CN112479193A - Graphene surface charged modification method - Google Patents
Graphene surface charged modification method Download PDFInfo
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- CN112479193A CN112479193A CN202011500139.4A CN202011500139A CN112479193A CN 112479193 A CN112479193 A CN 112479193A CN 202011500139 A CN202011500139 A CN 202011500139A CN 112479193 A CN112479193 A CN 112479193A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 61
- 238000002715 modification method Methods 0.000 title claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000000701 coagulant Substances 0.000 claims abstract description 16
- 238000011282 treatment Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 22
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 239000003431 cross linking reagent Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000292 calcium oxide Substances 0.000 claims description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 11
- 239000011787 zinc oxide Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical group CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910001290 LiPF6 Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a graphene surface charged modification method, which comprises a plurality of preparation steps: comprises a step 1, a step 2, a step 3 and a step 4. And 3, continuously heating the mixture obtained in the step two, adding an initiator, a coagulant and a silane coupling agent, evaporating to remove an organic solvent, heating to completely solidify the high molecular polymer, fully stirring and granulating in the heating process to obtain the graphite composite material with the surface coated with the high molecular polymer, cooling to room temperature, and carrying out conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer cooled in the step 3. The invention has the advantages of ensuring that the polymer is completely coated on the graphite surface and ensuring that the coating amount is the same each time.
Description
Technical Field
The invention relates to the technical field of graphene modification methods, in particular to a graphene surface charged modification method.
Background
Carbon is known to form many different allotropes (allotropes). Allotropes such as diamond (where a face-centered cubic lattice decorates the motif of two sp 3-hybridized tetrahedrally arranged carbon atoms per primary unit cell) or graphite (where sp 2-hybridized carbon atoms are hexagonally arranged to form planar sheets, with adjacent sheets held together by weak van der waals interactions) have long been known. Other carbon-based structures such as graphene, buckminsterfullerenes (buckminsterfullerenes), carbon nanotubes, carbon nanoribbons, diamond-like carbon, and amorphous carbon have only recently been discovered.
Graphene has attracted particular attention because of its unusual electronic, thermal and mechanical properties. One particular graphene material is known as 2D graphene. This is a single two-dimensional sp-bonded sheet of carbon atoms arranged in a hexagonal lattice, essentially a single graphite monolayer. 2D graphene is a zero gap semiconductor with a resistivity of about 10-6 Ω cm at room temperature and electron mobility greater than 15000cm 2/Vs. 2D graphene is finding application in electronics, but especially in the nanoscale electronics field. However, there are significant challenges in scaling up 2D graphene fabrication methods, which typically require exfoliation of graphite and transfer of exfoliated graphene sheets to a substrate, or complex deposition methods involving physical or chemical vapor deposition combined with post-deposition annealing treatment.
The invention patent of China (a modified graphite and a preparation method thereof, CN1581544) discloses a graphite particle which has excellent heavy current performance and longer cycle life, and the particle is characterized in that graphite core material particles are immersed in a polymer surface modifier solution for stirring treatment, separation, sieving, solidification and carbonization, but the separation of a solvent in the method adopts filtration or centrifugation, which can not ensure that the polymer is completely coated on the graphite surface, and the coating amount of each time is difficult to ensure to be the same.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a graphene surface electrification modification method, which has the advantages of ensuring that a polymer is completely coated on the graphite surface and ensuring that the coating amount is the same each time.
In order to achieve the purpose, the invention provides the following technical scheme: a graphene surface charging modification method comprises the following steps:
step 1: dissolving a graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05-0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% -7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: (18-22);
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1-2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
Preferably, the high molecular polymer is epoxy resin.
Preferably, zinc oxide and calcium oxide are further added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
In conclusion, the invention has the following beneficial effects:
the invention combines the dipping and the solvent evaporation treatment in the heating and curing process, thereby simplifying the process; the prepared modified graphene solution does not agglomerate, does not need crushing treatment, reduces equipment investment and is beneficial to large-scale production; the modified graphite, especially the modified natural graphite, as the carbon negative electrode material has longer cycle life and better heavy current discharge performance, and zinc oxide and calcium oxide are added to enhance the overall physical performance.
Detailed Description
The present invention is further explained.
Example 1: a graphene surface charging modification method comprises the following steps:
step 1: dissolving a graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 18;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
Example 2: a graphene surface charging modification method comprises the following steps:
step 1: dissolving a graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.1% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 6% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 20;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1.5 percent of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
Example 3: a graphene surface charging modification method comprises the following steps:
step 1: dissolving a graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 22;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the design concept of the present invention should be included in the scope of the present invention.
Claims (3)
1. A graphene surface electrification modification method is characterized by comprising the following steps: the method comprises the following steps:
step 1: dissolving a graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05-0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% -7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: (18-22);
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1-2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
2. The method for modifying the surface charge of the graphene according to claim 1, wherein: the high molecular polymer is epoxy resin.
3. The method for modifying the surface charge of the graphene according to claim 1, wherein: zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
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| CN202011500139.4A CN112479193A (en) | 2020-12-17 | 2020-12-17 | Graphene surface charged modification method |
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| CN202011500139.4A CN112479193A (en) | 2020-12-17 | 2020-12-17 | Graphene surface charged modification method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112429728A (en) * | 2020-12-17 | 2021-03-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene material suitable for cold spraying |
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| CN107868191A (en) * | 2017-11-06 | 2018-04-03 | 华南师范大学 | A kind of method of modifying of graphene |
| CN108299681A (en) * | 2018-01-05 | 2018-07-20 | 广东纳路纳米科技有限公司 | A kind of method of high polymer cladding two-dimensional nano sheet material |
| CN109455710A (en) * | 2018-12-29 | 2019-03-12 | 西北大学 | A method of the functional monomer polymeric modification graphene based on non-covalent bond |
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2020
- 2020-12-17 CN CN202011500139.4A patent/CN112479193A/en active Pending
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| CN101209837A (en) * | 2006-12-27 | 2008-07-02 | 宁波杉杉新材料科技有限公司 | Modification method of graphite and modified graphite |
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| CN112429728A (en) * | 2020-12-17 | 2021-03-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene material suitable for cold spraying |
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Application publication date: 20210312 |