CN103540786B - Preparation method of graphene/copper-nickel nano composite material - Google Patents
Preparation method of graphene/copper-nickel nano composite material Download PDFInfo
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- CN103540786B CN103540786B CN201310528409.6A CN201310528409A CN103540786B CN 103540786 B CN103540786 B CN 103540786B CN 201310528409 A CN201310528409 A CN 201310528409A CN 103540786 B CN103540786 B CN 103540786B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 29
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910000570 Cupronickel Inorganic materials 0.000 title claims abstract description 15
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000002815 nickel Chemical class 0.000 claims abstract description 14
- 150000001879 copper Chemical class 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 230000003750 conditioning effect Effects 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002086 nanomaterial Substances 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- -1 softex kw Chemical compound 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of nano inorganic functional materials, and relates to a preparation method of a graphene/copper-nickel nano composite material. The preparation method comprises the following steps: first, placing graphene oxide in deionized water for ultrasonic centrifugation to obtain a graphene suspension; then, dissolving sodium hydroxide in deionized water to prepare alkaline liquor; then, respectively dissolving copper salt and nickel salt in deionized water, stirring till copper salt and nickel salt are fully dissolved, and preparing copper salt and nickel salt liquor; placing the prepared alkaline liquor, and copper salt and nickel salt liquor in a flask to uniformly stir, and adding ethanediamine, hydrazine hydrate and a surface treating agent to stir, and then adding into the graphene suspension for reaction; cleaning, centrifugalizing and drying products obtained by reaction for 2-3 hours to obtain the graphene/copper-nickel nano composite material. The graphene/copper-nickel nano composite material is simple in preparation process, convenient to operate, low in cost, environment-friendly and easy for production on a large scale.
Description
Technical field:
The invention belongs to nano inorganic functional material preparing technical field, relate to a kind of preparation method of graphene/copper-nicknano nano composite material, both made full use of the premium properties of Graphene, and again in conjunction with copper nickel metal material electromagnetically, made this composite have electro-magnetic wave absorption performance.
Background technology:
Along with the development of science and technology, various electronic product is day by day universal in daily life, thing followed electromagnetic radiation and electromagnetic pollution are extensively present in the surroundings of people, greatly have impact on the life of people, therefore in the urgent need to preparing the electromagnetic wave absorbent material (abbreviation absorbing material) of function admirable, to reduce electromagnetic pollution; Simultaneously, absorbing material will play a significant role in the military affairs trial of strength of countries in the world, in modern war, weaponry stealthyization can break existing attacking and defending general layout, improves viability and the fighting efficiency of weapon, such as, when multi-section radar or communication apparatus use simultaneously, can signal disturbing be produced between each equipment, can interference be reduced at equipment surface coating electromagnetic wave absorbent material, improve the performance of each equipment.Therefore the absorbing material that processability is excellent is in civilian or all have great importance in Military Application.
In recent years, Graphene caused the extensive concern of scientist because of the performance of its uniqueness, and the two dimensional crystal structure that single-layer graphene is made up of hexatomic ring is a kind of semiconductor not having energy gap, has higher electron mobility (2 × 10
5cm
2/ V), large specific area (2600m
2/ g) and high mechanical strength (130GPa), therefore Graphene has potential application prospect in fields such as nano electron device, gas sensor and composites, in electromagnetic absorption, compared with other material with carbon elements, as CNT and carbon black, Graphene has larger specific area, thus provides larger electro-magnetic wave contacts area, is conducive to electromagnetic absorption.Less at the application report in electro-magnetic wave absorption field about Graphene at present, and complicated process of preparation, process is loaded down with trivial details.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence, seek to design the preparation method that a kind of Graphene/copper nickel composite function nano material is provided, adopt one-step synthesis to reduce copper ion and nickel ion simultaneously and prepare graphene/copper-nicknano nano composite material, both the premium properties of Graphene had been made full use of, tie again copper nickel metal material electromagnetically, made this composite have unique electro-magnetic wave absorption performance.
To achieve these goals, concrete preparation process of the present invention is:
(1), existing Hummers method is adopted to prepare graphene oxide;
(2), first graphene oxide is placed in deionized water, ultrasonic 12 hours, and gets supernatant liquor after centrifugal 4 minutes under 8000rpm condition, obtain the graphene suspension that graphene oxide concentration is 0.05g/L ~ 5g/L;
(3), again NaOH is dissolved in deionized water for stirring to solution clarify and be cooled to room temperature preparation obtain the alkaline solution that pH is 10 ~ 13; Then mantoquita and nickel salt are dissolved in respectively deionized water for stirring to dissolving completely, it is 0.1 ~ 1mol/L copper salt solution and nickel salt solution that preparation obtains concentration;
(4), step (3) is prepared the alkaline solution, copper salt solution and the nickel salt solution that obtain to be placed in flask according to the ratio that volume ratio is 30:0.1:0.3 and to stir, add in flask again 0.1 ~ 1mL weight percent concentration be 99% ethylenediamine, 0.02 ~ 0.5mL weight percent concentration be after 80% hydrazine hydrate and surface conditioning agent stir, add the graphene suspension that step (2) obtains, continue to stir, under 50 ~ 95 DEG C of temperature conditions, react 0.5 ~ 12h, wherein the mol ratio of surface conditioning agent and nickel salt is 3 ~ 50:1;
(5) the product washed with de-ionized water, by step (4) be obtained by reacting 3-5 time, under the condition of 8000 revs/min after centrifugal 5 minutes, the baking oven putting into 60 ~ 80 DEG C prepares graphene/copper-nicknano nano composite material after dry 2 ~ 3 hours.
The mantoquita that the present invention relates to is copper nitrate or copper chloride; Nickel salt is nickel nitrate or nickel chloride; Surface conditioning agent is the combination of one or more in urea, hexadecylamine, lauryl sodium sulfate, softex kw (CTAB), hexamethylenetetramine, polyvinylpyrrolidone (PVP), polyethylene glycol.
The pattern of the copper nickel nano material in graphene/copper-nicknano nano composite material prepared by the present invention is linear or spherical, and wherein the diameter of linear copper nickel nanometer is 2 ~ 500nm, and length is 5nm ~ 100 μm; The diameter of spherical copper nickel nanometer is 2nm ~ 1 μm.
The present invention compared with prior art, by graphene/copper-nicknano nano composite material one-step synthesis, reaches object quick, energy-conservation, simple to operate, both can reduce preparation cost, can obtain again the Graphene composite functional material of Load Balanced, good dispersion; Its preparation technology is simple, and easy to operate, cost is low, and environmental friendliness is easy to large-scale production.
Accompanying drawing illustrates:
Fig. 1 is SEM (SEM) picture of graphene/copper-nicknano nano composite material prepared by the embodiment of the present invention 1.
Fig. 2 is X-ray diffraction (XRD) the test curve schematic diagram of the graphene/copper-nicknano nano composite material being the embodiment of the present invention 1 preparation.
Fig. 3 is the absorbing property test result curve synoptic diagram of graphene/copper-nicknano nano composite material prepared by the embodiment of the present invention 1.
Fig. 4 is SEM (SEM) picture of graphene/copper-nicknano nano composite material prepared by the embodiment of the present invention 2.
Fig. 5 is the absorbing property test result curve synoptic diagram of graphene/copper-nicknano nano composite material prepared by the embodiment of the present invention 2.
Detailed description of the invention:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment 1:
The present embodiment is with Xiao Suan Tong ﹑ Xiao Suan Nie ﹑ graphene oxide for graphene/copper-nicknano nano composite material prepared by raw material, and wherein, the pattern of copper nickel nano material is linear; Its concrete preparation process is:
(1), traditional Hummers method is adopted to prepare graphene oxide;
(2), 20mg graphene oxide is placed in 100mL deionized water, ultrasonic 12h, the centrifugal 4min of 8000rpm, get supernatant liquor, supernatant liquor is dispersed individual layer or multilayer graphene oxide preferably, the Graphene of bottom is dried and weighs, show that the concentration of graphene oxide in supernatant liquor is 0.4g/L;
(3), take 70g NaOH and be dissolved in deionized water for stirring and clarify to solution, be cooled to room temperature, be mixed with the strong alkali solution that concentration is 7mol/L; Take 0.6g nitrate trihydrate copper again and 0.73g six water nickel nitrate is dissolved in deionized water respectively, be stirred to and dissolve completely, be mixed with copper nitrate solution and the 0.5mol/L nickel nitrate solution of 0.5mol/L;
(4), getting 60mL sodium hydroxide solution is put in there-necked flask, get 0.2mL copper nitrate solution, 0.6mL nickel nitrate solution, 0.6mL ethylenediamine (99wt%) and 0.05mL hydrazine hydrate (80wt%) to be again put in flask respectively and to stir, then be that 0.4g/L graphene oxide 60mL pours in flask and stirs by concentration, be incubated 2h after being warming up to 80 DEG C and react;
(5), by the product washed with de-ionized water that obtains 3-5 time, be positioned over dry 3h in 70 DEG C of baking ovens after centrifugation, obtain the graphene/copper-nicknano nano composite material powder of black.
Embodiment 2:
The present embodiment is with Xiao Suan Tong ﹑ Xiao Suan Nie ﹑ graphene oxide for graphene/copper-nicknano nano composite material prepared by raw material, and wherein, copper nickel appearance of nano material is spherical; Its concrete preparation process is:
(1), traditional Hummers method is adopted to prepare graphene oxide;
(2), 20mg graphene oxide is placed in 100mL deionized water, ultrasonic 12h, the centrifugal 4min of 8000rpm, get supernatant liquor, supernatant liquor is dispersed individual layer or multilayer graphene oxide preferably, dried by the Graphene of bottom and weigh, the concentration calculating graphene oxide in supernatant liquor is 0.4g/L;
(3), take 70g NaOH and be dissolved in deionized water for stirring and clarify to solution, be cooled to room temperature, preparation becomes the strong alkali solution that concentration is 7mol/L; Take 0.604g nitrate trihydrate copper and 0.727g six water nickel nitrate again and be dissolved in deionized water for stirring respectively to dissolving completely, be mixed with copper nitrate solution and the 0.5mol/L nickel nitrate solution of 0.5mol/L;
(4), get 60mL sodium hydroxide solution and be put in there-necked flask, 0.2mL copper nitrate solution, 0.6mL nickel nitrate solution, 0.6mL ethylenediamine (99wt%), 0.05mL hydrazine hydrate (80wt%) and 0.43g urea are put in flask respectively and stir; Be that 0.4g/L graphene oxide 60mL pours in flask and stirs again by concentration, be incubated 6h after being warming up to 70 DEG C and react;
(5), by the product washed with de-ionized water that obtains 3-5 time, after centrifugation, be positioned over dry 3h in 70 DEG C of baking ovens, obtain the graphene/copper-nicknano nano composite material powder of black.
Claims (3)
1. a preparation method for graphene/copper-nicknano nano composite material, is characterized in that concrete preparation process is:
(1), existing Hummers method is adopted to prepare graphene oxide;
(2), first graphene oxide is placed in deionized water, ultrasonic 12 hours, and gets supernatant liquor after centrifugal 4 minutes under 8000rpm condition, obtain the graphene suspension that graphene oxide concentration is 0.05g/L ~ 5g/L;
(3), again NaOH is dissolved in deionized water for stirring to solution clarify and be cooled to room temperature preparation obtain the alkaline solution that pH is 10 ~ 13; Then mantoquita and nickel salt are dissolved in respectively deionized water for stirring to dissolving completely, it is 0.1 ~ 1mol/L copper salt solution and nickel salt solution that preparation obtains concentration;
(4), step (3) is prepared the alkaline solution, copper salt solution and the nickel salt solution that obtain to be placed in flask according to the ratio that volume ratio is 30:0.1:0.3 and to stir, add respectively in flask again 0.1 ~ 1mL weight percent concentration be 99% ethylenediamine, 0.02 ~ 0.5mL weight percent concentration be after 80% hydrazine hydrate and surface conditioning agent stir, add the graphene suspension that step (2) obtains, continue to stir, under 50 ~ 95 DEG C of temperature conditions, react 0.5 ~ 12h, wherein added surface conditioning agent and the mol ratio of nickel salt are 3 ~ 50:1;
(5) the product washed with de-ionized water, by step (4) be obtained by reacting 3-5 time, under the condition of 8000 revs/min after centrifugal 5 minutes, the baking oven putting into 60 ~ 80 DEG C prepares graphene/copper-nicknano nano composite material after dry 2 ~ 3 hours.
2. the preparation method of graphene/copper-nicknano nano composite material according to claim 1, is characterized in that the mantoquita related to is copper nitrate or copper chloride; Nickel salt is nickel nitrate or nickel chloride; Surface conditioning agent is one or more the combination in urea, hexadecylamine, lauryl sodium sulfate, softex kw, hexamethylenetetramine, polyvinylpyrrolidone and polyethylene glycol.
3. the preparation method of graphene/copper-nicknano nano composite material according to claim 1, it is characterized in that the pattern of copper nickel nano material in the graphene/copper-nicknano nano composite material prepared is linear or spherical, wherein the diameter of linear copper nickel nanometer is 2 ~ 500nm, and length is 5nm ~ 100 μm; The diameter of spherical copper nickel nanometer is 2nm ~ 1 μm.
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| CN104569097B (en) * | 2014-12-17 | 2018-01-12 | 浙江理工大学 | The preparation method and applications of copper nano-wire graphene complex modified electrode |
| CN104475753B (en) * | 2014-12-29 | 2016-06-29 | 黑龙江大学 | Liquid phase reduction prepares graphene-supported nanometer of Cu3.8The method of Ni alloy |
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| CN105695788B (en) * | 2016-04-08 | 2017-11-21 | 上海和伍复合材料有限公司 | A kind of graphene enhancing nickel-base composite material and preparation method thereof |
| CN107037091B (en) * | 2016-11-15 | 2019-03-12 | 许美凤 | A kind of preparation method of electric transducer |
| CN106591822B (en) * | 2016-11-28 | 2018-10-19 | 广东工业大学 | A kind of graphene strengthens the preparation method and application of copper-based composite coating |
| CN106636711B (en) * | 2016-12-15 | 2018-06-29 | 中国航空工业集团公司北京航空材料研究院 | A kind of preparation method of graphene enhancing monel metal |
| CN108264041B (en) * | 2016-12-31 | 2019-12-24 | 哈尔滨工业大学 | Graphene oxide/copper oxide composite powder, preparation method thereof and preparation method of graphene/copper composite material with micro-layered structure |
| CN106993403B (en) * | 2017-04-18 | 2020-07-24 | 郑州航空工业管理学院 | Bar-shaped CuNi compound loaded graphene wave-absorbing material and preparation method thereof |
| CN108624775A (en) * | 2018-04-20 | 2018-10-09 | 西安理工大学 | A kind of the graphene enhancing Cu-base composites and preparation method of supported copper |
| CN109181175A (en) * | 2018-09-12 | 2019-01-11 | 芦露华 | A kind of fever composite material and preparation method of graphene and bimetal nano line |
| CN110039848B (en) * | 2019-04-16 | 2021-08-06 | 广州金穗芯能科技有限公司 | Graphene-loaded nickel nanoparticle composite structure and preparation method thereof |
| CN110922742A (en) * | 2019-10-31 | 2020-03-27 | 深圳市超导新材料有限公司 | Novel transparent conductive film and preparation method thereof |
| CN113927041B (en) * | 2021-09-17 | 2022-10-11 | 中国科学院深圳先进技术研究院 | Graphene copper-based composite material and preparation method and application thereof |
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| KR101337994B1 (en) * | 2010-04-14 | 2013-12-06 | 한국과학기술원 | Graphene/metal nanocomposite powder and method of manufacturing thereof |
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| CN103263921A (en) * | 2013-06-04 | 2013-08-28 | 中国科学院山西煤炭化学研究所 | Metal/graphene catalyst and preparation method thereof |
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