CN111474196B - Method for controlling deformation generated by sample preparation of transmission electron microscope - Google Patents
Method for controlling deformation generated by sample preparation of transmission electron microscope Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 74
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 201000009310 astigmatism Diseases 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
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Classifications
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- 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
- G01N23/20—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 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
-
- 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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/04—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 transmitting the radiation through the material and forming images of the material
-
- 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
- G01N23/20—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 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
-
- 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
- G01N23/20—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 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
Abstract
The present disclosure relates to preparation of electron microscope samples, and provides a method for controlling deformation generated by preparation of transmission electron microscope samples, comprising: providing a focused ion beam based system for obtaining a sample of electronic components disposed on a substrate; performing pre-thinning treatment to thin the electronic element sample to a first thickness of 1.3-1.7 microns; thinning the electronic element sample to a second thickness by a tilting angle and a first diaphragm hole, wherein the tilting angle is (+/-) (0.5-1.5 degrees), and the second thickness is 700-900 nanometers; a second thinning process of thinning the electronic component sample to a third thickness of 250 to 350 nm at the tilting angle and at the second diaphragm aperture; and a third thinning process of thinning the electronic component sample to a fourth thickness of 100 nm or less at the tilting angle and at the third diaphragm aperture; wherein the first aperture is larger than the second aperture, and the second aperture is larger than the third aperture.
Description
Technical Field
The disclosure relates to the technical field of transmission electron microscope sample preparation, and in particular relates to a method for controlling sample deformation of an electronic element sample in a sample preparation and thinning process.
Background
Transmission Electron Microscope (TEM) samples typically need to be thinned below 100 nanometers (nm), and today the most convenient and efficient method of preparation is by focused ion beam system (FIB) cutting to give flakes. In a focused ion beam system, a high-energy gallium ion beam is accelerated to reach the surface of a sample at each stage of magnetic lenses under the drive of accelerating voltage, and the incident ions exchange energy with surface atoms, so that the cutting function is achieved. The sample needs to be thinned on two sides, and finally a thin sample with the thickness smaller than 100 nanometers is obtained.
However, during the preparation of a transmission electron microscope sample, the sample is very subject to deformation with a gradual decrease in sample thinness. For example, referring to FIG. 1, there is shown a deformation of a sample during sample preparation, resulting in a hole in the sample; referring to FIG. 2, the sample is shown deformed during the sample preparation process, resulting in cracking of the sample; and referring to fig. 3, a transmission electron microscope image of a deformed sample is shown, and damage to the microstructure of the sample is observed. Therefore, the deformation can affect the structure of the sample, and also affect the focusing of the sample during observation by a transmission electron microscope, thereby seriously affecting the quality of sample preparation and the efficiency of sample preparation.
In a conventional method for thinning a sample of a transmission electron microscope, for example, when the thickness of the sample is about 1.5 micrometers (um), the sample is thinned by tilting the sample by 2 degrees, two sides (i.e., front side and rear side) of the sample are thinned to about 1 micrometer, two sides are thinned to about 600 nanometers by tilting the sample by 1.5 degrees, two sides are thinned to about 300 nanometers by tilting the sample by 1 degree, and then the tilting angle is changed to 0.5 degree for final thinning, so as to obtain a thin sample of the transmission electron microscope with the thickness smaller than 100 nanometers.
However, although the above-mentioned conventional method can obtain a large effective observation area, i.e., an area with a thickness of less than 100 nm in the sample, the requirement for the technical skill of the tester is high, and the probability of deformation of the prepared thin sample is high and the failure rate is also high. Fig. 4 shows a top view of a sample from a sample preparation process in which the sample is thinned in an angle-decreasing manner, showing that the sample has serious deformation. It is clear that the known methods of preparing a sample for a perspective electron microscope are not ideal.
Disclosure of Invention
In order to solve the problem that the sample of the transmission electron microscope is easy to deform during preparation, the probability of deformation of the sample is reduced by fixing the tilting angle during thinning treatment.
The present disclosure provides a method for controlling deformation generated by sample preparation of a transmission electron microscope, comprising: providing a focused ion beam based system for obtaining a sample of electronic components disposed on a substrate; performing pre-thinning treatment to thin the electronic element sample to a first thickness of 1.3-1.7 microns; thinning the electronic element sample to a second thickness by a tilting angle and a first diaphragm hole, wherein the tilting angle is (+/-) (0.5-1.5 degrees), and the second thickness is 700-900 nanometers; a second thinning process of thinning the electronic component sample to a third thickness of 250 to 350 nm at the tilting angle and at the second diaphragm aperture; and a third thinning process of thinning the electronic component sample to a fourth thickness of 100 nm or less at the tilting angle and at the third diaphragm aperture; wherein the first aperture is larger than the second aperture, and the second aperture is larger than the third aperture.
The technical scheme of the disclosure has the beneficial effects that the deformation probability of the sample is reduced, and the efficiency and the success rate of sample preparation are effectively improved.
Drawings
Aspects of the disclosure may be best understood from the following detailed description when read with the accompanying drawing figures. It is noted that according to common practice in the industry, the 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. 1 is an image of a sample prepared in a conventional sample preparation manner.
FIG. 2 is an image of a sample prepared in a conventional sample preparation manner.
FIG. 3 is an image of a sample prepared in a conventional sample preparation manner.
FIG. 4 is a top view of a sample during preparation in a conventional sample preparation manner.
Fig. 5 is a flow chart of a method of preparing a sample of transmissive electronic elements, according to some embodiments of the present disclosure.
Fig. 6 is a further flowchart of step S100 of fig. 5, according to some embodiments of the present disclosure.
Fig. 7A is a schematic diagram of an electronic component sample secured to a copper sheet according to some embodiments of the present disclosure.
FIG. 7B is an image of an electronic device sample mounted on a copper sheet according to one embodiment of the present disclosure.
Fig. 8A-8D are schematic illustrations of different steps of a method of preparing a sample of a transmissive electronic component, according to some embodiments of the present disclosure.
FIG. 9 is a schematic view of tilt angles for low voltage cleaning of a sample, according to some embodiments of the present disclosure.
Fig. 10 is an image of a sample prepared according to some embodiments of the present disclosure.
Fig. 11 is an image of a sample prepared, wherein the tilt angle of the fixed sample is 0.5 degrees during the thinning process, according to some embodiments of the present disclosure.
Fig. 12 is an image of a sample prepared, wherein the tilt angle of the fixed sample is 0.8 degrees during the thinning process, according to some embodiments of the present disclosure.
Fig. 13 is an image of a sample prepared according to some embodiments of the present disclosure, wherein the tilt angle of the fixed sample is 1 degree during the thinning process.
Fig. 14 is an image of a sample prepared, wherein the tilt angle of the fixed sample is 1.3 degrees during the thinning process, according to some embodiments of the present disclosure.
Fig. 15 is an image of a sample prepared according to some embodiments of the present disclosure, wherein the tilt angle of the fixed sample is 1.5 degrees during the thinning process.
Symbol description
10 method of
102 sample
104 copper sheet
106 tungsten weld
108 area to be analyzed
D1 first thickness
D2 second thickness
D3 third thickness
D4 fourth thickness
S100 step
S102, step
S104, step
S106, step
S108, step
S200, step
S300 step
S400 step
S500 step
S600 step
S700 step
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, while indicating the present disclosure, are intended for purposes of illustration only and are not intended to limit the scope of the claims.
Referring to fig. 5, a flow chart of a method of preparing a sample for a transmission electron microscope is shown, according to some embodiments.
In step S100 of the method 10, a sample of electronic components disposed on a substrate based on a focused ion beam system is provided.
In some embodiments, as shown in fig. 6, the step S100 may specifically include the following steps S102 to S108.
In step S102, an initial sample of electronic components is provided, which may be a sample comprising semiconductor, glass, flexible material, metal/ceramic, etc.
In step S104, the initial sample is made into a sample sheet, and the sample sheet is subjected to surface pretreatment to obtain a sample to be treated for later use. In some embodiments, the sample may be formed into a 1 cm x1 cm pellet, mounted on a sample stage, surface gold plated for 30 seconds to 90 seconds, such as 40 seconds or 60 seconds, before the sample is introduced into the device sample compartment. Specifically, the sample sheet was fixed to the sample stage using a double-sided carbon conduction voltage.
In step S106, a focused ion beam system aperture astigmatism correction is performed. And adjusting instrument parameters to optimize the resolution of focused ion beam imaging and the astigmatic correction of the diaphragm aperture. Specifically, for better processing, astigmatic X/Y electrical centering is performed on 5 diaphragm apertures of 550 microns, 300 microns, 150 microns, 80 microns, and 30 microns, using acceleration voltages of 20KeV to 40KeV, for example 25KeV, 30KeV, or 35 KeV.
In step S108, the sample to be processed prepared in step S104 is processed by using a focused ion beam system to prepare a sample of electronic components disposed on a substrate (e.g., copper sheet). In some embodiments, the acquired sample is fixed to a copper sheet, such as a copper mesh dedicated to focused ion beam sampling. Fig. 7A is a schematic view of the electronic component sample being fixed to the copper sheet, and the electronic component sample 102 being fixed to the copper sheet 104 by soldering. Fig. 7B shows an image of an electronic component sample secured to a copper sheet according to one embodiment.
Referring to fig. 5, in step S200 of the method 10, a non-sample area on the substrate is selected to adjust the electron beam, the aperture, and the astigmatism in the focused ion beam system to a predetermined state. In some embodiments, inactive areas (non-sample areas) on the copper sheet are selected for electron beam electrical centering, diaphragm electrical centering, astigmatic X/Y electrical centering at low voltages, followed by diaphragm Kong Duijiao. In some embodiments, the acceleration voltage for aperture focusing is 20KeV to 40KeV, such as 25KeV, 30KeV, or 35KeV, and 3 aperture apertures of 150 microns, 80 microns, and 30 microns are astigmatic X/Y electrically centered.
In step S300 of method 10, the sample is pre-thinned to a first thickness. In the pre-thinning process, the sample is treated with the ion beam on both sides (i.e., the front and back sides of the sample) separately without tilting the sample at an angle. Fig. 8A shows a schematic diagram of pre-thinning of a sample, sample 102, secured to copper sheet 104 via tungsten weld 106. The region 108 to be analyzed in the sample 102 is pre-thinned to a first thickness D1. In some embodiments, the acceleration voltage is 20KeV to 40KeV, such as 25KeV, 30KeV, or 35KeV, the aperture is 150 microns, and the dwell time is set to 3 microseconds. The first thickness D1 is about 1.3 microns to about 1.7 microns, for example 1.5 microns.
And then, the sample tilting angle of the pre-thinning is set to be proper parameters according to the sample requirement, and the sample is thinned in stages. In some embodiments, to increase the sample preparation efficiency, a 20KeV to 40KeV acceleration voltage (e.g., 20, 30, 40KeV acceleration voltage) is used in combination with a series of parameters, including different aperture selection, dwell time, and processing time, to perform the transmission electron microscope sample thinning in stages.
In step S400 of the method 10, a first thinning process is performed to thin the sample to a second thickness at a tilting angle of ± (0.5 degrees to 1.5 degrees) and the first diaphragm aperture. Fig. 8B is a schematic diagram showing the sample subjected to the first thinning process, and the region to be analyzed 108 in the sample 102 is thinned to a second thickness D2. In some embodiments, the second thickness D2 is 700 nanometers to 900 nanometers, for example 800 nanometers. In some embodiments, the dwell time of the focused ion beam for the first thinning process is 3 microseconds to 10 microseconds, e.g., 3 microseconds.
In step S500 of the method 10, a second thinning process is performed to thin the sample to a third thickness at a fixed tilting angle and a second diaphragm. Fig. 8C is a schematic diagram showing the sample subjected to the second thinning process. The region 108 to be analyzed in the sample 102 is thinned to a third thickness D3. In this step, the tilting angle of the sample is the same as that of step S400, i.e., the tilting angle of the sample is not changed. In some embodiments, the third thickness D3 is 250 nanometers to 350 nanometers, e.g., 300 nanometers. In some embodiments, the dwell time of the focused ion beam for the second thinning process is 3 microseconds to 10 microseconds, e.g., 3 microseconds.
In step S600 of the method 10, a third thinning process is performed to thin the sample to a fourth thickness at a fixed tilting angle and a third diaphragm. Fig. 8D is a schematic diagram showing the sample subjected to the third thinning process. The region 108 to be analyzed in the sample 102 is thinned to a fourth thickness D4. In this step, the tilting angle of the sample is the same as that of step S400 and step S500, i.e., the tilting angle of the sample is not changed. In some embodiments, the fourth thickness D4 is less than or equal to 100 nanometers, such as 50 nanometers, 60 nanometers, 70 nanometers, 80 nanometers, 90 nanometers, or 100 nanometers. In some embodiments, the dwell time of the focused ion beam for the third thinning process is 3 microseconds to 10 microseconds, e.g., 3 microseconds.
Fig. 8D is a schematic diagram showing the sample subjected to the third thinning. And (3) thinning the electronic element sample to a fourth thickness D4 by setting the residence time and the processing time at a fixed tilting angle and the third diaphragm hole. In some embodiments, the fourth thickness is less than or equal to 100 nanometers, such as 50 nanometers, 60 nanometers, 70 nanometers, 80 nanometers, 90 nanometers, or 100 nanometers.
In step S700 of the method 10, the thinned electronic component sample is subjected to a low voltage cleaning process to reduce irradiation damage of the electronic component sample. In the process of processing and thinning the area to be analyzed of the sample by utilizing gallium ions, the gallium ions under high-speed voltage are very easy to generate irradiation damage to the surface of the sample or deposit reversely and adhere to the surface of the sample, so that the analysis of the nano structure of the sample is difficult. By cleaning the surfaces on both sides of the thinned sample with low voltage, the irradiation damage layer on the surface of the sample can be reduced or even eliminated.
FIG. 9 is a schematic view showing the tilting angle of the sample for the low voltage cleaning process. First, the sample is tilted at a first angle a, and one surface of the sample 102 is processed at a low acceleration voltage, for example, in an upward (∈) direction. Then the sample is tilted by a second angle b, the other side of the sample 102 is processed with the same lower acceleration voltage, the processing direction is for example downward (∈). The second angle a is different from the first angle b in direction but has the same tilting angle value.
In some embodiments, the acceleration voltage of the low voltage cleaning process is 2 to 5KeV, the first angle a is (+/-) (5 to 12 degrees), the second angle b is (+/-) (5 to 12 degrees), the residence time of the focused ion beam is 1 microsecond to 10 microseconds, and the processing time is 30 seconds to 3 minutes. Preferably, the low voltage cleaning parameters are acceleration voltage of 5KeV, aperture of 80 microns, residence time of 3 microseconds, tilting angle of plus or minus 10 degrees and processing time of 2 minutes.
After the low voltage cleaning process is completed, the sample is prepared, and the structure of the sample can be observed by a perspective electron microscope.
Fig. 10 shows a top view of a thinned sample at a fixed tilt angle, showing that the sample is not significantly deformed, and therefore the deformation is substantially negligible.
More specifically, in step S400 to step S600, a suitable tilting angle may be selected according to the size of the area to be analyzed of the electronic device, and the thinning process may be sequentially performed.
Preferably, if the width of the area to be analyzed of the electronic component sample is less than 3 μm, a fixed tilting angle of 0.5 degrees to 0.6 degrees is selected for thinning, for example, 0.5 degrees, or 0.6 degrees. Fig. 11 shows a sample made by thinning at a fixed tilt angle of 0.5 degrees, showing that the sample is not significantly deformed, and thus the resulting effective viewing area meets the requirements of a transmission electron microscope.
Preferably, if the width of the area to be analyzed of the electronic component sample is 3 to 5 μm, a fixed tilting angle of 0.7 degrees to 0.9 degrees is selected for thinning, for example, 0.7 degrees, 0.8 degrees, or 0.9 degrees. Fig. 12 shows a sample made by thinning at a fixed tilt angle of 0.8 degrees, showing that the sample is not significantly deformed, and thus the resulting effective viewing area meets the requirements of a transmission electron microscope.
Preferably, if the width of the area to be analyzed of the electronic component sample is 5 to 8 μm, a fixed tilting angle of 0.9 degrees to 1.1 degrees is selected for thinning, for example, 0.9 degrees, 1 degree, or 1.1 degrees. Fig. 13 shows a sample made by thinning at a fixed tilt angle of 1 degree, showing that the sample is not significantly deformed, and thus the effective viewing area is in line with the requirements of a transmission electron microscope.
Preferably, if the width of the area to be analyzed of the electronic component sample is 8 to 12 μm, a fixed tilting angle of 1.2 degrees to 1.4 degrees is selected for thinning, for example 1.2 degrees, 1.3 degrees, or 1.4 degrees. Fig. 14 shows a sample made by thinning at a fixed tilt angle of 1.3 degrees, showing that the sample is not significantly deformed, and thus the resulting effective viewing area meets the requirements of a transmission electron microscope.
Preferably, if the width of the area to be analyzed of the electronic component sample is 12 to 15 μm, a fixed tilting angle of 1.4 degrees to 1.5 degrees is selected for thinning, for example, 1.4 degrees or 1.5 degrees. Fig. 15 shows a sample made by thinning at a fixed tilt angle of 1.5 degrees, showing that the sample is not significantly deformed, and thus the resulting effective viewing area meets the requirements of a transmission electron microscope.
In order to make the above-mentioned parameter debugging and analysis method of the present disclosure more comprehensible, the following detailed description of the specific operation method of the present disclosure is given with reference to the embodiments.
The preparation in the early stage is to start the focused ion beam system in advance to stabilize the instrument state for 30 minutes, avoid current fluctuation generated in the sample preparation of a transmission electron microscope and influence the sample preparation effect, and in the embodiment, a silicon wafer is selected as a test sample.
Preparing a test sample, namely preparing the test sample into a size of 1 cm x1 cm, placing the test sample on a non-magnetic metal sample table, fixing the test sample on the sample table by utilizing double-sided carbon conductive adhesive, placing the test sample in a gold plating machine for sputtering for 40 seconds, and placing the test sample in a sample cabinet for standby.
And (3) sample injection: after the focused ion beam system is stable, the sample stage is arranged on the object stage, and the sample to be detected is sent into the sample chamber for observation through the sample injection rod.
And (3) preparing a transmission electron microscope sample, namely opening a transmission electron microscope sample preparation program, focusing a diaphragm Kong Zhuge in the program, moving a program pattern to an analysis position to start processing, and obtaining a pattern with a tungsten layer plated on the surface layer with a certain thickness. The sample table is rotated for 58 degrees, a processing program set is opened, a diaphragm hole is set to 300 microns, processing and cutting are conducted on the bottom of the pattern, and only the left side is connected with the sample main body to achieve a fixing effect. And (3) feeding a sampling needle, moving the sampling needle and contacting the right surface of the pattern, and welding and fixing the sampling needle and the sample by adopting a tungsten deposition method. The diaphragm aperture was switched to 150 microns, the left side of the analysis area was cut off, the sampling needle was lifted to remove the sample block, the sampling needle was withdrawn and the sample stage was repositioned.
And (3) placing a clean copper sheet on the sample rod, fixing the copper sheet, selecting a position where a sample is to be placed after the sample rod enters the sample bin, moving the sample to the middle of the screen, feeding a sampling needle (carrying the sample), placing the sample on the copper sheet, and welding and fixing the bottom edge of the sample and the copper sheet by adopting a tungsten deposition method. Cutting off the sampling needle to separate the sampling needle from the sample, and withdrawing the sampling needle; the 150 micron, 80 micron, and 30 micron diaphragms Kong Zhuge are refocused.
Pre-thinning treatment the sample was pre-thinned on both sides (i.e., front and back sides) using a processing voltage of 40KeV and a diaphragm aperture of 150 microns to thin the sample to about 1.5 microns.
After the first thinning process, the sample tilting angle was set to 1 degree, and the sample was thinned back and forth to about 800 nm using a processing voltage of 40KeV and a diaphragm aperture of 150 μm.
A second thinning process followed by thinning the sample back and forth to about 300 nanometers using a processing voltage of 40KeV and a stop aperture of 80 microns.
And thirdly, thinning the sample back and forth to be less than 100 nanometers by using a processing voltage of 40KeV and a diaphragm hole of 30 micrometers.
The low-voltage cleaning treatment, namely, selecting an accelerating voltage of 5KeV and a diaphragm aperture of 80 microns, carrying out electron beam electric centering, diaphragm electric centering and astigmatic X/Y electric centering under low voltage, then tilting the thinned sample to +10 DEG, wherein the retention time (Dwell time) is 3 microseconds (us), the processing time is 2 minutes, the processing direction is +.C (upward), the processing area is set to be slightly larger than the effective observation area, and processing is started after the setting is completed; subsequently, the thinned sample was tilted to-10 degrees, the retention time was 3 μs, the processing time was 2 minutes, the processing direction was +.sup.i (downward), and the processing was started after the completion of the setting.
And then the sample preparation is completed, the sample rod is withdrawn, and the copper sheet is taken down for observation by a transmission electron microscope.
In summary, the embodiments and examples of the present disclosure adopt a fixed angle thinning method without reducing the preparation efficiency of a transmission electron microscope sample, and a suitable tilting angle is selected to thin the sample, so as to reduce deformation of the sample in the sample preparation process, further eliminate interference and influence of the deformation of the sample on the analysis result of the nanostructure, effectively improve quality of the prepared sample, and meet the requirement of high-precision analysis.
The foregoing description of the preferred embodiments and examples of the invention is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (9)
1. A method for controlling deformation produced by transmission electron microscope sample preparation, comprising:
step S100, obtaining an electronic element sample arranged on a substrate based on a focused ion beam system, wherein the electronic element sample is manufactured to be 1 cm x1 cm, the surface of the electronic element sample is plated with gold for 30 seconds to 90 seconds, and the electronic element sample is fixed on a sample stage by using a double-sided carbon conduction voltage;
step 200, performing astigmatic correction on the diaphragm aperture of the focused ion beam system, which comprises the following steps:
using acceleration voltages of 25KeV, 30KeV and 35KeV to carry out astigmatism correction on diaphragm holes of 550 microns, 300 microns, 150 microns, 80 microns and 30 microns;
step S300, performing a pre-thinning process to thin the electronic component sample to a first thickness, wherein the first thickness is 1.5 μm,
the pre-thinning treatment uses a processing voltage of 40KeV and a diaphragm hole of 150 micrometers to pre-thin two sides of the electronic element sample, wherein the two sides are a front side and a rear side;
step S400, a first thinning process, in which the electronic component sample is thinned to a second thickness at a tilting angle of + -0.5 degrees to 1.5 degrees and at a first diaphragm aperture, wherein the second thickness is 800 nanometers, wherein the first thinning process uses a processing voltage of 40KeV and a diaphragm aperture of 150 micrometers to thin the electronic component sample back and forth,
step S500, a second thinning process for thinning the electronic component sample to a third thickness of 300 nm at the same tilting angle as the first thinning process and at a second aperture, wherein the second thinning process uses a processing voltage of 40KeV and an aperture of 80 μm to thin the electronic component sample back and forth, and
step S600, thinning the electronic element sample to a fourth thickness which is less than or equal to 100 nanometers at the same tilting angle as the first thinning process and at a third diaphragm aperture, wherein the third thinning process uses a processing voltage of 40KeV and a diaphragm aperture of 30 micrometers to thin the electronic element sample back and forth;
wherein the electronic component sample of the steps S400 to S600 has a region to be analyzed having a width,
when the width of the area to be analyzed is less than 3 micrometers, the tilting angle is 0.5 degrees to 0.6 degrees;
when the width of the region to be analyzed is 3 to 5 micrometers, the tilting angle is 0.7 degrees to 0.9 degrees;
when the width of the region to be analyzed is 5 to 8 micrometers, the tilting angle is 0.9 degrees to 1.1 degrees;
when the width of the region to be analyzed is 8 to 12 micrometers, the tilting angle is 1.2 degrees to 1.3 degrees;
when the width of the region to be analyzed is 12 to 15 micrometers, the tilting angle is 1.4 degrees to 1.5 degrees;
step S700, a low voltage cleaning process, wherein,
selecting an acceleration voltage of 5KeV and a diaphragm aperture of 80 microns, performing electron beam electric centering, diaphragm electric centering and astigmatic X/Y electric centering under low voltage, then tilting the thinned electronic element sample to +10 DEG, keeping for 3 microseconds, processing for 2 minutes, setting the processing direction to be upward, setting the processing area to be slightly larger than the effective observation area, and starting processing after setting is completed; and then tilting the thinned electronic component sample to-10 ℃, wherein the retention time is 3 microseconds, the processing time is 2 minutes, the processing direction is downward, and the processing is started after the setting is completed.
2. The method of claim 1, wherein the first aperture is 150 microns, the second aperture is 80 microns, and the third aperture is 30 microns.
3. The method of claim 1, wherein an acceleration voltage of the first thinning, the second thinning, and the third thinning is 20 to 40KeV.
4. The method of claim 1, further comprising a low voltage cleaning process after the third thinning process to accelerate the voltage by 2KeV to 5 KeV.
5. The method for controlling deformation of a sample preparation for a transmission electron microscope according to claim 4, wherein the aperture of the low voltage cleaning process is 80 μm, and wherein the tilting angle of the sample for electronic components is + -5 degrees to 12 degrees.
6. The method for controlling distortion produced by a sample preparation of a transmission electron microscope of claim 1, wherein the pre-thinning aperture is 150 microns.
7. The method for controlling deformation of a sample preparation for a transmission electron microscope according to claim 1, wherein the pre-thinning process comprises:
and (3) not tilting the angle of the electronic element sample, and thinning the two sides of the electronic element sample.
8. The method of controlling distortion in a transmission electron microscope sample preparation according to claim 1, wherein the ion beam residence time of the pre-thinning process is 3 microseconds to 10 microseconds.
9. The method of controlling distortion produced by a sample preparation of a transmission electron microscope of claim 1, wherein the ion beam residence time of the first thinning process, the second thinning process, and the third thinning process is 3 microseconds to 10 microseconds.
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