CN109015157B - Pre-thinning device for metal sample and pre-thinning method for metal sample - Google Patents
Pre-thinning device for metal sample and pre-thinning method for metal sample Download PDFInfo
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- CN109015157B CN109015157B CN201810539441.7A CN201810539441A CN109015157B CN 109015157 B CN109015157 B CN 109015157B CN 201810539441 A CN201810539441 A CN 201810539441A CN 109015157 B CN109015157 B CN 109015157B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/10—Single-purpose machines or devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B55/00—Safety devices for grinding or polishing machines; Accessories fitted to grinding or polishing machines for keeping tools or parts of the machine in good working condition
- B24B55/02—Equipment for cooling the grinding surfaces, e.g. devices for feeding coolant
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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
- G01N23/02—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
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Abstract
The invention relates to the technical field of thinning of Transmission Electron Microscope (TEM) samples. The pre-thinning device for the metal sample comprises a base body and a replacing part which are matched with each other. The pre-thinning method comprises the following steps: cleaning and drying the metal sheet to be thinned, and attaching the large lower bottom surface of the replacement part to the surface of the metal opposite to the surface to be thinned; the combination of the replacement part and the metal sheet is embedded with the matrix in a twisting manner, after water is injected through the through hole of the matrix, the surface to be thinned of the metal sheet is thinned by utilizing a friction mechanism which moves relative to the metal sheet; after thinning by 0.05 +/-0.02 mm each time, detaching the combination of the replacement part and the metal sheet and heating the combination to 200 +/-20 ℃ for melting; and selecting a new replacement part, taking the opposite side surface of the to-be-thinned surface of the metal sheet as a new thinned surface, and repeating the steps until the thickness is less than or equal to 0.05 mm. The TEM metal sample thinning method provided by the invention can facilitate the clamping of the sample to be thinned while thinning the metal sample, reduce the possibility of the fracture of the disassembled metal sheet and flatten the surface of the metal sample.
Description
Technical Field
The invention relates to the technical field of sample thinning of Transmission Electron Microscopes (TEM), in particular to a cheap and environment-friendly pre-thinning device and method for manually preparing metal samples of TEM (TEM) by using a 3D printing material laboratory.
Background
Transmission Electron Microscopy (TEM), a Transmission Electron Microscope, projects an accelerated and focused beam of electrons onto a very thin sample, where the electrons collide with atoms in the sample and change direction, thereby producing solid angle scattering. The size of the scattering angle is related to the density and thickness of the sample, so that images with different light and shade can be formed. Generally, the resolution of a transmission electron microscope is 0.1 to 0.2nm, and the magnification is several tens of thousands to millions of times, and the transmission electron microscope is used for observing an ultra-microstructure, i.e., a structure which is smaller than 0.2 μm and cannot be seen clearly under an optical microscope, and is also called a sub-microstructure. Transmission electron microscopes are used in many applications in material science and biology. Because electrons are easy to scatter or be absorbed by an object, the penetrating power is low, the density, the thickness and the like of a sample can influence the final imaging quality, and a thinner ultrathin slice is required to be prepared, wherein the thickness is usually 50-100 nm. The sample to be observed with the transmission electron microscope needs to be processed thinly.
The following requirements are made for a sample to be tested in accordance with the inspection requirements of a transmission electron microscope: 1. the samples were sufficiently thin (10-200 nm). 2. Providing a representative field of view to be viewed. 3. The structure and composition of the sample cannot be changed (e.g., mechanical damage, chemical reaction, tissue transformation). 4. Meets the requirement of vacuum environment, has certain conductivity, can endure the irradiation of electron beams, and the like.
Metal samples for transmission electron microscopy typically have the following processing sequence: 1. wire cutting-preparing a thin sheet with a thickness of about 0.20-0.30 mm. 2. Mechanical grinding and thinning: the sheet was ground to about 100 μm with metallographic sandpaper, but was not too thin to prevent damage to the sheet. 3. Chemical polishing pre-thinning, namely thinning the central area of the wafer to about 50 mu m from one side or two sides of the wafer; a disk having a diameter of 3mm was cut out from the sheet. 4. And final thinning by double-spraying electrolysis (polishing liquid: 10% perchloric acid alcohol solution; sample is refined by acetone or absolute alcohol).
For many colleges and laboratories, TEM is not a common detection means, so data are usually obtained by sending the data to a detection center for detection. Meanwhile, most detection centers cannot provide manufacturing service for an excessively thick metal sample because the manufacturing period of the metal sample is too long, and therefore the sample needs to be pre-thinned by themselves. The problems of difficult clamping and difficult fixing release are easily caused by the pre-thinning of the metal sheet, so the invention solves the problems.
PLA (polylactic acid), which is often used for 3D printing, is a new bio-based and renewable biodegradable material, made using starch raw materials proposed by renewable plant resources (such as corn). The starch raw material is saccharified to obtain glucose, the glucose and certain strains are fermented to prepare high-purity lactic acid, and the polylactic acid with certain molecular weight is synthesized by a chemical synthesis method. The development of PLA has resulted from the large-scale popularization of FDM type 3D printers, the price of which has been reduced to 40 rmb/kg from $ 1000/kg, and which is good in heat exposure, high in strength, stable in performance, appropriate and stable in melting temperature range, environmentally friendly, and has good biodegradability, and the atmosphere is good (faint fragrance) when heated. And are therefore increasingly used throughout the plastics sector. And thus is used as a 3D additive material in the present invention.
Disclosure of Invention
The invention aims to provide a cheap and environment-friendly pre-thinning device and method for manually preparing a Transmission Electron Microscope (TEM) metal sample by using a 3D printing material laboratory, which are used for solving the problems of difficult clamping and difficult fixing release during pre-thinning of a metal sheet.
The invention provides a pre-thinning device for a metal sample, which is characterized by comprising a base body and a plurality of replacing parts; the water injection hole is formed in the center of the top of the base body, the water storage tank is formed in the base body, the bottom of the water storage tank comprises a peripheral annular structure and a central convex curved surface, four circular water outlet holes are uniformly formed in the annular structure at the bottom of the water storage tank, the bottom of the base body is of an inwards-concave step structure, and four cylindrical clips are arranged on the outer side wall of the step structure;
the replacement part is of a hollow step structure without a top and a bottom, a Z-shaped channel is formed in the inner side wall of the replacement part, and four special-shaped water outlets which are centrosymmetric are formed in the bottom of the replacement part; the inner sides of the cylindrical clamp and the replaceable part of the base body are provided with Z-shaped channels which can be twisted and embedded;
the basal body and the plurality of replacement parts are manufactured by using PLA materials through a 3D printer.
Preferably, the cylindrical clip of the base body and the bottom of the base body are provided with circular water outlet holes which are not on the same vertical plane passing through the central axis of the base body.
The second purpose of the invention is to provide a method for preparing a transmission electron microscope metal sample by using the pre-thinning device, which comprises the following steps:
(1) cleaning a metal sheet to be thinned;
(2) drying the metal sheet to be thinned, and pasting the center of the large bottom surface of the replacement part opposite to the surface to be thinned of the metal to the center by using double-sided adhesive;
(3) the combination of the replacement part and the metal sheet is embedded with the base body according to the torsion of the channel, after water is injected through the through hole of the base body, the surface to be thinned of the metal sheet is thinned by utilizing a friction mechanism which moves relative to the metal sheet;
(4) after thinning by 0.05 +/-0.02 mm each time, detaching the combination of the replacement part and the metal sheet from the base body, placing the metal sheet on an iron wire net in an upward manner, heating the combination of the replacement part and the metal sheet to 200 +/-20 ℃ through the iron wire net, and melting the combination of the replacement part and the metal sheet, and then taking down the metal sheet by using tweezers;
(5) and (4) selecting a new replacement part, taking the opposite side face of the to-be-thinned face of the metal sheet as a new thinned face, and repeating the steps (1) - (4) until the thickness is less than or equal to 0.05 mm.
Preferably, the step (1) of cleaning the metal sheet to be thinned specifically comprises the following steps: cleaning the metal sheet to be thinned by using clear water, and cleaning the metal sheet to be thinned by using absolute ethyl alcohol;
preferably, when the metal sheet is thinned in the step (3), the metal sheet flows out through the water outlet holes by water stored in the water storage tank inside the base body, and the metal sheet is cooled; it should be noted that the water storage tank inside the machine body is not empty.
Preferably, each 0.05 +/-0.02 mm of thinning is realized by polishing with 240-mesh sand paper on a polishing and grinding machine with 1000 revolutions per minute for 2-5 minutes.
Preferably, the area of the double-sided adhesive tape is larger than that of the metal sheet to be thinned.
Compared with the prior art, the invention has the following remarkable advantages:
(1) the device for manually pre-thinning the cheap and environment-friendly TEM metal sample in a laboratory is manufactured in an extremely simple and economical 3D printing mode.
(2) The problem of treat that attenuate sheetmetal is difficult to the centre gripping that appears when laboratory is attenuate in advance is solved.
(3) The problem of easy fragmentation and scrapping when the thickness of the metal sheet in thinning is reduced to be less than 0.2mm and then the fixation is released when pre-thinning in a laboratory is solved.
Drawings
FIG. 1a is an orthographic three-axis view of a substrate design schematic of a cheap and environmentally friendly pre-thinning apparatus for the laboratory manual preparation of Transmission Electron Microscope (TEM) metal samples using 3D printed materials according to the present invention.
Fig. 1b is an isometric view of a schematic representation of a replacement design for an inexpensive, environmentally friendly pre-thinning apparatus for the manual preparation of Transmission Electron Microscope (TEM) metal samples using 3D printed materials laboratories, in accordance with the present invention.
FIG. 2a is a front view of a schematic design of a substrate of an inexpensive and environmentally friendly pre-thinning apparatus for the manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials in a laboratory according to the present invention;
FIG. 2b is a right side view of a schematic substrate design of an inexpensive and environmentally friendly pre-thinning apparatus for the manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials in a laboratory according to the present invention;
FIG. 2c is a schematic top view of a substrate design of an inexpensive and environmentally friendly pre-thinning apparatus for the laboratory manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials according to the present invention;
FIG. 2D is a perspective view of a schematic design of a substrate of the inexpensive and environmentally friendly pre-thinning apparatus for the laboratory manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials according to the present invention;
FIG. 2e is a front view of a schematic design of a replacement part of the inexpensive and environmentally friendly pre-thinning apparatus for manually preparing a Transmission Electron Microscope (TEM) metal sample using a 3D printing material laboratory according to the present invention;
FIG. 2f is a right side view of a schematic design of a replacement part of the inexpensive and environmentally friendly pre-thinning apparatus for manually preparing a Transmission Electron Microscope (TEM) metal sample using a 3D printed material laboratory according to the present invention;
FIG. 2g is a schematic top view of a replacement design of the inexpensive and environmentally friendly pre-thinning apparatus for the manual preparation of Transmission Electron Microscope (TEM) metal samples using 3D printed materials in the laboratory according to the present invention;
FIG. 2h is a perspective view of a schematic design of a replacement part of the inexpensive and environmentally friendly pre-thinning apparatus for manually preparing a Transmission Electron Microscope (TEM) metal sample using a 3D printing material laboratory according to the present invention;
FIG. 2i is a perspective view of a schematic design of a substrate of an inexpensive and environmentally friendly pre-thinning apparatus for the laboratory manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials according to the present invention;
FIG. 2j is a perspective view of a schematic design of a replacement part of the inexpensive and environmentally friendly pre-thinning apparatus for manually preparing a Transmission Electron Microscope (TEM) metal sample using a 3D printing material laboratory according to the present invention;
FIG. 3a is a physical representation of the substrate of the inexpensive and environmentally friendly pre-thinning apparatus for the laboratory manual preparation of Transmission Electron Microscopy (TEM) metal samples using 3D printed materials in accordance with the present invention;
FIG. 3b is a diagram of a replacement part of the cheap and environmentally friendly pre-thinning apparatus for manually preparing a Transmission Electron Microscope (TEM) metal sample by using a 3D printing material laboratory according to the present invention;
FIG. 4a is a top view of a pre-thinned finished product of a metal test sample of the inexpensive, environmentally friendly pre-thinning apparatus and method for manually preparing a Transmission Electron Microscope (TEM) metal sample in a 3D printed material laboratory according to the present invention;
FIG. 4b is a side view of a pre-thinned finished product of a metal sample of the cheap and environmentally friendly pre-thinning apparatus and method for manually preparing a Transmission Electron Microscope (TEM) metal sample by using a 3D printing material laboratory according to the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
The method for preparing the transmission electron microscope metal sample by using the pre-thinning device comprises the following steps:
the first step is as follows: using a 3D printer to make one substrate out of PLA material ] and making enough replacements with reduced thickness as required. The manufacturing requirements are shown in FIGS. 1a-3 b: the center of the top of the base body is provided with a water injection hole 1, the inside of the base body is provided with a water storage tank 2, the bottom of the water storage tank 2 is provided with an upward convex curved surface, the bottom of the base body is provided with four circular water outlet holes 3, and the side surface of the bottom of the base body is provided with four cylindrical clips 4; the inner side of the replacement part is provided with a Z-shaped channel 5, and the bottom of the replacement part is provided with four special-shaped water outlet holes 6 which are centrosymmetric; the cylindrical clip 4 of the base body and the inner side of the replacement part are provided with Z-shaped channels 5 which can be twisted and embedded; the cylindrical clamp 4 of the base body and the bottom of the base body are provided with circular water outlet holes 3 which are not on the same vertical plane passing through the central axis of the base body.
The second step is that: and cleaning the metal sheet to be thinned by using clear water, and cleaning the metal sheet to be thinned by using absolute ethyl alcohol.
The third step: and drying the metal sheet to be thinned by using an electric hair drier, and pasting the center of the lower bottom large surface of the replacement part and the opposite surface of the metal sheet to be thinned with double-sided adhesive to the center, wherein the area of the double-sided adhesive is larger than that of the metal sheet to be thinned.
The fourth step: and twisting and embedding the combination of the replacement part and the metal sheet and the base body according to the channel, thinning the surface to be thinned by utilizing the polishing and grinding integrated machine after water is injected through the through hole of the base body, and paying attention to the fact that a water storage tank in the machine body cannot be empty during thinning.
The fifth step: after thinning by 0.05 +/-0.02 mm, namely polishing and grinding for 2-5 minutes by using 240-mesh sand paper on a polishing and grinding integrated machine with the speed of 1000 revolutions per minute, dismounting the combination of the replacement part and the metal sheet from the base body, placing the metal sheet on an iron wire net upwards, heating the combination of the replacement part and the metal sheet to 200 +/-20 ℃ for melting through the iron wire net, taking down the metal sheet by using tweezers, cooling the metal sheet by water, and drying.
And a sixth step: and selecting a new replacement part, taking the opposite side face of the to-be-thinned face of the metal sheet as a new thinned face, and repeating the steps until the thickness is less than or equal to 0.05mm, as shown in fig. 4a and 4 b.
Claims (7)
1. A pre-thinning device for a metal sample is characterized by comprising a base body and a plurality of replacement parts; the water injection hole (1) is formed in the center of the top of the base body, the water storage tank (2) is formed in the base body, the bottom of the water storage tank (2) comprises a peripheral annular structure and a central convex curved surface, four circular water outlet holes (3) are uniformly formed in the annular structure at the bottom of the water storage tank (2), the bottom of the base body is of an inward-concave step structure, and four cylindrical clips (4) are arranged on the outer side wall of the step structure;
the replacement part is of a hollow step structure with no top and bottom, a Z-shaped channel (5) is formed in the inner side wall of the replacement part, and four special-shaped water outlets (6) which are centrosymmetric are formed in the bottom of the replacement part; the cylindrical clip (4) of the base body and the inner side of the replacement part are provided with Z-shaped channels (5) which can be twisted and embedded;
the basal body and the plurality of replacement parts are manufactured by using PLA materials through a 3D printer.
2. A pre-thinning apparatus for metal samples according to claim 1, characterized in that the cylindrical clip (4) of the base body and the circular water outlet hole (3) formed at the bottom of the base body are not in the same vertical plane passing through the central axis of the base body.
3. Method for preparing a transmission electron microscopy metal sample using a pre-thinning apparatus according to claim 1 or 2, characterized in that the method comprises the following steps:
(1) cleaning a metal sheet to be thinned;
(2) drying the metal sheet to be thinned, and pasting the center of the large bottom surface of the replacement part opposite to the surface to be thinned of the metal to the center by using double-sided adhesive;
(3) the combination of the replacement part and the metal sheet is embedded with the base body according to the Z-shaped channel in a twisting mode, after water is injected through the through hole of the base body, the surface to be thinned of the metal sheet is thinned by utilizing a friction mechanism which moves relative to the metal sheet;
(4) after thinning by 0.05 +/-0.02 mm each time, detaching the combination of the replacement part and the metal sheet from the base body, placing the metal sheet on an iron wire net in an upward manner, heating the combination of the replacement part and the metal sheet to 200 +/-20 ℃ through the iron wire net, and melting the combination of the replacement part and the metal sheet, and then taking down the metal sheet by using tweezers;
(5) and (4) selecting a new replacement part, taking the opposite side face of the to-be-thinned face of the metal sheet as a new thinned face, and repeating the steps (1) - (4) until the thickness is less than or equal to 0.05 mm.
4. The method for preparing a transmission electron microscope metal sample by using the pre-thinning apparatus according to claim 3, wherein the step (1) of cleaning the metal sheet to be thinned specifically comprises the following steps: and cleaning the metal sheet to be thinned by using clear water, and cleaning the metal sheet to be thinned by using absolute ethyl alcohol.
5. The method for preparing a transmission electron microscope metal sample by using the pre-thinning apparatus according to claim 3, wherein when thinning is performed in the step (3), the metal sheet is cooled by allowing water stored in a water storage tank inside the substrate to flow out through a water outlet; it should be noted that the water storage tank inside the machine body is not empty.
6. The method for preparing a transmission electron microscope metal sample by using the pre-thinning apparatus according to claim 3, wherein each 0.05mm plus or minus 0.02mm thinning is realized by polishing with 240-mesh sand paper on a polishing and grinding integrated machine with 1000 revolutions per minute for 2-5 minutes.
7. Method for preparing a transmission electron microscope metal sample using a pre-thinning apparatus according to claim 3, characterized in that the area of the double sided adhesive tape is larger than the metal sheet to be thinned.
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CN108693005B (en) * | 2018-05-30 | 2020-07-31 | 扬州大学 | Simple and rapid semi-screw-rod-top-cone type ultrahigh-speed negative-pressure environment-friendly hot-embedding laboratory device and using method thereof |
CN115078431A (en) * | 2022-06-16 | 2022-09-20 | 中国核动力研究设计院 | Preparation method of transmission electron microscope sample based on zirconium alloy after self-ion irradiation |
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CN201225969Y (en) * | 2008-06-20 | 2009-04-22 | 北京科技大学 | Transmission electric mirror sample chemical thinning clamper |
CN201442215U (en) * | 2009-04-03 | 2010-04-28 | 大连交通大学 | Mechanical pre-thinning device used for transmission electron microscopy sample preparation process |
CN105467652A (en) * | 2014-09-30 | 2016-04-06 | 住友化学株式会社 | Polarizing plate, liquid crystal display device and organic electroluminescence display device |
CN105575825A (en) * | 2015-12-24 | 2016-05-11 | 合肥祖安投资合伙企业(有限合伙) | Chip packaging method and packaging assembly |
JP2016127139A (en) * | 2014-12-26 | 2016-07-11 | 花王株式会社 | Polishing particles for polishing silicon oxide film |
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CN201225969Y (en) * | 2008-06-20 | 2009-04-22 | 北京科技大学 | Transmission electric mirror sample chemical thinning clamper |
CN201442215U (en) * | 2009-04-03 | 2010-04-28 | 大连交通大学 | Mechanical pre-thinning device used for transmission electron microscopy sample preparation process |
CN105467652A (en) * | 2014-09-30 | 2016-04-06 | 住友化学株式会社 | Polarizing plate, liquid crystal display device and organic electroluminescence display device |
JP2016127139A (en) * | 2014-12-26 | 2016-07-11 | 花王株式会社 | Polishing particles for polishing silicon oxide film |
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