CN116593266A - Method for preparing nano mechanical test sample by utilizing focused ion beam - Google Patents
Method for preparing nano mechanical test sample by utilizing focused ion beam Download PDFInfo
- Publication number
- CN116593266A CN116593266A CN202310374600.3A CN202310374600A CN116593266A CN 116593266 A CN116593266 A CN 116593266A CN 202310374600 A CN202310374600 A CN 202310374600A CN 116593266 A CN116593266 A CN 116593266A
- Authority
- CN
- China
- Prior art keywords
- ion beam
- focused ion
- sample
- substance
- detected
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000010884 ion-beam technique Methods 0.000 title claims abstract description 130
- 238000012360 testing method Methods 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000002243 precursor Substances 0.000 claims abstract description 44
- 238000005498 polishing Methods 0.000 claims abstract description 35
- 239000000126 substance Substances 0.000 claims description 112
- 238000005520 cutting process Methods 0.000 claims description 52
- 230000002093 peripheral effect Effects 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 26
- 238000000605 extraction Methods 0.000 claims description 11
- 230000006835 compression Effects 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 47
- 239000002689 soil Substances 0.000 description 14
- 238000012669 compression test Methods 0.000 description 13
- 238000007373 indentation Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 238000012545 processing Methods 0.000 description 9
- 238000010894 electron beam technology Methods 0.000 description 8
- 238000003466 welding Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- 210000000078 claw Anatomy 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000012798 spherical particle Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000012491 analyte Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The application relates to the technical field of nano mechanical testing, in particular to a method for preparing a nano mechanical test sample by utilizing a focused ion beam, which comprises the following steps: extracting a sample precursor from a region to be measured of an object to be measured by using a focused ion beam, wherein the sample precursor meets the following condition requirements: 1) Having opposed first and second surfaces; and 2) the surface area of the first surface is 100 μm 2 ～2500μm 2 The method comprises the steps of carrying out a first treatment on the surface of the And fixing the second surface on a sample bearing device, adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam, so that the focused ion beam bombards the first surface at an incident angle of 86-94 degrees to finish polishing, and preparing a nano mechanical test sample. The sample prepared by the method can be used for nano mechanical test.
Description
Technical Field
The application relates to the technical field of nano mechanical testing, in particular to a method for preparing a nano mechanical test sample by utilizing a focused ion beam.
Background
The nano mechanical test is a key technical means for obtaining the mechanical properties of the micro-nano area of the material. The nanoindentation instrument is widely applied to mechanical property tests (such as hardness, plasticity, toughness, elastic modulus, fatigue characteristics and the like) of micro-nano level areas (such as grains, interfaces, cracks, second phases and the like) on the surface of a material by virtue of extremely high load and displacement resolution.
Because the nano mechanical test of the micro-nano area of the material is carried out on the micro-nano scale, compared with the traditional mechanical test, the method has extremely high precision requirement, and the preparation of the sample suitable for the nano mechanical test has extremely high difficulty.
Disclosure of Invention
Based on the above, the application provides a method for preparing a nano mechanical test sample by utilizing a focused ion beam, which has the following technical scheme:
a method for preparing a nanomechanical test sample using a focused ion beam, comprising the steps of:
extracting a sample precursor from a region to be measured of an object to be measured by using a focused ion beam, wherein the sample precursor meets the following condition requirements: 1) Having opposed first and second surfaces; and 2) the area of the first surface is 100 μm 2 ～2500μm 2 ；
And fixing the second surface on a sample bearing device, adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam, so that the focused ion beam bombards the first surface at an incident angle of 86-94 degrees to finish polishing, and preparing a nano mechanical test sample.
In some of these embodiments, the polishing comprises a first polishing and a second polishing;
the first polishing includes the steps of: adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to first bombard the first surface at an incident angle of 88-92 degrees;
the second polishing includes the steps of: and adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to bombard the first surface at an incident angle of 86-94 degrees.
In some of these embodiments, the first bombarded ion beam voltage is 20 kV-30 kV and the ion beam current is 1.5 nA-12 nA; and/or the voltage of the ion beam of the second bombardment is 20 kV-30 kV, and the current of the ion beam is 80 pA-1.5 nA.
In some of these embodiments, the first surface is spaced from the second surface by a distance of 10 μm to 50 μm.
In some embodiments, the method for extracting a sample precursor from a region to be measured of the object using a focused ion beam comprises the steps of:
and determining a to-be-detected area of the to-be-detected object according to the requirement on the sample precursor, pre-cutting the to-be-detected area substance and the surrounding area substance by utilizing a focused ion beam, connecting the to-be-detected area substance by utilizing an extraction device, and completely cutting the to-be-detected area substance and the surrounding area substance by utilizing the focused ion beam to obtain the sample precursor.
In some embodiments, pre-cutting the substance of the area to be detected from the substance of the peripheral area comprises the steps of:
retaining the connection between a part of the side surface of the substance in the region to be detected and the substance in the peripheral region, and cutting the rest of the side surface and the substance in the peripheral region;
cutting the bottom of the substance in the region to be detected and the substances in the peripheral region;
and cutting the side surface of the to-be-detected area connected with the substances in the peripheral area and the substances in the peripheral area, and reserving the connection between the substances in the to-be-detected area and the substances in the peripheral area.
In some embodiments, the distance to be cut between one side bottom edge and the opposite side bottom edge of the bottom of the substance in the area to be detected is greater than 20 μm.
In some embodiments, the cutting the substance bottom of the region to be detected from the substance in the peripheral region includes the steps of:
taking the bottom edge of one side of the substance in the region to be detected as a starting line, cutting the substance from outside to inside for the second time by taking the bottom edge of the other opposite side as the starting line after the substance is cut from outside to inside for half the distance to be cut, and completely cutting off the connection between the bottom of the substance in the region to be detected and the substances in the peripheral region.
In some of these embodiments, the cut surfaces of the first outside-in cut and the second outside-in cut are the same or intersect.
In some of these embodiments, the test object satisfies one or more of the following conditions:
1) Is granular; and 2) amorphous material.
In some of these embodiments, after polishing, the method further comprises the steps of:
a microcolumn is processed on the first surface using the focused ion beam for microcolumn compression testing.
Compared with the traditional scheme, the application has the following beneficial effects:
the application prepares the sample precursor with larger first surface area, then bombards the first surface by utilizing the focused ion beam to finish polishing, in the process, the position relation between the first surface and the focused ion beam is particularly adjusted, and the application discovers that: when the focused ion beam bombards the first surface at an incident angle of 86-94 degrees, the polishing effect on the large-area first surface is achieved, the polished first surface can meet the requirement of higher flatness of the nano mechanical test, the micro column compression test and the nano indentation test can be carried out, and the nano mechanical test is completed. The preparation method of the nano mechanical test sample is suitable for amorphous particle to-be-tested substances with complex structures and larger component differences, and provides an effective method for nano mechanical test of the substances.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present application and to more fully understand the present application and its advantageous effects, the following brief description will be given with reference to the accompanying drawings, which are required to be used in the description of the embodiments. It is evident that the figures in the following description are only some embodiments of the application, from which other figures can be obtained without inventive effort for a person skilled in the art.
FIG. 1 is a practical operation diagram and schematic diagram of how to adjust the position of a sample carrier;
FIG. 2 is a scanning electron microscope image of a lunar soil particle sample of example 1;
FIG. 3 is a side view image of the substance in the area to be measured after precutting in example 1;
FIG. 4 is a top view of the pre-cut test area material of example 1;
FIG. 5 is an image of sample precursors lifted by a nanomachining arm in example 1;
FIG. 6 is an image of sample precursors transferred by a nanomachining arm onto an M-shaped gripper of a FIB-specific support network in example 1;
FIG. 7 is a side view image of a sample of the nanomechanical test of example 1;
FIG. 8 is a front view image of a sample of the nanomechanical test of example 1;
FIG. 9 is a front view of the sample after nanoindentation testing in example 1;
FIG. 10 is a front view of the sample before and after the microcolumn compression test of the experimental group in example 2;
fig. 11 is a front view of the sample before and after the microcolumn compression test of the control group in example 2.
Detailed Description
The present application will be described in further detail with reference to specific examples. The present application may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
Terminology
Unless otherwise indicated or contradicted, terms or phrases used herein have the following meanings:
in the present application, reference to "optional", "optional" refers to the presence or absence of the "optional" or "optional" means either of the "with" or "without" side-by-side arrangements. If multiple "alternatives" occur in a technical solution, if no particular description exists and there is no contradiction or mutual constraint, then each "alternative" is independent.
In the present application, references to "further", "still further", "particularly" and the like are used for descriptive purposes and indicate that the application is not to be interpreted as limiting the scope of the application.
In the application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present application, a numerical range (i.e., a numerical range) is referred to, and optional numerical distributions are considered to be continuous within the numerical range and include two numerical endpoints (i.e., a minimum value and a maximum value) of the numerical range and each numerical value between the two numerical endpoints unless otherwise specified. Where a numerical range merely refers to integers within the numerical range, including both end integers of the numerical range, and each integer between the two ends, unless otherwise indicated, each integer is recited herein as directly, such as where t is an integer selected from 1 to 10, and where t is any integer selected from the group of integers consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10. Further, when a plurality of range description features or characteristics are provided, these ranges may be combined. In other words, unless otherwise indicated, the ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In the present application, the incident angle refers to an angle between a beam current of the focused ion beam and a normal line of the first surface when the focused ion beam bombards the first surface.
The nano mechanical test for representing the mechanical properties of the micro-nano area of the material can be carried out according to different purposes by referring to the following two methods:
the first method is to process micro-nano area of the material into micro-column with certain size, to perform compression test of the micro-column, and to obtain the indexes of compressive strength, plastic deformation performance, shearing strength, etc. through the compression stress-strain curve.
The second method is to finely grind or polish the micro-nano area of the material, and perform nano indentation test to obtain indexes such as hardness, young modulus, plastic work, fracture toughness and the like.
The microcolumn compression test requires that the microcolumn outer surface processed by the micronano-scale region of the material is smooth and clean, no obvious crack or damage exists at the bottom of the microcolumn, and the microcolumn is prevented from being deformed or broken in advance during the compression test to obtain an abnormal result; the nano indentation test requires that the micro-nano level region of the material be finely ground or polished before the test, and aims to eliminate the influence of surface roughness on the nano indentation test result and reduce the discreteness of the test result. The preparation of the sample for the nano mechanical test has high precision requirement.
The focused ion beam is a micro-nano processing system which utilizes an electromagnetic lens to focus the ion beam into a very small size and has micro-cutting capability, and the cutting precision of the focused ion beam can reach 4nm at present. When the focused ion beam bombards the sample, its high density energy is transferred to atomic molecules in the sample, causing the sample to be cut by high energy sputtering.
One embodiment of the present application provides a method for preparing a nanomechanical test sample using a focused ion beam, comprising the steps of:
extracting a sample precursor from a region to be measured of an object to be measured by using a focused ion beam, wherein the sample precursor meets the following condition requirements: 1) Having opposed first and second surfaces; and 2) the surface area of the first surface is 100 μm 2 ～2500μm 2 ；
And fixing the second surface on a sample bearing device, adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam, so that the focused ion beam bombards the first surface at an incident angle of 86-94 degrees to finish polishing, and preparing a nano mechanical test sample.
In this embodiment, a sample precursor with a larger first surface area is prepared first, and then the first surface is bombarded by the focused ion beam to finish polishing, in this process, the positional relationship between the first surface and the focused ion beam is specifically adjusted, and through the research of the present application, it is found that: when the focused ion beam bombards the first surface at an incident angle of 86-94 degrees, the polishing effect on the large-area first surface is achieved, the polished first surface can meet the requirement of higher flatness of the nano mechanical test, the micro column compression test and the nano indentation test can be carried out, and the nano mechanical test is completed. The preparation method of the nano mechanical test sample is suitable for amorphous particle to-be-tested substances with complex structures and larger component differences, and provides an effective method for nano mechanical test of the substances.
It will be appreciated that the surface area of the first surface is 100 μm 2 、500μm 2 、1000μm 2 、1500μm 2 、2000μm 2 And 2500 μm 2 Any one of the two numerical end-point ranges including two numerical end-points.
Optionally, the object to be measured is in the form of particles. Further alternatively, the particle diameter of the particulate analyte is 20 μm to 90 μm. It will be appreciated that the test object may be a spherical particle, an ellipsoidal particle, a polyhedral particle, or other regular or irregular particle.
For micron-sized particles, it is generally difficult to prepare a sample for a microcolumn compression test, because the microcolumn compression test needs to process microcolumns with a certain size, the shape of the object to be tested is greatly influenced, and particularly, the arc-shaped surface at the bottom of the particle seriously influences the test precision and stability; it is also generally difficult to prepare nanoindentation test samples because it is difficult to obtain a flat surface from particles by conventional grinding and polishing. Therefore, for the to-be-measured object of the particles with the micron-sized particle, a method for effectively obtaining the nano-mechanical test sample thereof is lacking. However, by the method of this embodiment, particles are cut by the focused ion beam to obtain a cubic sample precursor, then the positional relationship between the focused ion beam and the surface to be measured is adjusted, and polishing of the surface to be measured is completed by bombardment of the focused ion beam, so that samples suitable for microcolumn compression tests and nanoindentation tests are prepared, and nanomechanical tests are performed.
Optionally, the distance between the first surface and the second surface is 10 μm to 50 μm. I.e. the column length of the microcolumn can reach 40 μm.
Optionally, the object to be measured is an amorphous material. It is understood that the analyte may be amorphous particles.
Generally, the components of each region in the amorphous material are complex and have large differences, the amorphous particle structure is complex, and the difficulty in preparing the nano mechanical test sample is relatively high, but the nano mechanical test sample of the object to be tested can be obtained by the method of the embodiment.
In some examples, the test object is lunar soil particles. The moon is subjected to impact action of meteorites for up to one hundred million years to melt, crush and lithology bedrock, and the outermost layer of the moon forms finely crushed lunar soil particles due to extreme conditions (such as extremely large temperature difference change, solar wind, cosmic ray radiation and the like) of the moon, and the moon contains rock fragments, meteorites, amorphous substances and abundant minerals, so that the moon is amorphous spherical particles, and the mechanical property research on the lunar soil amorphous spherical particles is helpful for revealing the mechanism of influence of space weathering on amorphous forming process and performance, and has important guiding significance for the preparation and synthesis of high-strength and high-stability amorphous materials. Generally, the lunar soil particles have low amorphous substance content, the mechanical properties of the lunar soil particles cannot be measured and analyzed by the conventional method, but the method of the embodiment can utilize the high resolution of the focused ion beam to select and cut the lunar soil particles to obtain an amorphous sample suitable for nano mechanical test, and then the amorphous sample is subjected to nano indentation test to obtain information such as modulus, hardness and the like.
In some examples, the object to be detected may be other particles such as metal particles, ceramic particles, amorphous glass particles, etc., and the method of the present embodiment has a wide application range, and is also applicable to particles of various forms, compositions, and structures.
Optionally, the method for extracting the sample precursor from the region to be measured of the object to be measured by using the focused ion beam comprises the following steps:
and determining a to-be-detected area of the to-be-detected object according to the requirement on the sample precursor, pre-cutting the to-be-detected area substance and the surrounding area substance by utilizing a focused ion beam, connecting the to-be-detected area substance by utilizing an extraction device, and completely cutting the to-be-detected area substance and the surrounding area substance by utilizing the focused ion beam to obtain the sample precursor.
It can be understood that the focused ion beam processing system according to this embodiment is an electron beam-ion beam dual beam combined system, and the target particles can be selected as the object under the electron beam window according to the size requirement of the sample precursor, and then the area to be measured on the object can be selected.
It will be appreciated that when the target particles cannot be morphologically observed and selected as the test object, the target particles can be selected as the test object according to the particle composition using the spectrometer. Optionally, the energy spectrum acquisition parameters are set as follows: the voltage of the electron beam is 20 kV-30 kV, the working distance is 3.5 mm-4.5 mm, and the effective characteristic X-ray photon counting rate is more than 10000cps.
According to the resistivity of the object to be measured, the area to be measured on the object to be measured is selected by the following two methods.
When the resistivity of the object to be detected is less than 450nΩ & m, under the condition that the electron beam voltage is 5 kV-30 kV under the electron beam window of the FIB-SEM dual-beam combined system, selecting target particles as the object to be detected by utilizing a secondary electron or back scattering mode, and selecting a region to be detected on the object to be detected.
When the resistivity of the sample is more than or equal to 450nΩ & m, the method further comprises the step of performing metal spraying treatment on the object to be detected, wherein after the metal spraying treatment, the secondary electron or back scattering mode is utilized to select the area to be detected of the sample under the condition that the voltage is 5 kV-30 kV under the electron beam window of the FIB-SEM double-beam system. Further alternatively, the thickness of the sprayed metal is 5nm to 50nm. The metal spraying aims to avoid the drift of a processing window in the preparation process of the nano mechanical test sample and influence the processing precision.
After determining the region to be detected of the object to be detected, pre-cutting the substance in the region to be detected and the substance in the peripheral region by utilizing the focused ion beam.
Optionally, pre-cutting the substance in the area to be detected from the substance in the peripheral area includes the following steps:
retaining the connection between a part of the side surface of the substance in the region to be detected and the substance in the peripheral region, and cutting the rest of the side surface and the substance in the peripheral region;
cutting the bottom of the substance in the region to be detected and the substances in the peripheral region;
and cutting the side surface of the to-be-detected area connected with the substances in the peripheral area and the substances in the peripheral area, and reserving the connection between the substances in the to-be-detected area and the substances in the peripheral area.
It can be understood that the remaining side surface of the substance in the area to be detected and the substance in the peripheral area can be vertically cut, and after pre-cutting, a cutting area similar to a concave shape can be formed in the overlooking direction, so that the stability of the sample can be improved, and the sample is prevented from shaking or collapsing when the bottom is subsequently cut.
Optionally, when the residual side surface of the substance in the region to be detected and the substance in the peripheral region are cut, the voltage of the ion beam is 20 kV-30 kV, and the current of the ion beam is 11 nA-80 nA.
Based on the dimensional requirements for the sample precursor, in some examples, the substance bottom side of the region to be detected is more than 20 μm away from the opposite side. At this time, the cutting distance is long.
When the cutting distance is longer, optionally, cutting and separating the substance bottom of the to-be-detected area from the substance of the peripheral area includes the following steps:
taking the bottom edge of one side of the substance in the region to be detected as a starting line, cutting the substance from outside to inside for the second time by taking the bottom edge of the other opposite side as the starting line after the substance is cut from outside to inside for half the distance to be cut, and completely cutting off the connection between the bottom of the substance in the region to be detected and the substances in the peripheral region.
Further alternatively, the cut surfaces of the first outside-in cut and the second outside-in cut are the same or intersect.
It will be appreciated that when the two cut surfaces are identical, the bottom is planar after cutting; when the two cutting surfaces intersect, the bottom is non-planar after cutting. In some examples, the first outside-in cut and the second outside-in cut are both oblique cuts, and after the cuts, the bottom is a wedge-shaped cross section.
Optionally, the voltage of the ion beam is 20 kV-30 kV, and the current of the ion beam is 1.5 nA-45 nA when the ion beam is cut from outside to inside for the first time and/or cut from outside to inside for the second time.
Optionally, when the last side surface of the substance in the area to be detected and the substance in the peripheral area are partially cut, the voltage of the ion beam is 20 kV-30 kV, and the current of the ion beam is 1.5 nA-45 nA.
After precutting, the material in the region to be measured and the material in the peripheral region remain small part of the connection without cutting off, and an L-shaped notch is formed when seen from one side.
And (3) contacting one end, far away from the connection with the peripheral area substances, of the substances in the area to be detected by using the extraction device, welding the extraction device and the substances in the area to be detected together by depositing welding materials, and then cutting off small part of connection between the substances in the area to be detected and the substances in the peripheral area by using a focused ion beam so as to completely cut the substances in the area to be detected and the substances in the peripheral area, thereby obtaining a sample precursor.
It will be appreciated that the extraction device may be a nanomachined arm.
Alternatively, the ion beam voltage is 15 kV-30 kV and the ion beam current is 77 pA-280 pA when the welding material is deposited.
Alternatively, the welding material is Pt or C.
The two opposing sides of the sample precursor obtained in this embodiment may be referred to as a first surface and a second surface, respectively, and in some examples, the side remaining in the precut described above is referred to as the second surface and the side opposite thereto is referred to as the first surface.
The sample precursor is slowly lifted by the extraction device, then the second surface of the sample precursor is used as a contact surface, the sample precursor is transferred to the sample bearing device, the welding material is deposited on the contact surface of the second surface and the sample bearing device, and the sample precursor is fixed on the sample bearing device.
It will be appreciated that the central axis of the extraction device (nanomachining arm) may be rotated 180 ° in order to transfer the sample precursor onto the sample carrier device with the second surface of the sample precursor as the contact surface.
Optionally, the sample carrying device is an M-shaped claw of a FIB specific support mesh.
Alternatively, the ion beam voltage is 15 kV-30 kV and the ion beam current is 77 pA-280 pA when the welding material is deposited.
It will be appreciated that after the sample precursor is secured to the sample carrier means, the extraction means is separated from the sample precursor by means of an ion beam and the extraction means is removed.
Alternatively, when the extraction device and the sample precursor are separated by an ion beam, the voltage of the ion beam is 20 kV-30 kV, and the current of the ion beam is 1.5 nA-12 nA.
Connecting a sample bearing device carrying a sample precursor to a sample stage, adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam, so that the focused ion beam bombards the first surface at an incident angle of 86-94 degrees, and polishing is finished to prepare a nano mechanical test sample.
Unlike the thinning of small area sample, the focusing ion beam may be utilized to polish large area sample after the incident angle between the focusing ion beam and the first surface is regulated, and the surface roughness of the large area first surface is lowered under the condition of small thickness variation.
Optionally, the polishing comprises a first polishing and a second polishing;
the first polishing includes the steps of: adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to first bombard the first surface at an incident angle of 88-92 degrees;
the second polishing includes the steps of: and adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to bombard the first surface at an incident angle of 86-94 degrees.
The first polishing is favorable for removing a damaged layer on the surface of the sample precursor, which is caused by cutting by a high-current ion beam; the second polishing is advantageous for further improving the surface flatness.
Further alternatively, the first bombarded ion beam voltage is 20 kV-30 kV and the ion beam current is 1.5 nA-12 nA.
Further alternatively, the second bombarded ion beam voltage is 20 kV-30 kV and the ion beam current is 80 pA-1.5 nA.
In some examples, based on the limitations of the sample stage rotation angle, the position of the sample carrier device may be adjusted by:
referring to fig. 1, a sample stage carrying a FIB-specific support net is taken out of a FIB system, the FIB-specific support net is adjusted from a horizontal position to a vertical position so that the plane of the FIB-specific support net is perpendicular to the plane of the sample stage, then the sample stage is put into the FIB system again, and the position of the FIB-specific support net is adjusted by adjusting the tilting angle of the sample stage. It will be appreciated that when the FIB specific support grid is placed horizontally on the sample stage, the FIB specific support grid cannot achieve the desired tilt angle (e.g. approximately parallel to the direction of the ion beam) under rotation of the sample stage due to the limitations of the rotation angle of the sample stage, whereas when the FIB specific support grid is placed vertically on the sample stage, the FIB specific support grid can achieve the desired tilt angle (e.g. approximately parallel to the direction of the ion beam) under rotation of the sample stage.
In this embodiment, the focused ion beam is used to select and cut the area to be measured of the object to be measured, so as to obtain a sample suitable for the nano mechanical test, the sample with a smooth and clean surface can be obtained by the method, and the sample carrying device are fastened and welded together, so that the subsequent microcolumn compression test/nano indentation test can be smoothly performed.
It will be appreciated that after polishing, the sample can be used directly for nanoindentation testing.
When the sample is subjected to a microcolumn compression test, the polishing method further comprises the following steps:
a microcolumn is processed on the first surface using the focused ion beam for microcolumn compression testing.
Alternatively, when a microcolumn is machined on the first surface using a focused ion beam, the voltage of the ion beam is 20kV to 30kV and the current of the ion beam is 80pA to 45nA.
The method of the embodiment has high precision and high efficiency, is a novel preparation method for preparing the nano mechanical test sample, and enables the mechanical property test and analysis of particles with various shapes and complex components to be possible.
The following examples are further offered to illustrate, but not to limit, the materials used in the examples are commercially available, and the equipment used is commercially available, and the processes involved are routinely selected by those skilled in the art without any specific description.
Example 1 preparation of nanomechanical test samples of lunar soil samples
Referring to fig. 2 to 9, the present embodiment provides a method for preparing a nano mechanical test sample of lunar soil particles by using a focused ion beam, comprising the following steps:
1. selection of particles to be detected
The lunar soil particle sample is placed on a sample table, under the condition that the electron beam voltage is 5kV under the condition that the electron beam window of a FIB-SEM dual-beam combined system (the inclination angle of the sample table is 0 DEG), spherical amorphous particles in the lunar soil particle sample are selected as objects to be detected by utilizing a secondary electron mode, and referring to FIG. 2, the lunar soil particle sample is a scanning electron microscope image, the middle spherical particles are the objects to be detected, the areas to be detected on the objects to be detected are determined, and the lunar soil particle sample is from the five classes of the Chang E.
2. Pre-cutting of particles to be detected
Tilting the sample stage to be opposite to the direction of the ion beam (the tilt angle of the sample stage is 54 degrees), and under the conditions that the voltage of the ion beam is 30kV and the current is 45nA, vertically cutting three sides of a substance in a region to be detected and the substance in a peripheral region by utilizing the ion beam, and reserving the connection between the last side and the substance in the peripheral region; tilting the sample table to be opposite to the electron beam direction (the tilt angle of the sample table is 0 °), at this moment, the distance to be cut between the bottom edge of one side of the bottom of the substance in the region to be detected and the bottom edge of the opposite side is 28 μm, under the conditions that the ion beam voltage is 30kV and the current is 12nA, taking the bottom edge of one side of the substance in the region to be detected as a starting line, rotating the lunar soil particle sample by 180 degrees to turn to the bottom edge of the opposite side after the first time of cutting from outside to inside to half the distance to be cut, taking the bottom edge of the other side as the starting line, cutting from outside to inside to the second time of cutting until the connection between the bottom of the substance in the region to be detected and the substance in the region below is completely cut, and taking the bottom as a wedge-shaped section after cutting; and then under the conditions that the ion beam voltage is 30kV and the current is 12nA, the last side face of the substance in the region to be detected and the substance in the peripheral region are partially cut, the connection between the last side face of the substance in the region to be detected and the substance in the peripheral region is reserved, see fig. 3 and 4, fig. 3 is a side view of the substance in the region to be detected after precutting, an L-shaped notch is formed in the cutting region of the bottom and the last side face, fig. 4 is a top view of the substance in the region to be detected after precutting, and the cutting regions of the three side faces are formed into concave-shaped notches. And the distance to be cut between the bottom edge of one side of the bottom of the substance in the area to be detected and the bottom edge of the opposite side is 28 mu m, and the bottom is a wedge-shaped section after cutting.
3. Transfer and immobilization of sample precursors
And (3) moving the nano manipulator to one end, far away from the last side, of the substances in the to-be-detected area, contacting the end, under the conditions that the ion beam voltage is 30kV and the current is 80pA, welding the nano manipulator and the substances to be detected together by depositing Pt, and then cutting off a small part of connection between the last side of the substances in the to-be-detected area and the substances in the peripheral area under the conditions that the ion beam voltage is 30kV and the current is 12nA, so that the substances in the to-be-detected area and the substances in the peripheral area are completely cut, and obtaining a sample precursor, see FIG. 5.
Slowly lift the manipulator together with the sample, rotate the manipulator 180 ° around its central axis so as to have the last side as the final sideA second surface, which is brought into contact with an M-shaped claw of a FIB-specific support net which is also placed on a sample stage, and Pt is deposited at the contact position of the second surface and the M-shaped claw of the support net under the conditions that the voltage of the ion beam is 30kV and the current is 80pA, a sample precursor is fixed on the M-shaped claw, then the ion beam is used for cutting and separating the manipulator and the sample precursor under the conditions that the voltage is 30kV and the current is 1.5nA, and then the manipulator is slowly removed, wherein the surface of the sample precursor opposite to the second surface is taken as a first surface, the first surface and the second surface are parallel, the distance between the first surface and the second surface is 14.7 mu M, and the surface area of the first surface is 900 mu M 2 。
4. Surface polishing of sample precursors
And taking out the sample table carrying the FIB special supporting net from the FIB system, adjusting the FIB special supporting net from horizontal placement to vertical placement, enabling the plane of the FIB special supporting net to be perpendicular to the plane of the sample table, and then putting the sample table carrying the FIB special supporting net into the FIB system again.
And adjusting the tilting angle of the sample stage to enable the focused ion beam to bombard the first surface at an incident angle of 88 degrees, wherein the voltage of the first bombarded ion beam is 30kV, the current is 12nA so as to finish the first polishing, removing a damaged layer on the surface of the sample precursor, which is caused by cutting by the heavy current ion beam, and then adjusting the tilting angle of the sample stage to enable the focused ion beam to bombard the first surface at an incident angle of 86 degrees, wherein the voltage of the second bombarded ion beam is 30kV, the current is 280pA so as to finish the second polishing, further improving the surface flatness, and obtaining a sample suitable for nano mechanical testing, wherein a side view image is shown in fig. 7, a front view image is shown in fig. 8, and a dotted line elliptical area in fig. 8 is a nano mechanical testing area.
Nanoindentation test was performed in the above test area, and the result is shown in fig. 9. The indentation morphology rule is visible from the indentation amplification part, and compared with fig. 8, the sample is free from shaking, collapse and damage after the nanoindentation test, so that the nanomechanical test sample obtained by the method can be suitable for the nanoindentation test.
Example 2 preparation of nanomechanical test sample of lithium Battery cathode particles
Experimental group: the experimental group is basically the same as example 1, except that the test object is lithium battery positive electrode particles, and after step four, step five is added, and step one to step four of the experimental group refer to step one to step four of example 1, and step five is as follows:
5. microcolumn processing
Tilting the sample table to be opposite to the direction of the ion beam (the tilt angle of the sample table is 54 ℃), processing an annular pit on the polished first surface under the conditions of the ion beam voltage of 30kV and the current of 12nA, and processing the middle convex part of the annular pit into a microcolumn under the conditions of the ion beam voltage of 30kV and the current of 1.5nA to obtain a sample suitable for nano mechanical test. As shown in FIG. 10, the front view of the sample after micro-column processing shows that the micro-columns are regular and have small size difference at different height positions, and the outer surface is smooth and has no cracks.
With continued reference to fig. 10, it can be seen that typical slip fracture occurs after the microcolumn is compressed, and no abnormal collapse occurs in the whole sample, which indicates that the nano mechanical test sample obtained by the method can be applied to microcolumn compression test.
Control group: and the control group is the same as the experimental group in the lithium battery anode particles, the first to fourth steps are not performed, the fifth step of the experimental group is directly referred to, a pit reserved with a microcolumn is processed on the surface of the particles, a sample suitable for nano mechanical test is obtained, and a front view image of the sample after the microcolumn processing is shown in fig. 11.
As can be seen from the continued reference to fig. 11, the bottom of the particle is curved and cannot be in uniform contact with the underlying support material, so that the stress of the particle cannot be uniformly transferred to the underlying support material when the microcolumn is compressed, and the particle is caused to collapse due to rollover and abnormal breakage of the microcolumn. Therefore, the granular sample cannot be directly processed into microcolumns for nano mechanical test.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the application, which are described in detail and are not to be construed as limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (11)
1. A method for preparing a nano-mechanical test sample by using a focused ion beam, comprising the following steps:
extracting a sample precursor from a region to be measured of an object to be measured by using a focused ion beam, wherein the sample precursor meets the following condition requirements: 1) Having opposed first and second surfaces; and 2) the surface area of the first surface is 100 μm 2 ～2500μm 2 ；
And fixing the second surface on a sample bearing device, adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam, so that the focused ion beam bombards the first surface at an incident angle of 86-94 degrees to finish polishing, and preparing a nano mechanical test sample.
2. The method of preparing a nanomechanical test sample using a focused ion beam of claim 1, wherein the polishing comprises a first polishing and a second polishing;
the first polishing includes the steps of: adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to first bombard the first surface at an incident angle of 88-92 degrees;
the second polishing includes the steps of: and adjusting the position of the sample bearing device and/or the emission angle of the focused ion beam to enable the focused ion beam to bombard the first surface at an incident angle of 86-94 degrees.
3. The method of preparing a nanomechanical test sample using a focused ion beam of claim 2, wherein the first bombarded ion beam voltage is 20 kV-30 kV and the ion beam current is 1.5 nA-12 nA; and/or the voltage of the ion beam of the second bombardment is 20 kV-30 kV, and the current of the ion beam is 80 pA-1.5 nA.
4. A method of preparing a nanomechanical test sample using a focused ion beam according to any one of claims 1-3, wherein the distance between the first surface and the second surface is 10 μιη to 50 μιη.
5. A method of preparing a nanomechanical test sample using a focused ion beam according to any one of claims 1 to 3, wherein the method of extracting a sample precursor from a region of interest of the test object using a focused ion beam comprises the steps of:
and determining a to-be-detected area of the to-be-detected object according to the requirement on the sample precursor, pre-cutting the to-be-detected area substance and the surrounding area substance by utilizing a focused ion beam, connecting the to-be-detected area substance by utilizing an extraction device, and completely cutting the to-be-detected area substance and the surrounding area substance by utilizing the focused ion beam to obtain the sample precursor.
6. The method of preparing a nanomechanical test sample using a focused ion beam of claim 5, wherein pre-cutting the material of the region to be detected from the material of the surrounding region comprises the steps of:
retaining the connection between a part of the side surface of the substance in the region to be detected and the substance in the peripheral region, and cutting the rest of the side surface and the substance in the peripheral region;
cutting the bottom of the substance in the region to be detected and the substances in the peripheral region;
and cutting the side surface of the to-be-detected area connected with the substances in the peripheral area and the substances in the peripheral area, and reserving the connection between the substances in the to-be-detected area and the substances in the peripheral area.
7. The method of preparing a nanomechanical test sample using a focused ion beam according to claim 6, wherein the distance to be cut of one side bottom edge and the opposite side bottom edge of the bottom of the substance in the region to be detected is greater than 20 μm.
8. The method of preparing a nanomechanical test sample using a focused ion beam of claim 7, wherein the cutting of the bottom of the substance of the region to be detected from the substance of the surrounding region comprises the steps of:
taking the bottom edge of one side of the substance in the region to be detected as a starting line, cutting the substance from outside to inside for the second time by taking the bottom edge of the other opposite side as the starting line after the substance is cut from outside to inside for half the distance to be cut, and completely cutting off the connection between the bottom of the substance in the region to be detected and the substances in the peripheral region.
9. The method of preparing a nanomechanical test sample using a focused ion beam of claim 8, wherein the cut surfaces of the first outside-in cut and the second outside-in cut are the same or intersect.
10. The method of preparing a nanomechanical test sample using a focused ion beam according to any one of claims 1-3, 6-9, wherein the test object satisfies one or more of the following conditions:
1) Is granular; and 2) amorphous material.
11. The method for preparing a nano-mechanical test sample using a focused ion beam according to any one of claims 1 to 3 and 6 to 9, further comprising the steps of, after polishing:
a microcolumn is processed on the first surface using the focused ion beam for microcolumn compression testing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310374600.3A CN116593266A (en) | 2023-04-10 | 2023-04-10 | Method for preparing nano mechanical test sample by utilizing focused ion beam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310374600.3A CN116593266A (en) | 2023-04-10 | 2023-04-10 | Method for preparing nano mechanical test sample by utilizing focused ion beam |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116593266A true CN116593266A (en) | 2023-08-15 |
Family
ID=87588821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310374600.3A Pending CN116593266A (en) | 2023-04-10 | 2023-04-10 | Method for preparing nano mechanical test sample by utilizing focused ion beam |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116593266A (en) |
-
2023
- 2023-04-10 CN CN202310374600.3A patent/CN116593266A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Inkson | Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) for materials characterization | |
| Holzer et al. | Review of FIB-tomography | |
| Giannuzzi et al. | A review of focused ion beam milling techniques for TEM specimen preparation | |
| Bach | Application of ion sputtering in preparing glasses and their surface layers for electron microscope investigations | |
| NL2025431B1 (en) | Method for Preparing Multiple TEM Thin Slice Samples from Micron-sized Single Particle In Situ | |
| Tokitani et al. | Plasma wall interaction in long-pulse helium discharge in LHD–Microscopic modification of the wall surface and its impact on particle balance and impurity generation | |
| Moreau et al. | A Transmission Electron Microscopy Study of Silica and Kerogen Biosignatures in ̃1. 9 Ga Gunflint Microfossils | |
| Lombardo et al. | Focused ion beam preparation of samples for X-ray nanotomography | |
| O'connor et al. | The amorphous character and particle size distributions of powders produced with the Micronizing Mill for quantitative x‐ray powder diffractometry | |
| Abuhaikal | Nano-chemomechanical assessment of rice husk ash cement by wavelength dispersive spectroscopy and nanoindentation | |
| Frazer et al. | Evaluation of the mechanical properties of TRISO particles using nanoindentation and ring compression testing | |
| Santos et al. | Application of advanced (S) TEM methods for the study of nanostructured porous functional surfaces: A few working examples | |
| CN116593266A (en) | Method for preparing nano mechanical test sample by utilizing focused ion beam | |
| Baryakhtar et al. | Radiation damages and self-sputtering of high-radioactive dielectrics: spontaneous emission of submicronic dust particles | |
| Hyde et al. | Microstructural and isotopic analysis of shocked monazite from the Hiawatha impact structure: development of porosity and its utility in dating impact craters | |
| CN112649624A (en) | Preparation method of planar TEM sample | |
| CN112730006B (en) | Preparation method of pore surface ion channel contrast sample | |
| Plitzko et al. | Deposition-free Cryo-FIB Lift-out Transfer for Cryo-Electron Tomography Specimen Preparation | |
| Montone et al. | A new method for preparing powders for transmission electron microscopy examination | |
| Dunzik-Gougar et al. | Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles | |
| CN116735316A (en) | Method for preparing transmission electron microscope sample by utilizing focused ion beam | |
| Heikinheimo et al. | Towards high-fidelity fuel pellet fracture modelling in current and new fuel designs | |
| McDonald | An evaluation of the mechanical properties and microstructure in uranium dioxide doped with oxide additives | |
| CN114518375A (en) | Method for preparing low-order lignite HRTEM thin slice sample based on focused ion beam | |
| Robertson | Impact of ion irradiation damage on SiC and ZrN mechanical properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |