WO2012123216A1 - Spectroscopie de rayons x - Google Patents

Spectroscopie de rayons x Download PDF

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Publication number
WO2012123216A1
WO2012123216A1 PCT/EP2012/052754 EP2012052754W WO2012123216A1 WO 2012123216 A1 WO2012123216 A1 WO 2012123216A1 EP 2012052754 W EP2012052754 W EP 2012052754W WO 2012123216 A1 WO2012123216 A1 WO 2012123216A1
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WO
WIPO (PCT)
Prior art keywords
sample
electron beam
electron
light
electron source
Prior art date
Application number
PCT/EP2012/052754
Other languages
German (de)
English (en)
Inventor
Evangelos Papastathopoulos
Holger Wegendt
Lucian Stefan
Christian Thomas
Original Assignee
Carl Zeiss Microscopy Gmbh
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
Application filed by Carl Zeiss Microscopy Gmbh filed Critical Carl Zeiss Microscopy Gmbh
Publication of WO2012123216A1 publication Critical patent/WO2012123216A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00—Microscopes
    • G02B21/36—Microscopes arranged for photographic purposes or projection purposes or digital imaging or video purposes including associated control and data processing arrangements
    • G02B21/365—Control or image processing arrangements for digital or video microscopes
    • G02B21/367—Control or image processing arrangements for digital or video microscopes providing an output produced by processing a plurality of individual source images, e.g. image tiling, montage, composite images, depth sectioning, image comparison
    • 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
    • H01J37/16—Vessels; Containers
    • H01J37/165—Means associated with the vessel for preventing the generation of or for shielding unwanted radiation, e.g. X-rays
    • 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
    • H01J37/22—Optical or photographic arrangements associated with the tube
    • H01J37/226—Optical arrangements for illuminating the object; optical arrangements for collecting light from the object
    • 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
    • H01J37/244—Detectors; Associated components or circuits therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/071—Investigating materials by wave or particle radiation secondary emission combination of measurements, at least 1 secondary emission
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/079—Investigating materials by wave or particle radiation secondary emission incident electron beam and measuring excited X-rays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/307—Accessories, mechanical or electrical features cuvettes-sample holders
    • 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
    • H01J2237/244—Detection characterized by the detecting means
    • H01J2237/2445—Photon detectors for X-rays, light, e.g. photomultipliers

Definitions

  • the invention relates to a device for the spectroscopic evaluation of X-radiation in the analysis of a sample.
  • the X-radiation is produced by the interaction of an electron beam with the sample material.
  • the inventive device is particularly suitable for elemental analysis and element qualification in material microscopy, z. In metallurgy and particle analysis.
  • the elemental analysis is a method for controlling the purity of metallic and non-metallic material by determining the elements contained therein, such as carbon, hydrogen, nitrogen or sulfur. A distinction is made between qualitative elemental analysis, in which only the constituents are determined, and quantitative elemental analysis, in which the mass fractions of the found elements are determined.
  • EDX energy dispersive X-ray spectroscopy
  • XRF quential X-ray fluorescence analysis
  • LIBS laser induced breakdown spectroscopy
  • US Pat. No. 6,452,177 B1 describes an electron beam-based material analysis system which is particularly suitable for investigations under atmospheric pressure. Disadvantageously, no light microscopic observation of the sample is possible with this system. Furthermore, the sample area, in which the material analysis takes place, with an analysis point diameter> 100 ⁇ relatively large, so closely spaced structures with a size over 100 ⁇ can not be distinguished from each other. In addition, there is no shielding for the X-radiation, and the time for a measurement is relatively large.
  • the object of the invention is to develop a device for sample analysis by X-ray spectroscopy of the type described above so that the analysis of a sample can be made immediately after or during the light microscopy enlarged representation of the sample. Another object is to avoid the continuous supply of the gas. According to the invention, such a device comprises
  • an electron source from which an electron beam can be aligned with a region of the specimen selected by means of the light-microscopic arrangement
  • an X-ray detector designed to detect the resulting by the interaction of the electron beam with the sample material X-ray radiation
  • Means are provided, through which the sample area to be analyzed
  • a shield is present, which covers the measuring range at least during the
  • the shield is formed as a U-shaped housing and arranged in the device that the opening of the U-shape seen in the direction of gravity is down.
  • the housing forms an upwardly closed measuring chamber, from which a protective gas, which is lighter than air and in the presence of which the sample is examined, can not escape.
  • a protective gas which is lighter than air and in the presence of which the sample is examined.
  • a further advantage results from the fact that due to this embodiment according to the invention a complete, hermetic isolation of the measuring point from the surrounding atmosphere - in contrast to the prior art - is no longer absolutely necessary.
  • a hermetic shield can be provided by appropriate design of the sample support or by additional shielding.
  • an evaluation unit which analyzes the X-ray radiation spectrally
  • a control unit which generates control commands for the light-microscopic arrangement, the electron source, the X-ray detector and the evaluation unit so that the automation of the sample analysis can be carried out as far as possible.
  • the measurement range for the spectroscopic measurement phase is determined on the basis of the light-optical measurement of the sample.
  • the device according to the invention In contrast to the prior art, it is possible with the device according to the invention to carry out both the light microscopic and the electron beam excited examination, without a significant interruption of the workflow is required because of a change between two locally separate devices. As a further advantage, no vacuum environment is required in the X-ray analysis with the device according to the invention, since the sample is examined in the presence of a protective gas under or near ambient pressure.
  • helium as a protective gas in this context allows - both due to the weak scattering of electrons and due to the lower absorption of low-energy X-radiation - the implementation of EDX elemental analysis with a spatial resolution in the range of 1 ⁇ ⁇ 100 ⁇ , while the propagation distance of the electrons or the distance between the sample and the electron source is in the millimeter range. Due to this uncritical positioning of the sample to the electron source higher throughput rates in the analysis of a series of samples are possible with the device according to the invention.
  • the device according to the invention is equipped with adjusting devices for displacing the sample relative to the observation beam path of the light-microscopic device, to the electron beam and to the X-ray radiation detector.
  • the adjusting devices are connected to the control unit and the evaluation unit, so that, depending on the task underlying the analysis and the observation and / or analysis result, setting commands for moving the sample or for displaying the result of the analysis can be generated and output.
  • the device according to the invention can be equipped with means for focusing or collimating the electron beam onto the selected region of the sample.
  • an optoelectronic arrangement preferably consisting of a light source or a laser source and a photodetector arranged in the reception area of the laser light, should be provided.
  • a laser-optical aiming beam in the visible wavelength range, it is easy to mark or calibrate the electron impact location on the specimen.
  • a phosphorescent element may be used for the same purpose.
  • the electron source and the X-ray detector can be designed as an EDX analysis module.
  • the spot size of the focused on the sample electron beam is 5 ⁇ to 100 ⁇ , and the working distance and the distance of the last component of the electron source to the sample is in the measuring position or during the measurement phase 500 ⁇ to 2000 ⁇ . Both components are fixed and connected to a measuring chamber.
  • the selected sample area is centered under the electron source and the X-ray spectrum is automatically evaluated.
  • the sample is thereby displaced relative to the light-microscopic arrangement and the analysis module with the aid of a sliding table, which can preferably be automatically positioned in the coordinates ⁇ , ⁇ , ⁇ .
  • the coordinates of the selected sample area for analysis are identified on the basis of the light microscopic image.
  • this sample area is positioned under the fixed electron source and irradiated to perform the measurement according to the measurement task.
  • a laser range finder or at least one light barrier is provided to avoid collision of the sample with the electron source.
  • This protective arrangement is designed with a measuring accuracy in the micrometer range and is preferably coupled to a cut-off mechanism which optionally stops the relative movement between the sample and the electron source.
  • the sample is shielded from the environment during the analysis by the shield.
  • an aperture can additionally be provided for safe shielding of the X-ray radiation.
  • a gas for example Helium
  • the supplied gas displaces the air present in the chamber volume, which causes a smaller scattering of the electron radiation and absorption of the detection radiation with a constant ambient pressure and with which the spatial resolution and the detection efficiency of the device can be optimized.
  • helium is lighter than the atmospheric air, due to the downwardly open shape of the measuring chamber, the supplied helium remains trapped in the measuring chamber and does not constantly have to be refilled even slightly.
  • a reduction of the air atmosphere within the shield to, for example, 1 to 300 hPa conceivable.
  • the partial evacuation in a similar way as a protective gas atmosphere, ensures a reduced scattering of the electrons and absorption of the detection radiation.
  • the shield is advantageously provided with a closing control mechanism, for example comprising sensors in the form of inductive proximity switches, which control the approach of the underlying plate or the shielding sample carrier and ensure via the control unit that the electron source is switched on only when the shield is completely closed can be.
  • a closing control mechanism for example comprising sensors in the form of inductive proximity switches, which control the approach of the underlying plate or the shielding sample carrier and ensure via the control unit that the electron source is switched on only when the shield is completely closed can be.
  • the radiation shielding is effected by the proximity of the U-shaped upper part of the chamber to the sample carrier, which can be designed, for example, as a sample table.
  • the mutually facing surfaces of the chamber and sample carrier are advantageously designed flat.
  • the chamber is dimensioned larger than the sample carrier, and this is thus placed from below in the chamber.
  • the sample carrier has a centrally arranged device for receiving the sample, which can be designed to be height-adjustable.
  • the chamber facing surface of this device is raised relative to the peripheral sample support surfaces.
  • this device in the Z direction that is, in the direction of the optical axis, be made movable in such a way that the chamber facing surface of the central device relative to the peripheral sample carrier surfaces is raised and lowered.
  • this device is dimensioned so that it can be placed from below in the chamber.
  • the sample table projects beyond the chamber, so that upon closing the chamber comes into contact with the peripheral surfaces of the sample holder.
  • the U-shaped part of the measuring chamber is equipped with movable mechanical elements, which allow a complete closure of the measuring chamber, as will be explained in more detail below.
  • the electron source in the region between the exit position of the electrons and the point of impact on the sample is equipped with an electron-permeable membrane, which consists for example of Si 3 N 4 .
  • the distance between the membrane and the sample surface is, for example, 0.1 mm to 2 mm.
  • means for analyzing selected regions of the sample with ions which, starting from an ion source, serve to excite the sample substance instead of the excitation with electrons.
  • Another conceivable variant is the investigation of the luminescence generated by the electron beam in the sample with the aid of a luminescence detector via the light microscope, but also of a separate detector.
  • a microscopically small sample area can be analyzed in a spatially resolved manner, wherein a point analysis is possible within a few seconds due to the intended beam strengths.
  • the arrangement according to the invention has the following advantages:
  • the sample remains unaffected during elemental analysis. This is an advantage with respect to the study of unstable samples such. B. of particle filters for the residual soil analysis.
  • FIG. 1 shows the basic structure of the device according to the invention for the direct X-ray spectroscopic analysis of a sample 1 including a light-microscopic arrangement for the visual selection of a sample region to be analyzed.
  • a microscope objective 2 and its optical axis 17 are shown by the light-microscopic arrangement.
  • Light microscopes and their beam paths are known per se and therefore require no further explanation at this point.
  • FIG. 1 also shows an electron source 3 which emits an electron beam 4 which is directed onto an area of the sample 1 to be analyzed. Owing to the interactions of the electron beam 4 with the sample material, X-radiation 5 is produced, which is characteristic for the element-specific composition of the sample 1 within the interaction volume.
  • the X-ray emission emanating from the sample 1 during electron irradiation is analyzed spectrally with an X-ray detector 6.
  • X-ray detector 6 can For example, a cooled Si (Li) detector or silicon drift detector can be used.
  • the X-ray detector 6 is brought as close as possible to the electron impact point, so that the X-ray radiation is detected from a large solid angle.
  • the electron source 3 is made compact. It consists of an electron emitter and an electrode arrangement for accelerating and focusing the electron beam.
  • the electron energy is advantageously 0.1 to 30 KeV.
  • a length of a simple electrode arrangement of ⁇ 3 mm is sufficient. Free electrons are generated in an electron emitter, for example, which are then accelerated along the acceleration path and concentrated in a single lens before they exit through the aperture. In a very simplified embodiment, it is also possible to dispense with the single lens by cutting off the electron beam 4 only through the aperture, although a smaller current is to be accepted.
  • the electron optics may, for example, consist of a layer system of conductive and insulating layers, wherein the conductive layers are set to different potentials, so that the free electrons are bundled, accelerated and focused by the resulting fields.
  • the electron beam 4 are compared to a scanning electron microscope not so high demands.
  • a beam width of a few micrometers is sufficient, since the spatial resolution, which is determined by the interaction volume, is usually not better due to the energy used for the analysis.
  • the electron beam 4 can remain aligned with the sample during the measuring phase and does not have to be scanned over the sample 1, which means a reduction of the technical complexity.
  • Within the electron source 3 there is a vacuum, so that free electrons can be generated and used with as few scattering processes as possible for the excitation of X-radiation.
  • the electron source 3 is preferably located in an encapsulated vacuum tube, which is kept in a high vacuum state.
  • the electron source 3 is designed in such a way that the generation of the free electrons takes place in the upper region, which is then focused towards the lower end by means of an electron optics or shaped with the aid of at least one aperture to the intended beam diameter. Finally, the electrons will leave the electron source 3 through a suitable device, for example through a Si 3 N 4 membrane.
  • the distance between the sample 1 and the exit opening of the electrons, such as a membrane, is for example 0.5 mm.
  • the electron source 3 can be arranged to be movable in the direction of the sample 1. The reverse variant is possible.
  • a regulation of this distance can be provided. For example, for conductive samples 1, this distance may be controlled based on electrical resistance or impedance measurement.
  • the X-ray radiation 5 is detected by means of the X-ray detector 6.
  • the output signal of the X-ray detector 6 is applied to an evaluation unit (not shown) and is analyzed there by means of suitable software, after which a classification of, for example, determined particles or inclusions in metal samples is carried out. Finally, the corresponding element distribution in the analyzed sample area can be visually perceptible displayed on a monitor or stored as a measurement protocol or printed output.
  • the entire system is controlled by a central processing unit that controls the light microscope assembly and receives and processes its data.
  • this arithmetic unit is also connected to the electron source 3, the X-ray detector 6 and the drives for a carriage 10 which can be moved in the coordinates X, Y and Z, on which a sample table 7 with the sample 1 is located.
  • Sample table and slide can also be formed into a structural unit fused (not shown).
  • the electron source 3 and the X-ray detector 6 are enclosed by a housing 8 and thus designed as an EDX analysis module. As shown in FIG. 1, the housing 8 is provided with an opening 9 arranged at the bottom as seen in the direction of gravity.
  • the sample table 7 with the sample 1 is moved out of the region of the microscope objective 2 and displaced in the direction X until the region of the sample to be analyzed 1 in the optical axis 1 1 of the electron source 3 is located.
  • the drive of the carriage 10 is then controlled so that its displacement in the direction Z is carried out until the surface of the sample is immersed in the helium atmosphere.
  • a minimum distance between the housing 8 and the sample table 7 is present to ensure the mobility of the sample during the spectroscopic measurement phase.
  • the opening 9 is not completely closed by the sample table 7.
  • the measurement volume within the housing 8 remains shielded anyway, since the height the specimen surface is higher than the lower edge of the U-shaped housing 8.
  • the profile of the specimen stage may be peripherally lowered to provide more effective shielding. With this shield, the electron source 3, the X-ray detector 6, and the sample area to be analyzed are sufficient but not completely separated from the surrounding free atmosphere.
  • a control mechanism can thereby ensure an automatic and secure closure of the shield and only switch on the electron source 3 or start the sample analysis only if the closure has taken place correctly.
  • the range for the X-ray analysis is fixedly connected to the light microscopic arrangement, and the moving distance of the carriage 10 in the direction X always corresponds to the distance between the optical axis 17 of the microscope objective 2 and the optical axis 1 1 of the electron source 3.
  • the under the microscope objective 2 selected sample area with the analyzed sample area is identical.
  • one or more locations of the sample at which e.g. different particles or inclusions are located automatically, for example via an image recognition software, or manually identified, whereby the coordinates (X, Y and / or Z) of the sample sites are detected. These are then analyzed sequentially spectroscopically. Fast movements are possible by using adjusted limit switches.
  • sample surfaces can be detected manually or automatically by means of a series of overlapping images and calculated by the processing unit into a tiled image. It is also possible to detect the coordinates of points of interest found on a tile image and then to analyze them sequentially spectroscopically.
  • the device according to the invention is optionally equipped with a gas supply 12, which is provided in particular for charging the volume within the closed housing 8 with helium in order to effect a small scattering of the electrons.
  • the feed takes place via a line 13 from a gas reservoir, not shown, through an outer wall of the housing 8.
  • a valve 14 is arranged, which is controlled by the control unit of the arrangement.
  • FIG. 2 shows a variant of the exemplary embodiment explained above with reference to FIG.
  • the same reference numbers are used again for the same assemblies, which have already been explained with reference to FIG. 1, in FIG. 2 - and also subsequently in FIGS. 3 and 4.
  • the EDX analysis module is connected to a shield in the form of an annular telescope housing 16, which is designed so that before the start of the sample analysis due to the relative movement between the EDX analysis module and the carriage 1 0, a closure of the volume within the housing 8 with higher security.
  • a seal 18 is additionally provided here.
  • the seal may be elastic, for example made of rubber as a circumferential sealing ring or, for example, as a brush seal. Any other design is possible as well.
  • the light barrier formed by a light source 19 and a photodetector 20 and associated with the arithmetic unit and at least one traversing device of the carriage 10, the specimen table 7 and / or the preferably central device arranged inside the specimen table therefore becomes an automatic control of the positioning taken care of the sample area to be analyzed.
  • the light barrier is expediently arranged at a minimum distance below the outlet opening. As soon as the light barrier registers an approaching obstacle, the movement device is stopped via the computing unit.
  • the light barrier can also serve or also serve to optimally position the sample area to be analyzed in the focus of the electron beam 4.
  • the electron source 3 is only turned on and the sample analysis is only started when the sample 1 is positioned in the focus of the electron beam 4.
  • a gas supply 12 is optionally available for the purpose already described.
  • FIG. 3 shows a further exemplary embodiment in which the EDX analysis module is constructed in such a miniaturized manner that the sample analysis can be carried out while the sample 1 is still in the position under the microscope objective 2.
  • a closing device here again an annular telescopic housing 16 is provided with a seal 18.
  • the irradiation of the electrons takes place by means of a channel 21 through the telescope housing 1 6 therethrough.
  • the x-ray radiation 5 passes through the channel 21 to the x-ray detector 6.
  • a gas supply 12 is likewise optionally present here.
  • the electron source 3 is only switched on and the sample analysis is only started if the closure has been carried out correctly.
  • FIG. 4 shows an embodiment variant of the embodiment explained above with reference to FIG. 3, in which, however, a housing 22 fixedly connected to the carriage 10 is provided. which surrounds the sample 1 and through the outer wall of the channel 21 is passed. Likewise, a gas supply 12 is passed through the outer wall of the housing 22.
  • the housing 22 has an opening at the top, which is closed with a cover 23 when the carriage 10 is moved in the direction Y, so that in this case too, a sufficiently closed measuring volume is formed.
  • the electron source 3 is only switched on and the sample analysis is started only when the closure has been carried out correctly.
  • an aperture 24 is still present here, which further increases the effect of shielding against the emission of X-radiation.

Abstract

L'invention concerne un dispositif d'analyse spectroscopique d'un rayonnement X (5) lors de l'analyse d'un échantillon (1). Le rayonnement X (5) est généré par l'interaction entre un rayon électronique (4) et la matière échantillon. Le dispositif selon l'invention est en particulier conçu pour l'analyse d'éléments et la qualification d'éléments lors de la microscopie de matière, par exemple en métallurgie ou lors de l'analyse de particules. Le dispositif selon l'invention comprend : un système à microscopie optique conçu pour inspecter l'échantillon (1), une source d'électrons (3) à partir de laquelle un rayon électronique (4) peut être orienté sur une zone de l'échantillon (1) sélectionnée au moyen du système à microscopie optique, et un détecteur à rayons x (6) conçu pour détecter le rayonnement x (5) généré par l'interaction entre le rayon électronique (4) et la matière échantillon. Des moyens sont prévus pour disposer la zone d'échantillon à analyser dans le plan focal d'un objectif du système à microscopie optique pendant la phase d'inspection et dans la zone du rayon électronique (4) et dans la zone de réception du détecteur à rayons X (6) pendant une phase de mesure, ainsi qu'un blindage se présentant sous la forme d'un boîtier en U (8).
PCT/EP2012/052754 2011-03-17 2012-02-17 Spectroscopie de rayons x WO2012123216A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201110005732 DE102011005732B4 (de) 2011-03-17 2011-03-17 Einrichtung zur Röntgenspektroskopie
DE102011005732.3 2011-03-17

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