CN104085887A - Chemical vapor deposition method for preparing graphene - Google Patents
Chemical vapor deposition method for preparing graphene Download PDFInfo
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- CN104085887A CN104085887A CN201410364096.XA CN201410364096A CN104085887A CN 104085887 A CN104085887 A CN 104085887A CN 201410364096 A CN201410364096 A CN 201410364096A CN 104085887 A CN104085887 A CN 104085887A
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Abstract
The invention provides a chemical vapor deposition method for preparing graphene, which comprises the following steps: 1. preparing a copper-nickel alloy film on the monocrystalline silicon surface by a copper/nickel double-target magnetron sputtering process; 2. transferring the monocrystalline silicon substrate, of which the surface is deposited with the copper-nickel alloy film, into a chemical vapor deposition reaction furnace, and introducing helium into the reaction furnace to eliminate air in the reaction furnace; 3. heating the substrate to 400-600 DEG C within 20-40 minutes, and introducing helium until the pressure in the reaction furnace is 5-10 Torr; 4. introducing hydrogen into the reaction furnace, and injecting benzene into the reaction furnace; 5. while keeping the pressure in the reaction furnace at 5-10 Torr, after the benzene injection is finished, stopping introducing the hydrogen, introducing helium into the reaction furnace, cooling the monocrystalline silicon substrate with the copper-nickel alloy film to room temperature at the rate of 20 DEG C/minute, and continuing introducing helium for 10 minutes; and 6. taking out the substrate on which the graphene film is grown.
Description
Technical field
The present invention relates to a kind of method of preparing Graphene, particularly a kind of employing process for preparing graphenes by chemical vapour deposition.
Background technology
Graphene, i.e. the monoatomic layer of graphite, be carbon atom by the two-dirnentional structure of honeycomb arrangement, be also to form other low dimension carbon materials as the elementary cell of soccerballene, carbon nanotube.According to the number of plies, Graphene can be divided into single-layer graphene, double-layer graphite alkene, few layer graphene.The research of Graphene is long-standing, but the Geim of the Graphene Ze Shiyou Univ Manchester UK of real independent stable existence etc. obtain by the high oriented graphite of tape stripping.After Graphene is found, because its excellent performance and huge application prospect have caused the research boom in the fields such as physics and Materials science.But controlledly synthesis has the grapheme material problem of specific morphology not still to be resolved.Based on this, the research of Graphene still rests on fundamental research field, and the large-scale application of distance still has a segment distance.
Yet the realization of Graphene physicals and potential application be unable to do without the preparation of high quality, low cost, extensive Graphene.The current main method of preparing Graphene has: micromechanics stripping method, chemical Vapor deposition process, SiC surface greying method, organic molecule dispersion method, ion graft process, solvent-thermal method, oxidation reduction process, C doping liberation method etc.Micromechanics stripping method is to adopt ionic fluid to material surface etching, and by mechanical force, material surface is peeled off and prepared Graphene.But due to complex process, the Graphene productive rate of preparation is low, can not meet industrialization demand, has limited to a certain extent large-scale production.Chemical Vapor deposition process is to utilize chemical reaction at substrate surface, to form the film growth method of graphene film, the existing CH that passes through
4the CO that decomposes, reduces generates gaseous carbon atom, and product is deposited on substrate surface, generates two-dimentional graphene film.Due to CH
4decomposition temperature is very high, and this method can only be applicable to resistant to elevated temperatures a few materials substrate.SiC surface greying method is under ultrahigh vacuum(HHV), 4H-SiC or 6H-SiC to be heated to more than 1300 ℃, and after the Si atom of SiC plane of crystal is evaporated, carbon atom generation reconstruct just can generate two-dimentional graphene film on single crystalline Si face.The graphene film thickness that this method prepares is only 1～2 carbon atomic layer, has high carrier mobility.But in the Graphene for preparing in this way of profit, do not observe quantum hall effect, and the electronic property on Graphene surface is subject to the impact of SiC substrate very large, further research is still underway.Organic molecule dispersion method obtains graphite a kind of method of Graphene in organic solvent for ultrasonic dispersion, the Graphene defect that this method obtains is few, but concentration is not high.First ion graft process prepares compound between graphite layers, then in organic solvent, disperses to prepare Graphene, and it is lower that this method is prepared Graphene dispersity.Solvent-thermal method is that reactant is added to solvent, utilize solvent under higher than critical temperature and emergent pressure, can dissolve the character of most materials, can be that the reaction that can not occur under normal condition under high pressure can be carried out with lower temperature, or acceleration.This method development time is short, and present stage, many theory and technology problems still can not break through, and needs further to be explored.Oxidation reduction process is the graphene oxide that graphite oxidation is obtained disperseing in solution, then prepares Graphene with reductive agent reduction; Its cost is low, productive rate is high, but the graphite that strong oxidizer complete oxidation is crossed is difficult to reduce completely, causes performance, especially the electroconductibility loss of energies such as its some physics, chemistry.C doping liberation method is the GaAs material that utilizes MBE growth C doping, by improving temperature, GaAs is decomposed, and wherein C atom is separated out formation Graphene, and this method controllability is very low, and the Graphene mass ratio of generation is lower, still in the stage of fumbling.This just requires to improve existing preparation technology's level, and the preparation of Graphene at present remains the technical barrier in this field.
Chemical vapour deposition is a kind of deposition technique the most frequently used in semi-conductor industry.This side's ratio juris is the mode by chemical reaction, utilize the various energy such as heating, plasma excitation or optical radiation, in reactor, make the chemical substance of gaseous state or steam condition on gas phase or gas-solid interface, through chemical reaction, form the technology of solid deposited thing.
Summary of the invention
The invention provides a kind of process for preparing graphenes by chemical vapour deposition, by providing a kind of copper nickel to take the cupronickel substrate that is ratio in 53: 47 to improve Graphene in the suprabasil speed of growth.The preparation of Graphene is mainly divided into two kinds from growth mechanism: 1) charcoal mechanism is analysed in carburizing: the metal base for nickel etc. with higher molten carbon amount, the carbon atom that carbon source cracking produces infiltrates in metal base when high temperature, when cooling, from its inside, separate out nucleation again, and then growing graphene; 2) surface growth mechanism: the metal base for copper etc. with lower molten carbon amount, the carbon atom that under high temperature, gaseous carbon source cracking generates is adsorbed on metallic surface, and then nucleating growth becomes " Graphene island ", and obtain continuous graphene film by the two dimension on " Graphene island " merging of growing up.In this case, the temperature of cupronickel substrate is within the scope of 400～600 ℃, surface growth mechanism is deferred in the growth of Graphene, and compare as substrate with adopting fine copper film, adopting the ratio of cupronickel in substrate is 53: 47 o'clock, the speed of growth of graphene film is the fastest.Nickel has played the effect that promotes Graphene growth in Graphene process of growth.
For achieving the above object, the present invention is achieved through the following technical solutions:
A process for preparing graphenes by chemical vapour deposition, it is by following technical process:
Step 1, to select silicon single crystal be substrate, adopts the sputtering power of copper target and nickel target to be respectively 120～200W, 80～100W and take copper, the two target magnetic control co-sputtering methods of nickel and prepare thickness as 3～5 μ m cupronickel films at monocrystalline silicon surface;
Step 2, there is the monocrystal silicon substrate of cupronickel film to be transferred in the Reaktionsofen of chemical vapour deposition (CVD) surface deposition, in described Reaktionsofen, pass into the helium that flow velocity is 500sccm, continue to pass into 10min, drain the air in described Reaktionsofen;
Step 3, substrate is risen in 20～40min to 400～600 ℃, in described Reaktionsofen, continue to pass into helium afterwards, control pressure in described Reaktionsofen within the scope of 5～10Torr;
In step 4, maintenance CVD, the pressure of Reaktionsofen is within the scope of 5～10Torr, base reservoir temperature, at 400～600 ℃, passes into hydrogen afterwards in described Reaktionsofen, and the flow of hydrogen is 200～300sccm, to benzene injection in described Reaktionsofen, the injection speed of benzene is 100～150 μ l/min;
In step 5, maintenance CVD, the pressure of Reaktionsofen is within the scope of 5～10Torr, after benzene has been injected, stop passing into hydrogen, in described Reaktionsofen, pass into helium afterwards, the monocrystal silicon substrate that deposits cupronickel film is down to room temperature with 20 ℃/min speed, continues afterwards to pass into helium 10min;
Step 6, taking-up growth have the substrate of graphene film.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, described step 1 monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries under nitrogen environment.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, and the sputtering power of copper target 120～150W preferably in described step 1, the sputtering power of nickel target is 90～100W preferably.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, copper in described step 1, the two target magnetic control co-sputtering methods of nickel are in the condition of monocrystalline silicon surface deposited copper nickelalloy, and design parameter is as follows: sputtering chamber back end vacuum tightness is 5.0 * 10
-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, in described step 3, the temperature of cupronickel substrate is 400～500 ℃.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, in described step 4, the injection speed of benzene is constant speed, the injection speed of benzene is 120 μ l/min preferably.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, the flow that described step 5 passes into helium is 400～600sccm, preferably 450～500sccm.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, shifts in described step 6 method of graphene film in cupronickel substrate:
Step 1, polymethylmethacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface;
Step 2, drip and to have the sample of PMMA to put into FeCl
3in solution, after the cupronickel of sample erodes, the Graphene sample that scribbles PMMA swims in FeCl
3on solution;
Step 3, the graphene film that scribbles PMMA are put into acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, with copper mesh, picks up or transfer in other substrates to be measured.
A kind of process for preparing graphenes by chemical vapour deposition provided by the invention; its beneficial effect comprises: this preparation method's technical process is simple; production input cost is low; base reservoir temperature is lower, and consumes energy is few, and the copper nickel substrate of selection proper ratio has improved the speed of growth of graphene film; suitability for scale production; and the Graphene product of preparation: Area comparison is large, and quality purity is higher, and transmittance is high.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to specification sheets word.
Embodiment 1
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, is to make by following steps:
Step 1, to select silicon single crystal be substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries under nitrogen environment, and copper, the two target magnetic control co-sputtering methods of nickel are 5.0 * 10 in sputtering chamber back end vacuum tightness
-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that 120W, nickel target sputtering power are that under 90W condition, at monocrystalline silicon surface, to prepare thickness be 4 μ m cupronickel films;
Step 2, there is the monocrystal silicon substrate of cupronickel film to be transferred in the Reaktionsofen of chemical vapour deposition (CVD) surface deposition, in described Reaktionsofen, pass into the helium that flow velocity is 500sccm, continue to pass into 10min, drain the air in described Reaktionsofen;
Step 3, substrate is risen in 20min to 400 ℃, in described Reaktionsofen, continue to pass into helium afterwards, control pressure in described Reaktionsofen at 10Torr;
Step 4, keep the pressure of Reaktionsofen in CVD at 10Torr, base reservoir temperature, at 400 ℃, passes into hydrogen afterwards in described Reaktionsofen, and the flow of hydrogen is 200sccm, and to benzene injection in described Reaktionsofen, the injection speed of benzene is 120 μ l/min;
In step 5, maintenance CVD, the pressure of Reaktionsofen is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, in described Reaktionsofen, pass into helium afterwards, the flow of helium is 500sccm, the monocrystal silicon substrate that deposits cupronickel film is down to room temperature with 20 ℃/min speed, continues afterwards to pass into helium 10min;
Step 6, taking-up growth have the substrate of graphene film.
Step 7, graphene film not damaged is shifted: 1) polymethylmethacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl
3in solution, after the cupronickel of sample erodes, the Graphene sample that scribbles PMMA swims in FeCl
3on solution,
3) graphene film that scribbles PMMA is put into acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, with copper mesh, picks up or transfer in other substrates to be measured.
Embodiment 2
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, is to make by following steps:
Step 1, to select silicon single crystal be substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries under nitrogen environment, and copper, the two target magnetic control co-sputtering methods of nickel are 5.0 * 10 in sputtering chamber back end vacuum tightness
-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that 135W, nickel target sputtering power are that under 90W condition, at monocrystalline silicon surface, to prepare thickness be 4 μ m cupronickel films;
Step 2, there is the monocrystal silicon substrate of cupronickel film to be transferred in the Reaktionsofen of chemical vapour deposition (CVD) surface deposition, in described Reaktionsofen, pass into the helium that flow velocity is 500sccm, continue to pass into 10min, drain the air in described Reaktionsofen;
Step 3, substrate is risen in 20min to 400 ℃, in described Reaktionsofen, continue to pass into helium afterwards, control pressure in described Reaktionsofen at 10Torr;
Step 4, keep the pressure of Reaktionsofen in CVD at 10Torr, base reservoir temperature, at 400 ℃, passes into hydrogen afterwards in described Reaktionsofen, and the flow of hydrogen is 200sccm, and to benzene injection in described Reaktionsofen, the injection speed of benzene is 120 μ l/min;
In step 5, maintenance CVD, the pressure of Reaktionsofen is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, in described Reaktionsofen, pass into helium afterwards, the flow of helium is 500sccm, the monocrystal silicon substrate that deposits cupronickel film is down to room temperature with 20 ℃/min speed, continues afterwards to pass into helium 10min;
Step 6, taking-up growth have the substrate of graphene film.
Step 7, graphene film not damaged is shifted: 1) polymethylmethacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl
3in solution, after the cupronickel of sample erodes, the Graphene sample that scribbles PMMA swims in FeCl
3on solution,
3) graphene film that scribbles PMMA is put into acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, with copper mesh, picks up or transfer in other substrates to be measured.
Embodiment 3
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, is to make by following steps:
Step 1, to select silicon single crystal be substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries under nitrogen environment, and copper, the two target magnetic control co-sputtering methods of nickel are 5.0 * 10 in sputtering chamber back end vacuum tightness
-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that 150W, nickel target sputtering power are that under 90W condition, at monocrystalline silicon surface, to prepare thickness be 4 μ m cupronickel films;
Step 2, there is the monocrystal silicon substrate of cupronickel film to be transferred in the Reaktionsofen of chemical vapour deposition (CVD) surface deposition, in described Reaktionsofen, pass into the helium that flow velocity is 500sccm, continue to pass into 10min, drain the air in described Reaktionsofen;
Step 3, substrate is risen in 20min to 400 ℃, in described Reaktionsofen, continue to pass into helium afterwards, control pressure in described Reaktionsofen at 10Torr;
Step 4, keep the pressure of Reaktionsofen in CVD at 10Torr, base reservoir temperature, at 400 ℃, passes into hydrogen afterwards in described Reaktionsofen, and the flow of hydrogen is 200sccm, and to benzene injection in described Reaktionsofen, the injection speed of benzene is 120 μ l/min;
In step 5, maintenance CVD, the pressure of Reaktionsofen is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, in described Reaktionsofen, pass into helium afterwards, the flow of helium is 500sccm, the monocrystal silicon substrate that deposits cupronickel film is down to room temperature with 20 ℃/min speed, continues afterwards to pass into helium 10min;
Step 6, taking-up growth have the substrate of graphene film.
Step 7, graphene film not damaged is shifted: 1) polymethylmethacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl
3in solution, after the cupronickel of sample erodes, the Graphene sample that scribbles PMMA swims in FeCl
3on solution,
3) graphene film that scribbles PMMA is put into acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, with copper mesh, picks up or transfer in other substrates to be measured.
The cupronickel component that in above-mentioned three embodiment, different sputtering powers obtain is in Table 1:
Graphene product index prepared by above-mentioned 3 embodiment sees the following form 2
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment describing.
Claims (8)
1. a process for preparing graphenes by chemical vapour deposition, is characterized in that, comprising:
Step 1, to select silicon single crystal be substrate, adopts the sputtering power of copper target and nickel target to be respectively 120～200W, 80～100W and take copper, the two target magnetic control co-sputtering methods of nickel and prepare thickness as 3～5 μ m cupronickel films at monocrystalline silicon surface;
Step 2, there is the monocrystal silicon substrate of cupronickel film to be transferred in the Reaktionsofen of chemical vapour deposition (CVD) surface deposition, in described Reaktionsofen, pass into the helium that flow velocity is 500sccm, continue to pass into 10min, drain the air in described Reaktionsofen;
Step 3, substrate is risen in 20～40min to 400～600 ℃, in described Reaktionsofen, continue to pass into helium afterwards, control pressure in described Reaktionsofen within the scope of 5～10Torr;
In step 4, maintenance CVD, the pressure of Reaktionsofen is within the scope of 5～10Torr, base reservoir temperature, at 400～600 ℃, passes into hydrogen afterwards in described Reaktionsofen, and the flow of hydrogen is 200～300sccm, to benzene injection in described Reaktionsofen, the injection speed of benzene is 100～150 μ l/min;
In step 5, maintenance CVD, the pressure of Reaktionsofen is within the scope of 5～10Torr, after benzene has been injected, stop passing into hydrogen, in described Reaktionsofen, pass into helium afterwards, the monocrystal silicon substrate that deposits cupronickel film is down to room temperature with 20 ℃/min speed, continues afterwards to pass into helium 10min;
Step 6, taking-up growth have the substrate of graphene film.
2. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, described step 1 monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries under nitrogen environment.
3. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, the sputtering power of copper target 120～150W preferably in described step 1, and the sputtering power of nickel target is 90～100W preferably.
4. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, copper in described step 1, the two target magnetic control co-sputtering methods of nickel are in the condition of monocrystalline silicon surface deposited copper nickelalloy, and design parameter is as follows: sputtering chamber back end vacuum tightness is 5.0 * 10
-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa.
5. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, in described step 3, the temperature of cupronickel substrate is 400～500 ℃.
6. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, in described step 4, the injection speed of benzene is constant speed, and the injection speed of benzene is 120 μ l/min preferably.
7. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, the flow that described step 5 passes into helium is 400～600sccm, preferably 450～500sccm.
8. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, is characterized in that, shifts in described step 6 method of graphene film in cupronickel substrate:
Step 1, polymethylmethacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface;
Step 2, drip and to have the sample of PMMA to put into FeCl
3in solution, after the cupronickel of sample erodes, the Graphene sample that scribbles PMMA swims in FeCl
3on solution;
Step 3, the graphene film that scribbles PMMA are put into acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, with copper mesh, picks up or transfer in other substrates to be measured.
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| CN104328389A (en) * | 2014-10-24 | 2015-02-04 | 中国科学院合肥物质科学研究院 | Preparation method of graphene nano-net |
| CN104779015A (en) * | 2015-05-06 | 2015-07-15 | 南京汉能薄膜太阳能有限公司 | Preparation method for graphene transparent conducting thin film |
| CN106024111A (en) * | 2016-06-24 | 2016-10-12 | 成都天航智虹企业管理咨询有限公司 | Preparation method of conductive thin film |
| CN106158145A (en) * | 2016-06-24 | 2016-11-23 | 成都天航智虹企业管理咨询有限公司 | A kind of preparation method of graphene conductive film |
| CN106706710A (en) * | 2015-11-11 | 2017-05-24 | 中国科学院上海微***与信息技术研究所 | Nitrogen oxide gas sensor based on sulphur-doped graphene, and preparation method thereof |
| CN108033439A (en) * | 2018-01-02 | 2018-05-15 | 电子科技大学 | A kind of graphene low temperature preparation method of plasmaassisted sputtering solid-state carbon source |
| CN113148992A (en) * | 2021-03-31 | 2021-07-23 | 哈尔滨金纳科技有限公司 | Preparation method of small-size graphene |
| CN114107914A (en) * | 2021-11-12 | 2022-03-01 | 航天特种材料及工艺技术研究所 | Preparation method and application of graphene/metal film composite material |
| CN114867549A (en) * | 2019-12-19 | 2022-08-05 | 海科材料有限公司 | Method for preparing porous graphene membrane and membrane prepared using same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104328389A (en) * | 2014-10-24 | 2015-02-04 | 中国科学院合肥物质科学研究院 | Preparation method of graphene nano-net |
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| CN104779015A (en) * | 2015-05-06 | 2015-07-15 | 南京汉能薄膜太阳能有限公司 | Preparation method for graphene transparent conducting thin film |
| CN106706710A (en) * | 2015-11-11 | 2017-05-24 | 中国科学院上海微***与信息技术研究所 | Nitrogen oxide gas sensor based on sulphur-doped graphene, and preparation method thereof |
| CN106024111A (en) * | 2016-06-24 | 2016-10-12 | 成都天航智虹企业管理咨询有限公司 | Preparation method of conductive thin film |
| CN106158145A (en) * | 2016-06-24 | 2016-11-23 | 成都天航智虹企业管理咨询有限公司 | A kind of preparation method of graphene conductive film |
| CN108033439A (en) * | 2018-01-02 | 2018-05-15 | 电子科技大学 | A kind of graphene low temperature preparation method of plasmaassisted sputtering solid-state carbon source |
| CN114867549A (en) * | 2019-12-19 | 2022-08-05 | 海科材料有限公司 | Method for preparing porous graphene membrane and membrane prepared using same |
| CN113148992A (en) * | 2021-03-31 | 2021-07-23 | 哈尔滨金纳科技有限公司 | Preparation method of small-size graphene |
| CN113148992B (en) * | 2021-03-31 | 2022-10-25 | 哈尔滨金纳科技有限公司 | Preparation method of small-size graphene |
| CN114107914A (en) * | 2021-11-12 | 2022-03-01 | 航天特种材料及工艺技术研究所 | Preparation method and application of graphene/metal film composite material |
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