CN116715231A - Method for transferring graphene film to grid - Google Patents
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- CN116715231A CN116715231A CN202310462319.5A CN202310462319A CN116715231A CN 116715231 A CN116715231 A CN 116715231A CN 202310462319 A CN202310462319 A CN 202310462319A CN 116715231 A CN116715231 A CN 116715231A
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- graphene film
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- water
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000012546 transfer Methods 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 238000005086 pumping Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 9
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 9
- 238000003958 fumigation Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 6
- 230000005294 ferromagnetic effect Effects 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 3
- -1 sodium alkyl sulfonate Chemical class 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 229940071145 lauroyl sarcosinate Drugs 0.000 claims description 2
- 238000011056 performance test Methods 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 68
- 239000007788 liquid Substances 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of ionization films, in particular to a method for transferring a graphene film to a grid. The method comprises the following steps: and (3) floating the graphene film from water, adding a surfactant, pumping water to cover the graphene film on a grid of a transfer platform, and performing drying and heat treatment to transfer the graphene film to obtain the graphene film grid. The invention can improve the adhesion capability of the graphene film on the discontinuous substrate such as the grid mesh, reduce the damage of the graphene film and improve the coverage rate.
Description
Technical Field
The invention relates to the technical field of ionization films, in particular to a method for transferring a graphene film to a grid.
Background
The most widely used method in the measurement of spatial particle composition is the transmission TOF (time of flight) method, which measures the basic principle of particle composition as follows: the particles first pass through an electric device after entering the instrumentSeparating the film to generate a start signal (t 1 ) The particles then continue to fly, and the impact sensor generates a termination signal (t 2 ) By measuring the time difference between the two signals to obtain the flight time of the particle, the mass of the particle can be reversely deduced by combining the energy information of the particleThereby determining the particle type.
In this method, the material and thickness of the ionization film affect the emission properties such as the emission energy of the particles, and thus the measurement result. The reduction of the film thickness and the optimization of the material are beneficial to reducing the detection energy lower limit and improving the energy resolution, imaging resolution and mass spectrum resolution. At present, the conventional carbon film is widely used, and the thickness of the carbon film is generally 0.5-3.0 mug/cm -2 (about 3-17 nm) to somewhat limit the lower end of the detectable particle energy range. In order to further lower the lower limit of the energy of the particles that can be detected based on the prior art, the next generation of ionized thin film materials need to have a lower thickness than carbon films.
Graphene was discovered in 2004 as a novel two-dimensional material. The monoatomic layer thickness of graphene is only 0.34-nm, and the extremely low thickness makes it promising as a next generation ionization thin film candidate material following a traditional carbon film. Whether graphene or a traditional carbon film, the particle transmission needs to be attached to a supporting grid for working. When a graphene film manufactured by using a Chemical Vapor Deposition (CVD) method is transferred onto a grid by using the existing method, the problem of lower coverage rate, namely more damage, is often faced, so that the application of the graphene in the aspect of particle detection is affected.
The problem of low coverage rate of the graphene film transferred onto the grid is mainly caused by insufficient adhesion of the graphene film to the grid wires of the grid, so that the improvement of the adhesion of the graphene film to the grid wires in the transfer process becomes a key for improving the coverage rate. Unlike continuous substrates such as glass and silicon wafers, the grid acts as a discontinuous substrate and the area available for attachment is much smaller than that of a continuous substrate. Therefore, in the case that the area of the non-continuous substrate to be attached is far smaller than that of the continuous substrate, in order to avoid damage and improve coverage rate, the adhesion of the graphene film to the grid wires needs to be improved by various means, and the adhesion of the graphene film to the grid mesh is enhanced.
Therefore, an effort is needed to solve the problem of insufficient adhesion in the process of transferring the graphene film to the grid, and realize high coverage rate transfer of the graphene film to the grid.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for transferring a graphene film to a grid, which is used for testing the transmission performance of particles by transferring the graphene film to the grid with high coverage rate through various means for enhancing the adhesiveness of the graphene film.
The invention provides a method for transferring a graphene film to a grid, which comprises the following steps:
and (3) floating the graphene film from water, adding a surfactant, pumping water to cover the graphene film on a grid of a transfer platform, and performing drying and heat treatment to transfer the graphene film to obtain the graphene film grid.
Preferably, the graphene film is coated with a coating, and the material of the coating comprises PMMA.
Preferably, the step of removing the coating of the graphene film by fumigation after drying and heat treatment; the fumigation solvent comprises one or more of acetone, chloroform (chloroform), isopropanol IPA and ethyl acetate.
Preferably, the surfactant comprises one or more of fatty alcohol polyoxyethylene ether AEO, sodium alkyl sulfonate, sulfo fatty acid ester and lauroyl sarcosinate, and the addition amount of the surfactant is 0.01-0.1ml.
Preferably, the central part of the transfer platform is provided with a through hole, and the bottom of the transfer platform part is provided with a channel.
Preferably, the transfer table is a smooth metal part made of ferromagnetic stainless steel.
Preferably, the through hole is a round platform through hole, the top opening of the round platform through hole is smaller than the bottom opening, and four channels leading to four sides are arranged at the bottom of the transfer platform.
Preferably, the included angle between two opposite bus bars on the axial section of the round platform through hole is 30-150 degrees.
The invention provides a graphene film grid mesh, which is prepared by the preparation method.
The invention provides application of the graphene film grid mesh in the aspect of particle transmission performance test.
The main means for improving the adhesiveness of the graphene film are to eliminate the surface tension of the water surface by using a surfactant, to use a transfer platform, to perform vacuum heat treatment and to use gaseous acetone fumigation.
The invention uses the surfactant to help eliminate the surface tension of the water surface, so that tiny water drops remained due to the surface tension can not be generated in the process of pumping water to cover the graphene film. If the tiny water drops remain between the graphene film and the grid mesh, uneven coverage of the graphene film can be caused, wrinkles can be caused after the water is dried, and finally damage is caused.
The transfer platform is a metal part made of ferromagnetic stainless steel, a through hole is formed in the center of the metal part, meanwhile, four channels leading to each side are formed in the bottom of the transfer platform, the upper surface of the transfer platform is high in flatness, and burrs are avoided at the through hole. The ferromagnetic nature of the transfer platform facilitates the use of magnets to secure the transfer platform in the petri dish. The central circular truncated cone-shaped through hole is used for avoiding forming a capillary tube, is favorable for reducing capillary effect, and enables water in the through hole to be discharged along with the decline of the outside water surface. The four channels facilitate the drainage of water from the interior of the component from the surroundings and also facilitate the suction of residual water from the interior through the channel opening. The high requirement of the upper surface on flatness and no burrs are used for preventing the graphene film from being damaged by the upper surface when the graphene film is attached to the upper surface. And when the grid is placed on the transfer platform, the bonding between the graphene film and the grid after water pumping is realized more favorably than when the grid is placed on other surfaces (such as a quartz glass plate, a polymer film and the like).
The heat treatment is vacuum heat treatment, and the vacuum heat treatment process is beneficial to softening the coating (such as PMMA) to a certain extent, so that the graphene film can be spontaneously relaxed, and the damage of the graphene film after the coating is removed in suspended areas such as meshes due to incapability of spontaneous relaxation is avoided.
According to the invention, the liquid solvent is converted into the gas state for fumigation, so that the problem of liquid surface tension caused by immersion washing by using the liquid solvent (such as liquid acetone) can be avoided, and when the immersion washing is performed by using the liquid solvent, the graphene film suspended at the meshes can be torn to cause damage due to the existence of the surface tension of the solvent. This problem is effectively avoided during fumigation of the liquid solvent to a gaseous state to remove the coating (e.g., PMMA).
Compared with the prior art, the invention has the advantages that:
the invention can improve the adhesion capability of the graphene film on the discontinuous substrate such as the grid mesh, reduce the damage of the graphene film, and improve the coverage rate which can reach more than 96%.
Drawings
FIG. 1 is a block diagram of a transfer platform of the present invention;
FIG. 2 is a bottom view of the transfer platform of the present invention;
figure 3 is a cross-sectional view A-A of figure 2 according to the present invention.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the accompanying drawings and examples.
The invention provides a method for transferring a graphene film onto a grid for a particle transmission test with high coverage rate, which comprises the following transferring steps: firstly, floating a graphene film spin-coated with PMMA from water, eliminating surface tension by using a surfactant, then, pumping water to enable the graphene film to be covered on a grid mesh arranged on a special transfer platform, then, performing drying and vacuum heat treatment operation, and finally, removing the PMMA coating by using a gaseous acetone fumigation mode to finish transfer of the graphene film.
Specifically, the method comprises the following steps:
1) Preparing a substrate:
preparing a clean small culture dish, placing a transfer platform in the culture dish, fixing the culture dish at the bottom of the culture dish, placing the culture dish with the transfer platform on a table top in an overhead manner, taking out a target copper net, placing the target copper net at a through hole position of the transfer platform in an upward direction, ensuring that a grid net area completely covers through hole holes, and injecting ultrapure water into the culture dish to enable the water surface to be over the upper surface of the transfer platform; the transfer platform is a square metal part made of ferromagnetic stainless steel, a round platform through hole is formed in the center portion, the top opening of the through hole is smaller, the bottom opening is larger, meanwhile, four channels leading to four sides are formed in the bottom of the part, and the upper surface of the part is high in flatness and free of burrs at the through hole. The angle between the two opposite generatrix on the axial section of the circular truncated cone through hole is preferably 61.08 degrees.
2) And (3) water floating separation:
taking out a graphene film (the upper surface of which is provided with a layer of spin-coated PMMA serving as a support), fixing the graphene film on a glass plate, obliquely placing the glass plate into a large crystallization dish, slowly injecting ultrapure water into the crystallization dish, stopping injecting water when the liquid level gradually approaches to the graphene film region, adding 0.03mL of surfactant AEO into the water, fishing out the part which cannot be rapidly dissolved from the water, continuing slowly injecting water, stopping injecting water when the liquid level completely separates the graphene film from a non-woven fabric attachment surface and is completely supported by the water surface, removing bubbles behind the graphene film, fishing up the graphene film after the bubbles are removed, adding 0.05mL of surfactant AEO into the culture dish where the substrate is positioned, and then placing the graphene film into the water of the culture dish, so that the graphene film is supported by the water surface in the culture dish.
3) And (3) water pumping covering: the position of the graphene film is adjusted to enable the graphene film to float right above the target copper net, then pumping water is started to enable the graphene film to descend along with the water surface, the pumping speed is reduced when the graphene film approaches the target copper net, the position of the graphene film is adjusted at any time, the graphene film can completely cover the target copper net, the graphene film covers the target copper net and the upper surface area of a nearby transfer platform, the conventional pumping speed can be recovered when the graphene film is completely attached and cannot slide at the position of the transfer platform, pumping water is continued until water in a culture dish is pumped, and then the water in the culture dish is completely absorbed from a channel outlet on the side surface of the transfer platform.
4) Drying and heat treatment:
taking out a transfer platform with a target copper net, the upper surface of which is covered with a graphene film, putting the transfer platform into a dry culture dish, naturally airing in air, putting the aired transfer platform with the culture dish into an oven, covering a culture dish cover, drying under the air atmosphere, thoroughly removing moisture, taking out and checking the condition after cooling to room temperature, putting the culture dish with the cover back into the oven again after finishing, vacuumizing for 10 minutes, maintaining a vacuum state, heating to above the PMMA glass transition temperature, maintaining, cooling to room temperature after heat treatment is finished, and taking out.
5) Fumigating with acetone:
pouring liquid acetone into a beaker, heating the acetone, fumigating by using acetone steam, and dissolving and removing the PMMA coating above the graphene film to obtain the graphene film grid mesh.
The coverage rate of the graphene film in the graphene film grid is 96% -99%.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and are not limiting. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the appended claims.
Claims (10)
1. A method for transferring a graphene film to a grid, comprising the steps of:
and (3) floating the graphene film from water, adding a surfactant, pumping water to cover the graphene film on a grid of a transfer platform, and performing drying and heat treatment to transfer the graphene film to obtain the graphene film grid.
2. The method of claim 1, wherein the graphene film is coated with a coating, the material of the coating comprising PMMA.
3. The method according to claim 2, wherein the method further comprises: removing the coating of the graphene film by fumigation after drying and heat treatment; the fumigation solvent comprises one or more of acetone, chloroform, isopropanol and ethyl acetate.
4. The method according to claim 1, wherein the surfactant comprises one or more of fatty alcohol polyoxyethylene ether, sodium alkyl sulfonate, sulfofatty acid ester and lauroyl sarcosinate, and the amount of the surfactant added is 0.01-0.1ml.
5. The method of claim 1, wherein the transfer platform has a through hole in a central portion thereof and a channel in a bottom portion of the transfer platform member.
6. The method of claim 1, wherein the transfer platform is a smooth metal part made of ferromagnetic stainless steel.
7. The method of claim 1, wherein the through-hole is a frustoconical through-hole having a smaller top opening than a bottom opening, and the transfer platform has four channels opening to four sides at the bottom.
8. The method of claim 7, wherein the included angle between two opposing bus bars on the axial cross section of the frustoconical through hole is 30 ° -150 °.
9. A graphene film grid, characterized in that it is prepared by the preparation method of any one of claims 1 to 8.
10. Use of the graphene film grid of claim 9 in a particle transmission performance test.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310462319.5A CN116715231B (en) | 2023-04-26 | 2023-04-26 | Method for transferring graphene film to grid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310462319.5A CN116715231B (en) | 2023-04-26 | 2023-04-26 | Method for transferring graphene film to grid |
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| Publication Number | Publication Date |
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| CN116715231A true CN116715231A (en) | 2023-09-08 |
| CN116715231B CN116715231B (en) | 2024-01-30 |
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| CN116715231B (en) | 2024-01-30 |
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