CN104724697A - New microwave assisted preparation method of graphene oxide - Google Patents
New microwave assisted preparation method of graphene oxide Download PDFInfo
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- CN104724697A CN104724697A CN201410422552.1A CN201410422552A CN104724697A CN 104724697 A CN104724697 A CN 104724697A CN 201410422552 A CN201410422552 A CN 201410422552A CN 104724697 A CN104724697 A CN 104724697A
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- graphite powder
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000013019 agitation Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 3
- 230000002687 intercalation Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000005304 joining Methods 0.000 claims description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 230000005855 radiation Effects 0.000 abstract description 6
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Abstract
The invention discloses a new microwave assisted preparation method of graphene oxide, which mainly comprises the following steps: 1) mixing graphite with an oxidant potassium permanganate in a strong acid environment; 2) preparing graphite oxide by using unreported low-power microwave radiation assisted intercalated graphite oxide powder; and 3) carrying out ultrasonic stripping on the graphite oxide in deionized water so as to obtain a graphene oxide sol. The yield of graphene oxide is higher than 95%. Compared with the prior art, the method disclosed by the invention is simple in preparation process, and especially through microwave radiation assisted graphite intercalated oxidation, the preparation time is greatly shortened; materials are fully reacted, so that the yield is increased; and the reproducibility is good, and an effect of large-scale production can be achieved.
Description
Technical field
The present invention relates to the novel method that a kind of microwave-assisted prepares graphene oxide.
Background technology
Graphene has sp
2six side's conjugated structures of hydridization, it is a kind of stable two dimensional crystal material, because it is in electricity, optics, the aspect such as calorifics and mechanics shows many excellent properties, greatly excite the research enthusiasm of association area scientific research personnel, in recent years about this material at energy storage [M.Pumera.Graphene-based nanomaterials for energy storage [J] .Energy Environ.Sci., 2011, (4), 668-674], liquid crystal device [P.Blake, P.D.Brimicombe, R.R.Nair, T.J.Booth.Graphene-Based Liquid Crystal Device [J] .Nano Lett., 2008, 8 (6): 1704-1708], electron device (N.O.Weiss, H.Zhou, L.Liao, Y.Liu.Graphene:An Emerging Electronic Material [J] .Adv.Mater., 2012, 24 (43): 5782-825] and support of the catalyst [M.M.Liu, R.Z.Zhang, and W.Chen.Graphene-Supported Nanoelectrocatalysts for Fuel Cells:Synthesis, Properties, and Applications [J] .Chem.Rev., 2014, 114 (10): 5117-5160] etc. the applied research report in field increases sharply, demonstrate the application prospect that this material is wide.
At present, the preparation method of Graphene has chemical Vapor deposition process, epitaxial growth method, mechanically peel method and oxidation reduction process.Because oxidation reduction process preparation technology is simple, with low cost, can be mass, so have high researching value.
Graphene oxide is that products therefrom is peeled off in the oxidation of lamellar graphite powder, due to its Two-dimensional Carbon skeleton and edge containing the oxy radical such as great amount of hydroxy group, carboxyl, even, stable Monolayer Dispersion system [D.R.Dreyer can be formed in water, A.D.Todd, C.W.Bielawski.Harnessing the chemistry of graphene oxide [J] .Chem.Soc.Rev., 2014,43:5288-5301].And these oxy radicals are easy and some chemical substances react, obtain modified graphene and graphene-based matrix material, as people such as Feng Yan, zinc oxide-redox graphene matrix material [Y.Feng by solvent-thermal method fabricated in situ, N.N.Feng, Y.Z.Wei, G.Y.Zhang.An in situ gelatin-assisted hydrothermal synthesis of ZnO – reduced graphene oxide composites with enhanced photocatalytic performance under ultraviolet and visible light [J] .RSC Adv., 2014, 4:7933-7943].Exactly because graphene oxide has above-mentioned good physical compatibility performance and Chemical bond performance, make it not only can be prepared Graphene by direct-reduction batch, also more how may for synthetic graphite olefinic base material provides.
There is the multiple method preparing graphene oxide at present, such as: publication number is the patent of CN103539108A is prepare graphite oxide by two-step penetration method, is then peeled off and prepares graphene oxide; Daniela C. etc. are that crystalline flake graphite oxidation is obtained graphite oxide by oxygenant under mixing acid environment and heating condition with potassium permanganate, then obtained graphene oxide [D.C.Marcano is peeled off, D.V.Kosynkin, J.M.Berlin.Improved Synthesis of Graphene Oxide [J] .ACS Nano, 2010,4 (8): 4806-4814]; The positive light of Zou etc. then pass through ultrasonic wave added Hummers legal system for graphene oxide [Zou Zhengguang, Yu Huijiang, Long Fei, Fan Yanhuang. ultrasonic wave added Hummers legal system is for graphene oxide [J]. Chinese Journal of Inorganic Chemistry, 2011,27 (9): 1753-1757], but these methods exist or complicated operation, length consuming time, or poor reproducibility, or degree of oxidation is uneven etc. not enough.Therefore, develop a kind of high-level efficiency, high yield, good stability, operating process is manageable, and to prepare graphite oxide new technology significant.
Summary of the invention
It take Graphite Powder 99 as the novel method that graphene oxide prepared by raw material that the present invention proposes a kind of; the method overcome low, the material reaction of productive rate that existing graphene oxide technology of preparing exists not exclusively, react uneven, the drawback such as length consuming time; and preparation process favorable reproducibility, is applicable to the needs of low cost, large-scale production.
The present invention is achieved by the following technical programs:
(1) be 800rmin at rotating speed
-1~ 2000rmin
-1magnetic agitation under, added in strong acid with strong oxidizer potassium permanganate by Graphite Powder 99 respectively and mix, wherein Graphite Powder 99 can be crystalline graphite powder, natural graphite powder, expanded graphite powder or expansible black lead powder; Potassium permanganate consumption is 1g Graphite Powder 99 potassium permanganate 3g ~ 6g; Strong acid can be the commercially available vitriol oil, also can be the mixing acid of the commercially available vitriol oil and strong phosphoric acid, V in mixing acid
the vitriol oil: V
strong phosphoric acid>=4:1, the mass concentration of the vitriol oil and strong phosphoric acid is all not less than 92%, and the consumption of acid is the sour 30ml ~ 100ml of 1g Graphite Powder 99.
(2) controlling stir speed (S.S.) is 800rmin
-1~ 2000rmin
-1, be 3kWm by power density
-2~ 10kWm
-2microwave irradiation step (1) gained mixed solution 15min ~ 85min, carry out microwave-assisted Graphite Powder 99 intercalation oxidation.
(3) joining in ice by step (2) gained reaction solution, the ice that 1g Graphite Powder 99 40ml ~ 150ml water is formed, is 500rmin at rotating speed
-1~ 1000rmin
-1magnetic agitation under, be hydrolyzed at 80 DEG C ~ 100 DEG C temperature reaction 30min ~ 70min;
(4) be 800rmin at rotating speed
-1~ 2000rmin
-1magnetic agitation under, use 0.2 ~ 2ml mass percentage to be the H of 30% by 1g Graphite Powder 99
2o
2consumption, in step (3) gained reaction solution, add H
2o
2, centrifugation gained throw out is first the hydrochloric acid washing precipitate of 5 ~ 20% with mass percentage, then with deionized water washing sediment to pH>=5, and it is dry under lower than the condition of 100 DEG C, obtains graphite oxide.
(5) step (4) gained graphite oxide is joined deionized water for ultrasonic to peel off, 1g graphite oxide deionized water 100ml ~ 350ml, ultrasonic power is 300W ~ 500W, and ultrasonic splitting time is 1h ~ 4h, centrifugal removing insoluble impurities, obtains graphene oxide colloidal sol.
Method of the present invention assists graphite intercalation to be oxidized by microwave radiation, and not only preparation process is simple, the more important thing is to substantially reduce the reaction times compared with existing synthetic method; and material reaction is abundant; production efficiency significantly improves, favorable reproducibility, can accomplish scale production.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the graphene oxide of preparation in embodiment 1.
Fig. 2 is transmission electron microscope (TEM) photo of the graphene oxide of preparation in embodiment 1.
Fig. 3 is the XRD figure spectrum of the graphene oxide of preparation in embodiment 2.
Fig. 4 is transmission electron microscope (TEM) photo of the graphene oxide of preparation in embodiment 2.
Fig. 5 is the XRD figure spectrum of the graphene oxide of preparation in embodiment 3.
Fig. 6 is transmission electron microscope (TEM) photo of the graphene oxide of preparation in embodiment 3.
Embodiment
The present invention is further illustrated below in conjunction with example, but and not as limiting to the invention.
Embodiment 1
Get the 50ml vitriol oil in beaker, at ice-water bath and 1000rmin
-1respectively to wherein adding 1g crystalline graphite powder and 4g potassium permanganate under agitation condition, be placed in microwave reaction instrument after mixing, control stir speed (S.S.) is 1000rmin
-1, be 8kWm by power density
-2microwave radiation 40min, then being added by reaction solution in the ice that 50ml water forms, is 800rmin at rotating speed
-1magnetic agitation and 98 DEG C of water bath condition under hydrolysis reaction 30min.Reaction solution is moved apart water-bath, is 900rmin at rotating speed
-1magnetic agitation downhill reaction liquid in drip the H that 0.5ml mass concentration is 30%
2o
2, centrifugation goes out precipitation, is first the hydrochloric acid washing precipitation twice of 10% by mass concentration, then is precipitated to pH=5 with deionized water wash.Precipitation is placed in air dry oven, and dry 24h at 90 DEG C, obtains graphite oxide.Taking 0.3g graphite oxide joins in 100ml distilled water, and control ultrasonic power is 400w, ultrasonic stripping 2h, and the insoluble impurity of centrifugal segregation, obtains graphene oxide colloidal sol, and graphene oxide yield is 95.4%.The XRD figure spectrum preparing gained graphite oxide is shown in Fig. 1, and its XRD figure spectrum only has the characteristic peak of graphite oxide (001), in 2 θ=11.6 °, ° not to occur the peak of graphite, illustrate that graphite is converted into graphite oxide completely in 2 θ=26.4.Fig. 2 is shown in by the TEM photo preparing gained graphene oxide, is shown as complete laminated structure.
Embodiment 2
Getting 100ml volume ratio is V
the vitriol oil: V
strong phosphoric acidthe mixing acid of=9:1 in beaker, at room temperature and 1800rmin
-1respectively to wherein adding 1g crystalline graphite powder and 6g potassium permanganate under agitation condition, be placed in microwave reaction instrument after mixing, control stir speed (S.S.) is 1900rmin
-1, be 3.8kWm by power density
-2microwave radiation 80min, then being added in the ice that 150ml water forms, is 1000rmin at rotating speed
-1magnetic agitation and 90 DEG C of water bath condition under hydrolysis reaction 60min.Reaction solution is moved apart water-bath, is 1400rmin at rotating speed
-1magnetic agitation downhill reaction liquid in drip the H that 1ml mass concentration is 30%
2o
2, centrifugation goes out precipitation, is first the hydrochloric acid washing precipitation twice of 15% by mass concentration, then is precipitated to pH=5 with deionized water wash.Precipitation is placed in air dry oven, dry 24h at 80 DEG C, arrives to obtain graphite oxide.Taking 0.4g graphite oxide joins in 100ml distilled water, and control ultrasonic power is 500w, ultrasonic stripping 1h, and the insoluble impurity of centrifugal segregation, obtains graphene oxide colloidal sol, and graphene oxide yield is 98.1%.The XRD figure spectrum preparing gained graphite oxide is shown in Fig. 3, and Fig. 4 is shown in by the TEM photo preparing gained graphene oxide.
Embodiment 3
Getting 50ml volume ratio is V
the vitriol oil: V
strong phosphoric acidthe mixing acid of=4:1 in beaker, at room temperature and 1200rmin
-1add 1g expanded graphite powder and 3g potassium permanganate respectively to it under agitation condition, be placed in microwave reaction instrument after mixing, control stir speed (S.S.) is 1200r/min, is 10kWm by power density
-2microwave radiation 15min, then being added in the ice that 100ml water forms, is 500rmin at rotating speed
-1magnetic agitation and under 80 DEG C of water bath condition hydrolysis reaction 60min.Reaction solution is moved apart water-bath, is 1800rmin at rotating speed
-1magnetic agitation under in reaction solution, drip the H that 0.2ml mass concentration is 30% while stirring
2o
2, centrifugation, is first the hydrochloric acid washing precipitation twice of 10% by mass concentration, then is precipitated to pH=6 with deionized water wash.Precipitation is placed in air dry oven, and dry 48h at 60 DEG C, obtains graphite oxide.Take 1g graphite oxide and add in 100ml water that to control ultrasonic power be 500w, ultrasonic stripping 2h, the undissolved impurity of centrifugal segregation obtains graphene oxide colloidal sol.Graphene oxide yield is 95.0%.The XRD figure spectrum preparing gained graphite oxide is shown in Fig. 5, and Fig. 6 is shown in by the TEM photo preparing gained graphene oxide.
Claims (2)
1. microwave-assisted prepares a novel method for graphene oxide, it is characterized in that synthesis step is as follows:
(1) be 800rmin at rotating speed
-1~ 2000rmin
-1magnetic agitation under, added in strong acid with strong oxidizer potassium permanganate by Graphite Powder 99 respectively and mix, wherein Graphite Powder 99 can be crystalline graphite powder, natural graphite powder, expanded graphite powder or expansible black lead powder; Potassium permanganate consumption is 1g Graphite Powder 99 potassium permanganate 3g ~ 6g; Strong acid can be the commercially available vitriol oil, also can be the mixing acid of the commercially available vitriol oil and strong phosphoric acid, V in mixing acid
the vitriol oil: V
strong phosphoric acid>=4:1, the mass concentration of the vitriol oil and strong phosphoric acid is all not less than 92%, and the consumption of acid is the sour 30ml ~ 100ml of 1g Graphite Powder 99.
(2) with microwave irradiation step (1) gained mixed solution, the oxidation of microwave-assisted Graphite Powder 99 intercalation is carried out.
(3) joining in ice by step (2) gained reaction solution, the ice that 1g Graphite Powder 99 40ml ~ 150ml water is formed, is 500rmin at rotating speed
-1~ 1000rmin
-1magnetic agitation under, be hydrolyzed at 80 DEG C ~ 100 DEG C temperature reaction 30min ~ 70min.
(4) be 800rmin at rotating speed
-1~ 2000rmin
-1magnetic agitation under, use 0.2ml ~ 2ml mass percentage to be the H of 30% by 1g Graphite Powder 99
2o
2consumption, in step (3) gained reaction solution, add H
2o
2, after centrifugation is carried out to gained throw out, then be the hydrochloric acid washing precipitate of 5 ~ 20% with mass percentage, finally with deionized water washing sediment to pH>=5, it is dry under lower than the condition of 100 DEG C, obtain graphite oxide.
(5) step (4) gained graphite oxide is joined deionized water for ultrasonic to peel off, 1g graphite oxide deionized water 100ml ~ 350ml, ultrasonic power is 300W ~ 500W, and ultrasonic splitting time is 1h ~ 4h, centrifugal removing insoluble impurities, obtains graphene oxide colloidal sol.
2. a kind of microwave-assisted as claimed in claim 1 prepares the novel method of graphene oxide, it is characterized in that, in step (2), during with microwave irradiation step (1) gained mixed solution, need be 800rmin in stir speed (S.S.)
-1~ 2000rmin
-1, Microwave Power Density is 3kWm
-2~ 10kWm
-2condition under carry out, radiated time is 15min ~ 85min.
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| CN104724697B CN104724697B (en) | 2016-08-31 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088391A (en) * | 2015-07-17 | 2015-11-25 | 黑龙江大学 | Poly(p-phenylene vinylene)/graphene composite nanofiber material and preparation method thereof |
| CN106082197A (en) * | 2016-06-21 | 2016-11-09 | 哈尔滨工业大学 | A kind of method of microwave Fast back-projection algorithm graphite oxide and application |
| CN106477572A (en) * | 2016-10-24 | 2017-03-08 | 上海电力学院 | A kind of method that ultrasonic wave added method prepares graphene oxide |
| WO2018024196A1 (en) * | 2016-08-02 | 2018-02-08 | 福建新峰二维材料科技有限公司 | Preparation method for graphene nanometer material |
| CN108101034A (en) * | 2018-01-18 | 2018-06-01 | 莆田市超维二维科技发展有限公司 | A kind of device and method using microwave irradiation one-step method volume production graphene |
| CN109181654A (en) * | 2018-09-13 | 2019-01-11 | 江苏成康石墨烯科技有限公司 | A kind of graphene-based composite heat conduction film and preparation method thereof and its application |
| CN109562931A (en) * | 2016-04-13 | 2019-04-02 | 绿色纳米技术实验室有限责任公司 | The low cost and fast method of graphene and graphene oxide are largely prepared with rich carbon natural material |
| CN112174122A (en) * | 2020-09-30 | 2021-01-05 | 李素红 | Antibacterial graphene nano knife and preparation method and application thereof |
| CN112452686A (en) * | 2020-12-11 | 2021-03-09 | 安徽威能电源科技有限公司 | Surface treatment method for improving antistatic performance of electronic component |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088391A (en) * | 2015-07-17 | 2015-11-25 | 黑龙江大学 | Poly(p-phenylene vinylene)/graphene composite nanofiber material and preparation method thereof |
| CN109562931A (en) * | 2016-04-13 | 2019-04-02 | 绿色纳米技术实验室有限责任公司 | The low cost and fast method of graphene and graphene oxide are largely prepared with rich carbon natural material |
| CN109562931B (en) * | 2016-04-13 | 2023-09-08 | 绿色纳米技术实验室有限责任公司 | Low-cost and rapid method for preparing graphene and graphene oxide in large quantity by using carbon-rich natural material and application thereof |
| CN106082197A (en) * | 2016-06-21 | 2016-11-09 | 哈尔滨工业大学 | A kind of method of microwave Fast back-projection algorithm graphite oxide and application |
| WO2018024196A1 (en) * | 2016-08-02 | 2018-02-08 | 福建新峰二维材料科技有限公司 | Preparation method for graphene nanometer material |
| CN106477572A (en) * | 2016-10-24 | 2017-03-08 | 上海电力学院 | A kind of method that ultrasonic wave added method prepares graphene oxide |
| CN108101034A (en) * | 2018-01-18 | 2018-06-01 | 莆田市超维二维科技发展有限公司 | A kind of device and method using microwave irradiation one-step method volume production graphene |
| CN109181654A (en) * | 2018-09-13 | 2019-01-11 | 江苏成康石墨烯科技有限公司 | A kind of graphene-based composite heat conduction film and preparation method thereof and its application |
| CN112174122A (en) * | 2020-09-30 | 2021-01-05 | 李素红 | Antibacterial graphene nano knife and preparation method and application thereof |
| CN112452686A (en) * | 2020-12-11 | 2021-03-09 | 安徽威能电源科技有限公司 | Surface treatment method for improving antistatic performance of electronic component |
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|---|---|
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