CN116789127A - Transfer method of graphene film - Google Patents
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- CN116789127A CN116789127A CN202310890378.2A CN202310890378A CN116789127A CN 116789127 A CN116789127 A CN 116789127A CN 202310890378 A CN202310890378 A CN 202310890378A CN 116789127 A CN116789127 A CN 116789127A
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- graphene film
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 229920006254 polymer film Polymers 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000004528 spin coating Methods 0.000 claims abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 22
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 17
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 17
- 229910052594 sapphire Inorganic materials 0.000 claims description 13
- 239000010980 sapphire Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- -1 polymethacrylamide Polymers 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 230000006378 damage Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 235000012431 wafers Nutrition 0.000 description 25
- 239000010949 copper Substances 0.000 description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 229920006112 polar polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a transfer method of a graphene film, which comprises the following steps: spin-coating a high polymer film on the surface of a graphene film directly grown on a metal substrate; attaching a thermal release tape TRT on the polymer film to form a TRT/polymer film/graphene film/metal substrate composite structure; separating the TRT/polymer film/graphene film from the metal substrate; attaching the TRT/polymer film/graphene film to a target substrate; heating and releasing the thermal release tape TRT to obtain a polymer film/graphene film/target substrate composite structure, and continuously maintaining the polymer film/graphene film/target substrate composite structure after TRT is removed on a heat table; and washing with water to remove the high polymer film, thereby obtaining the graphene film/target substrate composite structure. The damage degree to the graphene film is smaller, the graphene film with higher integrity can be obtained, the operation is simple and convenient, the raw materials are environment-friendly, and the industrialization is facilitated.
Description
Technical Field
The invention belongs to the field of carbon materials, and particularly relates to a transfer method of a graphene film.
Background
Currently, graphene transfer methods are of a wide variety. The conventional chemical etching growth substrate transfer method is to place the graphene wafer coated with the polymer film in an etching solution for tens of hours at the expense of the growth substrate, completely etch copper, and separate the graphene and copper wafers.
Another common method is a bubbling method, and the method utilizes hydrogen bubbles generated between the growth substrate and the graphene after being electrified to realize decoupling of the graphene and the growth substrate so as to achieve the effect of complete separation.
For the two methods, the operation is complex, and the batch operation is difficult to carry out; organic waste liquid or alkali solution is difficult to treat and has great harm to the environment.
In the prior art, PVP and PVA are sequentially spin-coated on graphene, washed by absolute ethyl alcohol, dried, treated by water vapor at 75 ℃, dried and placed in deionized water at 75 ℃ for five times. The defect of this scheme is that different polymers need to be spin-coated step by step to reach the purpose that can separate graphene from the metal substrate, spin-coating process is complicated, and in last polymer cleaning process, need wash more than 5 times at least, the aftertreatment process is complicated.
In addition, the graphene can not be peeled off from the substrate by directly spin-coating PVP or PVA, or the peeled graphene has very poor quality, and the application requirement of graphene transfer can not be met.
The invention aims to develop a graphene wafer transfer method suitable for industrial production. The method has high repeatability, and ensures the quality of graphene transfer; the used raw materials aim to be harmless and low-toxic to operators, and the produced waste liquid and waste are environment-friendly; the operation steps are simple, and the process compatibility is strong.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a transfer method of a graphene film, which is suitable for transferring large-area graphene, has small damage to graphene, is simple and environment-friendly in process and is beneficial to industrial production. The specific scheme is as follows:
the transfer method of the graphene film specifically comprises the following steps:
s1, spin-coating a high polymer film on the surface of a graphene film directly grown on a metal substrate;
s2, attaching a thermal release tape TRT on the polymer film to form a TRT/polymer film/graphene film/metal substrate composite structure;
s3, separating the TRT/polymer film/graphene film from the metal substrate;
s4, attaching the TRT/polymer film/graphene film to a target substrate;
s5, heating and releasing the thermal release tape TRT to obtain a polymer film/graphene film/target substrate composite structure, and continuously maintaining the polymer film/graphene film/target substrate composite structure after TRT is removed on a heat table;
s6, washing with water to remove the high polymer film, and obtaining the graphene film/target substrate composite structure.
The polymer is one or more of polyvinyl alcohol PVA, polyvinylpyrrolidone PVP, polyacrylic acid, polymethacrylic acid, polyacrylamide, polymethacrylamide, polymethacrylate, polyacrylate and copolymer thereof; preferably polyvinyl alcohol PVA or polyvinylpyrrolidone PVP; still more preferred is polyvinyl alcohol PVA.
According to an embodiment of the present invention, before step S1, the method further includes: and (3) pre-oxidizing the graphene film/metal substrate composite structure in an alcohol/water solution.
According to the invention, the graphene wafer is subjected to oxidation treatment in advance, so that the binding force between the metal substrate and the graphene film is reduced, and the separation difficulty of the graphene film and the metal substrate is reduced; on the other hand, the treated graphene can be completely peeled off by adopting a water-soluble polar polymer such as PVA, and the graphene is easy to dissolve in water, so that the washing times are small after the transfer is completed, and the integrity of the graphene film is improved.
According to one embodiment of the present invention, the alcohol is one or more of methanol and ethanol.
According to one embodiment of the invention, the volume ratio of alcohol/water in the alcohol/water solution is 1:1.
According to an embodiment of the invention, the metal substrate is one of Cu, ni, pt, ru or an alloy thereof; alternatively, the metal substrate is a composite structure of one or an alloy of Cu, ni, pt, ru and sapphire.
According to an embodiment of the present invention, step S1 specifically includes: dissolving a polymer in water, and uniformly covering the surface of the graphene film with the polymer solution by using a spin coater; wherein the rotating speed is 300-5000rpm, the temperature is normal temperature, and the spin coating times are 1 time. The mass concentration of the polymer solution is 3wt% to 20wt%, preferably 8wt%.
According to one embodiment of the invention, in step S3, the separation is performed by mechanical stripping at a speed of not more than 10cm/S, preferably 0.1cm/S to 10cm/S.
According to an embodiment of the present invention, in step S4, the bonding mode is static pressure, rolling or vacuum bonding.
The bonding gap is made to have no air bubbles by bonding.
According to one embodiment of the invention, the thickness of the polymer film is 50 nm-10 μm; preferably 100nm to 1. Mu.m.
According to one embodiment of the present invention, in step S5, the heating release temperature is 20 to 200 ℃, and the release time is within 10 hours, preferably 1 to 600 minutes.
According to an embodiment of the present invention, in step S5, the PVA/graphene film/target substrate composite structure after TRT removal is continuously maintained on a heat stage; the heating temperature is controlled to be 100-140 ℃, preferably 120 ℃; the heating time is controlled within 10 hours, preferably 0.1 to 600 minutes.
By continuing to remain on the hot stage for a period of time, the graphene film may be brought into conformal contact with the target substrate.
According to an embodiment of the present invention, in step S6, the washing time is controlled within 120min, preferably 0.5min to 120min.
The washing water is preferably laboratory grade II pure water or ultrapure water.
According to one embodiment of the invention, the graphene film has a size of 2 to 10 inches, preferably 2 to 8 inches. Such as 2 inches, 4 inches, 6 inches, 8 inches.
According to an embodiment of the present invention, the graphene film of the present invention is a graphene film prepared by a conventional CVD method, and the number of layers is preferably 1 to 100, and more preferably 1 to 20.
According to one embodiment of the present invention, the target substrate is a conventional target substrate in the art, such as a silicon wafer.
The beneficial effects are that:
according to the invention, by adopting the technical scheme of combining the pre-oxidation treatment of the graphene wafer with the specific water-soluble polar organic polymer film, the graphene and the metal substrate can be separated only by physical stripping, and chemical means such as etching are not required; and in the subsequent photoresist removing process, normal-temperature clean water can be used for washing, heating is not needed, and washing times are less. Therefore, compared with the prior art, the technical scheme of the invention has the advantages that the damage degree to the graphene film is smaller, the graphene film with higher integrity can be obtained, the operation is simple and convenient, the raw materials are environment-friendly, and the industrialization is facilitated. In addition, compared with other schemes (such as a scheme of alternately coating PVA and PVP and the like) in the prior art, the technical scheme of the invention is more beneficial to realizing the transfer of the large-area graphene film.
Drawings
FIG. 1 is a schematic diagram of a graphene film transfer flow scheme of the present invention;
FIG. 2 is a photomicrograph of a graphene film after transfer of example 1;
FIG. 3 is a photograph of a graphene film after transfer of example 1;
FIG. 4 is a photomicrograph of a graphene film after transfer of example 2;
fig. 5 is a photomicrograph of graphene after transfer without oxidation treatment of comparative example 1.
Detailed Description
The present invention will be further illustrated by the following examples. It should also be understood that the following examples are given by way of illustration only and are not to be construed as limiting the scope of the invention, since various insubstantial modifications and adaptations of the invention to those skilled in the art based on the foregoing disclosure are intended to be within the scope of the invention and the specific process parameters and the like set forth below are merely one example of a suitable range within which one skilled in the art would choose from the description herein without being limited to the specific values set forth below.
Example 1
As shown in fig. 1, the graphene film/copper/sapphire wafer is oxidized in ethanol water solution for 5 hours, taken out and lightly blow-dried with high-purity nitrogen for standby. Polyvinyl alcohol (molecular weight 31K) is dissolved in water, the mass concentration is 8wt%, a spin coater is used for uniformly covering the surface of a 4-inch graphene film/copper/sapphire wafer with a polyvinyl alcohol (PVA) solution, the rotating speed is 2000rpm, the temperature is normal temperature, and the spin coating is carried out for 1 time. The PVA thickness was 150nm. And then, laminating a Thermal Release Tape (TRT) on the PVA by using a rolling mode to obtain the TRT/PVA/graphene film/copper/sapphire composite structure. Fixing the composite structure on a flat plate, and slowly stripping the composite structure of the TRT/PVA film/graphene wafer film from the copper/sapphire growth substrate by using tweezers. The copper/sapphire growth substrate is washed by a small amount of deionized water, dried by high-purity nitrogen and used for the subsequent regrowth of the high-quality graphene wafer film. The obtained composite layer of TRT/PVA film/graphene film is rolled and attached to a silicon wafer containing an oxide layer with the thickness of 285nm, and then the silicon wafer is heated and released on a hot table at 120 ℃ to remove the TRT, and the silicon wafer is heated for 90min continuously. And then washing to remove the glue, wherein the washing mode is to soak the silicon wafer in water for 2.5min, and drying the silicon wafer by nitrogen to obtain the 4-inch graphene film on the transferred silicon wafer.
As can be seen from fig. 2 and 3, the graphene film obtained by transfer by the transfer method of the present invention has a complete structure.
Example 2
As shown in fig. 1, the graphene film/copper/sapphire wafer is oxidized in ethanol water solution for 5 hours, taken out and lightly blow-dried with high-purity nitrogen for standby. Polyvinylpyrrolidone (molecular weight 1300K) is dissolved in water, the mass concentration is 6wt%, a spin coater is used for uniformly covering the polyvinylpyrrolidone (PVP) solution on the surface of a 4-inch graphene film/copper/sapphire wafer, the rotating speed is 2000rpm, the temperature is normal temperature, and spin coating is carried out for 1 time. PVP thickness was 200nm. And then laminating a Thermal Release Tape (TRT) on PVP in a rolling way to obtain the TRT/PVP/graphene film/copper/sapphire composite structure. Fixing the composite structure on a flat plate, and slowly stripping the composite structure of the TRT/PVP film/graphene wafer film from the copper/sapphire growth substrate by using tweezers. The copper/sapphire growth substrate is washed by a small amount of deionized water, dried by high-purity nitrogen and used for the subsequent regrowth of the high-quality graphene wafer film. And (3) laminating the obtained TRT/PVP film/graphene film composite layer on a silicon wafer containing an oxide layer with the thickness of 285nm by rolling, heating and releasing at 120 ℃ on a hot table to remove the TRT, and continuously heating for 90min. And then washing to remove the glue, wherein the washing mode is to soak the silicon wafer in water for 2.5min, and drying the silicon wafer by nitrogen to obtain the 4-inch graphene film on the transferred silicon wafer. The transferred graphene photo is shown in fig. 4, and it can be seen that the transferred graphene film maintains higher integrity although the transferred graphene film is slightly damaged compared with example 1.
Comparative example 1
Other conditions were the same as in example 1 except that the graphene film/copper/sapphire wafer was not subjected to oxidation treatment. The photo of the graphene photo obtained by transfer is shown in fig. 5, and it can be seen that the graphene obtained by transfer by the method is seriously damaged compared with examples and 2.
Unless otherwise defined, all terms used herein are intended to have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are intended to be illustrative only and not to limit the scope of the invention, and various other alternatives, modifications, and improvements may be made by those skilled in the art within the scope of the invention, and therefore the invention is not limited to the above embodiments but only by the claims.
Claims (10)
1. The transfer method of the graphene film is characterized by comprising the following steps of:
s1, spin-coating a high polymer film on the surface of a graphene film directly grown on a metal substrate;
s2, attaching a thermal release tape TRT on the polymer film to form a TRT/polymer film/graphene film/metal substrate composite structure;
s3, separating the TRT/polymer film/graphene film from the metal substrate;
s4, attaching the TRT/polymer film/graphene film to a target substrate;
s5, heating and releasing the thermal release tape TRT to obtain a polymer film/graphene film/target substrate composite structure, and continuously maintaining the polymer film/graphene film/target substrate composite structure after TRT is removed on a heat table;
s6, washing with water to remove the high polymer film, so as to obtain a graphene film/target substrate composite structure;
the polymer is one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid, polymethacrylic acid, polyacrylamide, polymethacrylamide, polymethacrylate, polyacrylate and copolymer thereof; preferably polyvinyl alcohol or polyvinylpyrrolidone; still more preferably, polyvinyl alcohol.
2. The transfer method according to claim 1, further comprising, prior to step S1: and (3) pre-oxidizing the graphene film/metal substrate composite structure in an alcohol/water solution.
3. The transfer method according to claim 2, wherein the alcohol is one or more of methanol and ethanol.
4. The transfer method of claim 1, wherein the metal substrate is one of Cu, ni, pt, ru or an alloy thereof; alternatively, the metal substrate is a composite structure of one or an alloy of Cu, ni, pt, ru and sapphire.
5. The transfer method according to claim 1, wherein in the step S4, the bonding means is static pressure, rolling or vacuum bonding.
6. The transfer method according to claim 1, wherein the thickness of the polymer film is 50nm to 10 μm; preferably 100nm to 1. Mu.m.
7. Transfer method according to claim 1, characterized in that in said step S5, the heating release is carried out at a temperature of 20-200 ℃ for a release time of less than 10 hours, preferably 1-600 min.
8. Transfer method according to claim 1, characterized in that in step S6 the washing time is within 120min, preferably between 0.5min and 120min.
9. The transfer method according to claim 1, wherein the graphene film has a size of 2 to 10 inches, preferably 2 to 8 inches.
10. Transfer method according to claim 1, characterized in that the number of layers of the graphene film is 1-100, preferably 1-20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310890378.2A CN116789127A (en) | 2023-07-19 | 2023-07-19 | Transfer method of graphene film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310890378.2A CN116789127A (en) | 2023-07-19 | 2023-07-19 | Transfer method of graphene film |
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| Publication Number | Publication Date |
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| CN116789127A true CN116789127A (en) | 2023-09-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310890378.2A Pending CN116789127A (en) | 2023-07-19 | 2023-07-19 | Transfer method of graphene film |
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| CN (1) | CN116789127A (en) |
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- 2023-07-19 CN CN202310890378.2A patent/CN116789127A/en active Pending
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