WO2005003735A1 - 薄片試料作製方法および複合荷電粒子ビーム装置 - Google Patents
薄片試料作製方法および複合荷電粒子ビーム装置 Download PDFInfo
- Publication number
- WO2005003735A1 WO2005003735A1 PCT/JP2004/009868 JP2004009868W WO2005003735A1 WO 2005003735 A1 WO2005003735 A1 WO 2005003735A1 JP 2004009868 W JP2004009868 W JP 2004009868W WO 2005003735 A1 WO2005003735 A1 WO 2005003735A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- ion beam
- focused ion
- sample
- side wall
- focusing
- Prior art date
Links
Classifications
-
- 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
- H01J37/3002—Details
- H01J37/3005—Observing the objects or the point of impact on the object
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- 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
- H01J37/304—Controlling tubes by information coming from the objects or from the beam, e.g. correction signals
-
- 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
-
- 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
- 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
- H01J2237/31745—Etching microareas for preparing specimen to be viewed in microscopes or analyzed in microanalysers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
Definitions
- the present invention relates to a method for producing a thin section sample for observation with a transmission electron microscope.
- Thin-film preparation method for forming flakes on the surface of a sample such as a semiconductor device Thin-film preparation method for forming flakes on the surface of a sample such as a semiconductor device
- thin sections were prepared by using a focused ion beam irradiation system and an electron beam irradiation system to perform a desired part of the sample surface by sputtering etching with a focused ion beam using a composite device consisting of a focused ion beam irradiation system and an electron beam irradiation system.
- a method is known in which a slice sample is taken out, and the taken-out slice sample is observed with a transmission electron microscope (for example, see Patent Document 1).
- Patent Literature 1 Japanese Patent Application Laid-Open No. Hei 7-174643 (page 2)
- Patent Literature 2 Japanese Patent Application Laid-Open No. H6-162074 (page 2)
- Patent Document 2 in order to make the thickness of a thin slice sample uniform, it is known to process the sample while tilting it. However, in such a processing method, there is no known method for controlling the thickness of the flake.
- the present invention provides a method of performing sputtering etching on a sample surface using a focused ion beam. A focused ion beam was scanned and irradiated, and the thickness of the slice was measured and the slice was prepared while confirming the thickness.
- processing is performed by combining a plurality of focused ion beams to reduce the time required for processing.
- the tilt direction of the stage is determined.
- the angle between the angle and the angle can be changed. This will be described with reference to FIG.
- the sample stage 7 is configured so as to be inclined in a plane direction including each of the beam barrels 1 and 3.
- it is configured to be inclined at least by 90 degrees different axes. This makes it possible to correct the inclination angle of the side wall with the first charged particle beam and, at the same time, immediately measure the thickness of the flake sample with the second charged particle beam.
- it also includes tilting in both directions.
- a twin-tilt or dual-beam device has a dual tilt configuration with two tilt axes.
- a method for preparing a thin section sample by forming a thin section by scanning and irradiating the sample surface with a focused ion beam and performing etching, and taking out the thin section.
- the second section is performed in a direction parallel to the side wall of the produced thin section.
- the surface of the thin section is observed under a microscope by scanning and irradiating a focused beam, the thickness of the thin section is measured, and it is confirmed that the thickness of the thin section has reached a predetermined thickness. The processing is terminated.
- the first focused ion beam is formed.
- the method for producing a slice sample according to the present invention includes the steps of: performing the second and third steps on the slice and the first side wall of the to-be-slided region to form the slice into a first desired thickness.
- a second third step is performed on a second side wall of the region to be thinned to form the predetermined thickness.
- the first focusing beam is irradiated onto the side wall so as to correct the inclination thereof.
- the sample is tilted to scan and irradiate a focused beam.
- a first focused ion is formed.
- a third step of measuring wherein the second step and the third step are performed simultaneously or alternately, and the thickness of the area to be a thin section is formed to a predetermined thickness. I do.
- a thin section is formed by scanning and irradiating the sample surface with a focused ion beam to perform etching, and by taking out the thin section, the thin section is obtained.
- a first processed region for exposing a first side wall of a region to be thinned under a first focused ion beam condition of a first focused ion beam is subjected to sputtering etching.
- a first step of sputtering and etching a second processing area for exposing a second side wall of the area to be flaked under a first focused ion beam condition of a second focused ion beam Simultaneously sputtering the second region to be processed under the first focused ion beam condition of the first focused ion beam, and simultaneously forming the first focused ion beam of the second focused ion beam.
- the sample is tilted so that the first focused beam is incident on the first side shot so as to correct the tilt, and the first focused beam is used by using the first focused beam.
- the first side wall is subjected to sputtering etching under the second focusing beam condition having a lower accelerating voltage and / or a lower beam current than the focusing beam condition.
- the focused ion beam irradiation is temporarily interrupted, the second focused ion beam is scanned and irradiated under the third focused ion beam condition, the surface of the thin section is observed with a microscope, and the thickness of the thin section is measured.
- the first focused ion beam is incident on the The sample is tilted so that the second side wall of the first focused beam is subjected to the sputtering etching under the second focused ion beam condition simultaneously with or simultaneously with the first focused ion beam irradiation.
- the thickness of the region to be formed is set to a desired thickness.
- a first focused ion beam column that focuses an ion beam generated from an ion source and scans and irradiates the sample surface
- an ion beam generated from the ion source Focused ion beam system consisting of a second focused ion beam column that focuses the sample and scans and irradiates the sample surface, and a sample stage on which the sample is placed and has a plurality of drive shafts and moves in a three-dimensional space
- the first focused ion beam emitted from the first focusing beam column and the second focused ion beam emitted from the second focusing beam column are:
- the sample stage placed on the sample stage is arranged so as to be irradiated at different angles to the same portion of the surface of the sample, and the sample stage includes at least the first focusing beam column and the sample tube.
- a first focused ion beam column for focusing an ion beam generated from an ion source and scanning and irradiating the sample surface with a beam.
- a second focused ion beam column that focuses the ion beam and scans and irradiates the sample surface
- an inert ion beam column that focuses an inert ion beam generated from an inert ion source and scans and irradiates the sample surface
- a composite focused ion beam system consisting of a sample stage on which a sample is placed and which moves in a three-dimensional space with multiple drive axes.
- the first focused ion beam column, the second focused ion beam column, and the inert beam column are disposed on the same plane, and the first focused ion beam column.
- a first focused ion beam irradiated more, a second focused ion beam irradiated from the second focused ion beam column, and an inert beam irradiated from the inert beam column
- the beam is arranged so as to irradiate the same portion of the surface of the sample placed on the sample stage at different angles, and the sample stage includes at least the first focusing ion beam column and the second
- the first plane with reference to a second plane perpendicular to the first plane formed by the focusing tube and the inactive lens tube Tilt to change the angle to And wherein the Rukoto.
- FIG. 1 shows an example of the configuration of a combined ion beam composite apparatus according to the present invention.
- FIG. 2 is an explanatory diagram relating to the operation of the sample stage used in the focused ion beam combined device according to the present invention.
- FIG. 3 shows an embodiment of the method according to the invention.
- FIGS. 4A and 4B are explanatory views showing the tilt direction of the sample stage.
- FIG. 4A is a front view
- FIG. 4B is a side view.
- a first focused ion beam column 1 that focuses ions generated from the liquid metal ion source with a focused ion optical system, focuses and scans the sample surface, and focuses ions generated from the liquid metal ion source. Focusing on the sample surface and scanning and irradiating with focusing on the sample surface 2 and an inert beam column 3 for generating an inert beam such as argon and irradiating the sample with the inert beam are attached to the sample chamber 4.
- the inside of the sample chamber is evacuated by the vacuum pump 5 to maintain a high vacuum state.
- a sample stage 7 on which the sample 6 is placed and moved is installed inside the sample chamber 4.
- the first focused ion beam column 1, the second focused ion beam column 2, and the inert ion beam column 3 are arranged on the same plane. Then, the first focused beam emitted from the first focused ion beam column 1 and the second focused beam emitted from the second focused ion beam column 2
- the inert ion beam emitted from the active ion beam column 3 is adjusted to intersect at one point on the surface of the sample 6 placed on the sample stage 7. At this time, the arrangement of the first focused ion beam column 1, the second focused ion tube column 2, and the inert ion beam column 3 may be interchanged.
- the sample stage 7 has a plurality of drive shafts and can move in a three-dimensional space with the sample 6 placed thereon.
- the first focusing ion beam column 1 With reference to a second plane 9 orthogonal to the first plane 8 including the second focused ion beam column 2 and the inert ion beam column 3, the crossing angle can be changed. I have.
- the range in which the intersection angle can be changed should be at least ⁇ 1 degree. This is the angle of inclination provided to erect the sample side wall perpendicular to the sample surface. The objective can be achieved if it can be experimentally tilted from this angle. That is, the inclination of the side wall surface of the sample can be corrected.
- the first focused ion beam emitted from the first focused ion beam column 1 to scan and irradiate the surface of the sample performs a sputter etching process on a region to be processed on the surface of the sample 6. Stop the simultaneous or primary focused ion beam Then, the second focused ion beam emitted from the second focused ion beam column 2 and scanned and irradiated on the surface of the sample is scanned and irradiated on the surface of the sample 6 including the region to be processed. Then, secondary charged particles such as electrons generated from the surface of the sample 6 are detected by a secondary charged particle detector (not shown in FIG. 1), and a scanning electron microscope image is obtained by a device control system (not shown). Become.
- first focused ion beam column 1 and the second focused ion beam column 2 can be switched. Furthermore, the first focused ion beam column 1 and the second focused ion beam column 2 can also perform the same sputtering etching at the same or different locations on the sample surface.
- the apparatus control system ends the irradiation of the sample with the first and second focusing beams.
- the inert ion beam emitted from the inert ion beam column 3 is irradiated around the flakes on the surface of the sample 6 to perform sputtering etching.
- the first or second focused beam was scanned and irradiated, and the periphery of the thin film was observed with a scanning ion microscope image, and the thickness of the slice became the set thickness.
- the apparatus control system ends the irradiation of the sample with the focused ion beam and the inert ion beam.
- FIG. 3 illustrates one embodiment of the method according to the present invention.
- processing frames 12a and 12b are set on both sides of the area 11 left as a slice on the sample surface.
- the processing frame 12a is sputtered with the first focused ion beam 101.
- the processing frame 12b is sputter-etched with the second focused ion beam 102.
- the processing frame 12b is sputtered by a first focused ion beam, and the processing frame 12a is processed by a second focused ion beam.
- the first focused ion beam and the second focused ion beam are on a plane orthogonal to the sample surface, and are arranged at positions where they are incident on the same location on the sample surface at different angles.
- the sputter etching process is performed under the first focused ion beam condition where the acceleration voltage is high and the etching speed is high.
- both sides of the region including the region 11 to be left as a flake are etched.
- a processing frame 13 is set on one side wall of the region 11 to be left as a thin section. Then, the sample is tilted, and the runner is irradiated with the first focused ion beam 101 under the second focused ion beam condition having a smaller beam diameter compared to the first focused beam condition. To perform sputter ring etching.
- the tilt angle shall be set so that the side wall of the slice is perpendicular to the sample surface.
- the second focused ion beam is scanned and irradiated under the third focused ion beam condition, and the surface of the thin section is irradiated. Is observed with a scanning ion microscope. Then, when the thickness of the flake reaches a predetermined thickness, the irradiation of the first and second focusing beams is terminated. Subsequently, as shown in FIG. 3C, a processing frame 14 is set on the other side wall side of the area 11 to be left as a thin section.
- the sample is tilted, and the first focused ion beam 101 is scanned and irradiated under the second focused ion beam condition to perform a sputtering etching process.
- the inclination angle at this time is Determined under the same conditions as the oblique.
- the second focused ion beam is scanned and irradiated under the third focused ion beam condition, and the surface of the thin section is observed with a scanning ion microscope. Then, when the thickness of the flake reaches a predetermined thickness, the irradiation of the first and second focused ion beams is completed.
- the thin section may be cut from the sample by processing the periphery of the thin section by a spacial etching process using the first and second focused ion beams.
- the acceleration voltage to a low voltage of 10 kV or less under the second focused ion beam condition. You may do it.
- the sample may be returned to a horizontal position, and the region 15 including the thin section may be irradiated with an inert ion beam. Then, the periphery of the thin section may be subjected to sputtering and etching. At that time, the first and second focused ion beams are scanned and irradiated around the thin section under the third focused ion beam condition, and the surface of the thin section is observed with a scanning ion microscope, and the thickness of the thin section is adjusted to a predetermined thickness. At this point, the irradiation of the focusing beam and the inert beam is terminated.
- the periphery of the flake is processed by spattering etching using a focused ion beam, and the flake is cut off from the sample.
- the thickness of the flake can be accurately controlled, and a flake sample can be produced in a short time.
- the focused ion beam was scanned and irradiated from a direction parallel to the side wall of the flake to observe the thickness of the flake, It is possible to obtain the effect that the uniformity of the thickness not only at the upper portion but also at the lower portion can be confirmed.
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
- Drying Of Semiconductors (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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US10/563,515 US7700367B2 (en) | 2003-07-08 | 2004-07-05 | Method of making lamina specimen |
EP04747336A EP1643232A4 (en) | 2003-07-08 | 2004-07-05 | METHOD FOR PREPARING THIN PIECES SPECIMENS AND COMPOSITE CHARGED PARTICLE BEAM DEVICE |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003-193512 | 2003-07-08 | ||
JP2003193512A JP3887356B2 (ja) | 2003-07-08 | 2003-07-08 | 薄片試料作製方法 |
Publications (1)
Publication Number | Publication Date |
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WO2005003735A1 true WO2005003735A1 (ja) | 2005-01-13 |
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Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/009868 WO2005003735A1 (ja) | 2003-07-08 | 2004-07-05 | 薄片試料作製方法および複合荷電粒子ビーム装置 |
PCT/JP2004/009870 WO2005003736A1 (ja) | 2003-07-08 | 2004-07-05 | 薄片試料作製方法および複合荷電粒子ビーム装置 |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/009870 WO2005003736A1 (ja) | 2003-07-08 | 2004-07-05 | 薄片試料作製方法および複合荷電粒子ビーム装置 |
Country Status (4)
Country | Link |
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US (1) | US7700367B2 (ja) |
EP (1) | EP1643232A4 (ja) |
JP (1) | JP3887356B2 (ja) |
WO (2) | WO2005003735A1 (ja) |
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- 2004-07-05 US US10/563,515 patent/US7700367B2/en active Active
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- 2004-07-05 WO PCT/JP2004/009870 patent/WO2005003736A1/ja active Application Filing
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US11491287B2 (en) | 2005-07-20 | 2022-11-08 | Manta Devices, Llc | Inhalation device |
US11672927B2 (en) | 2005-07-20 | 2023-06-13 | Manta Devices, Llc | Inhalation device |
US9919115B2 (en) | 2007-07-06 | 2018-03-20 | Manta Devices, Llc | Dose delivery device for inhalation with first and second portions to open a dose chamber |
CN103940643A (zh) * | 2013-01-18 | 2014-07-23 | 中芯国际集成电路制造(上海)有限公司 | Tsv样品的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
US7700367B2 (en) | 2010-04-20 |
EP1643232A1 (en) | 2006-04-05 |
EP1643232A4 (en) | 2008-05-14 |
JP3887356B2 (ja) | 2007-02-28 |
JP2005030799A (ja) | 2005-02-03 |
US20060157341A1 (en) | 2006-07-20 |
WO2005003736A1 (ja) | 2005-01-13 |
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