CN111474197A - Method for controlling contamination resulting from transmission electron microscope sample preparation - Google Patents

Method for controlling contamination resulting from transmission electron microscope sample preparation Download PDF

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Publication number
CN111474197A
CN111474197A CN202010302229.6A CN202010302229A CN111474197A CN 111474197 A CN111474197 A CN 111474197A CN 202010302229 A CN202010302229 A CN 202010302229A CN 111474197 A CN111474197 A CN 111474197A
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sample
copper sheet
area
ion beam
supporting copper
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CN202010302229.6A
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Chinese (zh)
Inventor
郑义明
李毅峰
杨詠钧
杨培华
谢忠诚
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TPK Touch Solutions Xiamen Inc
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TPK Touch Solutions Xiamen Inc
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Priority to CN202010302229.6A priority Critical patent/CN111474197A/en
Publication of CN111474197A publication Critical patent/CN111474197A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/02Investigating 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 transmitting the radiation through the material
    • G01N23/04Investigating 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 transmitting the radiation through the material and forming images of the material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025Sample holders or supports therefor

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  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present disclosure relates to electron microscope sample preparation, and provides a method for controlling contamination resulting from transmission electron microscope sample preparation, comprising: depositing a protective layer above a preset sample area of the element to be detected; cutting off a preset sample area to obtain a sample, wherein the sample is provided with an area to be measured; transferring and fixing the sample on a supporting copper sheet, wherein the area to be measured of the sample is not in contact with the supporting copper sheet directly below; thinning the area to be detected of the sample by using an ion beam; and performing low-voltage cleaning treatment on the area to be detected.

Description

Method for controlling contamination resulting from transmission electron microscope sample preparation
Technical Field
The present disclosure relates to the field of Transmission Electron Microscope (TEM) sample preparation technology, and more particularly to a method for controlling sample contamination during TEM sample preparation using a focused ion beam system (FIB).
Background
In the semiconductor field such as touch screens and integrated circuits, the requirement on analysis accuracy is higher along with the refinement of circuits. The transmission electron microscope has the advantage of high resolution and is widely applied. However, transmission analysis has a strict requirement on sample quality, and compared with the traditional transmission sample preparation methods such as ion thinning, electrolytic double-spraying, ultrathin slicing and the like, the focused ion beam system has unique advantages, can realize fixed-point sampling, and is more convenient for preparing transmission samples of a plurality of micro devices.
However, in the process of preparing a transmission sample by using a focused ion beam system, the sample has a pollution problem and the quality of the sample is influenced. The main pollution comes from: firstly, substrate pollution, wherein due to the fact that a sample is in contact with a copper sheet, during the thinning process, ion beams bombard the copper sheet while the sample is thinned, so that the situation that copper is reversely deposited to the bottom of the sample occurs at the final stage of thinning, and the sample is polluted; and secondly, irradiation damage and pollution, wherein the ion beam has energy, so that a damage and pollution layer can be generated on the sample in the thinning process.
FIG. 1A shows a conventional method for fixing a device sample to be tested on a supporting copper sheet. The conventional sample preparation method is to weld and fix the sample and the supporting copper sheet by tungsten deposition. The bottom of the sample is in direct contact with the supporting copper sheet or indirectly in contact with the supporting copper sheet through tungsten, so that copper is reversely deposited during the thinning process to pollute the sample.
FIG. 1B shows an image of a finished sample after the device sample to be tested is mounted on a supporting copper plate in a conventional manner, and many light-colored spots in the sample are observed, which indicates that the sample may have a contamination problem. FIG. 1C shows an image of the sample of FIG. 1B analyzed using an energy spectrometer to confirm that the majority of the contaminants are elemental copper.
Fig. 2A is a schematic diagram of a sample prepared with a focused ion beam system showing the first side 12 and the second side 14 of the sample 10 having irradiation damage. Because the two sides of the transmission electron microscope sample need to be thinned, a thin sample with smaller thickness is finally obtained; however, the existence of irradiation damage causes a damage layer to be formed on each side of the sample, which affects the signal of the transmission electron microscope and brings difficulty to the analysis of the sample nanostructure. Fig. 2B shows a transmission image of a sample prepared by a focused ion beam system in a conventional manner, and it is seen that the structure of the sample is distorted and cannot be accurately resolved.
The quality of the tem sample determines whether transmission high resolution, diffraction, etc. analysis can be achieved and the accuracy of the analysis of the components is improved. Therefore, aiming at the pollution problem existing in the preparation of the transmission sample, how to optimize the thinning mode and control the generation of sample pollution in the preparation process of the sample becomes a problem to be solved urgently in the technical field of sample preparation.
Disclosure of Invention
In order to solve the problem that the sample of the transmission electron microscope is easy to be polluted during preparation, the sample is fixed on the supporting copper sheet before thinning treatment, and the bottom of the area to be detected of the sample is not contacted with the supporting copper sheet, so that processing pollution caused by ion beam bombardment to the supporting copper sheet is reduced. Furthermore, after the sample is thinned, the two sides of the sample are cleaned and processed at low voltage so as to reduce or even eliminate the irradiation damage pollution generated by the ion beam.
One aspect of the present disclosure is a method for controlling contamination generated by tem sample preparation, comprising: depositing a protective layer above a preset sample area of the element to be detected; cutting off a preset sample area to obtain a sample, wherein the sample is provided with an area to be measured; transferring and fixing the sample on a supporting copper sheet, wherein the area to be measured of the sample is not in contact with the supporting copper sheet directly below; thinning the area to be detected of the sample by using an ion beam; and performing low-voltage cleaning treatment on the area to be detected.
The technical scheme of the disclosure achieves the beneficial effects that the degree of substrate pollution and irradiation damage pollution of the sample is reduced, so that a microstructure image of the element sample to be measured, which is analyzed with higher precision, can be obtained.
Drawings
Aspects of the present disclosure are best understood from the following detailed description when read with the accompanying drawings. It is noted that, in accordance with common practice in the industry, various features are not drawn to scale. In fact, the dimensions of the various features may be arbitrarily increased or reduced for clarity of illustration and discussion.
FIG. 1A shows an image of a sample mounted on a supporting copper sheet in a conventional manner.
Fig. 1B shows an image of a sample prepared in a conventional manner.
FIG. 1C shows the results of analyzing the sample of FIG. 1B using an energy spectrometer.
Fig. 2A shows a schematic diagram of a sample prepared with a focused ion beam.
Fig. 2B shows an image of a sample with significant radiation damage.
FIG. 3 is a flow chart of a method of preparing a transmissive device sample according to some embodiments of the present disclosure.
Fig. 4 is an image of a step in the process of preparing a sample with a focused ion beam system according to some embodiments of the present disclosure.
Fig. 5 is an image of a step in the process of preparing a sample with a focused ion beam system according to some embodiments of the present disclosure.
Fig. 6A is a schematic view of a sample side secured to a side wall of a supporting copper sheet according to some embodiments of the present disclosure.
Fig. 6B is an image of a sample side secured to a side wall of a supporting copper sheet according to some embodiments of the present disclosure.
Fig. 6C is an image of the sample of fig. 6B after thinning processing.
Fig. 7A is an image of a dimple formed in a supporting copper sheet according to some embodiments of the present disclosure.
Fig. 7B is a schematic view of a sample secured to both sides of a pit supporting a copper sheet according to some embodiments of the present disclosure.
Fig. 8 is an image of a step in the process of preparing a sample with a focused ion beam system according to some embodiments of the present disclosure.
Fig. 9A is a high resolution image of the sample before the low voltage cleaning process.
Fig. 9B is a high resolution image of the sample after the low voltage cleaning process.
Fig. 10 is an image of a completed sample prepared according to some embodiments of the present disclosure.
Fig. 11 is a diffraction analysis image of a sample prepared according to some embodiments of the present disclosure.
Fig. 12 is a high resolution analytical image of a sample prepared according to some embodiments of the present disclosure.
Fig. 13A-13F are sample component area distribution analysis images prepared according to some embodiments of the present disclosure.
Description of the symbols
10 sample
12 first side
14 second side
100 method
110 step of
120, step
130 step of
140 step (d)
150 step of
210 sample
220 supporting copper sheet
222 sample column
310 sample
320 supporting copper sheet
322 sample column
324 pits
Detailed Description
In order to make the objects, technical solutions and advantages of the present disclosure more apparent, the present disclosure is further described in detail below with reference to the accompanying drawings, embodiments and examples. It should be understood that the detailed description and examples described herein are intended for purposes of illustration only and are not intended to limit the scope of the claims.
Referring to fig. 3, a flow diagram of a method 100 of preparing a sample for a transmission electron microscope is shown, according to some embodiments.
In step 110 of the method 100, a protective layer is deposited over a predetermined sample area of the device under test. The protective layer is used for avoiding ion beams from contacting with the upper part of the sample in the subsequent thinning process, so that the surface layer of the upper part of the sample is prevented from being lost. In some embodiments, the protective layer is carbon or tungsten and has a thickness of 1 to 2 microns. In some embodiments, sufficient protection is obtained by controlling the beam current and time. Referring to fig. 4, an image of a protective layer deposited over a predetermined sample area of a device under test is shown.
In step 120 of the method 100, a predetermined sample region is cut off to obtain a sample, i.e. a region of interest (ROI) of the dut is obtained, wherein the sample includes the region under test observed by the transmission electron microscope. In some embodiments, a U-shaped cut is used to obtain a sample of the device under test, and the ion beam is used to cut the bottom and side surfaces of the predetermined sample area. Referring to fig. 5, an image of a preset sample area being processed in a U-cut manner is shown.
In step 130 of method 100, the sample is transferred and fixed to a supporting copper sheet, wherein the area of the sample to be measured is not in contact with the supporting copper sheet directly underneath. In other words, the bottom of the sample directly below the region to be measured does not contact the supporting copper sheet, and does not indirectly contact the supporting copper sheet through the deposited tungsten layer. Wherein a sample is extracted in situ in a focused ion beam system and then transferred to a supporting copper plate using a sample rod.
The present disclosure provides two ways to secure the sample to the supporting copper sheet to mitigate substrate contamination.
In some embodiments, sample preparation is performed using the side walls of a supporting copper sheet, with the sides of the sample being secured to the side walls of the supporting copper sheet via tungsten deposition. Thus, the bottom of the sample is in a suspended state. Referring to fig. 6A, a schematic view of fixing the side of the sample on the supporting copper sheet is shown. One side of the sample 210 is fixed to a sidewall of a sample column 222 supporting the copper sheet 220. Fig. 6B shows the image of the sample when mounted on a supporting copper sheet with a single edge.
In other embodiments, the supporting copper sheet is pre-treated to form the pits, after which the sample is fixed on both sides of the pits via tungsten deposition. The image of fig. 7A shows the pits formed in the supporting copper sheet. Fig. 7B shows a schematic view of the sample being held on both sides of the depression supporting the copper sheet. The sample pillar 322 supporting the copper sheet 320 has a recess 324, and the bottom of the sample 310 crosses both sides of the recess 324.
Further, in the subsequent thinning process, the ion beam thins both sides (i.e., the front side and the rear side) of the sample at the region to be measured of the sample, for example, as shown in fig. 8, in the image of fig. 8, the middle thinner region is the region to be measured of the sample. In some embodiments, the size of the pit on the supporting copper sheet is slightly larger than the area to be measured of the sample.
In some embodiments, the size of the pits is (5 to 12 microns) x (5 to 12) microns, for example, 8 microns x8 microns, or 10 microns x10 microns. In some embodiments, a suitable ion beam current, for example 60 to 70nA, is selected to sputter a pit in the supporting copper sheet prior to transferring the sample.
Thereafter, referring again to fig. 3, in step 140 of the method 100, the processed region of the sample is thinned with an ion beam. The thinning process of the sample may be divided into several stages, such as pre-thinning, coarse thinning, fine thinning, etc., to thin the sample to a thickness of less than 100 nanometers. In some embodiments, the front and back sides of the sample are treated separately at a processing voltage of 30 to 50KeV, for example a processing voltage of 40 KeV.
In some embodiments, when the sample is fixed by side edges to the supporting copper sheet, the ion beam is processed in a direction from top to bottom to thin the front side and the back side of the sample respectively when the thinning process is performed. Because the sample is far away from the bottom of the copper sheet, the ion beam cannot process the copper sheet when thinning, and the copper is prevented from being reversely deposited. Thus, contamination from the substrate supporting the copper sheet can be avoided. Fig. 6C shows an image of the sample of fig. 6B after thinning.
In other embodiments, when the sample is fixed on both sides of the pit for supporting the copper sheet, the area of the sample smaller than the width of the pit needs to be properly selected for thinning in the final thinning process when the sample is thinned by the ion beam. By controlling the processing depth of the ion beam and the tilting angle of the sample, the ion beam can not process the copper sheet. Or, the effect that the copper sheet is not processed by the ion beam can be realized by controlling the processing width during the thinning processing.
Thereafter, in step 150 of the method 100, a low voltage cleaning process is performed. Contamination due to irradiation damage is related to the acceleration voltage at which thinning is performed. Therefore, the irradiation damage pollution can be effectively eliminated by adding the low-voltage clearing treatment. In some embodiments, the low voltage cleaning process is performed at a tilt angle of ± (5 to 10 degrees), an acceleration voltage of 3 to 8KeV, a residence time of 1 to 10 microseconds, and a processing time of 30 seconds to 30 minutes. For example, in one embodiment, the sample is subjected to a 10 degree back and forth tilt, respectively, with the machine direction on one side from top to bottom and the machine direction on the other side from bottom to top, an acceleration voltage of 5KeV, a diaphragm aperture of 80 microns, a dwell time of 3 microseconds, and a machine time of 1 minute, and the front and back sides of the sample are subjected to low voltage cleaning, respectively.
Fig. 9A shows a high resolution image of a sample before a low voltage cleaning process. Fig. 9B shows a high resolution image of this sample after a low voltage cleaning process. The microstructure of the cleaned sample is clearer, which shows that the irradiation damage pollution is obviously reduced.
Fig. 10 is an image of a prepared sample, showing that the area to be measured of the sample has a complete structure and no deformation, and meets the sample requirements of the transmission electron microscope.
Embodiments of the present disclosure can effectively avoid the interference of contamination on the transmission electron microscope image, improve the quality of the prepared sample, realize the observation of atomic arrangement, and analyze the components on the nanometer scale, realize the analysis of transmission high resolution, diffraction, etc., and improve the accuracy of the component analysis, for example, as shown in the images of fig. 11 to 13F below.
Fig. 11 shows the results of diffraction analysis of the sample. It can be seen that the contamination due to sample preparation is reduced, thus obtaining a high quality sample, and then obtaining a clear high quality image.
Fig. 12 shows a high resolution analysis image of the sample. Because the pollution generated by sample preparation is reduced, a sample with high quality is obtained, and then a clear and high-quality image is obtained, so that the microstructure of the sample can be displayed.
Fig. 13A to 13F show analysis images of the composition profile of a sample, in which fig. 13A is a secondary electron image, fig. 13B is a titanium (Ti) profile image, fig. 13C is an aluminum (Al) profile image, fig. 13D is an oxygen (O) profile image, fig. 13E is a carbon (C) profile image, and fig. 13F is a nitrogen (N) profile image. Fig. 13A-13F show that the samples were sharp, free of noise caused by contamination of the substrate elements and reduced in the effects of irradiation damage.
In summary, the embodiments and examples of the disclosure control substrate contamination and irradiation damage contamination during sample preparation without reducing the sample preparation efficiency of the transmission electron microscope, thereby reducing interference and influence of contamination generated during sample preparation on images, effectively improving the quality of prepared samples, and meeting the requirement of high-precision analysis.
The above description is only exemplary of the preferred embodiment and examples of the present invention, and is not intended to limit the scope of the present invention, which is defined by the appended claims.

Claims (10)

1. A method for controlling contamination resulting from transmission electron microscope sample preparation, comprising:
depositing a protective layer above a preset sample area of an element to be detected;
cutting off the preset sample area to obtain a sample, wherein the sample is provided with an area to be detected;
transferring and fixing the sample to a supporting copper sheet, wherein the area to be measured of the sample is not in contact with the supporting copper sheet directly below;
thinning the region to be detected of the sample by using an ion beam; and
and carrying out low-voltage cleaning treatment on the area to be detected.
2. The method of claim 1, wherein the sample is transferred and fixed to the supporting copper sheet by:
and fixing one side edge of the sample on one side wall of the supporting copper sheet.
3. The method of claim 2, wherein the ion beam is directed from top to bottom in thinning the region of the sample to be measured with the ion beam.
4. The method of claim 1, wherein transferring and fixing the sample to a supporting copper plate comprises:
sputtering a pit on the supporting copper sheet by using an ion beam; and
and fixing two sides of the bottom of the sample on the supporting copper sheet respectively across the concave pits.
5. The method of claim 4, wherein the pits have a top-down length dimension of 5 to 12 microns and a top-down width dimension of 5 to 12 microns.
6. The method of claim 1, wherein said area of said sample to be measured is thinned by said ion beam, and said ion beam does not work into said supporting copper sheet.
7. The method of claim 1, wherein the low voltage cleaning process has an acceleration voltage of 3 to 8 KeV.
8. The method of claim 7, wherein the low voltage cleaning process is performed at a tilt angle of the sample of ± 5 degrees to ± 10 degrees.
9. The method of claim 7, wherein the low voltage cleaning is performed for a dwell time of 1 to 10 microseconds, a processing time of 30 seconds to 30 minutes, and a processing direction of either top-down or bottom-up.
10. The method of claim 1, wherein the protective layer is tungsten or carbon, and the protective layer has a thickness of 1 to 2 microns.
CN202010302229.6A 2020-04-16 2020-04-16 Method for controlling contamination resulting from transmission electron microscope sample preparation Pending CN111474197A (en)

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CN114166868A (en) * 2021-11-25 2022-03-11 中国科学院上海硅酸盐研究所 Preparation method of pollution-free electrode of transmission electron microscope in-situ electric field ultrathin sheet sample
CN114166868B (en) * 2021-11-25 2023-12-08 中国科学院上海硅酸盐研究所 Preparation method of pollution-free electrode for transmission electron microscope in-situ electric field ultrathin sample

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