EP1955356A2 - Sources d'ions, systemes et procedes associes - Google Patents

Sources d'ions, systemes et procedes associes

Info

Publication number
EP1955356A2
EP1955356A2 EP06837944A EP06837944A EP1955356A2 EP 1955356 A2 EP1955356 A2 EP 1955356A2 EP 06837944 A EP06837944 A EP 06837944A EP 06837944 A EP06837944 A EP 06837944A EP 1955356 A2 EP1955356 A2 EP 1955356A2
Authority
EP
European Patent Office
Prior art keywords
sample
ion
tip
gas
ion source
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP06837944A
Other languages
German (de)
English (en)
Inventor
Billy W. Ward
John A. Notte, Iv
Louis S. Farkas Iii
Randall G. Percival
Raymond Hill
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carl Zeiss Microscopy LLC
Original Assignee
Alis Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US11/385,136 external-priority patent/US20070228287A1/en
Priority claimed from US11/385,215 external-priority patent/US7601953B2/en
Application filed by Alis Corp filed Critical Alis Corp
Priority to EP11182539.4A priority Critical patent/EP2416342B1/fr
Publication of EP1955356A2 publication Critical patent/EP1955356A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/26—Bombardment with radiation
    • H01L21/263—Bombardment with radiation with high-energy radiation
    • H01L21/265—Bombardment with radiation with high-energy radiation producing ion implantation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/08—Ion sources; Ion guns
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/252—Tubes for spot-analysing by electron or ion beams; Microanalysers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching
    • H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching
    • H01J37/3056—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching for microworking, e.g. etching of gratings, trimming of electrical components
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/317—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation
    • H01J37/3174—Particle-beam lithography, e.g. electron beam lithography
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/3065—Plasma etching; Reactive-ion etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/02—Details
    • H01J2237/024—Moving components not otherwise provided for
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/06—Sources
    • H01J2237/08—Ion sources
    • H01J2237/0802—Field ionization sources
    • H01J2237/0807—Gas field ion sources [GFIS]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20221—Translation
    • H01J2237/20228—Mechanical X-Y scanning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20264—Piezoelectric devices
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/25—Tubes for localised analysis using electron or ion beams
    • H01J2237/2505—Tubes for localised analysis using electron or ion beams characterised by their application
    • H01J2237/2555—Microprobes, i.e. particle-induced X-ray spectrometry
    • H01J2237/2566—Microprobes, i.e. particle-induced X-ray spectrometry ion
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/262—Non-scanning techniques
    • H01J2237/2623—Field-emission microscopes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H01J2237/2812—Emission microscopes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/304—Controlling tubes
    • H01J2237/30433—System calibration
    • H01J2237/30438—Registration
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/304—Controlling tubes
    • H01J2237/30472—Controlling the beam
    • H01J2237/30477—Beam diameter
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/317—Processing objects on a microscale
    • H01J2237/31735—Direct-write microstructures
    • H01J2237/31737—Direct-write microstructures using ions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/317—Processing objects on a microscale
    • H01J2237/3174—Etching microareas
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/317—Processing objects on a microscale
    • H01J2237/3175—Lithography
    • H01J2237/31752—Lithography using particular beams or near-field effects, e.g. STM-like techniques
    • H01J2237/31755—Lithography using particular beams or near-field effects, e.g. STM-like techniques using ion beams

Definitions

  • the invention features a system that includes an ion source capable of interacting with a gas to generate an ion beam having a spot size with a dimension of three nm or less at a surface of a sample.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam having a brightness of 1x10 9 A/cm 2 sr or more at a surface of a sample.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam having a reduced brightness of 5x10 A/m srV or more at a surface of a sample.
  • the invention features an ion microscope capable of producing an image of a sample.
  • the sample is different from the ion microscope, and the image of the sample has a resolution of three nm or less.
  • the invention features an ion microscope that includes an ion source with an electrically conductive tip having a terminal shelf with 20 atoms or less.
  • the invention features a system that includes a gas field ion source with an electrically conductive tip with an average full cone angle of from 15° to 45°.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause particles to leave the sample.
  • the particles are selected from Auger electrons, secondary ions, secondary neutral particles, primary neutral particles, scattered ions and photons.
  • the system also includes at least one detector configured so that, during use, the at least one detector detects at least some of the particles to determine information about the sample.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause particles to leave the sample.
  • the system also includes at least one detector configured so that, during use, the at least one detector can detect at least some of the particles. For a given detected particle, the at least one detector produces a signal based on an energy of the given detected particle.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause secondary ions to leave the sample.
  • the system also includes at least one detector configured so that, during use, the at least one detector can detect at least some of the secondary ions.
  • the system further includes an electronic processor electrically connected to the at least one detector so that, during use, the electronic processor can process information based on the detected secondary ions to determine information about the sample.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause ions to leave the sample.
  • the system also includes at least one detector configured so that, during use, the at least one detector can detect the ions.
  • the interaction of the ion beam with the sample may cause secondary electrons to leave the sample, and, when the interaction of the ion beam with the sample causes secondary electrons to leave the sample, the at least one detector can detect at least some of the ions without detecting the secondary electrons.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause neutral particles to leave the sample.
  • the system also includes at least one detector configured so that, during use, the at least one detector can detect the neutral particles.
  • the interaction of the ion beam with the sample may cause secondary electrons to leave the sample, and, when the interaction of the ion beam with the sample causes secondary electrons to leave the sample, the at least one detector can detect at least some of the neutral particles without detecting the secondary electrons.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that can interact with a sample to cause photons to leave the sample.
  • the system also includes at least one detector configured so that, during use, the at least one detector can detect the photons.
  • the interaction of the ion beam with the sample may cause secondary electrons to leave the sample, and, when the interaction of the ion beam with the sample causes secondary electrons to leave the sample, the at least one detector can detect at least some of the photons without detecting the secondary electrons.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate an ion beam that is directed toward a sample.
  • the system also includes a charged particle source configured so that, during use, the charged particle source provides a beam of charged particles that is directed toward the sample.
  • the gas field ion source is different from the charged particle source.
  • the invention features a method that includes interacting an ion beam with a sample to cause multiple different types of particles to leave the sample, and detecting at least two different types of particles of the multiple different types of particles.
  • the multiple different types of particles are selected from secondary electrons, Auger electrons, secondary ions, secondary neutral particles, primary neutral particles, scattered ions and photons.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause particles to leave the sample.
  • the particles are selected from Auger electrons, secondary ions, secondary neutral particles, primary neutral particles, scattered ions and photons.
  • the method also includes detecting at least some of the particles to determine information about the sample.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause photons to leave the sample.
  • the method also includes detecting at least some of the photons, and determining information about the sample based on the detected photons.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause secondary ions to leave the sample.
  • the method also includes detecting at least some of the secondary ions.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause secondary neutral particles to leave the sample.
  • the method also includes detecting at least some of the secondary neutral particles or particles derived from the secondary neutral particles.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause Auger electrons to leave the sample. The method also includes detecting at least some of the Auger electrons. In one aspect, the invention features a method that includes forming a gas field ion source, and, after forming the gas field ion source, disposing the ion source into a chamber to provide a gas field ion system.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, the ion beam having a spot size with a dimension of 10 nm or less on a surface of a sample, and moving the ion beam from a first location on the surface of the sample to a second location on the surface of the sample, the first location being different from the second location.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and contacting a sample with the ion beam. The method also includes contacting the sample with a charged particle beam from a charged particle source.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample to cause particles to leave the sample.
  • the method also includes detecting at least some of the particles, and determining crystalline information about the sample based on the detected particles.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with an activating gas to promote a chemical reaction at a surface of a sample.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and using the ion beam to determine subsurface information about a semiconductor article. The method also includes editing the semiconductor article based on the sub-surface information.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and using the ion beam to determine information about a semiconductor article.
  • the ion beam has a spot size of 10 nm or less at a surface of the semiconductor article.
  • the method also includes editing the
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and using the ion beam to determine information about a lithography mask.
  • the ion beam has a spot size of 10 nm or less at a surface of the semiconductor article.
  • the method also includes repairing the lithography mask based on the information.
  • the invention features a method that includes using an ion beam to pattern a resist on a sample.
  • the ion beam has a spot size of 10 nm or less at the sample.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and interacting the ion beam with a sample including a feature.
  • the ion beam has a spot size of 50 nm or less on a surface of a sample.
  • the method also includes determining the size of the feature.
  • the invention features a method that includes exposing a sample to a focused ion beam, and generating a second ion beam by interacting a gas with a gas field ion source. The method also includes exposing the sample to the second ion beam.
  • the invention features a method that includes forming an electrically conductive tip of a gas field ion source when the gas field ion source is present within an ion microscope.
  • the invention features a system that includes an ion source. The system is capable of imaging the ion source in a first mode, and the system is capable of using the ion source to collect an image of a sample in a second mode. The sample is different from the ion source.
  • the invention features a sample manipulator that includes a housing, a disk supported by the housing, a member supported by the disk, the member having legs and a surface configured to support a sample, and a device.
  • the device contacts the member to move the sample in a first mode, and the device is not in contact with the member in a second mode.
  • the invention features a system that includes a gas field ion source and a sample manipulator.
  • the sample manipulator includes a housing, a disk supported by the housing, a member supported by the disk, the member having legs and a surface configured to support a sample, and a device.
  • the device contacts the member to move the sample in a first mode, and the device is not in contact with the member in a second mode.
  • the invention features a method that includes generating a first beam containing ions by interacting a gas with a gas field ion source, and removing non-singly charged chemical species from the first beam to form a second beam containing singly- charged ions.
  • the invention features a system that includes a gas field ion source capable of interacting with a gas to generate a beam comprising chemical species including charged chemical species.
  • the system also includes at least one biased electrode configured to cause beam paths of chemical species in the beam to diverge based on the charge of the chemical species.
  • the invention features a method that includes generating an ion beam by interacting a gas with a gas field ion source, and generating an electron beam using a system different from the gas field ion source.
  • the method also includes using both the ion beam and the electron beam to investigate a sample.
  • the invention features a method that includes generating a first ion beam by interacting a gas with a gas field ion source.
  • the first ion beam has a first current.
  • the method also includes using the first ion beam having the first current to prepare the gas field ion source for investigating a sample.
  • the method further includes generating a second ion beam by interacting a gas with the gas field ion source.
  • the second ion beam has a second current.
  • the method includes using the second ion beam to investigate the sample.
  • Embodiments may include one or more of the following advantages.
  • an ion source e.g., a gas field ion source
  • a gas field ion source can provide a relatively small spot size on the surface of a sample.
  • An ion microscope e.g., a gas field ion microscope using such an ion source can, for example, obtain an image of a sample with relatively high resolution.
  • an ion source e.g., a gas field ion source
  • a gas field ion source can have a relatively high brightness and/or a relatively high reduced brightness.
  • An ion microscope e.g., a gas field ion microscope using such an ion source can, for example, take a good quality image of a sample in a relatively short period of time, which can, in turn, increase the speed with which large numbers of samples can be imaged.
  • an ion microscope e.g., a gas field ion microscope
  • an ion microscope e.g., a gas field ion microscope
  • an ion microscope can be operated at relatively high temperature while still providing one or more of the above- mentioned advantages.
  • liquid nitrogen can be used as the coolant for the ion microscope. This can reduce the cost and/or complexity associated with using certain other coolants, such as liquid helium. This can also reduce potential problems associated with certain mechanical systems used with liquid helium coolant that can create substantial vibrations.
  • FIG. l is a schematic diagram of an ion microscope system.
  • FIG. 3 is a schematic representation of an enlarged side view of an embodiment of a tip apex.
  • FIG. 6 is a schematic representation of an enlarged top view of an embodiment of a W(111) tip.
  • FIG. 9 is a side view of a tip showing a radius of curvature measurement.
  • FIG. 10 is a flow chart showing an embodiment of a method of making a tip.
  • FIG. 1 IB is a bottom view of the support assembly of FIG. 1 IA.
  • FIG. 12 is a side view of an embodiment of a support assembly that includes a Vogel mount to support a tip.
  • FIG. 13 is a schematic view of an embodiment of a gas field ion source and ion optics.
  • FIG. 14 is a schematic view of an embodiment of an ion optical system.
  • FIG. 16 is a top view of an embodiment of a multi-opening aperture.
  • FIG. 17 is a cross-sectional view of an embodiment of a movement mechanism for a gas field ion microscope tip.
  • FIG. 18 is a schematic diagram of an Everhart-Thornley detector.
  • FIG. 19 is a cross-sectional view of a portion of a gas field ion microscope system including a microchannel plate detector.
  • FIGS. 2OA and 2OB are side and top views of a gold island supported by a carbon surface.
  • FIG. 2OC is a plot of average measured secondary electron total abundance as a function of ion beam position for the sample of FIGS. 2OA and 2OB.
  • FIG. 21 is a schematic diagram of a portion of a gas field ion microscope including a gas delivery system.
  • FIG. 22 is a schematic diagram of a portion of a gas field ion microscope including a flood gun.
  • FIG. 23 is a schematic diagram of a sample including a sub-surface charge layer.
  • FIG. 24 is a schematic diagram of a collector electrode for reducing surface charge on a sample.
  • FIG. 26 is a schematic diagram of a flood gun apparatus including a conversion plate for reducing surface charge on a sample.
  • FIG. 29 is a schematic diagram of an embodiment of a vibration-decoupled sample manipulator.
  • FIG. 30 is a schematic diagram of an embodiment of a vibration-decoupled sample manipulator.
  • FIG. 31 is a schematic diagram of an electrostatic filtering system for separating ions and neutral atoms in a particle beam.
  • FIG. 32 is a schematic diagram of an electrostatic filtering system for separating neutral atoms, singly-charged ions, and doubly-charged ions in a particle beam.
  • FIG. 33 is a schematic diagram of a filtering system that includes a dispersionless sequence of electric and magnetic fields for separating neutral atoms, singly-charged ions, and doubly-charged ions in a particle beam.
  • FIG. 34A is a schematic diagram showing an embodiment of helium ion scattering patterns from a surface.
  • FIG. 34B is a diagram showing plots of the relative abundance of scattered helium ions detected by the detectors in FIG. 34A.
  • FIG. 35B, 35E and 35H are plots of the total scattered helium ion yield for the systems shows in FIGS. 35A, 35D and 35G, respectively.
  • FIG. 35C, 35F and 351 are plots of the relative abundance of scattered helium ions detected by the detectors in FIGS. 35A, 35D and 35G, respectively.
  • FIG. 36 is a schematic diagram showing a portion of a gas field ion microscope including an arrangement of detectors for measuring scattered ions from a sample.
  • FIGS. 37A-37D are scanning electron microscope images an electrically conductive tip.
  • FIG. 38 is a digitized representation of the surface of an electrically conductive tip.
  • FIG. 39 is a plot of the slope of the slope of the surface shown in FIG. 38.
  • FIG. 42 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 43 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 44 is a scanning field ion microscope image of an electrically conductive tip.
  • FIG. 45 is a field ion microscope image of an electrically conductive tip having a trimer as the terminal shelf at its apex.
  • FIG. 46 is a scanning electron microscope image of an electrically conductive tip.
  • FIG. 47 is a field ion microscope image of an electrically conductive tip.
  • FIG. 48 is a field ion microscope image of an electrically conductive tip.
  • FIG. 49 is a field ion microscope image of an electrically conductive tip.
  • FIG. 50 is a scanning field ion microscope image of an electrically conductive tip having a trimer as the terminal shelf at its apex.
  • FIG. 51 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 52 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 53 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 54 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 55 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 57 is a schematic representation of a support for a tip.
  • FIG. 58 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 59A is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 59B is an image of a sample taken with a scanning electron microscope.
  • FIG. 60 is a graph of secondary electron current from a sample.
  • FIG. 61 A is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 61 B is an image of a sample taken with a scanning electron microscope.
  • FIG. 63 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 64 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 65 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 66 is an embodiment of a detector configuration configured to detect secondary electrons.
  • FIG. 67A is a graph of secondary electron intensity at varying sample locations based on the image in FIG. 59A.
  • FIG. 67B is a graph of secondary electron intensity at varying sample locations based on the image in FIG. 59B.
  • FIG. 68 is an image of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIGS. 69A-69C are images of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIG. 7OA is an image of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIG. 70 B is a polar plot showing the angular intensity of helium ions and helium atoms leaving the sample for the image of FIG. 7OA.
  • FIG. 71 A is an image of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIG. 72 is an image of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIG. 73 is an image of a sample taken with a helium ion microscope configured to detect helium ions and neutral helium atoms.
  • FIG. 74 is an image of a sample taken using a helium ion microscope configured to detect photons.
  • FIG. 75 is an image of a sample taken with a helium ion microscope configured to detect secondary electrons.
  • FIG. 76 is an expanded view of a portion of the image of FIG. 75.
  • FIG. 77 is a plot of image intensity as a function of pixel position for a line scan through the image of FIG. 76.
  • FIG. 81 is an image of a sample taken with a scanning electron microscope.
  • FIG. 82 is a plot of image intensity as a function of pixel position for a line scan through a portion of the image of FIG. 81.
  • a gas field ion source is a device that includes an electrically conductive tip (typically having an apex with 10 or fewer atoms) that can be used to ionize neutral gas species to generate ions (e.g., in the form of an ion beam) by bringing the neutral gas species into the vicinity of the electrically conductive tip (e.g., within a distance of about four to five angstroms) while applying a high positive potential (e.g., one kV or more relative to the extractor (see discussion below)) to the apex of the electrically conductive tip.
  • a high positive potential e.g., one kV or more relative to the extractor (see discussion below)
  • gas field ion source 120 can be maintained at a pressure of approximately 10 "10 Torr.
  • the background pressure rises to approximately 10 "5 Torr.
  • Ion optics 130 are maintained at a background pressure of approximately 10 '8 Torr prior to the introduction of gas into gas field ion source 120.
  • the background pressure in ion optics 130 typically increase to approximately 10 "7 Torr.
  • Sample 180 is positioned within a chamber that is typically maintained at a background pressure of approximately 10 "6 Torr. This pressure does not vary significantly due to the presence or absence of gas in gas field ion source 120.
  • gas source 110 is configured to supply one or more gases 182 to gas field ion source 120.
  • gas source 110 can be configured to supply the gas(es) at a variety of purities, flow rates, pressures, and temperatures.
  • at least one of the gases supplied by gas source 110 is a noble gas (helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe)), and ions of the noble gas are desirably the primary constituent in ion beam 192.
  • the current of ions in ion beam 192 increases monotonically as the pressure of the noble gas in system 100 increases.
  • this relationship can be described by a power law where, for a certain range of noble gas pressures, the current increases generally in proportion to gas pressure.
  • the pressure of the noble gas is typically 10 "2 Torr or less (e.g., 10 "3 Torr or less, 10 "4 Torr or less), and/or 10 "7 Torr or more (e.g., 10 "6 Torr or more, 10 "5 Torr or more) adjacent the tip apex (see discussion below).
  • it is desirable to use relatively high purity gases e.g., to reduce the presence of undesirable chemical species in the system).
  • the He when He is used, the He can be at least 99.99% pure (e.g., 99.995% pure, 99.999% pure, 99.9995% pure, 99.9999% pure).
  • the purity of the gases is desirably high purity commercial grade.
  • the additional gas(es) can be present at levels above the level of impurities in the noble gas(es), the additional gas(es) still constitute minority components of the overall gas mixture introduced by gas source 110.
  • the overall gas mixture can include 20% or less (e.g., 15% or less, 12% or less) Ne, and/or 1% or more (e.g., 3% or more, 8% or more) Ne.
  • the overall gas mixture can include from 5% to 15% (e.g., from 8% to 12%, from 9% to 11%) Ne.
  • the overall gas mixture can include 1% or less (e.g., 0.5% or less, 0.1% or less) nitrogen, and/or 0.01% or more (e.g., 0.05% or more) nitrogen.
  • the overall gas mixture can include from 0.01% to 1% (e.g., from 0.05% to 0.5%, from 0.08 to 0.12%) nitrogen.
  • the additional gas(es) are mixed with the noble gas(es) before entering system 100 (e.g., via the use of a gas manifold that mixes the gases and then delivers the mixture into system 100 through a single inlet).
  • the additional gas(es) are not mixed with the noble gas(es) before entering system 100 (e.g., a separate inlet is used for inputting each gas into system 100, but the separate inlets are sufficiently close that the gases become mixed before interacting with any of the elements in gas field ion source 120).
  • Gas field ion source 120 is configured to receive the one or more gases 182 from gas source 110 and to produce gas ions from gas(es) 182.
  • Gas field ion source 120 includes an electrically conductive tip 186 with a tip apex 187, an extractor 190 and optionally a suppressor 188.
  • the distance from tip apex 187 to surface 181 of sample 180 is five cm or more (e.g., 10 cm or more, 15 cm or more, 20 cm or more, 25 cm or more), and/or 100 cm or less (e.g., 80 cm or less, 60 cm or less, 50 cm or less).
  • the distance from tip apex 187 to surface 181 of sample 180 is from five cm to 100 cm (e.g., from 25 cm to 75 cm, from 40 cm to 60 cm, from 45 cm to 55 cm).
  • Electrically conductive tip 186 can be formed of various materials.
  • tip 186 is formed of a metal (e.g., tungsten (W), tantalum (Ta), iridium (Ir), rhenium (Rh), niobium (Nb), platinum (Pt), molybdenum (Mo)).
  • electrically conductive tip 186 can be formed of an alloy.
  • electrically conductive tip 186 can be formed of a different material (e.g., carbon (C)).
  • tip 186 is biased positively (e.g., approximately 20 kV) with respect to extractor 190, extractor 190 is negatively or positively biased (e.g., from -20 kV to +50 kV) with respect to an external ground, and optional suppressor 188 is biased positively or negatively (e.g., from -5 kV to +5 kV) with respect to tip 186.
  • tip 186 is formed of an electrically conductive material, the electric field of tip 186 at tip apex 187 points outward from the surface of tip apex 187. Due to the shape of tip 186, the electric field is strongest in the vicinity of tip apex 187.
  • the strength of the electric field of tip 186 can be adjusted, for example, by changing the positive voltage applied to tip 186.
  • un-ionized gas atoms 182 supplied by gas source 110 are ionized and become positively-charged ions in the vicinity of tip apex 187.
  • the positively-charged ions are simultaneously repelled by positively charged tip 186 and attracted by negatively charged extractor 190 such that the positively-charged ions are directed from tip 186 into ion optics 130 as ion beam 192.
  • Suppressor 188 assists in controlling the overall electric field between tip 186 and extractor 190 and, therefore, the trajectories of the positively- charged ions from tip 186 to ion optics 130.
  • the overall electric field between tip 186 and extractor 190 can be adjusted to control the rate at which positively-charged ions are produced at tip apex 187, and the efficiency with which the positively-charged ions are transported from tip 186 to ion optics 130.
  • the average cone direction of tip 300 can be 10° or less (e.g., 9° or less, 8° or less, 7° or less, 6° or less, 5° or less), and/or the average cone direction of tip 300 can be 0° or more (e.g., 1° or more, 2° or more , 3° or more, 4° or more). In certain embodiments, the average cone direction of tip 300 is from 0° to 10° (e.g., from 1° to 10°, from 3° to 10°, from 6° to 10°, from 2° to 8°, from 4° to 6°).
  • FIG. 10 is a flow chart for a process 400 of making a W(111) tip having a terminal atomic shelf that is a trimer.
  • a single crystal W(111) precursor wire is attached to a support assembly.
  • the W(111) precursor wire has a diameter of 3 mm or less (e.g., 2 mm or less, 1 mm or less), and/or 0.2 mm or more (e.g., 0.3 mm or more, 0.5 mm or more).
  • the W(111) precursor wire has a diameter of from 0.2 mm to 0.5 mm (e.g., from 0.3 mm to 0.4 mm, 0.25 mm).
  • Suitable precursor wires can be obtained, for example, from FEI Beam Technology (Hillsboro, OR).
  • the tip precursor can be in a form that is different from a wire.
  • the tip precursor can be formed of an electrically conductive material that has a protrusion that terminates in a crystalline structure.
  • the terminus of the protrusion can be a single crystal structure, for example, and can be formed of W(111), or formed of another material in a similar or different crystal orientation.
  • FIGS. 1 IA and 1 IB show perspective and bottom views, respectively, of an embodiment of a support assembly 520.
  • Support assembly 520 includes support posts 522a and 522b connected to a support base 524.
  • Posts 522a and 522b are connected to heater wires 526a and 526b, and a length of a W(111) precursor wire 528 is connected to heater wires 526a and 526b (e.g., via welding).
  • Posts 522a and 522b can be connected to auxiliary devices such as, for example, electric current sources (e.g., power supplies) to permit control of the temperature of W(111) precursor wire 528.
  • electric current sources e.g., power supplies
  • base 524, posts 522a and 522b, and heater wires 526a and 526b can generally be selected as desired.
  • a distance between posts 522a and 522b can be from 1 mm to 10 mm.
  • precursor wire 528 can be held in position by a support assembly that applies a compressive force to the wire.
  • FIG. 12 shows an exemplary support assembly 550 including a Vogel mount to secure precursor wire 528. Suitable Vogel mounts are available commercially from AP Tech (McMinnville, OR), for example.
  • Support assembly 550 includes a support base 556 and mounting arms 552 attached to base 556. To secure precursor wire 528, arms 552 are pried apart and spacers (e.g., formed of pyrolytic carbon) 554 are inserted into the space between the arms.
  • spacers e.g., formed of pyrolytic carbon
  • Mounting arms 552 can be formed from one or more electrically conducting materials.
  • the materials used to form arms 552 can also be chosen so that base 556 and arms 552 have a similar coefficient of thermal expansion, and so that arms 552 remain fixed in position relative to base 556 during temperature cycling of precursor wire 528.
  • arms 552 are formed from an alloy that includes iron, nickel, and cobalt. Suitable commercially available materials for forming arms 552 include
  • Spacers 554 are formed from a material such as pyrolytic carbon. Suitable pyrolytic carbon spacers are available from, for example, AP Tech (McMinnville, OR). Pyrolytic carbon spacers typically are formed of a series of flat carbon sheets stacked atop one another to create a laminar structure. In general, the resistivity of pyrolytic carbon varies according to direction, with the resistivity of the carbon in a direction perpendicular to the sheets (e.g., in a direction approximately normal to the planes of the stacked sheets) being higher than the resistivity along a direction in a plane parallel to the planes of the sheets.
  • spacers 554 can serve as heating elements for adjusting the temperature of . precursor wire 528.
  • step 404 precursor wire 528 is etched in an electrochemical bath to shape the tip of wire 528.
  • step 404 includes multiple sub-steps.
  • the first sub-step in the etching process can optionally be a cleaning step to remove surface contaminants from wire 528.
  • This etching process can involve disposing wire 528 in an electrochemical etch solution and exposing wire 528 to an alternating current (AC) voltage.
  • the solution can be a IN solution of sodium hydroxide (NaOH), and an AC voltage of 1 V can be used.
  • the entire support assembly e.g., support assembly 520 or 550
  • can be cleaned e.g., ultrasonically cleaned in water to remove certain remaining contaminants.
  • the next sub-step in step 404 is to optionally apply a resist material to a portion of wire 528.
  • the resist material is applied over a length of approximately 0.5 mm of wire 528, starting from the apex of wire 528.
  • Application of the resist material can be achieved, for example, by placing a drop of resist solution onto a clean surface and dipping wire 528 into the resist several times, allowing the resist to dry slightly between applications.
  • the applied resist limits the amount of precursor wire 528 that is etched during subsequent processing steps. Because formation of a subsequent tip on a precursor wire 528 often follows removal of a previous tip by etching, use of the resist material permits a larger number of tips to be formed on a given precursor wire before the wire is discarded.
  • the next sub-step in step 404 is to electrochemically etch precursor wire 528.
  • electrochemical etching procedures can be used. In some embodiments, the following electrochemical etching procedure is used.
  • the support assembly is placed in an etching fixture that includes a translation apparatus for translating the support assembly, a dish, and an electrode (e.g., a stainless steel electrode) that extends into the dish.
  • An etching solution is placed in the dish such that the solution is in contact with the electrode.
  • the support assembly is lowered toward the dish via the translation apparatus until the resist interface on wire 528 just contacts the etching solution.
  • Wire 528 is then lowered an additional amount (e.g., 0.2 mm) into the etching solution.
  • concentration of NaOH in the etching solution can be selected to vary the corrosion rate of precursor wire 528 and the chemical environment of the solution.
  • concentration of NaOH can be 0.1 M or more (e.g., 0.2 M or more, 0.5 M or more, 0.6 M or more, 0.8 M or more, 1.0 M or more, 1.2 M or more, 1.4 M or more, 1.6 M or more, 2.0 M or more, 2.5 M or more, 3.0 M or more), and/or 10.0 M or less (e.g., 9.0 M or less, 8.0 M or less, 7.0 M or less, 6.5 M or less, 6.0 M or less, 5.5 M or less, 5.0 M or less, 4.5 M or less, 4.0 M or less).
  • the etching solution can include a relatively small amount of surfactant.
  • surfactant can assist in promoting symmetric etching of precursor wire 528.
  • Suitable surfactants for this purpose include materials such as PhotoFlo 200, available from Eastman Kodak
  • the concentration of surfactant in the etching solution is 0.1 volume % or more (e.g., 0.2 volume % or more, 0.3 volume % or more, 0.4 volume % or more), and/or 2 volume % or less (e.g., 1 volume % or less, 0.8 volume % or less, 0.6 volume % or less).
  • an external power supply is connected to both wire 528 and the electrode, and a potential is applied across wire 528 and the electrode to facilitate an electrochemical corrosion reaction of wire 528.
  • the voltage can be applied from either an AC source or a direct current (DC) source.
  • the amplitude of the applied voltage can generally be selected as desired, based upon an empirical determination of an amplitude that produces a uniformly etched precursor wire 528.
  • the duration of AC pulses applied to the etching solution can generally vary as desired to promote controlled etching of wire 528.
  • pulses applied to the etching solution have a duration of 10 ms or more (e.g., 25 ms or more, 50 ms or more, 75 ms or more, 100 ms or more, 150 ms or more, 200 ms or more, 250 ms or more), and/or one second or less (e.g., 900 ms or less, 800 ms or less, 700 ms or less, 650 ms or less, 600 ms or less).
  • pulses applied to the etching solution have a duration of from 10 ms to one second (e.g., from 10 ms to 900 ms, from 10 ms to 800 ms, from 10 ms to 700 ms, from 10 ms to 600 ms).
  • pulses of varying duration and/or amplitude can be applied to the etching solution to cause erosion of precursor wire 528 in the region of the wire that contacts the solution.
  • a portion of the end of precursor wire 528 drops off into the etching solution, and the newly exposed, etched region of precursor wire 528 is processed further in subsequent steps.
  • a suitable etching regimen includes an initial application of approximately 100 AC pulses of amplitude 5 V, each pulse having a duration of approximately 580 ms. Thereafter, a series of approximately 60 pulses are applied, with each pulse having a duration of approximately 325 ms and an amplitude of 5 V. Then, pulses having a duration of 35 ms and an amplitude of 5 V are applied until a portion of the end of wire 528 drops off into the etching solution.
  • the immersion depth of precursor wire 528 can be adjusted.
  • the etching process leads to formation of a narrow-diameter region of precursor wire 528.
  • Adjusting the immersion depth of wire 528 can help ensure that the meniscus of the etching solution is positioned near a midpoint of the narrow-diameter region, which can enhance the probability of forming a relatively symmetric tip.
  • the drop-off point is approached (e.g., as the diameter in the narrow-diameter region becomes very small)
  • adjustment of the immersion depth is performed to ensure that the end of precursor wire 528 is not snapped off.
  • the first pulse can be from 1 V to 10 V (e.g., from 3 V to TV, 5V) with a duration of from 20 ms to 50 ms (e.g., from 30 ms to 40 ms, 35 ms), and the second pulse can be from 1 V to 10 V (e.g., from 3 V to 7V, 5 V) with a duration of from 10 ms to 25 ms (e.g., from 15 ms to 20 ms, 17 ms).
  • the next step 406 of process 400 is to examine the support assembly (and particularly, the etched tip of wire 528) to verify that the etched tip has suitable
  • determination of geometrical features includes obtaining profile images of the etched tip and calculating various geometrical parameters from data obtained from the profile images.
  • the inspection can be performed using a SEM, for example.
  • Profile images of the tip of wire 528 can be obtained at very high magnification, such as a magnification of 65,00OX, for example.
  • the measured geometrical parameters can include average tip radius of curvature, average cone direction, and average full cone angle, for example. At this point, if the shape of the etched tip is unsuitable, it may be possible to re-shape the tip slightly by inserting the assembly back into the etching fixture and lowering the etched tip of wire 528 toward the dish until the tip just contacts the etching solution.
  • step 408 the terminal shelf of the apex of the tip of etched wire
  • step 408 includes installing the support assembly in a FIM and evacuating the FIM.
  • the tip of wire 528 is cooled (e.g., to liquid nitrogen
  • the He gas is pumped out of the FIM chamber, and the bias on the tip of wire 528 is changed to being negative with respect to the common ground so that the apex of the tip of wire 528 emits electrons.
  • a detector which generates photons in response to incident electrons such as a phosphor-coated glass screen, is positioned to intercept electrons from the tip.
  • the generated photons are detected by a suitable detector (e.g., a CCD device, a photomultiplier tube, a photodiode, or another type of photon detector) and used to monitor electron emission from the tip.
  • the detector can be directly coupled to the photon-generating device.
  • the detector and photon-generating device are not directly coupled.
  • optical elements such as mirrors can be used to direct generated photons to the detector.
  • the voltage bias applied to the tip is adjusted until a desired electron current is measured (e.g., from 25 pA to 75 pA, from 40 pA to 60 pA, 50 pA).
  • the tip is then heated to a desired temperature (e.g., from 1000 K to 1700 K, from 1300 K to 1600 K, 1500 K), and the tip is monitored visually to detect light emitted from the tip in response to the application of both voltage and heat.
  • Light emission from the tip can be monitored, for example, using a mirror positioned to reflect light emitted by the tip toward a suitable photon detector (e.g., a CCD device, a photomultiplier tube, a photodiode, or another type of photon detector).
  • a suitable photon detector e.g., a CCD device, a photomultiplier tube, a photodiode, or another type of photon detector.
  • Heat can be applied to the tip using a variety of devices such as a resistive heating device (e.g., a filament heater), a radiative heating device, an inductive heating device, or an electron beam. From 15 seconds to 45 seconds (e.g., from 25 seconds to 35 seconds, 30 seconds) after the first appearance of light from the tip, both the applied potential and the heating device are turned off, yielding wire 528 with a trimer as its terminal atomic shelf.
  • a resistive heating device e.g., a filament heater
  • a radiative heating device e.g., an inductive heating device
  • an electron beam e.g., from 15 seconds to 35 seconds, 30 seconds
  • a gas can be used to sharpen the tip.
  • oxygen can be introduced into the FIM chamber to promote sharpening of a rounded W tip surface.
  • the sharpening gas e.g., oxygen
  • He is first pumped out of the FIM chamber and then the tip is heated to a temperature of between 1300K and 1700 K (e.g., 1500 K). The tip is maintained at 1500 K for between one and five minutes.
  • oxygen can be introduced into the chamber at a pressure of approximately 10 "5 Torr, while maintaining the temperature of the tip for approximately two minutes.
  • the temperature of the tip is then reduced to between 700 K and 1200 K (e.g., 1000 K), and the tip is maintained at that temperature for approximately two minutes.
  • the oxygen supply to the chamber is closed and oxygen is pumped out of the chamber until the oxygen pressure therein is less than 10 "7 Torr.
  • the tip is cooled to its normal operating temperature (e.g., approximately 77 K in some embodiments) and He is re-introduced into the FIM chamber.
  • a W trimer atop the tip corresponding to a W(111) facet is observed.
  • the W(111) wire having a terminal shelf that is a trimer can then be removed from the FIM and stored for future use.
  • system 200 can be used as the FIM.
  • the support assembly is installed within the ion source and system 200 is operated as a FIM, generally according to the procedure described in the preceding paragraphs.
  • the detector when operating system 200 in FIM mode, can be positioned either where sample 280 is normally positioned (i.e., sample 180 is not present in its normal position).
  • a flat sample with a relatively high secondary electron yield can be positioned where sample 180 is normally positioned, and the secondary electrons generated by the interaction of the He ions with the flat sample are detected because the intensity of the secondary electrons detected will generally scale with the intensity of the He ions incident on the flat sample.
  • system 200 can be operated in SFIM mode during the process of imaging/shaping the wire tip apex, hi such embodiments, the process is as described in the preceding paragraphs, except that alignment deflectors 220 and 222 are used to raster the ion beam across the surface of aperture 224 to generate a field emission pattern of the apex of the wire tip. Portions of the ion beam which pass through aperture 224 can optionally be focused by second lens 226, or remain unfocused.
  • SFIM mode an image of the wire tip is acquired pixei-by-pixel, and each measured pixel intensity corresponds to a portion of ion beam permitted to pass through aperture 224.
  • the pixel intensities together can be used to represent the field emission pattern of the tip as an image or, more generally, as a plurality of electrical signals.
  • the field emission pattern can then be used to assess various properties of the tip to determine its suitability for use in a gas field ion microscope.
  • the detector In SFIM mode, the detector can be located and of the type as described in the preceding paragraphs.
  • the detector can be a spatially integrating detector such as a photomultiplier tube or a photodiode.
  • microscope system 200 can be configured to operate in FIM and/or SFIM mode, as described above.
  • the re-sharpening process can be initiated or postponed.
  • other criteria can be used to determined when to initiate re-sharpening. For example, if the measured ion current from the tip falls below an established threshold value after a period of operation, re-sharpening can be initiated.
  • the tip can be field evaporated to remove atoms near the tip apex.
  • microscope system 200 can be configured to operate in FIM and/or SFIM mode, as discussed above, and the potential applied to the tip can be carefully adjusted to produce controlled field evaporation of tip atoms.
  • a field emission image of the tip can be obtained in FIM or SFIM mode by a detector (e.g., a phosphor-coupled photon detector, or a secondary electron detector configured to measured secondary electron emission from a flat sample) and monitored to determine when to halt the field evaporation process.
  • a detector e.g., a phosphor-coupled photon detector, or a secondary electron detector configured to measured secondary electron emission from a flat sample
  • the tip can be re- sharpened.
  • He gas is pumped out of microscope system 200 until the background He pressure is less than approximately 10 "7 Torr.
  • a negative electrical potential is applied to the tip to operate microscope system 200 in electron mode, and the tip is sharpened via heating as described previously.
  • a sharpening gas such as oxygen is introduced into microscope system 200, and the tip is heated in the presence of oxygen for a selected time, as described previously.
  • He gas is re-introduced into microscope system 200, and with the system configured to operated in FIM and/or SFIM mode, one or more images of the re-sharpened tip are captured to verify that the tip apex includes a trimer corresponding to a W(111) facet.
  • control system 170 After two minutes at 1500 K, control system 170 introduces oxygen gas into microscope system 200 by opening a valve on an oxygen gas source. The valve opening is adjusted to maintain an oxygen pressure of approximately 10 "5 Torr in microscope system 200. After two additional minutes, the temperature of the tip is reduced to 1100 K by control system 170 by regulating the flow of liquid nitrogen coolant into the system. After two minutes at 1100 K, control system 170 shuts off the oxygen supply to the system and cools the tip to liquid nitrogen temperature. At this point, FIM and/or SFIM images of the tip (measured by an operator) can be used to manually verify the presence of a W(111) at the apex of the tip.
  • the pressure of oxygen gas in the FIM chamber can be 10 "7 Torr or more (e.g., 10 "6 Torr or more, 10 "5 Torr or more, 10 “4 Torr or more), and/or 1 Torr or less (e.g., 10 "1 Torr or less, 10 "2 Torr or less, 10 "3 Torr or less).
  • the pressure of oxygen gas in the FIM chamber can be from 10 "8 Torr to 10 "2 Torr (e.g., from 10 "7 Torr to 10 "3 Torr, from 10 "6 Torr to 10 "4 Torr).
  • trimer as the terminal atomic shelf during tip sharpening.
  • gases and materials can also be used to promote formation of a trimer as the terminal atomic shelf during tip sharpening.
  • materials such as palladium, platinum, gold, and/or indium can be vapor deposited onto the surface of a rounded tip prior to re-sharpening. It is believed that these materials may promote more reliable trimer formation at the apex of the tip.
  • sharpening of a W tip can be achieved by controlled heating of the tip without the application of a field or the intentional addition of oxygen.
  • a W tip can be sharpened by the following steps: 1) install tip in FIM chamber; 2) reduce pressure in FIM chamber; 3) heat tip to IOOOK for five minutes; and cool (e.g., to liquid nitrogen temperature).
  • cool e.g., to liquid nitrogen temperature.
  • trace amounts of oxygen present on the tip as oxides may assist in sharpening the tip using heat.
  • an unsharpened tip can be exposed to a stream of oxygen, placed in a substantially oxygen-free environment, and sharpened by controlled heating.
  • one or more additional gases may be present during tip sharpening.
  • nitrogen gas may be present. Without wishing to be bound by theory, it is believed that nitrogen gas may assist in etching the tip to provide a more rounded structure with a terminal atomic shelf that is a trimer; such a structure is believed to be more stable than a less-rounded, trimer-terminated tip.
  • the nitrogen gas is introduced simultaneously with the oxygen gas.
  • the pressure of nitrogen gas in the FIM chamber can be 10 "8 Torr or more (e.g., 10 "7 Torr or more), and/or 10 "5 Torr or less (e.g., 10 "6 Torr). In certain embodiments, the pressure of nitrogen gas in the FIM chamber can be from 10 "5 Torr to 10 '8 Torr (e.g., from 10 "6 Torr to 10 "7 Torr).
  • the positive electrical potential applied to the sharpened tip is increased so that controlled field evaporation of the tip occurs.
  • the tip apex reassumes a rounded shape.
  • the rounded tip produces an emission pattern that is similar to the emission pattern of the tip after the initial field evaporation step.
  • the rounded tip is again sharpened in electron mode to produce a terminal atomic shelf that is a trimer (e.g., using the procedure described above).
  • one or more trimers can be removed from the sharpened tip using field evaporation techniques.
  • the top-most atomic layer on the sharpened tip which is formed by a three- atom shelf, can be removed to reveal an atomic shelf underneath that includes more than three atoms.
  • the newly exposed atomic shelf can be further field evaporated to produce a W atom trimer at its apex.
  • This newly formed trimer, along with additional trimers formed during field evaporation, can be evaporated.
  • This process leads to a layer-by-layer rounding of the tip in the vicinity of its apex. By rounding the tip, the electric field gradient near the tip apex is reduced, reducing the probability that tip atoms undergo field evaporation while microscope system 200 is operating, and increasing the stability and lifetime of the tip.
  • the apex 187 of tip 186 is aligned within system 200.
  • microscope system 200 is evacuated using one or more vacuum pumps, and then heat is applied to tip 187 to remove, for example, oxides, condensates, and/or any other impurities that may have adhered to the tip surface.
  • tip 186 is heated to a temperature of 900 K or more (e.g., 1000 K or more, 1100 K or more) for a duration of 10 s or more (e.g., 30 s or more, 60 s or more). Heating may also assist in re-faceting tip 186, in the event that the tip shape is compromised by the presence of impurities.
  • tip 186 With tip 186 glowing radiatively as a result of the applied heat, the tip is then roughly aligned with the longitudinal axis of ion optics 130 by observing light from tip 186 propagating along the longitudinal axis (e.g., by inserting a reflective element such as a mirror and directing a portion of the light to a detector such as a CCD camera).
  • the position and/or orientation of tip 186 can be changed by adjusting tip manipulator 208 to direct the light from tip 186 through ion optics 130.
  • microscope system 200 is configured to operate in FIM or SFIM mode by reducing the background pressure in vacuum housings 202 and 204, cooling tip 186 (e.g., to approximately liquid nitrogen temperature), and introducing a stream of He gas atoms into a region in the vicinity of tip 186 via gas source 110.
  • An image of the field emission pattern of He ions from tip 186 is measured by a suitably configured detector and based upon this image, tip manipulator 208 is used to align the field emission pattern with a longitudinal axis of ion optics 130, so that the field emission pattern of tip 186 is centered upon the longitudinal axis.
  • a centering test can be performed by changing the electrical potential applied to first lens 216 while observing the induced modulation of the field emission pattern of tip 186. If the size of the field emission pattern observed by the detector changes due to the variation of the electrical potential applied to lens 216, but the position of the center of the pattern does not change, then tip 186 is aligned with a longitudinal axis of first lens 216. Conversely, if the center position of the field emission pattern of tip 186 changes in response to the variation of the potential applied to first lens 216, then tip 186 is not centered on the longitudinal axis of first lens 216. Adjustments of the orientation and position of tip 186 via tip manipulator 208 can be repeated iteratively until tip 186 is sufficiently well aligned with the longitudinal axis of first lens 216. Typically, this centering test is performed without aperture 224 in position.
  • a fine alignment procedure can then be performed to ensure that He ions generated via the interaction of He gas atoms with the three-atom shelf at apex 187 of tip 186 pass through aperture 224.
  • the electrical potentials applied to deflectors 220 and 222 are adjusted so that 70% or more (e.g., 75% or more, 80% or more, 85% or more, 90% or more, 95% or more, 97% or more, 99% or more) of the He ions in ion beam 192 that pass through aperture 224 are generated via the interaction of He gas atoms with only one of the three trimer atoms at the apex of tip 186.
  • the adjustment of the potentials applied to deflectors 220 and 222 ensures that aperture 224 prevents 50% or more (e.g., 60% or more, 70% or more, 80% or more, 90% or more, 95% or more, 98% or more) of the He ions in ion beam 192 generated by the interaction of He gas atoms with the other two trimer atoms from reaching surface 181 of sample 180.
  • the He ion beam that passes through aperture 224 and exits ion optics 130 includes He atoms that were ionized primarily in the vicinity of only one of the three trimer atoms at the apex of tip 186.
  • microscope system 200 can be operated in He ion mode in step 412 of process 400.
  • the FIM detectors and/or other FIM componentry is moved so that sample 180 can be positioned for exposure to ion beam 192.
  • An electrical potential that is positive with respect to extractor 190 is applied to tip 186, and He gas is introduced into vacuum housing 202 via gas source 110. He ions generated via the interaction of He gas atoms with primarily one of the three trimer atoms at the apex of tip 186 are guided by ion optics 130 through aperture 224, and are directed to sample 180.
  • the potential applied to tip 186 is 5 kV or more (e.g., 10 kV or more, 15 kV or more, 20 kV or more). In certain embodiments, the potential applied to tip 186 is 35 kV or less (e.g., 30 kV or less, 25 kV or less). For example, in some embodiments, the potential applied to tip 186 is from 5 kV to 35 kV (e.g., from 10 kV to 30 kV, from 15 kV to 25 kV).
  • the He gas pressure is 10 "8 Torr or more (e.g., 10 "7 Torr or more, 10 '6 Torr or more, 10 "5 Torr or more).
  • the He gas pressure in microscope system 200 is 10 ⁇ - " l Torr or less (e.g., 10 "2 Torr or less, 10 "3 Torr or less, 10 "4 Torr or less).
  • the He gas pressure in microscope system 200 is from 10 "7 Torr to 10 "1 Torr (e.g., from 10 "6 Torr to 10 "2 Torr, from 10 "5 Torr to 10 "3 Torr).
  • tip 186 can be periodically monitored by operating microscope system 200 in FIM or SFIM mode, as discussed above. If the trimer structure remains intact at tip apex 187, then tip 186 can continue to be used to provide ion beam 192 to microscope system 200. However, under certain circumstances, FIM or SFIM imaging of tip 186 may reveal that the trimer structure is no longer intact on tip apex 187. In this case, tip 186 can first be field evaporated to round the tip and remove the damaged trimer structure, and then re- sharpened in situ (e.g., without removing tip 186 from microscope system 200) using a process as described above.
  • sample 180 can be removed from its position and a detector, such as a phosphor-coupled CCD detector, can be placed at the former location of sample 180.
  • a detector such as a phosphor-coupled CCD detector
  • a flat sample with a relatively high secondary electron yield can be translated into position in place of sample 180, and a suitable detector can be positioned and configured to detect secondary electrons that leave the sample due to the interaction of the He ions with the sample.
  • Aperture 224 can be removed (or a large diameter opening 225 can be selected) so that ions generated from the interaction of He gas atoms with tip 186 are not significantly obstructed.
  • a detector can be introduced as described for FIM imaging, and aperture 224 can be maintained in position.
  • Alignment deflectors 220 and 222 can be used to raster the ion emission pattern of tip 186 across aperture 224 to acquire an image of tip 186 in pixel-by-pixel fashion. Acquisition of one or more images of tip 186 can be automated by electronic control system 170, which can control placement of apertures, movement of samples and detectors, and electrical potentials applied to tip 186 and to alignment deflectors 220 and 222.
  • the alignment procedure described above typically aligns a longitudinal axis 207 of tip 186 with a longitudinal axis 132 of ion optics 130 so that the distance d between axes 207 and 132 at apex 187 of tip 186 is less than 2 mm (e.g., less than 1 mm, less than 500 ⁇ m, less than 200 ⁇ m).
  • the angle between axes 207 and 132 at apex 187 of tip 186 is 2° or less (e.g., 1° or less, 0.5° or less, 0.2° or less).
  • Extractor 190 includes an opening 191.
  • the shape of extractor 190 and of opening 191 can be selected as desired. Typically, these features are chosen to ensure that He ions are efficiently and reliably directed into ion optics 130.
  • extractor 190 has a thickness t e measured in the z direction, an opening 191 of width a measured in the x-direction, and is positioned a distance e measured in the z-direction from apex 187 of tip 186.
  • t e is 100 ⁇ rn or more (e.g., 500 ⁇ m or more, 1 mm or more, 2 mm or more), and/or t e is 10 mm or less (e.g., 7 mm or less, 5 mm or less, 3 mm or less).
  • the distance e between apex 187 of tip 186 and extractor 190 is 10 mm or less (e.g., 8 mm or less, 6 mm or less, 5 mm or less, 4 mm or less, 3 mm or less, 2 mm or less, 1 mm or less).
  • extractor 190 is positioned further in the +z direction than tip 186, as shown in FIG. 13.
  • extractor 190 is positioned further in the -z direction than tip 186.
  • tip 186 protrudes through extractor 190 and extends further along the z-axis in the +z direction than extractor 190.
  • extractor 190 is shown as having a particular configuration in FIG. 13, more generally, extractor 190 can be of any desired design.
  • opening 191 can have curved sides of any desired shape.
  • Extractor 190 can generally be biased either positively or negatively with respect to tip 186.
  • the electrical potential applied to extractor 190 is -10 kV or more (e.g., -5 kV or more, 0 kV or more), and/or 20 kV or less (e.g., 15 kV or less, 10 kV or less) with respect to tip 186.
  • suppressor 188 can also be present in the vicinity of tip 186.
  • Suppressor 188 can be used, for example, to alter the electric field distribution in the vicinity of tip 186 by adjusting the potential applied to suppressor 188. Together with extractor 190, suppressor 188 can be used to control the trajectory of He ions produced at tip 186.
  • Suppressor 188 has an opening of width k measured in the x-direction, a thickness t s measured in the z-direction, and is positioned at a distance s, measured in the z-direction, from the apex of tip 186.
  • k is three ⁇ m or more (e.g., four ⁇ m or more, five ⁇ m or more) and/or eight ⁇ m or less (e.g., seven ⁇ m or less, six ⁇ m or less).
  • t s is 500 ⁇ m or more (e.g., 1 mm or more, 2 mm or more), and/or 15 mm or less (e.g., 10 mm or less, 8 mm or less, 6 mm or less, 5 mm or less, 4 mm or less). In some embodiments, s is 5 mm or less (e.g., 4 mm or less, 3 mm or less, 2 mm or less, 1 mm or less).
  • suppressor 188 is positioned further along in the +z-direction than tip 186.
  • tip 186 is positioned further along in the +z-direction than suppressor 188, so that tip 186 extends through suppressor 188 in the +z-direction.
  • microscope system 200 can be configured so that after passing through extractor 190, the energy of the ions in ion beam 192 can be selected as desired.
  • the energy of the ions in ion beam 192 can be changed without changing the ion current. That is, the electrical potential applied to tip 186 can be adjusted to modify the average energy of ion beam 192 without substantially changing the ion beam current from ion beam 192.
  • ion beam 192 enters ion optics 130 via entry opening 133 from gas field ion source 120.
  • Ion beam 192 passes first through first lens 216.
  • the position and electrical potential of first lens 216 are generally selected to focus ion beam 192 to a cross-over point C, where point C is a distance p, measured in the z-direction, from aperture 224.
  • first lens 216 is positioned a distance f, measured in the z- direction, from entry opening 133.
  • the distance f is 5 mm or more (e.g., 10 mm or more, 15 mm or more), and/or 30 mm or less (e.g., 25 mm or less, 20 mm or less).
  • first lens 216 can be biased positively or negatively with respect to tip 186.
  • the electrical potential applied to first lens 216 is -30 kV or more (e.g., -20 kV or more, -10 kV or more), and/or 40 kV or less (e.g., 30 kV or less, 20 kV or less, 15 kV or less, 10 kV or less) relative to tip 186.
  • the distance p can be 1 mm or more (e.g., 5 mm or more, 10 mm or more), and/or 100 mm or less (e.g., 70 mm or less, 50 mm or less, 30 mm or less, 20 mm or less).
  • Changing the position of point C can change the size of ion beam 192 in the x- and/or y- directions at the position of aperture 224, which can selectively control the fraction of ions in ion beam 192 that pass through aperture 224.
  • cross-over point C can, in some embodiments, be positioned further in the +z-direction than aperture 224.
  • Alignment deflectors 220 and 222 are configured to direct a portion of ion beam
  • deflectors 220 and 222 can each be quadrupole electrodes, with the two quadrupole electrodes being arranged in series.
  • Deflectors 220 and 222 can each deflect He ion beam 192 in both x- and y- directions.
  • the electrical potentials applied to the electrodes of deflectors 220 and 222 can be adjusted to ensure that a portion of ion beam 192 passes through both aperture 224 and second lens 226.
  • the potentials applied to deflectors 220 and 222 are adjusted to achieve a particular alignment condition, and then the potentials remain static while microscope system 200 is in operation. Alignment of ion beam 192 through aperture 224 is assessed by observing ion beam 192 using a suitable detector configured, for example, to image aperture 224.
  • Deflectors 220 and/or 222 can also be adjusted so that the portion of ion beam 192 that passes through aperture 224 is aligned with a longitudinal axis of second lens 226.
  • the electrical potential applied to second lens 226 can be varied (commonly referred to as wobbling) and the results observed on the imaging detector. If, as a result of the changing potential applied to second lens 226, the image of ion beam 192 changes in size but not in position, then ion beam 192 is aligned through second lens 226. If the position of the center of ion beam 192 changes as a result of the changing potential, then ion beam 192 is not aligned with second lens 226. hi this case, the potentials applied to deflectors 222 and/or 220 can be further adjusted and the wobble test repeated, in iterative fashion, until alignment is achieved.
  • electrical potentials applied to various electrode elements of alignment deflectors 220 and 222 can be selected as desired to produce deflection of ion beam 192 to a particular location relative to both aperture 224 and second lens 226.
  • Each of the electrodes in deflectors 220 and 222 can be biased either positively or negatively with respect to a common external ground.
  • the electrical potential applied to any electrode can be 100 V or less (e.g., 75 V or less, 50 V or less) and/or 10 V or more (e.g., 25 V or more, 40 V or more) relative to a common external ground.
  • the electrical potential applied to any electrode in deflectors 220 and 222 can be from 10 V to 100 V (e.g., from 10 V to 75 V, from 10 V to 50 V) relative to a common external ground.
  • Aperture 224 is positioned relative to ion beam 192 to permit a fraction of the ions in ion beam 192 to pass therethrough. Typically, aperture 224 does not have an applied electrical potential.
  • the width w, measured in the x-direction, of opening 225 in aperture 224 is one ⁇ m or more (e.g., 2 ⁇ m or more, 5 ⁇ m or more, 10 ⁇ m or more, 15 ⁇ m or more, 20 ⁇ m or more, 25 ⁇ m or more, 30 ⁇ m or more), and/or 100 ⁇ m or less (e.g., 90 ⁇ m or less, 80 ⁇ m or less, 70 ⁇ m or less, 60 ⁇ m or less, 50 ⁇ m or less).
  • w is from one ⁇ m to 100 ⁇ m (e.g., from 5 ⁇ m to 90 ⁇ m, from 15 ⁇ m to 50 ⁇ m, from 20 ⁇ m to 50 ⁇ m).
  • the width of opening 225 in aperture 224 measured in the y direction is one ⁇ m or more (e.g., 2 ⁇ m or more, 5 ⁇ m or more, 10 ⁇ m or more, 15 ⁇ m or more, 20 ⁇ m or more, 25 ⁇ m or more, 30 ⁇ m or more), and/or 100 ⁇ m or less (e.g., 90 ⁇ m or less, 80 ⁇ m or less, 70 ⁇ m or less, 60 ⁇ m or less, 50 ⁇ m or less).
  • w is from one ⁇ m to 100 ⁇ m (e.g., from 5 ⁇ m to 90 ⁇ m, from 15 ⁇ m to 50 ⁇ m, from 20 ⁇ m to 50 ⁇ m).
  • Aperture 224 is positioned on aperture mount 234.
  • Aperture mount 234 permits translation of aperture 224 in the x-y plane, according to control signals received from electronic control system 170.
  • aperture mount 234 can also permit translation of aperture 224 in the z direction along longitudinal axis 132 of ion optics 130.
  • aperture mount 234 can permit tilting of aperture 224 with respect to the x-y plane. Tilting aperture 224 can be used to align a longitudinal axis of aperture 224 with longitudinal axis 132 of ion optics 130.
  • aperture 224 can include a plurality of openings having different widths w.
  • FIG. 15 is a top view (along the z-direction) of a disk- shaped aperture 224a that includes multiple openings 225a-225g.
  • Aperture 224a is configured to rotate about a pivot point 227 that coincides with the center of aperture 224a. The centers of each of openings 225a-225g are positioned at the same distance from pivot point 227.
  • An aperture opening of a particular size can therefore be selected by rotating aperture disk 224a such that a selected opening is positioned in the path of ion beam 192, and then translating aperture disk 224a, if desired, to ensure correct alignment of the opening with ion beam 192.
  • FIG. 15 is a top view (along the z-direction) of a disk- shaped aperture 224a that includes multiple openings 225a-225g.
  • Aperture 224a is configured to rotate about a pivot point 227 that coincides with
  • FIG. 16 is a top view (along the z-direction) of a rod-shaped aperture 224b that includes multiple openings 229a-229e extending through aperture 224b.
  • the aperture size can be chosen by selecting an opening in aperture 224b. This selection is performed by translating aperture 224b in a direction parallel to arrow 221 to align one of the openings 229a-229e with ion beam 192.
  • openings 225a-225g and 229a-229e have diameters that can be chosen as desired.
  • the diameter of any of the openings can be five ⁇ m or more (e.g., 10 ⁇ m or more, 25 ⁇ m or more, 50 ⁇ m or more) and/or 200 ⁇ m or less (e.g., 150 ⁇ m or less, 100 ⁇ m or less), hi certain embodiments, the diameters of openings 225a-225g and/or 229a-229e can be from five ⁇ m to 200 ⁇ m (e.g., five ⁇ m to 150 ⁇ m, five ⁇ m to 100 ⁇ m).
  • devices other than an aperture can be used to permit only a portion of the ions in ion beam 192 to pass through ion optics 130 and impinge on the surface of sample 180.
  • two perpendicular slits can be positioned in series along the flight path of the ion beam.
  • Astigmatism corrector 218 is generally configured, via its shape, position along the path of ion beam 192, and applied electrical potential, to reduce or eliminate astigmatism in ion beam 192. Although various components can be used to construct astigmatism corrector 218, astigmatism corrector 218 is typically an octupole electrode positioned between aperture 224 and scanning deflectors 219 and 221.
  • the eight electrodes of an octupolar astigmatism corrector are divided into two groups of four electrodes, with a first controller configured to adjust the voltages of four of the electrodes (e.g., the first group of four electrodes, positively biased with respect to tip 186) and a second controller that adjusts the voltages of the other four electrodes (e.g., the second group of four electrodes, negatively biased with respect to tip 186). Electrodes from the first and second electrode groups are arranged in alternating fashion to form the segments of the octupole, where adjacent segments have bias voltages of opposite signs. This arrangement of electrodes forms a cusp field which focuses ion beams propagating along a longitudinal axis of the octupole, and de-focuses off-axis ion beams.
  • each of the electrodes of the octupole can be configured independently, and astigmatism corrector 218 therefore permits sensitive control over ion beam 192.
  • the electrical potential applied to any of the electrodes of astigmatism corrector 218, relative to the common external ground can be -30 V or more (e.g., -20 V or more, -10 V or more, -5 V or more), and/or 30 V or less (e.g., 20 V or less, 10 V or less, 5V or less).
  • ion optics 130 include scanning deflectors 219 and 221. Scanning deflectors 219 and 221 are typically positioned between astigmatism corrector 218 and second lens 226, although in general, other arrangements of scanning deflectors 219 and 221 within ion optics 130 are also possible.
  • the negative potential bias relative to the common external ground can assist in accelerating electrons out of the hole or via and away from the sample, making detection of the electrons easier. In the absence of the negative bias, many of the secondary electrons might instead re-enter the sample at points along the hole or via walls, never escaping the hole or via to be detected.
  • Sample 180 can be positively biased, for example, when the ET detector is used to measure ions from the sample.
  • the magnitude of the electrical potential applied to bias the sample can be 5 V or more (e.g., 10 V or more, 15 V or more, 20 V or more, 30 V or more, 50 V or more, 100 V or more).
  • a microchannel plate detector can be used to amplify a flux of secondary electrons, neutral atoms, or ions from sample 180.
  • MicroChannel plates are typically formed from materials such as fused silica, and generally include a large number of small diameter channels arranged in the form of an array. Particles enter individual channels and collide with channel walls, generating free electrons. Typically, multiple free electrons are generated on each collision of a particle (neutral atom, ion, or electron) with a channel wall. As a result, a cascaded electron signal corresponding to an amplification of the input particle signal exits the microchannel plate.
  • Channeltron detectors can also be used to detect particles such as electrons, ions and neutral atoms leaving sample 180.
  • Channeltron detectors function by amplifying particle signals through multiple internal collisions in a manner similar to that described in connection with microchannel plate detectors. Measurement of relatively weak secondary electron, ion, or neutral atom fluxes from sample 180 is possible by measuring the amplified particle signals that are output by a channeltron detector (e.g., using electronic control system 170).
  • a channeltron detector e.g., using electronic control system 170.
  • Phosphor-based detectors which include a thin layer of a phosphor material deposited atop a transparent substrate, and a photon detector such as a CCD camera, a PMT, or one or more diodes, can be used to detect electrons, ions and/or neutral particles from sample 180. Particles strike the phosphor layer, inducing emission of photons from the phosphor which are detected by the photon detector. Phosphor-based detectors can be arranged in positions similar to those of detector 150 and/or detector 160 as depicted in FIGS. 1 and 5, depending upon the type of particle that is measured (see discussion above).
  • Electrostatic prism detectors in which an electric and/or magnetic field is used to deflect incident ions, where the amount of deflection depends on the energy of the ions, can be used to spatially separate ions with different energies.
  • Magnetic prism detectors may also be used to spatially separate ions based on the energy of the ions. Any of the suitable detectors discussed above (e.g., microchannel plates, channeltrons, and others) can then be used to detect the deflected ions.
  • Quadrupole detectors can also be used to analyze energies of ions from sample 180.
  • a radio-frequency (RF) field within the quadrupole ensures that ions having a chosen mass and energy propagate along a straight, undeflected trajectory within the quadrupole. Ions with a different mass and/or energy propagate along a curved trajectory within the quadrupole. From the deflected position of ions within the quadrupole analyzer, energies of the ions can be determined.
  • RF radio-frequency
  • the detectors disclosed above can also be configured to measure time-of-flight information for secondary electrons, ions, and neutral atoms.
  • ion beam 192 is operated in pulsed mode.
  • Ion beam 192 can be pulsed, for example, by rapidly changing the electrical potential applied to one or both of deflectors 220 and 222. By increasing these potentials, for example, ion beam 192 can be diverted from its usual path in ion optics 130 such that ion beam 192 is temporarily blocked by aperture 224. If the potentials of deflectors 220 and 222 are then returned to their normal values for a short time before being increased again, a pulse of He ions can be delivered to sample 180.
  • detectors 150 and 160 can be synchronized to a clock signal from electronic control system 170 that is based upon the temporal variation in potentials applied to deflectors 220 and/or 222.
  • the time interval between the launch of a He ion pulse and the detection of particles from sample 180 can be accurately measured. From known information about the time of propagation of the He ion pulse within ion optics 130, the time-of-flight of the detected particles between sample 180 and detectors 150 and/or 160 can be determined.
  • Measurement samples that include gold islands deposited on carbon, suitable for the resolution measurements described herein, are available commercially from Structure Probe Inc. (West Chester, PA), for example.
  • the ion microscope is operated such that it moves ion beam 192 linearly across a portion of the gold island, as well as the portions of the carbon surface on one side of the gold island (arrow 1730).
  • the intensity of secondary electrons is measured as a function of the location of the ion beam (FIG. 20C).
  • Asymptotic lines 1740 and 1750 are calculated (or drawn) corresponding to the average total abundance values for the carbon and gold, and vertical lines 1760 and 1770 are calculated (or drawn) corresponding to the locations where the total abundance is 25% and 75%, respectively, of the abundance difference between asymptotic lines 1740 and 1750.
  • the spot size of ion microscope 200 is the distance between lines 1760 and 1770.
  • the current of ion beam 192 at surface 181 of sample 180 is one nA or less (e.g., 100 pA or less, 50 pA or less), and/or 0.1 fA or more (e.g., one fA or more, 10 fA or more, 50 fA or more, 100 fA or more, one pA or more, 10 pA or more).
  • the current of ion beam 192 at surface 181 of sample 180 is from 0.1 fA to one nA (e.g., from 10 fA to 100 pA, from 100 fA to 50 pA).
  • d s will be a minimum value d 0 . That is, the spatial extent of the trajectories in a plane parallel to the x-y plane will be a minimum.
  • the diameter do of the minimum-diameter circle at point Z 0 is referred to as the virtual source size of microscope system 200.
  • the divergence and beam current of ion beam 192 in the FWHM region of ion beam 192 between extractor 190 and first lens 216, as discussed above, are measured.
  • brightness is calculated as beam current divided by the product of the virtual source size and the solid divergence angle of ion beam 192.
  • Ion beam 192 can have a relatively high reduced brightness at surface 181 of sample 180.
  • ion beam 192 can have a reduced brightness of 5x10 8 A/m 2 srV or more (e.g., IxIO 9 A/cm 2 srV or more, IxIO 10 A/cm 2 srV or more) at surface 181 of sample 180.
  • the reduced brightness of an ion beam is the brightness of the ion beam divided by the average energy of the ions in the ion beam at the position where the beam current is measured
  • Ion beam 192 is then translated linearly along the diameter of the gold island and the focused spot size, S f , of the ion beam is measured, as described above.
  • the convergence angle ⁇ can then be determined trigonometrically from the measurements of the focused and defocused spot sizes, along with the translation distance, as
  • the convergence half angle of ion microscope 200 is ⁇ /2.
  • the gas field ion source (tip 186, extractor 190 and optionally suppressor 188) is capable of interacting with gas atoms to generate an ion beam for a time period of one week or more (e.g., two weeks or more, one month or more, two months or more) with a total interruption time of 10 hours or less (e.g., five hours or less, two hours or less, one or less).
  • the gas field ion source may interact with gas atoms to generate the ion beam continuously for the entire time period (corresponding to a total interruption time of zero hours), but this is not necessary.
  • Such time periods correspond to an interruption time.
  • interruption times may occur one time or more than one time (e.g., two times, three, times, four times, five times, six times, seven times, eight times, nine times, 10 times).
  • the interruptions may be due, for example, to scheduled maintenance, unexpected maintenance, and/or down time between shifts (e.g., overnight down time).
  • the total of the interruption times is the total interruption time. As an example, if during the time period there are three interruption times, each of one hour, then the total interruption time is three hours.
  • the total interruption time is three hours.
  • the current of ion beam 192 at surface 181 of sample 180 varies by 10% or less (e.g., 5% or less, 1% or less) per minute.
  • Ion microscope 200 can have a relatively good resolution.
  • the resolution of ion microscope 200 can be 10 nm or less (e.g., nine nm or less, eight nm or less, seven nm or less, six nm or less, five nm or less, four nm or less, three nm or less, two nm or less, one nm or less).
  • the resolution of ion microscope 200 can be 0.05 nm or more (e.g., 0.1 nm or more, 0.2 nm or more, 0.25 nm or more, 0.5 nm or more, 0.75 nm or more, one nm or more, two nm or more, three nm or more).
  • the resolution of ion microscope 200 can be from 0.05 nm to 10 nm (e.g., from 0.1 nm to 10 nm, 0.2 nm to 10 nm, 0.25 nm to 3 nm, 0.25 nm to one nm, 0.1 nm to 0.5 nm, 0.1 nm to 0.2 nm).
  • the resolution of an ion beam refers to the size of the smallest feature that can be reliably measured from images obtained using the ion microscope.
  • a size of a feature is reliably measured if it can be determined to within an error of 10% or less of the actual size of the feature, and with a standard deviation in the measured size of less than 5% of the actual size of the feature, from ten images of the feature obtained under similar conditions.
  • Ion microscope 200 can be used to take a good quality image in a relatively short period of time.
  • ion microscope 200 can have a quality factor of 0.25 or more (e.g., 0.5 or more, 0.75 or more, one or more, 1.5 or more, two or more).
  • the quality factor is determined as follows.
  • the sample is imaged pixel-by-pixel by sub-dividing the surface of the sample into an x-y array of 512 pixels by 512 pixels.
  • the dwell time per pixel is 100 ns during the measurement.
  • the total abundance of secondary electrons from the sample is measured as a function of the position of the ion beam on the surface of the sample.
  • an average pixel intensity G 1 is determined, along with a standard deviation SD 1 from the distribution of Si pixel intensities.
  • an average pixel intensity G 2 is determined, along with a standard deviation SD 2 from the distribution of Cu pixel intensities.
  • the quality factor is calculated according to the equation
  • Surface 181 of sample 180 can undergo relatively little damage when exposed to ion beam 192.
  • surface 181 of sample 180 can have a value of 25 nm or less (e.g., 20 nm or less, 15 nm or less, 10 nm or less, five nm or less) according to the damage test.
  • the damage test is performed as follows. An atomically flat silicon (99.99% purity) sample with a four square ⁇ m field of view is imaged for 120 seconds while rastering the ion beam across the surface of the sample pixel-by-pixel using an ion beam current at the sample of 10 pA and a spot size of the ion beam at the sample of 10 nm or less.
  • the four square ⁇ m field of view is broken into a 512 pixel by 512 pixel array for rastering purposes.
  • the value of the damage test corresponds to the maximum distance of etching into the imaged portion of the silicon sample resulting from performing the damage test.
  • a sample that includes gold islands formed on a carbon substrate (as discussed previously in connection with measurement of the He ion beam spot size) is inserted into the He ion microscope, and a measurement of the He ion beam spot size is performed as discussed above.
  • the location of the sample along the z-axis is iteratively adjusted so that the position of the sample that yields the smallest He ion beam spot size is determined. This position along the z-axis is denoted Z f .
  • the spot size of the He ion beam at Z f is denoted SSf.
  • the sample is then translated in increments along the -z direction relative to Z f .
  • a gas field ion microscope e.g., He ion microscope
  • a gas field ion microscope can be used to distinguish elements in a sample having very close atomic numbers (Z values) using, for example, secondary electron yield, scattered ion abundance, and/or angle- and energy-resolved scattered ion detection.
  • the gas field ion microscope can be used to distinguish elements having atomic numbers (Z values) that differ only by one.
  • a gas field ion microscope e.g., He ion microscope
  • a gas field ion microscope can be used to distinguish elements in a sample having a very close masses using, for example, secondary electron yield, scattered ion abundance, and/or angle- and energy-resolved scattered ion detection.
  • the gas field ion microscope can be used to distinguish elements having masses that differ by one atomic mass unit or less (e.g., 0.9 atomic mass unit or less, 0.8 atomic mass unit or less, 0.7 atomic mass unit or less, 0.6 atomic mass unit or less, 0.5 atomic mass unit or less, 0.4 atomic mass unit or less, 0.3 atomic mass unit or less, 0.2 atomic mass unit or less, 0.1 atomic mass unit or less), m some embodiments, a sample may have domains formed of materials (e.g., alloys) having different average masses.
  • materials e.g., alloys
  • the gas field ion microscope can, for example, be used to distinguish domains of material having masses that differ only by one atomic mass unit or less (e.g., 0.9 atomic mass unit or less, 0.8 atomic mass unit or less, 0.7 atomic mass unit or less, 0.6 atomic mass unit or less, 0.5 atomic mass unit or less, 0.4 atomic mass unit or less, 0.3 atomic mass unit or less, 0.2 atomic mass unit or less, 0.1 atomic mass unit or less).
  • one atomic mass unit or less e.g., 0.9 atomic mass unit or less, 0.8 atomic mass unit or less, 0.7 atomic mass unit or less, 0.6 atomic mass unit or less, 0.5 atomic mass unit or less, 0.4 atomic mass unit or less, 0.3 atomic mass unit or less, 0.2 atomic mass unit or less, 0.1 atomic mass unit or less.
  • FIG. 21 is a schematic diagram of a portion of a gas field ion microscope that includes gas source 110 and a vacuum pump 734.
  • Gas source 110 includes a delivery tube 730 of length q and diameter n terminating in a delivery nozzle 736, and vacuum pump 734 includes an inlet port 732.
  • Nozzle 736 is positioned at a distance g from apex 187 of tip 186, and inlet port 732 is positioned at a distance 1 from apex 187 of tip 186.
  • g can be 10 mm or less (e.g., 9 mm or less, 8 mm or less, 7 mm or less).
  • g is 3 mm or more (e.g., 4 mm or more, 5 mm or more, 6 mm or more).
  • g can be from 3 mm to 10 mm (e.g., from 4 mm to 9 mm, from 5 mm to 8 mm).
  • 1 can be 100 mm or less (e.g., 90 mm or less, 80 mm or less, 70 mm or less, 60 mm or less, 50 mm or less).
  • 1 is 10 mm or more (e.g., 20 mm or more, 30 mm or more, 40 mm or more).
  • 1 can be from 10 mm to 100 mm (e.g., from 30 mm to 100 mm, from 40 mm to 80 mm).
  • the local pressure of He gas at the position of apex 187 of tip 186 is 10 "5 Torr or more (e.g., 10 "4 Torr or more, 10 "3 Torr or more, 10 "2 Torr or more, 10 "1 Torr or more, 1 Torr or more).
  • the overall pressure of He gas in microscope system can be reduced relative to systems that employ background
  • the overall He pressure in microscope system 200 can be 10 "4 Torr or less (e.g., 10 '5 Torr or less, 10 "6 Torr or less, 10 '7 Torr or less, 10 '8 Torr or less).
  • the distance 1 and the cross-sectional area of inlet port 732 are selected so that vacuum pump 734 captures un-ionized He atoms within a particular solid angle region of microscope system 200.
  • the solid angle subtended by inlet port 732 is 5° or more (e.g., 10° or more, 15° or more, 20° or more, 30° or more, 40° or more).
  • the ratio of the length q of delivery tube 730 to the diameter n of tube 730 can be selected to control the distribution of trajectories of He gas atoms delivered to tip 186.
  • the ratio q/n can be 3 or more (e.g., 4 or more, 5 or more, 6 or more) and/or 10 or less (e.g., 9 or less, 8 or less, 7 or less). In certain embodiments, the ratio q/n can be between 3 and 10 (e.g., between 3 and 9, between 4 and 9, between 4 and 8, between 5 and 8, between 5 and 7).
  • the gas delivery system can include more than one delivery tube and nozzle.
  • the gas delivery system can include two or more (e.g., three or more, four or more, five or more, six or more) gas delivery tubes.
  • Each of the multiple gas delivery tubes can be positioned to deliver He gas, in a relatively directed fashion, to tip 186.
  • the local pressure of He gas at the position of apex 187 of tip 186 can be increased even further.
  • One or more vacuum pumps can be used to remove un-ionized He gas from microscope system 200.
  • gas delivery tube 730 can be incorporated into another component of the system.
  • gas delivery tube 730 can be formed by one or more passageways (e.g., two or more passageways, four or more passageways, six or more passageways) for gas delivery in extractor 190 and/or suppressor 188.
  • one or more passageways (e.g., two or more passageways, four or more passageways, six or more passageways) for gas delivery can be provided in posts which support tip 186 (e.g., posts 522a/b and 552).
  • extractor 190 can include four passageways for gas delivery to tip 186.
  • the passageways can be equally spaced and arranged radially along a circumference of extractor 190 so that the opening of each passageway directly faces tip 186.
  • the length- to-diameter ratios of each of the passageways can be the same, or different.
  • a number of advantages can be realized by incorporating gas delivery tubes into other elements of microscope system 200. For example, using a metal tube 730 placed close to tip 186 for gas delivery can perturb electric fields in the vicinity of tip 186.
  • Incorporation of the gas delivery tube into another element of the microscope system can eliminate such perturbations.
  • the spatial region in the vicinity of tip 186 is typically crowded with electrodes and other devices for operation of microscope system 200.
  • gas delivery tube 730 By incorporating gas delivery tube 730 into another element of the system, crowding in the vicinity of tip 186 can be reduced.
  • He gas delivered via delivery tube 730 can be pre-cooled so that it is near the operating temperature of tip 186 when it enters microscope system 200.
  • a portion of delivery tube 730 can be placed in contact with a supply reservoir of coolant (e.g., liquid nitrogen) that is used to cool tip 186.
  • a supply reservoir of coolant e.g., liquid nitrogen
  • the material of the sample can be damaged by the positive charges.
  • certain materials are charge sensitive, and can react violently (e.g., explode) in the presence of excess positive (or negative) charge.
  • positive charging of the surface of the sample can cause inaccurate ion beam rastering. Deflection and deceleration of the incident ion beam as a result of the electric field created by positive charges at the surface of the sample can reduce the energy of the incident ions, and change their trajectories in difficult-to-predict fashion.
  • the surface of the sample can act as an electrostatic mirror for He ions, deflecting He ions away from the surface of the sample before the He ions reach the surface of the sample.
  • FIG. 22 shows a portion of a gas field ion microscope that includes a flood gun 840 configured to deliver an electron beam 842 to surface 181 of sample 180 while He ion beam 192 is incident on surface 181.
  • the electron flux on surface 181 can, in general, be controlled so that surface charging effects are counterbalanced by electron beam 842 to the extent desired.
  • FIG. 22 depicts ion beam 192 and electron beam 842 simultaneously impinging on surface 181 of sample 180
  • flood gun 840 can be configured to deliver electron beam 842 to sample 180 to create a charge layer 846 in a sub-surface region of sample 180 (FIG. 23).
  • Layer 846 has an average depth m below surface 181, and layer 846 has a thickness r measured in a direction normal to surface 181.
  • the depth m and thickness r, as well as the density of electrons in layer 846, can be controlled by the energy of the electrons in electron beam 842, the angle of incidence of the electrons in electron beam 842 with respect to surface 181, and the total dosage of electrons delivered to sample 180.
  • the average energy of the electrons in electron beam 842 when incident on surface 181, is adjustable.
  • the average energy of the electrons can be 500 eV or more (e.g., 1 keV or more, 2 keV or more), and/or 20 keV or less (e.g., 15 keV or less, 10 keV or less).
  • the average energy of the electrons in electron beam 842 when incident on surface 181, can be from 500 eV to 20 keV (e.g., from 1 keV to 15 keV, from 2 keV to 10 keV).
  • the angle of incidence ⁇ of the electrons in electron beam 842 with respect to surface 181 corresponds to the angle between a principal trajectory 850 of electron beam 842 and a normal 848 to surface 181.
  • ⁇ is 0° or more (e.g., 10° or more, 20° or more), and/or 80° or less (e.g., 70° or less, 60° or less).
  • ⁇ can be from 0° to 70° (e.g., from 0° to 10°, from 40° to 60°).
  • the total current of electrons delivered to sample 180 is 10 pA or more (e.g., 100 pA or more, 1 nA or more, 10 nA or more), and/or 100 ⁇ A or less (e.g., 10 ⁇ A or less, 1 ⁇ A or less, 500 nA or less, 100 nA or less).
  • the total current of electrons delivered to sample 180 can be from 10 pA to 1 ⁇ A (e.g., from 100 pA to 100 nA, from 1 nA to 10 nA).
  • m is 10 ran or more (e.g., 25 nm or more, 50 nm or more, 75 nm or more, 100 nm or more), and/or 500 nm or less (e.g., 400 nm or less, 300 nm or less, 200 nm).
  • m can be from 10 nm to 500 nm (e.g., from 25 nm to 500 nm, from 50 nm to 500 nm, from 75 nm to 400 nm, from 100 nm to 400 nm).
  • multiple flood guns can be used.
  • different flood guns can be used to expose different portions of surface 181 of sample 180 to electrons.
  • each flood gun can be used to expose the same portion of surface 181 to electrons.
  • different flood guns can be operated at different times.
  • one or more flood guns can be used to expose surface 181 to electrons before surface 181 is exposed to He ions (e.g., to form a subsurface charge layer), while one or more different flood guns can be used to expose surface 181 to electrons while surface 181 is also being exposed to He ions.
  • all the flood guns can be used to expose surface 181 to electrons before surface 181 is exposed to He ions (e.g., to form a sub-surface charge layer), whereas in certain embodiments all the flood guns can be used to expose surface 181 to electrons while surface 181 is also being exposed to He ions.
  • Other combinations may also be used.
  • combinations of one or more collector electrodes and one or more flood guns can be used.
  • one or more flood guns can be used to expose surface 181 of sample 180 to electrons before surface 181 is exposed to He ions (e.g., to form a sub-surface charge layer), and one or more collector electrodes can be used to neutralize charging at surface 181 while surface 181 is being exposed to He ions.
  • Other combinations are also possible.
  • flood gun 840 can be configured to deliver a very low energy beam of electrons 842 to sample 180.
  • electrons in beam 842 can have an average energy of about 50 eV or less.
  • the low energy electrons have low landing energies, and this limits the amount of negative charge that can accumulate on surface 181.
  • the average electron energy in electron beam 842 is 50 eV, once sample 180 charges to a potential of -50 V relative to the common ground, electrons from flood gun 840 will no longer land on the surface of the sample.
  • the energy of the low energy electrons from flood gun 840 the maximum accumulated negative charge on surface 181 of sample 180 can be controlled.
  • This method can be used to image non-conducting materials without depositing a layer of conductive material on top of the non-conducting material to prevent charging of the nonconducting material.
  • An example of this method is shown in FIG. 25.
  • Ion beam 192 is incident on surface 181 of sample 180, which is a dielectric material with relatively low electrical conductivity (e.g., sample 180 is not metallic).
  • Sample 180 is supported by sample manipulator 140, which is biased at an electrical potential of -600 V relative to the common external ground of microscope system 200. The electrical potential applied to manipulator 140 creates an electric field at surface 181 of sample 180.
  • FIGS. 27 A and 27B An example of the use of an embedded layer of negative charge is shown schematically in FIGS. 27 A and 27B.
  • ion beam 192 is incident on surface 181 of sample 180.
  • a plurality of secondary electrons 2012 are generated within the first few nanometers of sample 180.
  • many of the secondary electrons escape as free electrons 2014, which can be detected by a suitably configured detector.
  • incident He ions implant within sample 180, forming a positively-charged layer 2010 within sample 180.
  • secondary electrons 2012 are increasingly attracted toward layer 2010, and fewer and fewer secondary electrons 2012 escape sample 180 as free electrons 2014.
  • imaging of sample 180 via detection of secondary electrons can become increasingly difficult.
  • sample manipulator 140 can be configured to decouple sample 180 from other parts of system 200, thereby reducing the impact of external mechanical disturbances.
  • FIG. 28 shows a vibration-decoupled sample manipulator 140 that includes a guiding needle 906 supported by an actuator 908, with needle 906 and actuator 908 each located within a stage 904.
  • a support disk 902 is positioned atop stage 904, and a friction spider 900, which supports sample 180, is placed atop disk 902.
  • guiding needle 906 can have a substantially rectangular cross-sectional shape.
  • a rectangular cross-sectional shape may assist in ensuring that rotation of sample 180 and/or of spider 900 does not occur as spider 900 is translated in the x- and/or y-directions by guiding needle 906.
  • the materials used to form spider 900 and/or disk 902 can be selected so that an even higher static frictional force between these elements is present.
  • spider 900 and disk 902 can be magnetically coupled to increase the frictional force between these elements. Magnetic field coupling can be carefully implemented to ensure that the magnetic field is localized and does not disturb sample 180 or impinging ion beam 192.
  • FIG. 29 depicts a sample holder assembly 1510 for a microscope system.
  • Sample holder assembly 1510 reduces the use of bearings and helps reduce low frequency mechanical vibrations in the sample during operation.
  • Assembly 1510 includes a body 1511 having an opening 1512 to insert a sample.
  • Body 1511 is connected to arms 1518 through adjustable connectors 1522.
  • Arms 1518 support a sample stage 1514 using grips 1520.
  • Sample stage 1514 includes a surface disk 1516 having an aperture 1524.
  • Assembly 1510 may be connected to an ion microscope such that tip 186 is pointed towards aperture 1524 on sample stage 1514.
  • Body 1511 maybe formed from suitable rigid materials such as hardened steel, stainless steel, phosphor bronze, and titanium. Body 1511 may be sized and shaped to suit the particular needs of the application. As an example, the size and shape of body 1511 may be chosen for use with the microscope systems disclosed herein.
  • a sample may be introduced to assembly 1510 through opening 1512.
  • Sample stage 1514 is supported by arms 1518 connected to body 1511 along adjustable connectors 1522.
  • Adjustable connectors 1522 allow for vertical movement of arms 1518. Arms 1518 and sample stage 1514 can be moved in a vertical direction and locked in a specific position.
  • Connectors 1522 can be pneumatic or vacuum controlled such that arms 1518 and stage 1514 can be tightly locked in a desired vertical position.
  • Connectors 1522 can optionally include other types of connectors.
  • Sample stage 1514 is connected to arms 1518 using grip 1520.
  • Arm 1518 can have a shaft extending inwards such that grip 1520 of sample stage 1514 can clasp the shaft.
  • Grip 1520 can be pneumatically or vacuum operated such that stage 1514 can be tilted.
  • Grip 1520 can be controlled such that stage 1514 is tilted to a desired position. In some embodiments, after a desired position has been reached, grip 520 can be tightened such that sample stage 1514 is tightly locked in the desired tilted position.
  • Sample stage 1514 further includes surface disk 1516 having an opening 1524.
  • a sample may be placed on disk 1516 and a sample position control system can be introduced through opening 1524 to move the sample on the plane of disk 1516.
  • disk 1516 can be rotated about its center to rotate and move the sample located on the surface of the disk as desired.
  • Disk 1516 may be formed from suitable rigid materials including ceramic, glass and polymers.
  • FIG. 30 depicts a sample holder assembly for a microscope system.
  • the sample holder assembly of FIG. 30 is similar to the sample holder assembly of FIG. 29 with a spider 1600 placed on a surface of disk 1516.
  • Spider 1600 can have legs to allow it to be positioned on top of opening 1524.
  • spider 1600 can have an opening on a portion of the surface.
  • Spider 1600 can be formed from suitable rigid materials including ceramic, glass and polymers.
  • sample 180 can be moved in the z- direction, tilted, translated in the x-y plane, and rotated. If sample 180 is tilted and the tilt angle (e.g., the angle between ion beam 192 and a normal to the surface of sample 180) is relatively large, the inclined sample may not be in focus over the entire field of view of microscope system 200. As a result, the image of the sample obtained under these conditions may be out of focus and blurred at the areas outside of the center and vertical to the tilt axis.
  • the tilt angle e.g., the angle between ion beam 192 and a normal to the surface of sample 180
  • sample manipulator 140 can transmit tilt angle information for sample 180 to electronic control system 170.
  • tilt angle information can be entered manually by a system operator via a user interface.
  • Electronic control system 170 can determine, based upon the orientation of sample 180, a set of voltage corrections to apply to second lens 226 to dynamically change the focal length of lens 226 as ion beam 192 is scanned over the surface of tilted sample 180.
  • the lateral dimensions of the inclined sample are distorted due to the projection of the tilted sample on a plane surface and due to the difference in distance to the ion optics 130.
  • lateral dimensions of inclined sample surfaces may appear shorter that they actually are due to the orientation of sample 180 with respect to ion beam 192.
  • Another example is the keystone distortion of the image. The effect is that a rectangular feature is distorted so that the image of the rectangle appears to be keystone in its shape.
  • the electronic control system 170 can get the information about the tilt angle for sample 180 in the same way as described above.
  • Electronic control system 170 can determine, based upon the tilt of sample 180, adjustments of the scan amplitude to apply to scanning deflectors 219 and 221 to adapt the ion beam deflection as ion beam 192 is scanned over the surface of tilted sample 180 for an undistorted imaging of the surface of tilted sample 180.
  • these two distortion effects can be corrected by digital manipulation of the distorted image.
  • neutral particles e.g., He atoms
  • neutral particles can negatively impact the performance of the microscope system.
  • Doubly-charged He ions e.g., He 2+
  • gas field ion source 120 can also be produced in gas field ion source 120, either via double-ionization of He atoms in the vicinity of tip 186, or by collisions between He ions.
  • the focusing properties of doubly-charged He ions are different from singly-charged ions, and doubly-charged ions present in ion beam 192 can lead to larger spot sizes on sample 180 and other undesirable effects.
  • One approach to reducing the population of neutral particles in ion beam 192 involves reducing the probability that neutral particles will make their way into the ion beam. Such an approach can involve, for example, using directed gas delivery to tip 186 (see discussion above) to reduce the overall presence of un-ionized He gas atoms in microscope system 200.
  • FIG. 31 shows ion optics 130 in which deflector 220 is offset from longitudinal axis 132 of ion optics 130, and in which an additional deflector 223 is disposed.
  • He ion beam 192 includes He ions 192a and He atoms 192b.
  • the electrical potential applied to deflector 223 is adjusted to cause deflection of He ions 192a in the x-direction. He atoms 192b are unaffected by deflector 223, and are therefore undeflected. He atoms 192b are subsequently intercepted by collector 1016, which prevents He atoms 192b from passing through aperture 224.
  • the electrical potentials applied to deflectors 220 and 222 are also adjusted so that the trajectories of He ions 192a are re-aligned with longitudinal axis 132, and a portion of He ions 192a pass through aperture 224 and are incident on surface 181 of sample 180 as ion beam 192.
  • Other techniques may also be used to remove neutral particles from an ion beam.
  • such techniques involve deflecting the ions in the ion beam using electric and/or magnetic field(s), without deflecting the neutral particles.
  • combinations of electric and magnetic fields can be used to compensate for energy dependent spatial separation of ions resulting from ion deflection in ion optics 130.
  • various asymmetric ion column geometries e.g., bent ion columns
  • a bent column configuration of ion optics 130 can be used to separate He atoms, singly-charged He ions, and doubly-charged He ions.
  • Ion beam 192 enters ion optics 130 propagating along a direction that is tilted with respect to axis 132 of ion optics 130.
  • Ion beam 192 includes neutral He atoms, He + ions, and He 2+ ions.
  • An electrical potential is applied to deflector 223, deflecting He + ions in ion beam 192 so that after passing through deflector 223, the He + ions propagate along axis 132 as ion beam 192a.
  • neutral atoms are undeflected on passing through deflector 223.
  • Neutral atom beams 192b are undeflected and are intercepted at positions following each deflector by collectors 1016b. Doubly-charged He ions are deflected even further than He + ions, and multiple He + beams 192c are intercepted by collectors 1016c. As a result, He atoms, He + ions, and He + ions are spatially separated from one another, and the He + ions are directed toward sample 180 as ion beam 192, while the undesired beam constituents are blocked in ion optics 130.
  • the use of magnetic fields can lead to spatial separation of the trajectories of ions in ion beam 192 which have the same charge, but which correspond to different isotopes of the gas introduced by gas source 110.
  • gases such as He, which have a dominant naturally occurring isotope (e.g., greater than 90% relative abundance)
  • separation effects due to magnetic fields are typically small.
  • an isotope separator e.g., a block used to prevent undesired isotopes from traversing the length of ion optics 130
  • a collector 1016 that is used to block neutral atoms or doubly-charged ions can also be used to block unwanted isotopes in ion beam 192.
  • the interaction of the ion beam with the sample can cause different types of particles to leave the surface through various interactions as described below.
  • Such particles include secondary electrons, Auger electrons, scattered ions, primary neutral particles, X-ray photons, IR photons, visible photons, UV photons, secondary ions and secondary neutral particles.
  • One or more types of particles can be detected and analyzed to determine one or more different types of information about the sample.
  • Such types of information about the sample include topographical information about the surface of the sample, material constituent information about the surface of the sample, material constituent information about a sub-surface region of the sample, crystalline information about the sample, voltage contrast information about the surface of the sample, voltage contrast information about a sub-surface region of the sample, magnetic information about the sample, and optical information about the sample.
  • the term surface of a sample refers to the volume up to a depth of five nm or less.
  • Secondary electrons can be detected using one or more appropriate detectors capable of detecting electrons (see discussion above regarding types of detectors). If multiple detectors are used, the detectors may all be the same type of detector, or different types of detectors may be used, and may generally be configured as desired.
  • the detectors can be configured to detect secondary electrons leaving surface 181 of sample 180 (the surface on which the ion beam impinges), surface 183 of sample 180 (the surface on the opposite side from where the ion beam impinges) or both (see discussion above regarding configurations of detectors).
  • Detected secondary electron signals can be used to form an image of a sample.
  • the ion beam is raster-scanned over a field of view of the surface of the sample, and the secondary electron signal at each raster step (which corresponds to an individual pixel in an image) is measured by one or more detectors.
  • each detector remains in fixed position relative to the sample as the ion beam is raster-scanned over the field of view of the surface of the sample.
  • one or more detectors can be moved relative to the sample. For example, if a single detector is being used, moving the detector relative to the sample can yield angle-dependent information about the sample.
  • detecting the total abundance of secondary electrons can provide information regarding the topography of a sample.
  • the secondary electron total abundance at a given location on a surface generally depends upon the slope of the surface relative to the ion beam at that point. In general, the secondary electron total abundance is higher where the slope of the surface relative to the ion beam is higher (i.e., where the angle of incidence of the ion beam as measured from the surface normal is larger).
  • the change in the total abundance of secondary electrons as a function of the location of the ion beam on the surface of the sample can be correlated to a change in the slope of the surface, providing information regarding the topography of the surface of the sample.
  • detecting the total abundance of secondary electrons can yield material constituent information (e.g., elemental information, chemical environment information) about a sample, hi such embodiments, the information is predominantly related to the surface of the sample.
  • material constituent information e.g., elemental information, chemical environment information
  • each element or material in a given chemical environment will have a particular inherent secondary electron yield.
  • the secondary electron total abundance at a given location on a surface generally depends on the material present at that location. Therefore, the change in the total abundance of secondary electrons as a function of the location of the ion beam on the surface of the sample, can be correlated to a change in the element(s) and/or material(s) present at the surface of the sample, providing material constituent information about the surface of the sample.
  • specific materials in a sample can be identified based on quantitative measurements of secondary electron yields from the sample.
  • materials such as Al, Si, Ti, Fe, Ni 5 Pt, and Au have known secondary electron yields when exposed to a He ion beam under controlled conditions.
  • An ion microscope e.g., a gas field ion microscope
  • secondary electron yields for various materials are shown in Table I. The yields were measured at normal incidence of the He ion beam, and at an average ion energy of 21 keV.
  • the yields shown in Table I are typically scaled by a multiplicative factor that corresponds to the secant of the angle of incidence of the ion beam on the surface of the sample.
  • Other experimental conditions are described in the corresponding Example noted below.
  • detecting the total abundance of secondary electrons can yield voltage contrast information, which in turn, can provide information regarding the electrical conductivity properties and/or the electrical potential of an element and/or a material at the surface of a sample.
  • the secondary electron total abundance at a given location on the surface of a sample usually depends on the electrical properties of the material present at the surface of the sample. In general, less electrically conducting materials will tend to become positively charged over time while being exposed to an ion beam over time, whereas more electrically conducting materials will have less of a tendency to become positively charged over time while being exposed to an ion beam.
  • the secondary electron total abundance at a given location of the surface of a sample will tend to decrease over time for a material that is less electrically conducting (due to more surface charging resulting in fewer secondary electrons escaping the sample), while the secondary electron total abundance at a given location of the surface of the sample that is more electrically conducting will tend to undergo less reduction in secondary electron total abundance over time (due to less surface charging).
  • the change in the total abundance of secondary electrons as a function of the ion beam location at the sample surface can be correlated to the electrical conductivity of the material at that location, providing voltage contrast information about the surface of the sample.
  • Sub-surface voltage contrast effects can be provided by He ions which become embedded within sub-surface regions of the sample. As described in connection with FIGS. 27 A and 27B, sub-surface He ions can prevent secondary electrons generated in the sample from escaping the sample surface. Thus, contrast in secondary electron images of the sample can be due to sub-surface charging of the sample by incident He ions.
  • voltage contrast measurements can be used to determine whether portions of electrical devices and/or circuits are at different potentials when exposed to the ion beam due to the presence or absence of electrical connections between the portions, and therefore whether the devices and/or circuits are operating correctly or not.
  • detecting the total abundance of secondary electrons can provide crystalline information about a sample.
  • the total abundance of secondary electrons can vary depending on whether the ion beam is aligned with the crystal structure of the sample (e.g., aligned parallel to one of the unit vectors describing the crystal lattice) or not. If the ion beam is aligned with the crystal structure of the sample, the probability that ions in the ion beam can generally penetrate into a given distance into the sample without undergoing a collision with a sample atom (commonly referred to as channeling) is relatively high, resulting in a lower total abundance of secondary electrons.
  • the ions in the ion beam will have a lower probability of penetrating into the sample the given distance without undergoing a collision with a sample atom, resulting in a higher total abundance of secondary electrons. Therefore, the change in the total abundance of secondary electrons as a function of the ion beam location at the sample surface can be correlated to the crystalline information of the material at that location. For example, there may be regions of the sample surface where the secondary electron total abundance is substantially the same.
  • Such regions can, for example, have the same crystal orientation, and the size of the regions can provide grain size and/or crystal size information (e.g., in a polycrystalline sample that includes multiple, oriented crystal domains), and/or can provide information regarding strained regions of sample (whether amorphous or crystalline) because the magnitude of the secondary electron total abundance for a material of a given chemical composition (e.g., elemental composition, material composition) can depend on the strain of the material.
  • a material of a given chemical composition e.g., elemental composition, material composition
  • detecting the total abundance of secondary electrons can provide magnetic information about a sample.
  • the total abundance of secondary electrons can depend on the magnitude of a magnetic field adjacent the sample surface.
  • the magnetic field adjacent to the sample surface varies due to magnetic domains within the sample that produce local magnetic fields at the sample surface.
  • a static magnetic field is applied by an external magnetic field source, and magnetic domains within the sample produce local magnetic fields at the surface of the sample that introduce variations in the applied external magnetic field. In either case, variations in the local magnetic field at the surface of the sample can, for example, change the trajectories of secondary electrons ejected from the sample.
  • the change in secondary electron trajectories can correspond to an increase in the total abundance of secondary electrons when the trajectories of the secondary electrons are changed so that more secondary electrons are directed toward the detector(s), or the change in secondary electron trajectories can correspond to a decrease in the total abundance of secondary electrons when the trajectories of the secondary electrons are changed so that more secondary electrons are directed away from the detector(s).
  • the contrast that appears in a secondary electron image of the sample may be due to two or more of the mechanisms discussed above.
  • secondary electron images of certain samples can include contrast that is due in part to topographic variations in the sample surface, material constituent variations in the sample surface, voltage contrast variations in the sample surface, crystalline variations in the sample surface, and/or magnetic variations in the sample surface. Accordingly, it can be advantageous to combine information gained from measuring the secondary electron total abundance with information gained from measuring other types of particles to
  • Secondary electron imaging techniques can be applied to a variety of different classes of samples.
  • An example of such a class of materials is semiconductor articles, such as patterned wafers, which can include, for example, multiple electrical conductors surrounded by a matrix of insulating material.
  • Secondary electron imaging techniques can be used to identify defects in the device, such as incomplete electrical connections between conductors, and/or electrical shorts between circuit elements. More generally, secondary electron imaging techniques can be used for a wide range of ion beam testing applications of semiconductor articles. Optionally, this approach can similarly be used for purposes of mask repair.
  • the He ion source also provides a greater depth of focus than an electron source.
  • images of a sample obtained using an ion microscope e.g., a gas field ion microscope
  • Auger electron detection Another advantage of using an ion beam, as opposed to an electron beam, for Auger electron detection is that when using an electron beam the Auger electrons are detected on a baseline of backscattered electrons, and, using an ion beam, the
  • backscattered electrons are not present.
  • it can be possible to obtain a relatively high signal to noise ratio for detected Auger electrons while collecting a relatively small number of Auger electrons, which can reduce the amount of time it takes to obtain a relatively good quality Auger electron spectrum from a sample when using an ion beam.
  • a scattered ion is generated when an ion from the ion beam
  • scattered ions generally provide information about the surface of the sample.
  • the particular arrangement of the detector(s) generally depends on the type of information that is desired to be obtained.
  • topographical information about a sample surface can be obtained via detected scattered ions.
  • FIG. 34A generally depicts an embodiment of an approach to detecting scattered ions from different regions of a surface to determine topographical information about the surface of a sample.
  • FIG. 34A shows a sample 7010 having regions 7012, 7014 and 7016 with surfaces 7013, 7015 and 7017, respectively.
  • Scatter patterns 7020, 7030 and 7040 represent the angular distribution of ions scattered from surfaces 7013, 7015 and 7017, respectively, when the ion beam is perpendicularly incident thereon.
  • each of scatter patterns 7020, 7030 and 7040 is a cosine-type distribution.
  • 34B depicts the contribution to the relative intensities 7042 and 7052 (dashed line and dotted line, respectively) of scattered ions detected by detectors 7041 and 7050, respectively, arising from topographical effects.
  • the relative total abundance profiles from detectors 7041 and 7050 can be used to determine the topography of sample 7010.
  • the contribution to the total abundance of the scattered ions detected that is due to topography alone can be removed from the total abundance of the detected scattered ions to determine the contribution to the total detected scattered ions due to other effects (e.g., changing material across the surface of sample 7010).
  • topographic information is obtained from He ions that are scattered at large scattering angles.
  • topographic information from scattered ions is determined by detecting scattered ions at an angle of 60° or greater (e.g., 65° or greater, 70° or greater, 75° or greater) relative to the direction of the ion beam.
  • FIG. 34A depicts the use of two detectors, in some embodiments a single detector is used (e.g., detector 7041 or detector 7050). Alternatively, in certain embodiments, more than two (e.g., three, four, five, six, seven, eight) detectors can be used.
  • FIGS. 35A-35I generally depict various embodiments of approaches to detecting scattered ions from different regions of a surface to determine topographical information about the surface of a sample.
  • FIGS. 35A, 35D and 35G shows a sample 8050 having regions 8052, 8054, 8056 and 8058 with surfaces 8053, 8055, 8057, 8059 and 8061, respectively.
  • FIGS. 35H and 351 depict the total yield of scattered ions and the relative abundance of detected scattered ions when a top detector 80140 a relatively large acceptance angle for scattered ions is used to detect the scattered ions. As shown in FIG. 351, by selecting the appropriate acceptance angle of detector 80140, the relative abundance of the detected scattered ions is substantially the same across the sample.
  • the total abundance of scattered He ions from a tungsten atom at a surface of the semiconductor article will be approximately 25 times the total abundance of scattered ions from a silicon atom at the surface of the semiconductor article.
  • the total abundance of scattered He ions from a gold atom at a surface of the semiconductor article will be approximately 25 times the total abundance of scattered ions from a silicon atom at the surface of the semiconductor article.
  • Another approach to determining material constituent information about the surface of a sample by detecting scattered He ions involves measuring the scattered He ions in an energy-resolved and angle-resolved fashion.
  • second lens 226 focuses He ion beam 192 onto surface 181 of sample 180.
  • He ions 1102 scatter from surface 181 and are detected by detector 1100.
  • Detector 1100 is designed so that the angle and energy of each detected scattered He ion is known for each angle ⁇ within the acceptance angle of detector 1100.
  • the mass of the atom at the surface that scatters the scattered He ion can be calculated based on the following relationship:
  • E s is the energy of the scattered He ion
  • Ej is the incident energy of the He ion
  • M ⁇ e is the mass of the He ion
  • ⁇ s is the scattering angle
  • M a is the mass of the atom that scatters the He ion.
  • Detector 1100 can, for example, be an energy-resolving phosphor-based detector, an energy-resolving scintillator-based detector, a solid state detector, an energy-resolving electrostatic prism-based detector, an electrostatic prism, an energy-resolving ET detector, or an energy-resolving microchannel. In general, it is desirable for detector 1100 to have a substantial acceptable angle. In some embodiments, detector 1100 is stationary (e.g., an annular detector). In certain embodiments, detector 1100 can sweep through a range of solid angles.
  • the ions in the ion beam will have a lower probability of penetrating into the sample the given distance without undergoing a collision with a sample atom, resulting in a higher total abundance of scattered He ions. Therefore, the change in the total abundance of scattered He ions as a function of the ion beam location at the sample surface can be correlated to the crystalline information of the material at that location. For example, there may be regions of the sample surface where the scattered He ions' total abundance is substantially the same.
  • crystalline information about the surface of a sample can be obtained by exposing a region of the surface to an ion beam (without rastering the ion beam) and then measuring a pattern of the scattered He ions (e.g., similar to a Kikuchi pattern obtained due to backscattered electrons from a sample surface exposed to an electron beam).
  • the pattern of the scattered He ions can be analyzed to determine, for example, the orientation, lattice spacing, and/or crystal type (e.g., body centered cubic, face centered cubic) of the material at the location of the sample surface that is exposed to the ion beam.
  • Scattered ion imaging techniques can be applied to a variety of different classes of samples.
  • An example of such a class of materials is semiconductor articles, such as patterned wafers, which can include, for example, multiple electrical conductors surrounded by a matrix of insulating material.
  • Scattered ion imaging techniques can be used to identify defects in the device, such as incomplete electrical connections between conductors, and/or electrical shorts between circuit elements. Optionally, this approach can similarly be used for purposes of mask repair.
  • Another example of a sample class for which scattered ion imaging techniques can be used is metals and alloys. For example, images of samples that contain mixed materials such as alloys can be used to determine the surface distribution of each of the materials in the sample.
  • Yet another example of a sample class where scattered ion imaging techniques can be used is read/write structures for data storage. Additional examples of classes of materials for which scattered ion imaging techniques can be used are biological materials and pharmaceutical materials.
  • scattered ions are not formed when a sample surface is exposed to an electron beam of the type used in conventional SEMs, and thus none of the crystalline information or material constituent information obtainable via detected scattered He ions is available with such SEMs.
  • This is a significant advantage of a gas field ion microscope (e.g., a He ion microscope) as described herein relative to a conventional SEM.
  • a depth profile of material constituent information can be obtained by taking multiple He atom images of a sample at varying ion beam energies (probe depths).
  • tomographic reconstruction algorithms and/or techniques can be applied to the depth dependent information to perform tomographic reconstruction of the structure of the sample.
  • Primary neutral particle (e.g., He atom) techniques can be applied to a variety of different classes of samples.
  • An example of such a class of materials is semiconductor articles, such as patterned wafers, which can include, for example, multiple electrical conductors surrounded by a matrix of insulating material.
  • Primary neutral particle techniques can be used to identify defects in the device, such as incomplete electrical connections between conductors, and/or electrical shorts between circuit elements. Optionally, this approach can similarly be used for purposes of mask repair.
  • Another example of a sample class for which primary neutral particle imaging techniques can be used is metals and alloys. For example, images of samples that contain mixed materials such as alloys can be used to determine the surface distribution of each of the materials in the sample.
  • Yet another example of a sample class where primary neutral particle imaging techniques can be used is read/write structures for data storage. Additional examples of classes of materials for which primary neutral particle imaging techniques can be used are biological materials and pharmaceutical materials.
  • Primary neutral particles are generally not generated when a sample surface is exposed to an electron beam of the type used in conventional SEMs, and thus none of the crystalline information or material constituent information obtainable via detected scattered He ions is available with such SEMs. This is a significant advantage of a gas field ion microscope (e.g., a He ion microscope) as described herein relative to a conventional SEM.
  • a gas field ion microscope e.g., a He ion microscope
  • Typical photons of interest include X-ray photons, UV photons, visible photons and IR photons.
  • an IR photon is a photon having a wavelength of more than 700 nm to 100,000 run (e.g., from 1.2xlO ⁇ 5 keV to 1.7xlO "3 keV )
  • a visible photon is a photon having a wavelength of from more than 400 nm to 700 nm (e.g., from 1.8xlO "3 keV to 3xlO "3 keV)
  • a UV photon is a photon having a wavelength of more than 10 nm to 400 nm (e.g., from 3.IxIO "3 keV to 125 eV)
  • an X-ray photon is a photon having a wavelength of from 0.01 nm to 10 nm (e.g., from 125 eV to 125 keV).
  • such photons are
  • the photons can be detected using one or more appropriate detectors capable of detecting photons in a wavelength- resolved or energy-resolved fashion (see discussion above regarding types of detectors). If multiple detectors are used, the detectors may all be the same type of detector, or different types of detectors may be used, and may generally be configured as desired.
  • the detectors can be configured to detect photons leaving surface 181 of sample 180 (the surface on which the ion beam impinges), surface 183 of sample 180 (the surface on the opposite side from where the ion beam impinges) or both (see discussion above regarding
  • the system can include one or more optical elements (e.g., one or more lenses, one or more mirrors) that are adjacent the surface of the sample and that can direct the photons to the detector can be used (e.g., to increase the effective solid angle of detection of the detected photons).
  • optical elements e.g., one or more lenses, one or more mirrors
  • detecting the energy and/or wavelength of the photons can yield material constituent information (e.g., elemental information, chemical environment information) about a sample.
  • the information is predominantly related to the surface of the sample.
  • the photons emitted by the element or material will have a particular energy/band of energies and wavelength/band of wavelengths.
  • the energy and wavelength of the photons emitted from a given location on a surface generally depends on the material present at that location.
  • material constituent information about the sample can be obtained detecting photons by determining the de-excitation time of the sample material. This can be achieved, for example, by pulsing the ion beam to expose the sample to the ion beam for a brief period, followed by measuring the amount of time it takes to detect the photons, which relates to the de-excitation time of the sample material that emits the photons.
  • each element or material in a given chemical environment will have a particular de-excitation time period.
  • Crystalline information about a sample can be obtained using photon detection in combination with a polarizer because the polarization of the photons can depend upon the crystal orientation of the material in the sample.
  • the polarization of the photons emitted by a sample can be determined, providing information relating to the crystal orientation of the sample.
  • the information contained in the detected photons will predominantly be information about the surface of the sample.
  • detected photons can contain information relating to the sub-surface region of the sample.
  • detected photons can be used to determine optical properties of the sample.
  • the transparency of the sample to the photons can be investigated by manipulating the energy of the ions in the ion beam, and therefore their probe depth, and determining the corresponding impact on the intensity of the detected photons.
  • the detected photon intensity as a function of ion energy (probe depth) can yield information regarding the transparency of the sample to the photons.
  • Photon imaging techniques can be applied to a variety of different classes of samples.
  • An example of such a class of materials is semiconductor articles, such as patterned wafers, which can include, for example, multiple electrical conductors surrounded by a matrix of insulating material.
  • Photon imaging techniques can be used to identify defects in the device, such as incomplete electrical connections between conductors, and/or electrical shorts between circuit elements. Optionally, this approach can similarly be used for purposes of mask repair.
  • Another example of a sample class for which photon imaging techniques can be used is metals and alloys. For example, images of samples that contain mixed materials such as alloys can be used to determine the surface distribution of each of the materials in the sample.
  • Yet another example of a sample class where photon imaging techniques can be used is read/write structures for data storage. Additional examples of classes of materials for which photon imaging techniques can be used are biological materials and pharmaceutical materials.
  • Imaging samples using photons generated by exposure to a He ion beam can provide a number of advantages relative to photon imaging via other techniques, such as SEM.
  • the spot size of the He ion beam on the sample can be smaller than the spot size of an electron beam from a SEM.
  • the region of the sample that is exposed to the He ion beam is more carefully controlled than the exposed region in a SEM.
  • He ions are heavier than electrons, scattering events do not disperse He ions as readily within the sample as electrons are dispersed by scattering.
  • He ions incident on the surface of a sample can interact with the sample in a smaller interaction volume than electrons in a SEM.
  • photons detected in a gas field ion microscope e.g., a He ion microscope
  • a gas field ion microscope can arise from a smaller region than the region giving rise to photons in a SEM with a similar spot size.
  • the photons which are generated by the interaction of the sample and the He ion beam can correspond to a more localized interrogation of the surface of the sample (e.g., with less lateral averaging of material properties) than the photons generated in a SEM.
  • the He ion source also provides a greater depth of focus than an electron source.
  • images of a sample obtained using an ion microscope e.g., a gas field ion microscope
  • Detection of secondary ions from the sample can provide material constituent information about the sample via calculation of the masses of detected particles. In general, this information will correspond to material at the surface of the sample.
  • the mass(es) of the secondary ions is(are) determined using a combination of time-of-flight and a mass-resolved detector, such as a quadrupole mass spectrometer.
  • a mass-resolved detector such as a quadrupole mass spectrometer.
  • Such secondary ion detection can be performed as follows.
  • the ion beam is operated in pulsed mode by changing the electrical potentials applied to ion optical elements in the ion optics. Pulses of incident ions are incident on a surface of the sample.
  • a clock signal which determines the rate at which the ion optical element potentials are switched to turn the ion beam on and off, is also used as a reference time signal for the detector (see discussion above regarding detectors). In this manner, the time of flight of secondary ions from the sample to the detector can be accurately determined.
  • Secondary ion imaging techniques can be applied to a variety of different classes of samples.
  • An example of such a class of materials is semiconductor articles, such as patterned wafers, which can include, for example, multiple electrical conductors surrounded by a matrix of insulating material.
  • Secondary ion imaging techniques can be used to identify defects in the device, such as incomplete electrical connections between conductors, and/or electrical shorts between circuit elements. Optionally, this approach can similarly be used for purposes of mask repair.
  • sample class for which secondary ion imaging techniques can be used is metals and alloys.
  • images of samples that contain mixed materials such as alloys can be used to determine the surface distribution of each of the materials in the sample.
  • sample class where secondary ion imaging techniques can be used is read/write structures for data storage.
  • materials for which secondary ion imaging techniques can be used are biological materials and pharmaceutical materials.
  • Detection of secondary neutral particles (post-ionization) from the sample can provide material constituent information about the sample via calculation of the masses of detected particles. In general, this information will correspond to material at the surface of the sample.
  • the mass(es) of the secondary neutral particles (post- ionization) is(are) determined using a combination of time-of-flight and a mass-resolved no detector, such as a quadrupole mass spectrometer.
  • Such secondary neutral particle (post- ionization) detection can be performed as follows.
  • the ion beam is operated in pulsed mode by changing the electrical potentials applied to ion optical elements in the ion optics. Pulses of incident ions are incident on a surface of the sample.
  • a clock signal which determines the rate at which the ionization device (e.g., laser, electron beam) and/or ion optical element potentials are switched is also used as a reference time signal for the detector (see discussion above regarding detectors). In this manner, the time of flight of secondary neutral particles (post ionization) from the sample to the detector can be accurately determined.
  • the ionization device e.g., laser, electron beam
  • ion optical element potentials is also used as a reference time signal for the detector (see discussion above regarding detectors).
  • the mass of the particle can be calculated, and the type chemical species (e.g., atom) can be identified. This information is used to determine material constituent information for the sample.
  • compositions and related properties can have an important impact on the performance of the article. For example, in certain instances, if one or more of these parameters is outside an appropriate range, the article may be rejected because it cannot function as desired. As a result, it is generally desirable to have very good control over each step during
  • Regions of a semiconductor article can be formed of different types of material (electrically conductive, electrically non-conductive, electrically semiconductive).
  • the gas field ion microscope (e.g., He ion microscope) described herein can be used to investigate a semiconductor article at various steps (e.g., each step) in the fabrication process.
  • the gas field ion microscope e.g., He ion microscope
  • the gas field ion microscope can be used to determine topographical information about the surface of the semiconductor article, material constituent information of the surface of the semiconductor article, material constituent information about the sub-surface region of the semiconductor article, crystalline information about the semiconductor article, voltage contrast information about the surface of the semiconductor article, voltage contrast information about a sub-surface region of the sample, magnetic information about the semiconductor article, and/or optical information about the semiconductor article.
  • Photoresist e.g., polymer photoresist, such as poly(methyl methacrylate) (PMMA) or epoxy-based photoresists, allyl diglycol carbonate, or photosensitive glasses
  • PMMA poly(methyl methacrylate)
  • photosensitive glasses e.g., silicon dioxide, silicon dioxide, or silicon dioxide
  • PMMA poly(methyl methacrylate)
  • etchant epoxy-based photoresists, allyl diglycol carbonate, or photosensitive glasses
  • etching the non-etch resist regions of the material depositing appropriate materials (e.g., one or more electrically conductive materials, one or more non-electrically conductive materials, one or more semiconductive materials), and optionally removing undesired regions of material.
  • the patterning step involves exposing the photoresist to a radiation pattern of an appropriate wavelength so that some regions of the photoresist are etch resistant and other regions of the photoresist are not etch resistant.
  • the radiation pattern can be formed on the photoresist by forming an image of a mask onto the photoresist or covering certain regions of the photoresist with a mask, and exposing the uncovered regions of the photoresist through the mask.
  • an ion beam generated by the interaction of gas atoms with the gas field ion source (e.g., He ion source) described herein can be used to irradiate to pattern the photoresist to create desired etch-resistant regions and non-etch resistant regions. This can be achieved, for example, by rastering the ion beam across the photoresist so that desired regions of material are exposed to the ions (e.g., by turning the ion beam on at regions where exposure of the photoresist to radiation is desired and by turning the ion beam off at regions where exposure of the photoresist to radiation is not desired).
  • a semiconductor article can be fabricated in a maskless process.
  • the process can be performed without the use of mask, which can decrease the time, cost and/or complexity associated with fabrication of semiconductor articles.
  • the relatively large depth of focus of the ion beam can allow for patterning relatively thick photoresist materials (e.g., 2 ⁇ m or more thick, 5 ⁇ m or more thick, 10 ⁇ m or more thick, and or 20 ⁇ m or less thick).
  • the relatively deep penetration depth of ions that can be achieved with the ion beam can further assist in processing relatively thick photoresist materials, as well as assisting in good quality processing of more standard thickness photoresist materials.
  • the ion beam has higher resolution relative to what is generally achieved with an electron beam, allowing for the fabrication of smaller sized features with higher precision. Further, ion beam patterning of photoresist can be faster than electron beam patterning of photoresist.
  • a focused ion beam is commonly used during the fabrication of a semiconductor article to obtain a sample for inspection.
  • Gallium (Ga) ions are commonly used in the FIB.
  • a FIB can be used for a variety of reasons, such as cross-sectional imaging through a semiconductor article, circuit editing, failure analysis of a
  • a FIB can be used to deposit one or more materials on a sample (e.g., as an ion source in a chemical vapor deposition process).
  • the FIB is used to remove material from a semiconductor article via sputtering.
  • the FIB is used to slice through a semiconductor article to expose a cross-section of the article for subsequent imaging using the ion microscope.
  • the FIB is used to sputter away material from an article to form a trench or via in the article. This technique can be used, for example, to expose portions of the article that are underneath the article's surface.
  • a FIB can also be used as a selective sputtering tool to remove portions of a semiconductor article, such as portions of conductive material on the article.
  • a FIB is used to cut out a portion of a sample so that the portion can be subsequently analyzed (e.g., using TEM).
  • a gas field ion microscope e.g., a He ion microscope
  • a cross-beam tool with both a FIB instrument and a gas field ion microscope can be used so that the location of the FIB can be determined using the gas field ion microscope without moving the sample.
  • the gas field ion source can be used to image the sample and provide information that can be used to precisely position the FIB as desired.
  • Such an arrangement can offer numerous advantages relative to using a SEM to determine location of the FIB.
  • a SEM can result in a magnetic field adjacent the sample surface, which can result in isotope separation of the Ga ions, resulting more than one location of the FIB at the sample. In many instances, this problem results in the FIB and SEM being used in series rather than simultaneously. In contrast, however, a gas field ion microscope can be operated in the absence of such a magnetic field, thereby eliminating complications associated with Ga ion isotope separation, while also allowing the FIB and gas field ion microscope to be used
  • An additional advantage for using a gas field ion microscope is that it has a longer working distance than typically used with a SEM, while still maintaining very good resolution because the ion beam has a smaller virtual source than the electron beam. This can relieve certain spacing constraints that may exist for a tool that combines a FIB instrument and a SEM.
  • a further advantage of a gas field ion microscope as described herein is that it can be used to obtain sub-surface information about a sample, which can enhance the ability to precisely locate the FIB, whereas a SEM generally cannot provide such sub-surface information.
  • Gas assisted chemistry is commonly used during semiconductor fabrication to add material to and/or remove material from a given layer.
  • gas assisted chemistry can be used for semiconductor circuit editing - to repair damaged or incorrectly fabricated circuits formed in semiconductor articles.
  • Gas assisted chemistry can also be used in photolithographic mask repair, where material can be added to or removed from masks to repair defects which result from use or incorrect fabrication.
  • the process generally involves interacting electrons with an activating gas to form a reactive gas that can then participate in chemistry at the surface of a semiconductor article to add material to the surface, remove material from the surface, or both.
  • the electrons are generated as secondary electrons resulting from the interaction of a Ga ion beam with the sample and/or the electrons are generated as secondary electrons resulting from the interaction of an electron beam (e.g., produced by a SEM) with the sample.
  • an appropriate pumping system can be used to remove undesirable volatile products of the surface chemistry.
  • An ion beam can be used for this purpose where the ion beam sputters material from the sample.
  • an ion beam generated via the interaction of gas atoms with a gas field ion source as described herein can be used for sputtering a sample.
  • He gas ions may be used, it is typically preferable to use heavier ions (e.g., Ne gas ions, Ar gas ions, Kr gas ions, Xe gas ions) to remove material.
  • the ion beam is focused on the region of the sample where the material to be removed is located.
  • An advantage to using an ion beam to remove material is that the material can be removed in a relatively controlled and/or precise manner.
  • An additional advantage is that sputtering can be achieved without undesirable implantation of ions (e.g., such as often results when using Ga ion sputtering, where Ga implantation is a common undesired side effect of sputtering).
  • voids in certain features or layers may be inadvertently formed.
  • the voids can undesirably impact the properties (e.g., electrical, mechanical) of the feature and/or the overall device.
  • subsequent processing steps may open the void, and the void may, for example, fill with liquid and/or gaseous components. This can cause corrosion of the underlying structures, particle defects and/or residue defects on the surrounding wafer surface.
  • Discontinuities in the TiN x layer can result in significant void formation.
  • material e.g., dielectric material
  • trenches e.g., relatively high aspect ratio trenches
  • void formation can occur during dielectric filling of shallow trench isolation structures.
  • voids can be formed during the formation of electrically conductive lines of material (e.g., copper lines), which can result in undesirable reduction in electrical conductance. In some cases, such voids can result in a lack of electrical conductance where electrical conductance is desired.
  • a gas field ion microscope e.g., a He ion microscope
  • a gas field ion microscope can be used to investigate void formation by taking advantage of its ability to provide sub-surface information about a sample, such as a semiconductor article. This property can be used during the semiconductor article fabrication process to determine the existence and/or location of voids. This is a distinct advantage over using an electron beam because an electron beam generally does not provide this kind of sub-surface information for a sample.
  • Overlay shift registration generally refers to the alignment of a feature of a given layer of a semiconductor article with a feature in a different layer of the semiconductor article.
  • the formation of a semiconductor article generally involves the proper formation of many layers.
  • a semiconductor article contains well over 20 layers.
  • each layer can contain multiple different features, each of which is desirably located with high precision so that the semiconductor article can function properly.
  • a semiconductor article can contain lateral features, such as electrically conductive wires, which are in different layers and connected to each other by a via.
  • Critical dimension metrology refers to the measurement of the linear dimensions of features in a semiconductor article that can have a critical impact on the performance of the device.
  • features can include lines (e.g., lines of electrically conductive material, lines of electrically semiconductive conductive material, lines of electrically non-conductive material).
  • a semiconductor article can contain one or more features having a size dimension of 20 nm or less (e.g., 10 nm or less, five nm or less, four nm or less, three nm or less, two nm or less, one nm or less).
  • the size of the feature is measured multiple times to provide statistical information regarding the size of the feature.
  • He ion microscope systems disclosed herein can be used for critical dimension measurement.
  • the He ion beam can be raster-scanned over a region of a wafer, and the resulting image(s) of the wafer can be used to determine the critical dimension(s).
  • He ion microscope systems can provide a number of advantages relative to SEMs and other inspection systems.
  • He ion microscope images generally exhibit less edge blooming (generally, excessive signal, approaching the point of saturation of the detector, due to enhanced yield at topographic features with slopes nearly parallel to the beam) than comparable SEM images.
  • the reduced edge blooming is a result of the smaller interaction volume between He ions and the surface of the sample, relative to the interaction volume of electrons with the surface.
  • the incident He ions can be focused to a smaller spot size than a comparable incident electron beam.
  • the smaller beam spot size in combination with the smaller interaction volume, results in images of the sample having resolution that is superior to images produced with SEMs, and more accurate determination of critical dimensions of samples.
  • the depth of focus of a He ion beam is relatively large compared to a SEM.
  • the resolution of sample features at varying depths is more consistent when using an ion beam, as compared to an electron beam. Therefore, using an ion beam can provide information at various sample depths with better and more consistent lateral resolution than can be provided using an electron beam.
  • better critical dimension profiles can be achieved using an ion beam than can be achieved with an electron beam.
  • Imaging of the samples for determination of critical dimensions can be performed using scattered He ions. This provides the added advantage of material information in addition to high resolution distance determination.
  • a flood gun can be used to prevent excessive charging of the sample surface (see discussion above).
  • very low He ion beam currents e.g., 100 fA or less
  • the use of low ion currents reduces ion beam-induced damage to certain resist materials.
  • wafer samples selected for critical dimension measurement may first need to be sectioned (e.g., to measure a cross-sectional dimension of the sample).
  • heavier gases such as Ne and Ar can be used in the ion microscope to form an ion beam which can be used to slice through the sample.
  • a Ga- based FIB can be used to section the sample. Then, the microscope system can be purged of these gases and He can be introduced, so that critical dimension measurements are made with a He ion beam, avoiding sample damage during metrology.
  • Line edge roughness generally refers to the roughness of the edge of a line of material in a semiconductor article
  • line width roughness generally refers to the roughness of the width of a line of material in a semiconductor article. It can be desirable to understand these values to determine whether actual or potential problems exist in a given semiconductor article. For example, if adjacent lines formed of electrically conductive material have edges that bulge outward toward each other, the lines may contact each other resulting in a short.
  • line edge roughness and/or line width roughness can be desirable to understand the dimensions of line edge roughness and/or line width roughness to within five nm or less (e.g., four run or less, three nm or less, two nm or less, one nm or less, 0.9 nm or less, 0.8 nm or less, 0.7 nm or less, 0.6 nm or less, 0.5 nm or less).
  • the line edge roughness and/or line edge width is measured multiple times to provide statistical information regarding the size of the feature.
  • fabrication tolerances for parameters such as line edge roughness can be very high.
  • He ion microscope systems can provide a number of advantages relative to SEMs and other inspection systems.
  • He ion microscope images generally exhibit less edge blooming (generally, excessive signal, approaching the point of saturation of the detector, due to enhanced yield at topographic features with slopes nearly parallel to the beam) than comparable SEM images.
  • the reduced edge blooming is a result of the smaller interaction volume between He ions and the surface of the sample, relative to the interaction volume of electrons with the surface.
  • the relatively high yield of secondary electrons provided by an ion beam, as compared to an electron beam can result in a relatively high signal to noise ratio for a given current. This can, in turn, allow for sufficient information about the sample to be obtained in a relatively short period of time, increasing throughput for a given current.
  • the process of forming a semiconductor article typically involves stacking many different layers of material in a desired fashion, and performing appropriate processes on each layer. Generally, this involves depositing on and/or removing material from a given layer.
  • the final semiconductor article includes many different features in different layers (e.g., to form a desired circuit). In general, it is desirable for the features to be properly aligned for the final device to function as desired. Alignment marks are commonly used in semiconductor articles to assist in properly aligning features in a given layer with features in a different layer. However, using alignment marks can add extra steps to the overall fabrication process, and/or can introduce other complexities or expenses to the fabrication process.
  • the mere presence of the alignment marks means that there are areas and/or volumes of the semiconductor article that are not available for use (e.g., for the fabrication of active components).
  • an ion beam can be used to investigate the sub-surface region of a material. This property can be used to determine the location of certain features in a layer beneath a surface layer, allowing features in different layers of the semiconductor article to be aligned as desired without the use alignment marks.
  • the gas field ion microscope (e.g., the He ion microscope) described herein can be used to remove and/or deposit material (e.g., from an electrical circuit) using, for example, the gas assisted chemistry and/or sputtering techniques noted above.
  • An advantage of using an ion microscope to perform these processes is that the ion beam can also be used to assess the resulting product to determine, for example, whether the desired material was properly deposited or removed. This can reduce the cost and/or complexity associated with device fabrication, and/or increase the throughput of device fabrication.
  • Removal and/or addition of material capabilities can be combined to perform sub-surface circuit repair. To repair a sub-surface defect, material from the device is first removed down to a depth that exposes the defect. The defect is then repaired by either adding or removing material from the device. Finally, the overlying layers of the device are repaired, layer-by- layer, by adding appropriate thicknesses of new material.
  • the gas field ion microscope (e.g., the He ion microscope) described herein can provide particular advantages for circuit editing applications including small spot sizes and low ion currents for controlled and highly accurate editing of fabricated devices.
  • Photoresist e.g., polymer photoresist, such as poly(methyl methacrylate) (PMMA) or epoxy-based photoresists, allyl diglycol carbonate, or photosensitive glasses
  • PMMA poly(methyl methacrylate)
  • photosensitive glasses e.g., silicon dioxide, silicon dioxide, or silicon dioxide
  • PMMA poly(methyl methacrylate)
  • etchant epoxy-based photoresists, allyl diglycol carbonate, or photosensitive glasses
  • etching the non-etch resist regions of the material depositing appropriate materials (e.g., one or more electrically conductive materials, one or more non-electrically conductive materials, one or more semiconductive materials), and optionally removing undesired regions of material.
  • the patterning step involves exposing the photoresist to a radiation pattern of an appropriate wavelength so that some regions of the photoresist are etch resistant and other regions of the photoresist are not etch resistant.
  • the radiation pattern can be formed on the photoresist by forming an image of a mask onto the photoresist or covering certain regions of the photoresist with a mask, and exposing the uncovered regions of the photoresist through the mask.
  • Photolithographic masks used to fabricated integrated circuits and other microelectronic devices in the semiconductor industry can be fragile and/or expensive.
  • mask fabrication processes can be time-consuming and/or delicate.
  • fabrication errors produce mask defects.
  • mask defects can arise from handling and general use. If circuits or other devices were produced using the defective masks, the circuits or devices may not operate correctly. Given the time and expense required to fabricate a new mask, it may be more cost-effective to edit a defective mask than to fabricate an entirely new mask.
  • Mask defects generally include an excess of mask material in a region of the mask where there should be no material, and/or an absence of mask material where material should be present.
  • the gas field ion microscope e.g., the He ion microscope
  • the gas field ion microscope described herein may be used to inspect and/or repair a mask.
  • the gas field ion microscope e.g., He ion microscope
  • the gas field ion microscope can be used to inspect the mask to determine whether a defect and present, and, if a defect is present, where the defect is.
  • Many of the various advantageous featured provided by the gas field ion microscope (e.g., He ion microscope) disclosed herein are desirably used to image the mask.
  • the gas field ion microscope (e.g., He ion microscope) can be used during the repair process.
  • the gas field ion microscope can be used to position the mask relative to a FIB so that the FIB can be used to add and/or remove material from the mask using gas surface chemistry process and/or etching processes, such as described above.
  • the gas field ion microscope in addition to initially imaging the mask to determine the existence and/or location of a defect, can be used to add and/or remove material from the mask using gas surface chemistry process and/or etching processes, such as described above.
  • the gas field ion microscope can be used to conduct certain repair steps (add material, remove material) while another instrument (e.g., a FIB) is used to conduct other repair steps (add material, remove material).
  • (xi) Defect Inspection In general, during the process of fabricating a semiconductor article, the article is inspected for potential defects. Typically, the inspection is performed using an in-line tool which is always running and being fed wafers and that is fully automatic. The tool is often used to examine a small area of wafer whether there are regions where a defect will occur. This inspection is performed prior to defect review (see discussion below). The goal of defect inspection typically is to determine whether a defect may exist, as opposed to determining the exact nature of a given defect.
  • a region of a wafer is analyzed to see whether certain anomalous properties (e.g., voltage contrast properties, topographical properties, material properties) are exhibited by the sample, relative to other regions of the same wafer and/or to regions of other wafers.
  • certain anomalous properties e.g., voltage contrast properties, topographical properties, material properties
  • the coordinates e.g., X 5 Y coordinates
  • the location of the wafer is more carefully inspected during defect review.
  • a gas field ion microscope e.g., a He ion beam
  • a gas field ion microscope can be used to gather information about a sample during defect inspection.
  • Such a microscope can be used for relatively high throughput and high quality defect inspection.
  • the different contrast mechanisms provided by the gas field ion microscope e.g., He ion microscope
  • a sample is noted as having a potential defect during defect inspection, that sample is then submitted to defect review where the particular region(s) of the sample having the potential defect is(are) investigated to determine the nature of the defect. Based on this information, modifications to the process may be implemented to reduce the risk of defects in final product.
  • defect inspection is conducted at slower speed and higher magnification than defect review, and may be automated or conducted manually to obtain specific information regarding one or more defects. The information is used to attempt to understand why anomalous results were obtained during defect review, and the nature and cause of the defects that gave rise to the anomalous results.
  • the gas field ion microscope (e.g., He ion microscope) described herein can be used to investigate a semiconductor article at various steps (e.g., each step) in the fabrication process.
  • the gas field ion microscope e.g., He ion microscope
  • the gas field ion microscope can be used to determine topographical information about the surface of the semiconductor article, material constituent information of the surface of the semiconductor article, material constituent information about the sub-surface region of the semiconductor article, crystalline information about the semiconductor article, voltage contrast information about the surface of the semiconductor article, voltage contrast information about a sub-surface region of the semiconductor article, magnetic information about the semiconductor article, and/or optical information about the semiconductor article.
  • the different contrast mechanisms provided by the He ion microscope can permit visualization of defects that would otherwise not appear using SEM-based techniques.
  • He ion microscopes can be used to identify and examine metal corrosion in various devices and material. For example, metal fixtures and devices used in nuclear power plants, military applications, and biomedical applications can undergo corrosion due to the harsh environments in which they are deployed. He ion microscopes can be used to construct images of these and other devices based on the relative abundance of hydrogen (H) in the devices, which serves as reliable indicator of corrosion.
  • H hydrogen
  • Read/write heads used in magnetic storage devices are fabricated to extremely high tolerances and must be inspected for manufacturing defects prior to installation. These devices frequently have very high aspect ratios; the short sides of such devices can be as small as 1 nm.
  • He ion microscopes provide numerous advantages when used to image these devices during inspection. Among these are small spot sizes and interaction volumes, which can result in high resolution imaging of these tiny devices, a large depth of focus, which can allow in-focus imaging of the entire high- aspect-ratio device along its long dimension, and material information provided by measurement of scattered He ions and/or neutral atoms, which is used to verify that tiny circuit elements are properly connected.
  • a gas field ion microscope e.g., a He ion microscope
  • the gas field ion microscope can be used to image immuno-labeled cells and internal cell structures. The microscope can be used in this manner while providing certain advantages disclosed herein.
  • a therapeutic agent e.g., small molecule drug
  • a crystal e.g., as it comes out of solution. It can be desirable to determine the crystalline structure of the crystallized small molecule because this can, for example, provide information regarding the degree of hydration of the small molecule, which, in turn, can provide information regarding the bioavailability of the small molecule. In certain instances, the crystalline information may turn out to demonstrate that the small molecule is actually in an amorphous (as opposed to crystalline) form, which can also impact the bioavailability of the small molecule.
  • a gas field ion microscope e.g., a He ion microscope
  • a gas field ion microscope as described herein can be used to determine, for example, topographical information about a biological sample, material constituent information of a surface of a biological sample, material constituent information about the sub-surface region of a biological sample and/or crystalline information about a biological sample.
  • the microscope can be used in this manner while providing certain advantages disclosed herein.
  • any of the analysis methods described above can be implemented in computer hardware or software, or a combination of both.
  • the methods can be implemented in computer programs using standard programming techniques following the methods and figures described herein.
  • Program code is applied to input data to perform the functions described herein and generate output information.
  • the output information is applied to one or more output devices such as a display monitor.
  • Each program may be implemented in a high level procedural or object oriented programming language to communicate with a computer system.
  • the programs can be implemented in assembly or machine language, if desired. In any case, the language can be a compiled or interpreted language.
  • the program can run on dedicated integrated circuits preprogrammed for that purpose.
  • crystallographic orientations of W can also be used in a tip.
  • a W(112), W(110) or W(100) tip may be used.
  • the ion microscope (e.g., gas field ion microscope) can include appropriate componentry to allow the microscope to be used in- line for the analysis of samples, such as samples relevant to the semiconductor industry (e.g., wafer samples).
  • the ion microscope may be automated with a high-speed loadlock for standard sized semiconductor wafers.
  • the system may include a wafer stage capable of putting a portion of a sample wafer under the ion microscope at high speed.
  • the ion microscope may also include a scan system capable of high-speed rastering of metrology patterns.
  • the ion microscope may also include a charge neutralization scheme to reduce sample charging.
  • the ion microscope may also include a wafer height control module for adjusting working distances.
  • the system may be configured so that individual dies (e.g., having lengths on the order of 50mm) can be imaged.
  • a 25 mm length of emitter wire formed of single crystal W(111) was obtained from FEI Company (Hillsboro, OR). The emitter wire was trimmed to a 3 mm length and set aside.
  • a V-shaped heater wire was prepared as follows. A 13 mm length of polycrystalline tungsten wire (diameter 180 ⁇ m) was obtained from Goodfellow (Devon, PA) and cleaned by sonication for 15 minutes in distilled water to remove the carbon residue and other impurities. The wire was bent at its midpoint to form an angle of 115 degrees.
  • the region near the apex of the "V" was electrochemically etched to prepare it for welding in a IN aqueous solution of sodium hydroxide (NaOH) with an applied AC potential of 1 V and frequency 60 Hz for a duration of approximately 15 seconds.
  • NaOH sodium hydroxide
  • the heater wire was then removed from the etching solution, rinsed with distilled water, and dried.
  • the V-shaped heater wire was mounted in a fixture to ensure that the ends of the wire remained coplanar.
  • the emitter wire was spot welded to the V-shaped apex of the heater wire.
  • the two ends of the heater wire were spot welded to two posts of a support base of the type shown in FIGS. 1 IA and 1 IB.
  • the support base was obtained from AEI Corporation (Irvine, CA). The resulting assembly was then cleaned
  • the end of the emitter wire was etched by an electrochemical process as follows.
  • a resist material e.g., nail polish obtained from Revlon Corporation, New York, NY
  • a drop of resist was placed on the surface of a clean glass microscope slide, and the wire was dipped ten times into the resist solution, allowing the resist to dry slightly between each dipping. Care was taken to assure that the upper boundary of the resist was in the shape of a circle, and that the plane of the circle was maintained perpendicular to the axis of the wire.
  • the wire was allowed to dry for 1 hour in air.
  • the support base with the resist-coated emitter wire attached was then attached to an etching fixture that included: (a) a translation apparatus for vertically translating the support base; (b) a dish; and (c) a counter electrode, formed of stainless steel to minimize undesired chemical reactions, that extended into the dish.
  • the dish was filled with an etching solution to a level such that the solution was in contact with the counter electrode. Approximately 150 mL of solution was present in the etching fixture dish.
  • the orientation of the support base was adjusted to ensure that the longitudinal axis of the emitter wire was approximately parallel to the vertical direction (e.g., the direction along which the translation apparatus provided for translation of the support base).
  • a sequence of AC pulses at a frequency of 60 Hz was applied to the emitter wire to facilitate the electrochemical etching process.
  • Portions of the emitter wire which were immersed in solution but not covered by resist material began to etch away. Because the emitter wire was positioned so that only a small uncoated region of the wire above the edge of the photoresist material was immersed in solution, localized etching of the emitter wire in this region was observed. As the electrochemical reaction proceeded, the diameter of the wire in this region began to get narrower due to the etching process.
  • the tip boundary in each image was then determined as the set of nonzero-intensity (X, Y) points that formed a demarcation between image pixels corresponding to the tip and image pixels corresponding to the black (e.g., zero-intensity) background.
  • X, Y nonzero-intensity
  • One such set of (X 5 Y) points for one of the views of the tip is shown in FIG. 38. Similar sets of boundary points were determined for each of the eight perspective views of the tip.
  • FIG. 39 shows a graph of the calculated slope at points along the boundary curve as a function of X for the boundary curve shown in FIG. 38.
  • the calculations of the right radius, left radius, and tip radius of curvature were repeated for each of the eight perspective views of the tip.
  • the average tip radius was then calculated as the average of the tip radius of curvature measurements in all of the views of the tip.
  • the average tip radius was determined to be 62 nm.
  • the standard deviation of all of the tip left and right radii was also calculated, and expressed as a percentage of the average tip radius.
  • the eccentricity was determined to be 11.9%.
  • the cone angle of the tip in each of the eight perspective views was also determined.
  • left and right tangent points on the boundary curve were located on the left and right sides of the tip apex, respectively, at positions 1 ⁇ m from the tip apex, measured along the Y direction, as discussed previously.
  • the left cone angle of the tip in a particular view was then determined as the angle between a tangent to the boundary curve at the left tangent point and a line parallel to the Y axis and extending through the left tangent point.
  • the right cone angle of the tip in a particular view was determined as the angle between a tangent to the boundary curve at the right tangent point and a line parallel to the Y axis and extending through the right tangent point. Finally, the full cone angle was determined as the sum of the magnitudes of the left and right cone angles.
  • the FIM included a mounting area for the support assembly supporting the tip, a high voltage power supply for biasing the tip, an extractor adjacent to the tip, and a detector for recording ion emission patterns from the tip.
  • the support assembly including the tip was installed in the FIM and the FIM chamber was evacuated to a background pressure of 1x10 "8 Torr.
  • the tip was cooled to 77 K using liquid nitrogen as a coolant.
  • the source was heated to 900 K for 5 minutes to desorb condensates or other impurities that had formed on the tip during processing. Heating of the tip was accomplished by applying an electrical current to the heater wire to which the tip was welded. The current was applied using a power supply with constant power capabilities (Bertan Model IB-30A, available from Spellman High Voltage Inc., Hauppauge, NY). Temperature measurements were made using an optical pyrometer (obtained from Pyro Corporation, Windsor, NJ).
  • the tip was sharpened to obtain a terminal atomic trimer at the tip apex.
  • Helium gas was pumped out of the FIM chamber until the background pressure in the chamber was less than 1.2x10 " Torr.
  • the tip was then heated, via application of current to the heater wires as described above, to a temperature of 1500 K for 2 minutes.
  • Oxygen gas was introduced into the FIM chamber in the vicinity of the tip at a pressure of IxIO "5 Torr. After 2 minutes, the tip temperature was reduced to 1100 K. After 2 minutes at 1100 K, the oxygen supply was shut off and the tip was allowed to cool to approximately 77 K. During cooling, and about 15 minutes after the oxygen supply was shut off, the residual oxygen gas was pumped out of the FIM chamber until the background pressure in the chamber was less than 1.2xlO " ⁇ Torr.
  • the tip bias potential was further increased up to +28 kV. Field evaporation of the tip atoms continued during this process.
  • a bias potential of +28 kV another atomic trimer was obtained at the apex of the tip.
  • a FIM image of the second trimer is shown in FIG. 40.
  • the tip bias potential was reduced to attain the highest angular intensity in the FIM emission pattern. This occurred at a tip bias of +23 kV.
  • the highest angular intensity was determined by adjusting the tip bias to obtain the largest observed brightness of a selected atom in the FIM emission pattern.
  • the bias at which the highest angular emission intensity occurred was verified by measuring the He ion current from the trimer as the potential bias of the tip was adjusted. The He ion current was measured using a Faraday cup positioned in the path of the He ion beam.
  • Scanning deflectors configured as octupole electrodes, were positioned after the astigmatism corrector to permit rastering of the ion beam across the surface of a sample.
  • the second lens was positioned at a distance 150 mm from the aperture, and was used to focus the ion beam onto the surface of a sample.
  • the second lens was shaped as a truncated right-angled cone, with a full cone angle of 90°.
  • the tip was allowed to cool while maintaining the tip at a potential bias of +5 kV relative to the extractor. Once the tip had cooled to liquid nitrogen temperature, He gas was introduced into the tip region at a pressure of 1x10 "5 Torr.
  • the ion microscope system was run in SFIM mode, as described above, to generate an image showing the He ion emission pattern of the tip. The image indicated the shape of the tip to atomic precision.
  • the alignment electrodes were used to raster the ion beam generated from the tip over the surface of the aperture.
  • Sawtooth voltage functions were applied to each of the alignment deflectors to achieve rastering at a frame rate of 10 Hz, with a maximum voltage of the sawtooth functions of 150 V relative to the common external ground of the microscope system.
  • the raster pattern scanned 256 points in each of two orthogonal directions transverse to the axis of the ion optics. The astigmatism corrector and the scanning deflectors were not used in this imaging mode.
  • the scanning deflectors were used to raster the ion beam transmitted through the aperture over the surface of the sample.
  • a recognizable, high contrast feature (a copper grid) on the surface of the sample (part number 02299C-AB 5 obtained from Structure Probe International, West Chester, PA) was placed iri the path of the ion beam under the second lens, and secondary electron images of the feature were measured by the detector using the configuration discussed above.
  • the strength of the second lens was adjusted to roughly focus the ion beam on the sample surface; the potential bias applied to the second lens was about 15 kV, relative to the common external ground. The quality of the focus was assessed visually from the images of the sample recorded by the detector.
  • the alignment of the ion beam with respect to the axis of the second lens was evaluated by slowly modulating the strength of the second lens - at a frequency of 1 Hz and an modulation amplitude of about 0.1% of the operating voltage of the second lens - and observing the displacement of the feature.
  • the beam alignment in the final lens was optimized by adjusting the voltages of the alignment deflectors. The alignment was optimized when the position of the center of the image measured by the detector did not change significantly during modulation of the strength of the second lens.
  • the type of detector used, and the detector's settings, were selected according to the type of sample that was examined with the ion microscope.
  • an ET detector was used with a metal grid biased at about +300 V relative to the common external ground.
  • a scintillator internal to the ET detector was biased at +10 kV relative to the external ground, and the gain of the internal PMT adjusted to produce the largest possible signal without saturation.
  • a MCP detector obtained from Burle Electro-Optics, Sturbridge, MA was also used to detect secondary electrons and/or scattered He from samples.
  • the MCP grid, front face, and back face could each be biased relative to the external ground.
  • the image shown in FIG. 43 is an image of an aluminum post on a silicon substrate.
  • the image was acquired by detecting secondary electrons from the surfaces of the nanotubes.
  • the He ion beam current was 0.5 pA and the average ion energy was 24 keV.
  • the ion beam was raster-scanned with a dwell time of 200 ⁇ s per pixel.
  • the field of view at the surface of the sample was 1 ⁇ m, obtained by applying a maximum voltage of 1 V to the scanning deflectors.
  • a W(111) tip was mounted in a support assembly and electrochemically etched following the procedure described in Example 1.
  • a SEM image of the tip is shown in FIG. 46.
  • Geometrical characterization of the tip was performed according to the procedure in Example 1. For this tip, the average tip radius was determined to be 70 nm. The tip was accepted for use based on the criteria in Example 1.
  • the source assembly including the etched tip was installed into the FIM described in
  • Example 1 The configuration of the FIM was the same as the configuration discussed in Example 1, except where noted below.
  • the potential bias on the tip, relative to the extractor, was slowly increased up to a potential of +21.8 kV. Field evaporation of tip atoms occurred as the potential was increased. After reaching +21.8 kV, the tip potential was reduced to +19.67 kV.
  • the FIM image of the tip shown in FIG. 47 was acquired with the tip maintained at this potential. Using this image, the single crystal structure and correct orientation of the tip were verified.
  • the tip was sharpened to produce an atomic trimer at the apex.
  • Helium was pumped out of the FIM chamber, and the tip was heated by applying a constant current of 4.3 A to the tip for 20 seconds.
  • a tilted mirror installed in the FIM column and angled to re-direct light propagating along the column axis to a side port of the column, was used to observed the tip. No glow (e.g., photons emitted from the tip) was visible to the eye, so the tip was allowed to cool for 5 minutes.
  • the tip was heated by applying a constant current of 4.4 A to the tip for 20 seconds. No glow was visible to the eye, so the tip was allowed to cool for 5 minutes.
  • the tip was heated by applying a constant current of 4.5 A to the tip for 20 seconds. No glow was visible to the eye, so the tip was allowed to cool for 5 minutes. Then the tip was heated by applying a constant current of 4.6 A to the tip for 20 seconds. At this temperature, a glow was clearly visible from the tip. Thus, the current necessary to induce tip glow was established to be 4.6 A. The source was then allowed to cool for 5 minutes.
  • a negative bias was applied to the tip while monitoring electron emission current from the tip.
  • the bias was made increasingly negative until an electron emission current of 50 pA from the tip was observed.
  • the tip bias at this current was -1.98 kV.
  • the heating current of 4.6 A was applied to the tip.
  • Tip glow was again observed after about 20 seconds. Heating of the tip extended another 10 seconds after tip glow was observed.
  • the bias potential and heating current applied to the tip were then removed from the tip, and the tip was allowed to cool to liquid nitrogen temperature.
  • Some of the emitting atoms on the tip were loosely bound adatoms and were removed with increased field strength via field evaporation of tip atoms.
  • the tip bias was further increased, and first and second trimers were removed by field evaporation to +21.6 kV. After reaching this potential, the tip bias was reduced to +18.86 kV and the FIM image of the tip in FIG. 49 was recorded.
  • the tip was identified as viable and removed from the FIM. About one month later, the tip was mounted into a helium ion microscope configured as described in Example 1. The trimer was re-built and evaporated multiple times in a process as described in Example 1, except that no oxygen gas was used. Instead, the trimer rebuild process relied upon applying a specific negative potential bias to the tip (to produce an electron emission current of 50 pA), while simultaneously heating the tip with a 4.6 A current applied to the heater wire, resulting in visible glow of the heater wire for 20 seconds. The tip remained in the helium ion microscope and provided over four weeks of usage without the need to vent the system to service the tip.
  • FIG. 50 A SFIM image of a rebuilt trimer of the tip is shown in FIG. 50.
  • FIG. 51 An image of a semiconductor sample recorded using a He ion microscope with this tip is shown in FIG. 51. The sample was included lines of aluminum metal deposited on the surface of a silicon oxide substrate. An unknown coating was deposited atop each of these materials.
  • Scan voltages of maximum amplitude 1 V were introduced on the scanning deflectors to produce a 10 ⁇ m field of view on the sample.
  • the potentials of the first and second lenses, the alignment deflectors, and the astigmatism corrector were adjusted to control the portion of the He ion beam that passed through the aperture, and to control the quality of the beam focus at the sample position, as described in Example 1.
  • the sample was tilted and rotated during imaging to reveal the three dimensional nature and the details ofthe sidewalls.
  • FIG. 52 An image of another semiconductor sample taken using this tip is shown in FIG. 52.
  • the sample was a multilayer semiconductor device with surface features formed of a metal.
  • the image was recorded by measuring secondary electrons that left the sample of the sample due to the interaction of the sample with the incident He ions. Maximum scan voltages of 150 volts were applied to the scanning deflectors to produce a 1.35 mm field of view at the sample surface.
  • the sample was observed from a top down perspective, which shows many features on the surface of the sample.
  • a MCP detector with grid and front surface biased at +300 V relative to the common external ground was positioned at a distance 10 mm from the sample, and oriented parallel to the surface of the sample.
  • the He ion beam current was 15 pA and the average ion energy was 21.5 keV.
  • the ion beam was raster-scanned with a dwell time of 10 ⁇ s per pixel. 3.
  • the sample was a gold grid sample with topographic features (part number 02899G-AB, obtained from Structure Probe International, West Chester, PA).
  • the sample was imaged by measuring secondary electron emission from the sample surface in response to incident He ions.
  • a 40 mm diameter annual, chevron-type MCP detector (obtained from Burle Electro-Optics, Sturbridge, MA) was positioned at a distance 10 mm from the sample, and oriented parallel to the surface of the sample. The detector consumed a solid angle of about 1.8 steradians and was symmetric with respect to the ion beam. The detector was mounted directly to the bottom of the second lens, as shown in FIG. 66.
  • the front surface of the MCP was biased positively (+300 V) with respect to the common external ground, and there was also a positively biased (with respect to the common external ground) internal metal grid (+300 V).
  • the average ion energy was 20 keV. Images of the sample were measured with beam currents of 1 pA, 0.1 pA and 0.01 pA, respectively, and are shown in FIGS. 53, 54, and 55, respectively. The total image acquisition times were 33 seconds, 33 seconds, and 67 seconds, respectively.
  • Example 1 (compared to about 11 W required to heat the tip in Example 1 to 1500 K).
  • the tip was held relatively rigid with respect to the source base, due to the absence of a heater wire.
  • the natural vibration frequency of the support assembly was greater than 3 kHz.
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed in as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • the microscope system was configured to measure secondary electrons that left the sample due to the interaction of the sample with the incident He ions.
  • a MCP detector (similarly configured to the detector described in Example 3) was used to record sample images.
  • the sample was steel, and was spherical in shape and of uniform composition.
  • the He ion beam current was 1.0 pA and the average ion energy was 20 keV.
  • the ion beam was raster-scanned with a dwell time of 10 ⁇ s per pixel.
  • the maximum potentials applied to the scanning deflectors (about 100 V) yielded a field of view at the surface of the sample of about 1 mm.
  • FIGS. 59A and 59B Images of a second sample are shown in FIGS. 59A and 59B.
  • the imaging conditions for the sample shown in FIG. 59A were as discussed above in connection with the first sample in this example.
  • a tip was prepared following a procedure as described in Example 1 , and characterization of geometrical tip properties was performed as described in Example 1.
  • the He ion beam was intentionally defocused (to a spot size of 100 ran) to minimize any contamination or charging artifacts.
  • the screen bias potential was adjusted in increments from -30 V to +30 V, and the secondary electron current was measured for each bias potential. Each measurement was conducted with a He ion beam energy of 22.5 keV and a beam current of 13 pA.
  • the graph in FIG. 60 shows the results for a silicon sample. On the left of the graph, where the screen was biased negatively, all of the secondary electrons that left the sample due to the interaction of the sample with the incident He ions were returned to the silicon sample. The He ion beam current and the secondary electron current were approximately equal, so that negligible amounts of free secondary ions and scattered helium ions were produced.
  • FIG. 61 A is a secondary electron image of an alignment cross on the surface of a substrate, recorded using the helium ion microscope. Scan voltages of maximum amplitude of about 1.5 V were introduced on the scanning deflectors to produce a 15 ⁇ m field of view on the sample. A MCP detector was positioned at a distance of 10 mm from the sample, and oriented parallel to the surface of the sample. The grid and front face of the MCP were biased at +300 V, relative to the common external ground. The He ion beam current was 5 pA and the average ion energy was 27 keV. The ion beam was raster-scanned with a dwell time of 150 ⁇ s per pixel.
  • the measured signal was the result of secondary electrons generated at the surface of the sample by both scattered He ions and neutral He atoms. This assessment was verified by biasing the MCP and screen negative and noting that almost no signal was detected. Secondary electrons that left the sample due to the interaction of the sample with the incident He ions produced the image of the surface metal layer in FIG. 64. The image of the sub-surface metal layer is produced He ions that have penetrated into the sample and become neutralized. The neutral He atoms scatter from the sub-surface layer, and a fraction of them return to the surface where they produce secondary electrons upon their exit. This accounts for the blurred and dimmed image of the sub-surface features.
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • FIG. 65 An image of the sample is shown in FIG. 65.
  • the image shows distinctly brighter and darker grains.
  • the bright features correspond to surface topographic relief patterns, which enhance secondary electron production due to the topographic effects disclosed herein.
  • the contrasting image intensities of the various crystal grains were due to the relative orientations of the crystal domains with respect to the incident He ion beam.
  • the scattering probability at the surface was low, and so the ion beam penetrated deeply into the grain.
  • the secondary electron yield at the surface of the material was relatively lower, and the grain appeared darker in the image.
  • the tungsten lattice in a particular grain was oriented so that the He ion beam was incident upon a high index
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • the tip was then installed and configured in the He ion microscope.
  • the microscope system was configured as described in Example 1, with changes to the configuration noted below.
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • the tip was sharpened in the FIM using the procedure described in Example 1.
  • the tip was then installed and configured in the He ion microscope.
  • the microscope system was configured as described in Example 1, with changes to the configuration noted below.
  • a sample of sodium chloride (NaCl) was imaged using the photomultiplier tube detector.
  • the He ion beam current was 10 pA and the average He ion energy was 25 keV.
  • the sample was raster-scanned with a dwell time per pixel of 500 ⁇ s.
  • a maximum voltage of 150 V was applied to the scanning deflectors to yield a field of view at the sample surface of 1.35 mm.
  • each of the He ions generated at the tip continued to travel in a straight line, diverging from the tip.
  • the aperture intercepted most of the He ion beam and allowed only a small central portion of it to pass further down the remainder of the ion column.
  • the portion of the He ion beam that passed through the aperture was detected with the Faraday cup, yielding a measured He ion current of 5 pA passing through the aperture.
  • the angular intensity of the He ion beam was then calculated as the He ion beam current passing through the aperture (5 pA) divided by the solid angle of the aperture from the perspective of the tip.
  • the corresponding solid angle was calculated as 2.1 x 10 "6 steradians (sr). Based upon the solid angle, the angular intensity of the He ion beam was determined to be 2.42 ⁇ A /sr.
  • the virtual source size is generally smaller than the actual ionization area.
  • the virtual source size was determined using the general procedure discussed previously: by back-projecting asymptotic trajectories of 100 He ions once the ions were beyond the electric field region (e.g., the region in the vicinity of the tip and the extractor) of the ion source.
  • the back-projected trajectories moved closer to one another until they passed through a region of space in which they were most closely spaced with respect to one another, and then they diverged again.
  • the circular diameter of the closest spacing of the back-projected trajectories was defined to be the virtual source size.
  • the virtual source size can be considerably smaller.
  • the brightness of the ion source was 3.4 x lO 9 A/cm 2 sr.
  • the reduced brightness was calculated as the brightness divided by the voltage used to extract the beam (e.g., the voltage bias applied to the tip).
  • the tip to extractor voltage was 19 kV, and the reduced brightness was 1.8 x 10 9 A/m 2 srV.
  • the etendue is a measure of the product of the He ion beam's virtual source size and its angular divergence (as a solid angle). Using the brightness determined above, the etendue was determined to be 1.5 x 10 " cm sr. The reduced etendue is the etendue multiplied by the He ion beam voltage. The reduced etendue, based on the etendue calculated above, was determined (using the tip bias voltage of +19 kV) to be 2.8 x 10 "17 cm 2 srV. 17.
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • the tip was sharpened in the FIM using the procedure described in Example 1.
  • the tip was then installed and configured in the He ion microscope.
  • the microscope system was configured as described in Example 1, with changes to the configuration noted below.
  • FIG. 77 shows a graph on which pixel intensity values for one particular line (line #14) before smoothing (dots) and after smoothing (curve) are plotted.
  • the vertical axis corresponds to the image intensity, ranging from 0 (black) to 255 (white).
  • the horizontal axis corresponds to the pixel number, ranging from 0 (left edge) to 57 (right edge).
  • the center of the left to right light-to-dark transition was determined by locating the minimum value of the first derivative of the intensity line scan. For edges with a left to right dark-to-light transition, the center of the transition would have been found by determining the location of the maximum value of the first derivative of the intensity line scan.
  • Each line was then trimmed to contain just 21 pixels.
  • the trimming operation such that the transition point, the 10 pixels preceding the transition point, and the 10 pixels following the transition point were retained in each line.
  • Intensity values for the first five pixels in each trimmed line were averaged together and the average was identified as the 100% value.
  • Intensity values for the final five pixels in each trimmed line were averaged together and the average was identified as the 0% value.
  • the smoothed data from each line scan was then rescaled in terms of the 100% and 0% values.
  • the rescaled data from FIG. 77 is shown in FIG. 78.
  • a tip was prepared following a procedure as described in Example 1, and characterization of geometrical tip properties was performed as described in Example 1. The tip was accepted for use based on the criteria in Example 1.
  • the He ion beam current was 1 pA and the average He ion beam energy was 26 keV.
  • the He ion beam was raster-scanned over the surface of the sample with a dwell time per pixel of 100 ⁇ s.
  • a maximum potential of 1.30 V was applied to the scanning deflectors to yield a field of view at the surface of the sample of 13 ⁇ m.
  • FIG. 79 shows an image of the sample recorded using the measurement configuration described above.
  • Various features on the surface of the sample have measured intensities which are relatively uniform, and different from the intensity of the substrate.
  • Visual inspection of the edges of the surface features reveals that there are no apparent bright edge effects (e.g., edge blooming) which can lead to saturation of the signal chain, and can make the precise location of the edge difficult to find.
  • edge blooming e.g., edge blooming
  • FIG. 80 A horizontal line scan through one of the sample's surface features is shown in FIG. 80.
  • the horizontal axis of the line scan shows the pixel number, and the vertical axis indicates the measured image intensity at particular pixels.
  • the same sample was imaged in a Schottky Field Emission SEM (AMRAY model 1860) with a beam energy of 3 keV and a beam current of 30 pA, at a magnification of 30,000 X (corresponding to a field of view of about 13 um).
  • the resulting image is shown in FIG. 81, and a horizontal line scan through the same feature that was scanned in FIG. 80 is shown in FIG. 82.
  • the line scan in FIG. 82 showed significant bright edge effects, and the signal chain at the edges of the imaged surface feature was nearly saturated.
  • the SEM line scan does not show a relatively uniform steady state intensity level. Instead, the intensity level in the body of the feature is either decreasing or increasing everywhere but in a small region at the center of the feature.
  • the asymmetry of the SEM line scan indicates that time-dependent charging of the surface feature was occurring during SEM exposure.
  • the line scan image of the feature recorded by detecting scattered He ions and neutral He atoms shows considerably reduced edge effects, and no apparent charging artifacts.
  • Multiple measurements of a particular feature on the surface of the sample could also have been performed. If multiple measurements of a feature were made, it would have been possible to ascertain statistical data about the dimensions of the measured feature. For example, the mean feature width, the standard deviation of the feature width, and/or the mean and standard deviation of the location of the first edge and/or the second edge of the feature could have been measured. Fourier methods could also have been used to analyze the positions of the edges of one or more features to determine the spectrum of spatial wavelengths corresponding to the edge shapes.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured to expose a 100 ⁇ m 2 FOV on the surface of the sample to a He ion beam having a beam current of 1 pA, an average ion energy of 20 keV, and a beam spot size on the surface of the sample of 0.1% of the FOV.
  • a detector is configured to measure a total intensity of secondary electrons from the sample produced in response to the incident He ion beam.
  • the He ion beam is raster-scanned in discrete steps over the entire FOV region of the sample surface, and the total intensity of secondary electrons is measured as a function of the position of the He ion beam on the sample surface.
  • the measured crystalline information is then used to remove contributions to the secondary electron intensity measurements that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the corrected intensities of secondary electrons at a corresponding He ion beam position on the sample.
  • Topographic information is provided by the image, which shows the surface relief pattern of the sample in the FOV.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • the He ion beam is raster- scanned in discrete steps over the FOV region of the sample surface.
  • a detector is used to measured a total abundance of scattered He ions as a function of the position of the He ion beam on the sample surface.
  • the measured total abundance values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the total measured abundance of He ions at a corresponding He ion beam position on the sample.
  • Differently-oriented crystal grains at the surface of the sample have different yields of scattered He ions, and the image shows the differently-oriented crystal grains as variable gray levels. Using the information in the image, crystal grains and grain boundaries can be identified at the sample surface.
  • the total secondary electron intensity is measured as described in Example 19.
  • the measured crystalline information is then used to remove contributions to the secondary electron intensity measurements that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the corrected intensities of secondary electrons at a corresponding He ion beam position on the sample.
  • Topographic information is provided by the image, which shows the surface relief pattern of the sample in the FOV.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • the He ion beam is raster- scanned in discrete steps over the FOV region of the sample surface.
  • a detector is used to measured a total abundance of scattered He ions as a function of the position of the He ion beam on the sample surface.
  • the measured total abundance values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the total measured abundance of He ions at a corresponding He ion beam position on the sample.
  • Differently-oriented crystal grains at the surface of the sample have different yields of scattered He ions, and the image shows the differently-oriented crystal grains as variable gray levels. Using the information in the image, crystal grains and grain boundaries can be identified at the sample surface.
  • the He ion beam is scanned from one grain to another on the surface of the sample.
  • a two- dimensional detector is used to capture an image of scattered he ions from the surface of the sample.
  • Each two-dimensional image corresponds to a Kikuchi pattern for a particular crystal grain at the surface of the sample. Based on the Kikuchi pattern, the grain's crystal structure, lattice spacing, and crystal orientation can be determined. By measuring a single Kikuchi pattern for each grain rather than at each pixel throughout the FOV, a complete map of the sample's surface crystal structure is obtained in a shorter time.
  • the total secondary electron intensity is measured as described in Example 19.
  • the measured crystalline information is then used to remove contributions to the secondary electron intensity measurements that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the corrected intensities of secondary electrons at a corresponding He ion beam position on the sample.
  • Topographic information is provided by the image, which shows the surface relief pattern of the sample in the FOV.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 19.
  • a detector is configured to measure a total intensity of secondary electrons from the sample produced in response to the incident He ion beam.
  • the sample is tilted with respect to the He ion beam, so that the He ion beam is incident at a non-normal angle to the surface of the sample.
  • the He ion beam is raster-scanned in discrete steps over the entire FOV region of the sample surface, and the total intensity of secondary electrons is measured as a function of the position of the He ion beam on the sample surface.
  • the measured crystalline information is then used to remove contributions to the secondary electron intensity measurements that arise from crystal structure variations in the sample.
  • the corrected total intensity values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the corrected total intensities of secondary electrons at a corresponding He ion beam position on the sample.
  • Topographic information is provided by the image, which shows the surface relief pattern of the sample in the FOV. Tilting the sample with respect to the He ion beam can reveal topographic information that would otherwise remain hidden if the He ion beam was incident on the sample surface only at normal angles.
  • the sample tilt can then be adjusted so that the He ion beam is incident at a different non-normal angle to the surface of the sample, and the He ion beam is raster- scanned is discrete steps over the entire FOV region of the sample surface.
  • the total intensity of secondary electrons is measured as a function of the position of the He ion beam on the sample surface, and the measured crystalline information is used to remove contributions to the secondary electron intensity measurements that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct a second grayscale image of the sample corresponding to the second non-normal incidence angle of the He ion beam, where the gray level at a particular image pixel is determined by the corrected total intensities of secondary electrons at a
  • Crystalline information from the sample is measured as described in Example 20.
  • the total intensity of secondary electrons from the sample is measured as described in Example 22.
  • the measured crystalline information is used to remove contributions to the secondary electron intensity measurements, at each ion beam angle of incidence, that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct grayscale images of the sample as described in Example 22.
  • the information from the two images measured at different He ion beam angles of incidence can then be combined and used to determine quantitative three-dimensional topographic information about the surface of the sample.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 192.
  • Crystalline information from the sample is measured as described in Example 21.
  • the total intensity of secondary electrons from the sample is measured as described in Example 22.
  • the measured crystalline information is used to remove contributions to the secondary electron intensity measurements, at each ion beam angle of incidence, that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct grayscale images of the sample as described in Example 22.
  • the information from the two images measured at different He ion beam angles of incidence can then be combined and used to determine quantitative three-dimensional topographic information about the surface of the sample.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 19.
  • two or more detectors each oriented at a different angle and position with respect to the sample, are configured to measure a total intensity of secondary electrons from the sample produced in response to the incident He ion beam.
  • the He ion beam is raster-scanned in discrete steps over the entire FOV region of the sample surface, and the total intensity of secondary electrons is measured by each detector as a function of the position of the He ion beam on the sample surface.
  • the measured crystalline information is used to remove contributions to the secondary electron intensity measurements at each detector that arise from crystal structure variations in the sample.
  • the corrected total intensity values are used to construct a series of grayscale images of the sample, each image corresponding to one of the detectors, where the gray level at a particular pixel in a particular image is determined by the corrected total intensity of secondary electrons at a corresponding He ion beam position on the sample.
  • Information from the images measured by the multiple detectors can then be combined and used to determine quantitative three-dimensional topographic information about the surface of the sample.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 20.
  • To measure topographic information from the sample the total intensity of secondary electrons from the sample is measured as described in Example 25.
  • the measured crystalline information is used to remove contributions to the secondary electron intensity measurements, at each detector, that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct grayscale images of the sample as described in Example 25. Information from the images measured by the multiple detectors can then be combined and used to determine quantitative three-dimensional topographic information about the surface of the sample. 27. Measurement of Topographic and Crystalline Information from a Sample
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 21.
  • To measure topographic information from the sample the total intensity of secondary electrons from the sample is measured as described in Example 25.
  • the measured crystalline information is used to remove contributions to the secondary electron intensity measurements, at each detector, that arise from crystal structure variations in the sample.
  • the corrected total secondary electron intensity values are used to construct grayscale images of the sample as described in Example 25. Information from the images measured by the multiple detectors can then be combined and used to determine quantitative three-dimensional topographic information about the surface of the sample.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 19.
  • a detector configured to measure He ions is positioned to detect He ions scattered from the surface of the sample at large scattering angles.
  • the He ion beam is raster-scanned in discrete steps over the entire FOV region of the sample surface, and the total abundance of He ions is measured by the detector as a function of the position of the He ion beam on the sample surface.
  • the total abundance values are used to construct a grayscale image of the sample, where the gray level at a particular image pixel is determined by the total measured abundance of scattered He ions at a corresponding He ion beam position on the sample.
  • Topographic information is provided by the image, which shows the surface relief pattern of the sample in the FOV.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 20.
  • Topographic information from the sample is measured as described in Example 28.
  • the sample is fixed in position on a sample mount in a gas field ion microscope as described herein.
  • the gas field ion microscope is configured as described in Example 19.
  • Crystalline information from the sample is measured as described in Example 31.
  • Topographic information from the sample is measured as described in Example 28.

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Abstract

L'invention concerne des sources d'ions ainsi que des systèmes et des procédés associés.
EP06837944A 2005-12-02 2006-11-15 Sources d'ions, systemes et procedes associes Withdrawn EP1955356A2 (fr)

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US74195605P 2005-12-02 2005-12-02
US78439006P 2006-03-20 2006-03-20
US78438806P 2006-03-20 2006-03-20
US78433106P 2006-03-20 2006-03-20
US78450006P 2006-03-20 2006-03-20
US11/385,136 US20070228287A1 (en) 2006-03-20 2006-03-20 Systems and methods for a gas field ionization source
US11/385,215 US7601953B2 (en) 2006-03-20 2006-03-20 Systems and methods for a gas field ion microscope
US79580606P 2006-04-28 2006-04-28
US79920306P 2006-05-09 2006-05-09
PCT/US2006/044729 WO2007067328A2 (fr) 2005-12-02 2006-11-15 Sources d'ions, systemes et procedes associes

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WO2008152132A2 (fr) * 2007-06-15 2008-12-18 Interuniversitair Microelektronica Centrum Vzw (Imec) Appareil et procédé pour spectroscopie de masse à émission ionique secondaire
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