CN110739196B - Transmission electron microscope grid capable of being produced in batches and preparation method thereof - Google Patents
Transmission electron microscope grid capable of being produced in batches and preparation method thereof Download PDFInfo
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 89
- 239000002184 metal Substances 0.000 claims abstract description 89
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000005266 casting Methods 0.000 claims abstract description 29
- 238000005530 etching Methods 0.000 claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 238000001259 photo etching Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005498 polishing Methods 0.000 claims abstract description 7
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 17
- 229910001152 Bi alloy Inorganic materials 0.000 claims description 14
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 claims description 9
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 claims description 8
- PSMFTUMUGZHOOU-UHFFFAOYSA-N [In].[Sn].[Bi] Chemical compound [In].[Sn].[Bi] PSMFTUMUGZHOOU-UHFFFAOYSA-N 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 6
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 238000004627 transmission electron microscopy Methods 0.000 claims description 3
- 238000012512 characterization method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002390 adhesive tape Substances 0.000 description 4
- 238000010923 batch production Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
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- 239000004677 Nylon Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000001149 cognitive effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/06—Permanent moulds for shaped castings
- B22C9/061—Materials which make up the mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
- B22C9/24—Moulds for peculiarly-shaped castings for hollow articles
-
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/261—Details
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Abstract
The invention discloses a transmission electron microscope grid capable of being produced in batches and a preparation method thereof, wherein the transmission electron microscope grid comprises the following steps: 1) designing and processing a photoetching mask according to the grid-carrying requirement of the transmission electron microscope to obtain a required mask graph; 2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold; 3) heating the casting mould, then melting the low-melting-point metal, pouring the molten low-melting-point metal into the mould, and cooling to room temperature to solidify the metal; 4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then taking the cast metal mesh carrying framework out of the mold; 5) and covering an organic film on the metal grid framework to form the transmission electron microscope grid. According to the method, the micro-nano processing technology and the excellent characteristics of low-melting-point metal are combined, 200-3000-mesh electron microscope metal grid can be manufactured in batches, and a more flexible electron microscope grid solution is provided for the electron microscope characterization field.
Description
Technical Field
The invention relates to a transmission electron microscope grid capable of being produced in batches and a preparation method thereof, belonging to the field of transmission electron microscope characterization testing.
Background
The representation of the microstructure of the tested nanometer material and the various properties of the cognitive nanometer material are important foundations for promoting the application of the nanometer material and constructing a novel functional device. Among many test analysis techniques, thanks to ultra-high resolution, transmission electron microscopy has become one of the most important techniques for testing and characterizing the morphology, structure, composition and physical properties of nanomaterials.
In the transmission electron microscope test characterization, the transmission electron microscope carrier net is usually an indispensable component. The nano material to be tested and characterized is generally transferred and loaded on a carrier net of an electron microscope, then the carrier net is assembled into a sample rod, and then the sample rod is loaded into a cavity of a main body of a transmission electron microscope for characterization and analysis. Various commercially available transmission electron microscope carrying nets in the current market comprise nylon nets, metal carrying nets, silicon nitride carrying nets and the like; the metal grid is mostly made of copper, the skeleton of the copper grid is mainly realized by an etching method, the mesh number of the copper grid is usually 50-600 meshes, and some imported high-mesh copper grid skeletons can reach 1000-2000 meshes. For high numbers of copper mesh, products on the market today rely mainly on importation and are relatively expensive.
In addition, in an experiment for representing nano particles and nano wires with small sizes, the mesh number of the carrier net is generally expected to be further increased to reduce meshes, so that suspended loading of the nano particles and the nano wires is realized, an electron microscope carrier net with higher mesh number, designable mesh morphology and relatively low cost is required, however, the product is not available in the market, and the technical field is still blank at present.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a method for preparing a transmission electron microscope grid capable of being produced in batches, which can be used for manufacturing 200-3000-mesh electron microscope metal grids in batches by combining a micro-nano processing technology and the excellent characteristics of low-melting-point metal, and is beneficial to providing a more flexible electron microscope grid solution for the characterization field of electron microscopes.
The technical scheme is as follows: the invention provides a preparation method of a transmission electron microscope grid capable of being produced in batches, which comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of the transmission electron microscope to obtain a required mask graph;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold;
3) heating the casting mould, then melting the low-melting-point metal, pouring the molten low-melting-point metal into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then taking the cast metal mesh carrying framework out of the mold;
5) and covering an organic film on the metal grid framework to form the transmission electron microscope grid.
Wherein:
the number of meshes in the mask pattern in the step 1) is 200-3000 meshes, and the meshes are square holes, round holes or hexagonal holes.
The inner graph of the mask in the step 1) is in a circular shape with the diameter of 3 mm.
Etching the mask pattern into the silicon wafer to form a casting mold through an etching process in the step 1), wherein the etching depth is 20-50 microns.
The low-melting-point metal in the step 3) is a tin-indium-bismuth alloy, a lead-tin alloy or a bismuth-tin alloy, and the step 3) of heating the casting mold means heating to the melting point temperature of the low-melting-point metal of 50-150 ℃.
The step 4) of taking out the cast metal mesh carrying framework from the mold refers to taking out the cast metal mesh carrying framework from the mold by using a rubber belt.
The organic film in the step 5) is a square membrane or a collodion membrane, and the thickness of the organic film is 10-30 nm.
The invention also provides the transmission electron microscope grid prepared by the method, which consists of a metal grid framework prepared from low-melting-point metal and an organic film covered on the surface of the metal grid framework, wherein meshes in the metal grid framework are square holes, round holes or hexagonal holes, and the mesh number is 200-3000 meshes.
Wherein:
the transmission electron microscope carrier net is in a circular shape with the diameter of 3mm,
the low-melting-point metal is a tin-indium-bismuth alloy, a lead-tin alloy or a bismuth-tin alloy; the thickness of the metal mesh framework is 20-50 μm.
The organic film is a diamond film or a collodion film, and the thickness of the organic film is 10-30 nm.
Has the advantages that: compared with the prior art, the invention has the following advantages:
the transmission electron microscope grid capable of being produced in batches and the preparation method thereof provided by the invention have low requirements on technical level and equipment, can flexibly design the grid number and structure, have the advantages of simplicity in preparation, low cost and the like, are beneficial to providing a more flexible solution for electron microscope grids in the characterization field of electron microscopes, and further provide technical support for deep research on the morphology, structure, components and physical properties of nano materials.
The transmission electron microscope grid provided by the invention has the advantages of high mesh number, obvious price advantage, controllable internal graph and the like which cannot be met by the current market, so that the problems that the high-mesh grid in the market depends on import, the price is high and the like can be solved, and a more flexible electron microscope grid solution is provided for the electron microscope characterization field.
In the preparation method of the grid for the transmission electron microscope, the used materials are relatively low, the technical level is low, the requirements on the manufacturing environment and equipment are not high, and the grid can be produced in batch, so that the grid has the advantages of simplicity in manufacturing, low cost, high yield, convenience in use and the like.
Drawings
FIG. 1 is a schematic diagram of a method for manufacturing a transmission electron microscope grid capable of mass production according to the present invention;
FIG. 2 is a microscope picture of a transmission electron microscope grid prepared by the present invention, wherein a is an optical microscope picture of the transmission electron microscope grid, and b is a scanning electron microscope picture of the transmission electron microscope grid.
Detailed Description
The invention provides a transmission electron microscope grid capable of being produced in batches and a preparation method thereof, and by combining a micro-nano processing technology and the excellent characteristics of low-melting-point metal, 200-3000-mesh electron microscope metal grids can be produced in batches, which is helpful for providing a more flexible electron microscope grid solution for the characterization field of electron microscopes, and the further detailed description is provided in combination with the attached drawings.
Example 1
A method for preparing transmission electron microscope mesh in batch production comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of a transmission electron microscope to obtain a circular mask graph with the diameter of 3mm, wherein the mesh number in the graph is 200 meshes, and the mesh shape is a square hole;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold, wherein the etching depth is 20 microns;
3) heating the casting mould to 100 ℃, then melting the low-melting-point metal bismuth-tin alloy, pouring the molten low-melting-point metal bismuth-tin alloy into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then stripping the cast metal mesh carrying framework from the casting mold by using an adhesive tape;
5) covering a cubic film with the thickness of 10nm on the metal grid framework to form the transmission electron microscope grid.
The transmission electron microscope grid prepared by the method consists of a bismuth tin alloy metal grid framework and a diamond film covered on the surface of the bismuth tin alloy metal grid framework, the shape of the transmission electron microscope grid is a circle with the diameter of 3mm, the thickness of the metal grid framework is 20 mu m, meshes in the metal grid framework are square holes, the mesh number is 200 meshes, and the thickness of the diamond film is 10 nm.
Example 2
A method for preparing transmission electron microscope mesh in batch production comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of a transmission electron microscope to obtain a circular mask graph with the diameter of 3mm, wherein the mesh number in the graph is 600 meshes, and the mesh shape is a hexagonal hole;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold, wherein the etching depth is 30 microns;
3) heating the casting mould to 70 ℃, then melting the low-melting-point metal Sn-in-Bi alloy, pouring the molten low-melting-point metal Sn-in-Bi alloy into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then stripping the cast metal mesh carrying framework from the casting mold by using an adhesive tape;
5) covering a cubic film with the thickness of 30nm on the metal grid framework to form the transmission electron microscope grid.
The transmission electron microscope grid prepared by the method consists of a tin-indium-bismuth alloy metal grid framework and a square membrane covered on the surface of the tin-indium-bismuth alloy metal grid framework, the tin-indium-bismuth alloy metal grid framework is in a circular shape with the diameter of 3mm, the thickness of the metal grid framework is 30 micrometers, meshes in the metal grid framework are hexagonal holes, the mesh number is 600 meshes, and the thickness of the square membrane is 30 nm.
Example 3
A method for preparing transmission electron microscope mesh in batch production comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of a transmission electron microscope to obtain a circular mask graph with the diameter of 3mm, wherein the mesh number in the graph is 1000 meshes, and the mesh shape is a round hole;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold, wherein the etching depth is 40 mu m;
3) heating the casting mould to 150 ℃, then melting the low-melting-point metal lead-tin alloy, pouring the molten low-melting-point metal lead-tin alloy into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then stripping the cast metal mesh carrying framework from the casting mold by using an adhesive tape;
5) covering the metal mesh-carrying framework with collodion with the thickness of 10nm to form the transmission electron microscope mesh-carrying.
The transmission electron microscope carrier net prepared by the method consists of a lead-tin alloy metal carrier net framework and a collodion film covered on the surface of the lead-tin alloy metal carrier net framework, the shape of the lead-tin alloy metal carrier net framework is a circle with the diameter of 3mm, the thickness of the metal carrier net framework is 40 mu m, meshes in the metal carrier net framework are round holes, the mesh number is 1000 meshes, and the collodion film thickness is 10 nm.
Example 4
A method for preparing transmission electron microscope mesh in batch production comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of a transmission electron microscope to obtain a circular mask graph with the diameter of 3mm, wherein the mesh number in the graph is 3000 meshes, and the mesh shape is a square hole;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold, wherein the etching depth is 50 microns;
3) heating the casting mould to 50 ℃, then melting the low-melting-point metal Sn-in-Bi alloy, pouring the melted low-melting-point metal Sn-in-Bi alloy into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then stripping the cast metal mesh carrying framework from the casting mold by using an adhesive tape;
5) covering the metal mesh-carrying framework with collodion with the thickness of 30nm to form the transmission electron microscope mesh-carrying.
The transmission electron microscope grid prepared by the method consists of a Sn-in-Bi alloy metal grid framework and a collodion film covered on the surface of the Sn-in-Bi alloy metal grid framework, the Sn-in-Bi alloy metal grid framework is in a circular shape with the diameter of 3mm, the thickness of the metal grid framework is 50 mu m, meshes in the metal grid framework are square holes, the mesh number is 3000 meshes, and the collodion film thickness is 30 nm.
Claims (9)
1. A preparation method of transmission electron microscope grid capable of being produced in batches is characterized by comprising the following steps: the method comprises the following steps:
1) designing and processing a photoetching mask according to the grid-carrying requirement of the transmission electron microscope to obtain a required mask graph;
2) transferring the mask pattern onto a silicon wafer by a photoetching process, and etching the mask pattern into the silicon wafer by an etching process to form a casting mold;
3) heating the casting mould, then melting the low-melting-point metal, pouring the molten low-melting-point metal into the mould, and cooling to room temperature to solidify the metal;
4) polishing to remove redundant metal on the upper surface after the casting mold is filled, and then taking the cast metal mesh carrying framework out of the mold;
5) and covering an organic film on the metal grid framework to form the transmission electron microscope grid.
2. The method for preparing the transmission electron microscope mesh capable of being produced in batches according to claim 1, wherein the method comprises the following steps: the number of meshes in the mask pattern in the step 1) is 200-3000 meshes, and the meshes are square holes, round holes or hexagonal holes.
3. The method for preparing the transmission electron microscope mesh capable of being produced in batches according to claim 1, wherein the method comprises the following steps: etching the mask pattern into the silicon wafer to form a casting mold through an etching process in the step 2), wherein the etching depth is 20-50 DEG
。
4. The method for preparing the transmission electron microscope mesh capable of being produced in batches according to claim 1, wherein the method comprises the following steps: the low-melting-point metal in the step 3) is a tin-indium-bismuth alloy, a lead-tin alloy or a bismuth-tin alloy, and the step 3) of heating the casting mold refers to heating to the melting point temperature of the low-melting-point metal.
5. The method for preparing the transmission electron microscope mesh capable of being produced in batches according to claim 1, wherein the method comprises the following steps: the step 4) of taking out the cast metal mesh carrying framework from the mold refers to taking out the cast metal mesh carrying framework from the mold by using a rubber belt.
6. The method for preparing the transmission electron microscope mesh capable of being produced in batches according to claim 1, wherein the method comprises the following steps: the organic film in the step 5) is a square membrane or a collodion membrane, and the thickness of the organic film is 10-30 nm.
7. The transmission electron microscope grid prepared by the method for preparing the transmission electron microscope grid capable of being produced in batches according to the claims 1, 2, 3, 4, 5 or 6, is characterized in that: the transmission electron microscope carrier mesh consists of a metal carrier mesh framework prepared from low-melting-point metal and an organic film covered on the surface of the metal carrier mesh framework, wherein meshes in the metal carrier mesh framework are square holes, round holes or hexagonal holes, and the mesh number is 200-3000 meshes.
8. The grid for transmission electron microscopy according to claim 7, wherein: the low-melting-point metal is a tin-indium-bismuth alloy, a lead-tin alloy or a bismuth-tin alloy; the thickness of the metal net carrying framework is 20-50
。
9. The grid for transmission electron microscopy according to claim 7, wherein: the organic film is a diamond film or a collodion film, and the thickness of the organic film is 10-30 nm.
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| CN101276724B (en) * | 2007-03-30 | 2011-06-22 | 北京富纳特创新科技有限公司 | Transmission electron microscope micro grid and preparing method thereof |
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| Title |
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