CN108760438B - Preparation method of in-situ mechanical tensile sample of transmission electron microscope - Google Patents
Preparation method of in-situ mechanical tensile sample of transmission electron microscope Download PDFInfo
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- CN108760438B CN108760438B CN201810788822.9A CN201810788822A CN108760438B CN 108760438 B CN108760438 B CN 108760438B CN 201810788822 A CN201810788822 A CN 201810788822A CN 108760438 B CN108760438 B CN 108760438B
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 29
- 230000005540 biological transmission Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 56
- 239000010410 layer Substances 0.000 claims abstract description 18
- 238000002474 experimental method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 238000005520 cutting process Methods 0.000 claims abstract description 9
- 239000011241 protective layer Substances 0.000 claims abstract description 8
- 238000009966 trimming Methods 0.000 claims abstract description 6
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 238000007735 ion beam assisted deposition Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000005464 sample preparation method Methods 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 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
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A preparation method of a transmission electron microscope in-situ mechanical tensile sample comprises the steps of tilting a sample platform by 54 degrees in a focused ion beam system, depositing a Pt protective layer on a part to be cut of the sample, removing materials around the part to be cut of the sample by using an ion beam of 4nA to form a micron sheet, trimming the micron sheet by using the ion beam, tilting the sample platform by 28-38 degrees, welding the micron sheet on a manipulator on a stretching device, tilting the sample platform by-18-5 degrees, cutting the micron sheet into an I shape by using an ion beam of 2nA, enabling the middle part of the micron sheet to be 0.5-3.5 microns in width, depositing a Pt layer by using the ion beam, then thinning the micron sheet by using the ion beam to enable the thickness of the micron sheet to be 50-150nm, and carrying out an in-situ tensile experiment on the sample in the transmission electron microscope. The invention provides a preparation method of a transmission electron microscope in-situ mechanical tensile sample, which realizes the sample preparation of a transmission electron microscope in-situ mechanical tensile experiment of a block material.
Description
Technical Field
The invention relates to a preparation method of a transmission electron microscope in-situ mechanical tensile sample, in particular to a block material in-situ mechanical tensile test, and belongs to the technical field of transmission electron microscope in-situ nanometer mechanical test.
Background
In the aerospace and defense industries, high-performance equipment achieves service performance through high-performance parts, and the aerospace field also requires lightweight and miniaturization of parts. The mechanical and photoelectric properties of the parts can be reduced by a damaged layer generated by stress induction in the mechanical processing process of the parts, for example, the electrical properties of the devices can be reduced by an amorphous layer and a crystal damaged layer generated in the ultra-precision grinding process of a silicon wafer, and along with the development of miniaturization, the damaged layer plays an extremely important role in influencing the properties of the micro devices. Therefore, it is necessary to develop a new machining process and a new machining apparatus, to reduce the thickness of a damaged layer generated during machining, and to understand the mechanism of formation of the damaged layer is the basis for developing the new process and the new apparatus. Transmission electron microscope in-situ nano mechanics is an important method for researching a damaged layer forming mechanism, can be used for observing the deformation of a stress induction material and the damage forming and evolution processes in a transmission electron microscope in real time, and can be used for carrying out nano-scale control on displacement.
In-situ nano-mechanical research of a transmission electron microscope requires that the thickness of a sample is about 100nm, and the in-situ nano-mechanical research is divided into in-situ indentation, in-situ compression and in-situ stretching according to the loading mode of the sample. In-situ indentation experiments require small radius of curvature of the pressing pin, and a very thin sample is pressed by the extremely small pressing pin, so that the experiment difficulty is very high, and the stress analysis is also very difficult; in the in-situ compression experiment, the sample is bent before reaching the stress limit of the sample in the compression process, so that the sample is difficult to control; in the in-situ tensile experiment, because the axial tensile force is applied to the sample, the stress direction of the sample is not changed before the tensile stress limit is reached, but the difficulty of the in-situ tensile experiment of the transmission electron microscope is that the sample is difficult to prepare, the thickness of the sample is required to be about 100nm, and two ends of the sample are required to be fixed.
Disclosure of Invention
The invention adopts the focused ion beam to cut, transfer, fix and thin the sample, and realizes the sample preparation of the bulk material transmission electron microscope in-situ nanometer mechanical tensile experiment.
The technical scheme of the invention is as follows:
a preparation method of a transmission electron microscope in-situ mechanical tensile sample comprises the steps of tilting a sample platform by 54 degrees in a focused ion beam system, depositing a Pt protective layer on a part to be cut of the sample, removing materials around the part to be cut of the sample by using an ion beam of 4nA to form a micron sheet with the length of 8-12 mu m, the depth of 8-12 mu m and the thickness of 1.5-2.5 mu m, trimming the micron sheet by using an ion beam of 600pA-2nA, tilting the sample platform by 28-38 degrees, welding the micron sheet on a manipulator on a stretching device, tilting the sample platform by-18 to 5 degrees, cutting the micron sheet into an I shape by using an ion beam of 2nA, depositing a Pt layer with the thickness of 200-600nm by using the ion beam, then thinning the micron sheet by using an ion beam of 20-120pA to reduce the thickness of the micron sheet to 50-150nm, in-situ tensile experiments were performed on the samples in a transmission electron microscope. The invention provides a preparation method of a transmission electron microscope in-situ mechanical tensile sample, which realizes the sample preparation of a transmission electron microscope in-situ mechanical tensile experiment of a block material.
The sample is a block material with the length of 10 mu m-20mm, the width of 10 mu m-20mm and the height of 4 mu m-4 mm. Because the distance between the two ends of the sample fixed by the stretching device is 1.5-3 μm, the sample to be cut must be large enough, the length, the width and the height are required to be not less than 10 μm and not less than 4 μm, and the sample cannot be too large due to the limitation of a sample chamber of a focused ion beam system.
Fixing the sample on a horizontal sample table by using conductive adhesive, and fixing the stretching device on a 45-degree sample table by using the conductive adhesive. The focused ion beam system requires the sample to be conductive, so the sample is fixed by conductive adhesive, the sample is fixed on a horizontal sample table, and a stretching device is fixed on a 45-degree sample table, so that the sample is conveniently cut, transferred, fixed and thinned.
And (3) tilting the sample platform by 54 degrees in a focused ion beam system, and depositing a Pt protective layer on the part to be cut of the sample with the thickness of 200-600 nm. Because the included angle between the ion beam direction and the normal direction of the horizontal sample table is 54 degrees, the sample table should be tilted by 54 degrees, the damage of the ion beam to the sample in the cutting and thinning processes can be reduced by the protective layer, and the common protective layer is Pt which has stable chemical property.
And removing materials around the part to be cut of the sample by using an ion beam of 4nA to form a micron sheet with the length of 8-12 microns, the depth of 8-12 microns and the thickness of 1.5-2.5 microns. 4nA ion beam can bombard and remove sample materials with high efficiency, and the micro-sheet is too large or too thin and is easy to bend, so that the micro-sheet with the length of 8-12 mu m, the width of 8-12 mu m and the thickness of 1.5-2.5 mu m is selected.
Trimming the micron sheet by using an ion beam of 600pA-2nA, and compensating the sample platform by 1.5-2.5 degrees along the tilting direction. After cutting by using an ion beam of 4nA, a damaged layer is formed on the surface of the micron sheet, the surface of the micron sheet needs to be trimmed by using an ion beam of 600pA-2nA, and the ion beam needs to be tilted by 1.5-2.5 degrees for compensation because the ion beam has a convergence angle.
And (3) rotating the sample platform by 5-10 degrees, welding the micrometer sheet on a manipulator by using ion beam assisted deposition, cutting the micrometer sheet by using 600pA-2nA ion beams, and separating the micrometer sheet from the sample substrate. The tilting of the sample platform by 5-10 degrees is beneficial to observing and cutting the micron sheet in an ion beam mode, the ion beam of 600pA-2nA has small damage to the micron sheet, and the micron sheet can be cut off.
The sample stage is tilted by 9 degrees, and a layer of Pt with the thickness of 0.6-1.0 μm is deposited at the sample fixing position of the stretching device. Because the stretching device is fixed on the 45-degree sample platform, after the sample platform is tilted by 9 degrees, the normal direction of the stretching device is consistent with the ion beam direction, and a layer of Pt with the thickness of 0.6-1.0 μm is deposited at the sample fixing position of the stretching device, thereby being beneficial to thinning the welded sample.
And (3) rotating the sample platform by 28-38 degrees, and welding the micrometer sheet on the manipulator on the stretching device. The sample platform is tilted by 28-38 degrees, so that the micrometer sheet is parallel to the fixed position of the sample of the stretching device, and the welding of the micrometer sheet is convenient.
The sample platform is tilted to-18 to 5 degrees, the micrometer sheet is cut into an I shape by using an ion beam of 2nA, and the width of the middle part of the micrometer sheet is 0.5 to 3.5 mu m. The sample stage is tilted to-18 to 5 degrees, the ion beam direction can be perpendicular to the surface of the micrometer sheet, the micrometer sheet is cut into an I shape, the stress of the middle part of the micrometer sheet is maximum when the micrometer sheet is pulled, and the change characteristic of the micrometer sheet is most obvious in the stretching state.
The sample platform is horizontally rotated by 180 degrees, then is tilted by 8-18 degrees, a 200-600nm thick Pt layer is deposited by ion beams, then the micrometer sheet is thinned by using 20-120pA ion beams, the sample platform compensates for 1.5-2.5 degrees along the tilting direction during thinning, and the thickness of the micrometer sheet is thinned to 50-150 nm. The sample stage is rotated 180 degrees and then tilted 8-18 degrees, so that the micron sheet is parallel to the direction of the ion beam, the ion beam is favorable for thinning the micron sheet, a layer of Pt with the thickness of 200-600nm is deposited by the ion beam, then the ion beam with the thickness of 20-120pA is used for thinning the micron sheet, the damage of the ion beam to a sample in the thinning process can be reduced, the ion beam has a convergence angle, the ion beam needs to be tilted 1.5-2.5 degrees for compensation, the thickness of the micron sheet is 50-150nm, and the microstructure of the micron sheet can be observed under a transmission electron microscope.
Fixing the stretching device on a sample rod of a transmission electron microscope in-situ mechanical system, and carrying out in-situ stretching experiment on the sample in the transmission electron microscope.
The invention has the advantages that the focused ion beam system is adopted to cut, transfer, fix and thin the sample, thereby realizing the sample preparation of the transmission electron microscope in-situ nanometer mechanical tensile experiment.
Drawings
FIG. 1 is a top view of a scanning electron microscope after thinning a sample.
FIG. 2 is a front view of a scanning electron microscope after thinning a sample.
Detailed Description
The following further describes the specific embodiments of the present invention in combination with the technical solutions.
Examples
The sample is a nickel-based alloy block material, and the distance between the sample fixing positions of the stretching device is 2.3 mu m; fixing the sample and the stretching device on a horizontal sample table and a 45-degree sample table respectively by using conductive adhesives, tilting the sample table by 54 degrees in a focused ion beam system, and depositing a Pt protective layer with the thickness of 600nm on the part to be cut of the sample. Cutting the sample surface with 4nA ion beam to form micrometer pieces with length of 12 μm, depth of 10 μm and thickness of 2 μm; trimming the micrometer sheet by using 600pA ion beams, compensating the sample platform for 2 degrees along the tilting direction during trimming, tilting the sample platform for 10 degrees, welding the micrometer sheet on a manipulator by using ion beam assisted deposition, and cutting the micrometer sheet by using 2nA ion beams to separate the micrometer sheet from a sample substrate; tilting the sample platform by 9 degrees, and depositing a layer of Pt at the position of the stretching device where the sample is to be fixed, wherein the thickness of the Pt is 0.9 mu m; the sample platform is tilted by 33 degrees, and two ends of the micrometer sheet are welded on the stretching device; the sample platform is tilted to 0 degree, the micrometer sheet is cut into an I shape by using 2nA ion beams, and the width of the middle part of the micrometer sheet is 3 micrometers; the sample platform horizontally rotates 180 degrees, then turns 13 degrees, firstly uses ion beams to deposit a layer of Pt with the thickness of 600nm, then uses 120pA, 60pA and 20pA ion beams to thin the micrometer piece in sequence, the sample platform compensates 2 degrees along the turning direction when the micrometer piece is thinned, and finally the thickness of the micrometer piece is thinned to 86 nm.
Claims (1)
1. The utility model provides a tensile sample preparation method of transmission electron microscope normal position mechanics, cuts, shifts, fixes, attenuate to the sample with focused ion beam, carries out tensile experiment to the sample under the transmission electron microscope which characterized in that:
(1) the sample is a block material, the length is 10 mu m-20mm, the width is 10 mu m-20mm, and the height is 4 mu m-4 mm;
(2) fixing a sample on a horizontal sample table by using conductive adhesive, and fixing a stretching device on a 45-degree sample table by using the conductive adhesive;
(3) tilting the sample platform by 54 degrees in a focused ion beam system, and depositing a Pt protective layer on the part to be cut of the sample, wherein the thickness of the Pt protective layer is 200-600 nm;
(4) removing materials around a part to be cut of the sample by using 4nA ion beams to form a micron sheet with the length of 8-12 mu m, the depth of 8-12 mu m and the thickness of 1.5-2.5 mu m;
(5) trimming the micron sheet by using 600pA-2nA ion beams, and compensating the sample platform for 1.5-2.5 degrees along the tilting direction;
(6) the sample platform is tilted by 5-10 degrees, the micron sheet is welded on a manipulator by ion beam assisted deposition, the micron sheet is cut off by 600pA-2nA ion beams, and the micron sheet is separated from the sample substrate;
(7) tilting the sample platform by 9 degrees, and depositing a layer of Pt at the sample fixing position of the stretching device, wherein the thickness of the Pt is 0.6-1.0 mu m;
(8) the sample platform is tilted by 28-38 degrees, and the micron sheet on the manipulator is welded on the stretching device;
(9) the sample platform is tilted to-18-5 degrees, a 2nA ion beam is used for cutting the micrometer sheet into an I shape, and the width of the middle part of the micrometer sheet is 0.5-3.5 micrometers;
(10) horizontally rotating a sample table for 180 degrees, then tilting for 8-18 degrees, depositing a Pt layer with the thickness of 200-600nm by using an ion beam, then thinning the micrometer sheet by using an ion beam with the thickness of 20-120pA, compensating for 1.5-2.5 degrees along the tilting direction of the sample table during thinning, and thinning the micrometer sheet to 50-150 nm;
(11) fixing the stretching device on a sample rod of a transmission electron microscope in-situ mechanical system, and carrying out in-situ stretching experiment on the sample in the transmission electron microscope.
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| CN108760438B true CN108760438B (en) | 2020-08-14 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110057851B (en) * | 2019-05-17 | 2020-05-19 | 中国科学院地球化学研究所 | Method for in-situ preparation of micron-sized single-particle multiple TEM slice samples |
| CN112067405B (en) * | 2020-10-10 | 2022-12-23 | 南京南智先进光电集成技术研究院有限公司 | Preparation method of plane TEM sample and plane TEM sample |
| CN113125475B (en) * | 2021-03-19 | 2022-04-01 | 复旦大学 | Method for in-situ stress application in transmission electron microscope |
| CN114166588A (en) * | 2021-10-14 | 2022-03-11 | 浙江大学杭州国际科创中心 | Sample preparation method for in-situ tensile experiment of transmission electron microscope |
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