CN111620326A - Preparation method of fluorinated graphene material with adjustable fluorine content - Google Patents
Preparation method of fluorinated graphene material with adjustable fluorine content Download PDFInfo
- Publication number
- CN111620326A CN111620326A CN202010344637.8A CN202010344637A CN111620326A CN 111620326 A CN111620326 A CN 111620326A CN 202010344637 A CN202010344637 A CN 202010344637A CN 111620326 A CN111620326 A CN 111620326A
- Authority
- CN
- China
- Prior art keywords
- fluorinated graphene
- fluorine content
- steps
- following
- graphene material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
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
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- 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
- C01B32/10—Carbon fluorides, e.g. [CF]nor [C2F]n
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of a fluorinated graphene material with adjustable fluorine content, which comprises the following steps: (1) uniformly mixing the mixed metal salt and graphite fluoride, wherein the mixing method can be grinding or ball milling; wherein the mixed metal salt is NaCl and CaCl2、LiCl、BaCl2And ZnCl2(ii) the melting point of the mixed metal salt is less than 550 ℃; the mass ratio of the mixed metal salt to the graphite fluoride is 4: 1-1: 1; (2) placing the mixed product in a tube furnace to react for a period of time at 550 ℃; (3) and (3) ultrasonically stripping the reaction product in a mixed solution of an organic solvent and hydrogen fluoride, centrifugally separating out an upper layer solution, performing suction filtration and washing, and performing vacuum drying to obtain the fluorinated graphene. The synthetic method has the advantages of low requirement on equipment, simple process, strong operability and easy amplification.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to a preparation method of a fluorinated graphene material with adjustable fluorine content.
[ background of the invention ]
Since the first successful preparation of fluorinated graphene by the group of the project geom in 2010, fluorinated graphene attracts much attention due to its unique structure, excellent electrical properties and broad application prospects. The fluorinated graphene is a novel nano material in a graphene family, and fluorine atoms are introduced on the basis of retaining a two-dimensional planar structure of the graphene. The out-of-plane fluorine atoms interact with carbon atoms either covalently or ionically. The introduction of fluorine atoms not only reduces the surface energy of graphene and widens the band gap, but also endows the graphene with outstanding interface and physicochemical properties such as strong hydrophobicity, excellent mechanical properties and high stability. The fluorinated graphene has the structural and performance characteristics of two materials, namely graphene and teflon, is called as 'two-dimensional teflon', has the chemical properties similar to those of polytetrafluoroethylene, is very stable in chemical and physical properties, has the corrosion resistance of acid and alkali resistance, and has certain high temperature resistance. The unique properties enable the coating to have wide application prospects in the fields of ultrathin high-stability coatings, super-hydrophobic and oleophobic interfaces, lubricating materials, novel nano electronic devices, energy sources and the like. For example, it can be used for tunnel barriers or high quality insulators or barrier materials, as well as for light emitting diodes and displays. Meanwhile, the fluorinated graphene can be applied to the fields of lithium primary battery anode materials, stem cell growth support materials, magnetic resonance imaging, quantum dots, electrochemical sensing and the like.
The current methods for preparing fluorinated graphene can be divided into two types, one is a physical method, mainly a method for peeling off fluorinated graphite, the yield of the fluorinated graphene obtained by the method is not high, the fluorinated graphene is mostly a sheet with a small size, and an organic solvent or a reagent used in the peeling process is often toxic and difficult to remove. The other is a chemical process, mainly a graphene fluorination process, a graphene oxide fluorination process and an exfoliated graphite fluorination process. Some of the methods adopt graphene as a raw material, but the preparation is difficult and the price is high, so that the synthesis cost is too high; in addition, most of the fluorinating agents used are fluorine gas and XeF2And so on. The fluorination reagents have high toxicity, serious environmental pollution and difficult acquisition, and the reaction has higher requirements on equipment, experimental conditions and operation. At present, the research on fluorinated graphene is still in the initial stage, and the preparation method of fluorinated graphene is not mature. This also makes the large-scale preparation impossible and limits the application, so finding a suitable method for preparing fluorinated graphene is a research effort of many scientific researchersAnd (4) direction.
[ summary of the invention ]
The invention aims to solve the technical problem of providing a preparation method of a fluorinated graphene material with adjustable fluorine content, and the synthesis method has the advantages of low requirement on equipment, simple process, strong operability and easiness in amplification.
The invention is realized by the following steps:
a preparation method of a fluorinated graphene material with adjustable fluorine content comprises the following steps:
(1) uniformly mixing the mixed metal salt and graphite fluoride, wherein the mixing method can be grinding or ball milling;
(2) placing the mixed product in a tube furnace to react for a period of time at 550 ℃;
(3) and (3) ultrasonically stripping the reaction product in a mixed solution of an organic solvent and hydrogen fluoride, centrifugally separating out an upper layer solution, performing suction filtration and washing, and performing vacuum drying to obtain the fluorinated graphene.
Further, the mixed metal salt in the step (1) is NaCl and CaCl2、LiCl、BaCl2And ZnCl2Of said mixed metal salt has a melting point below 550 ℃.
Further, the mass ratio of the mixed metal salt to the graphite fluoride is 4: 1-1: 1.
further, in the step (1), if the mixing method is grinding, the grinding time is 30-120 minutes; if the mixing method is ball milling, the rotation speed of the ball milling is 200 and 600rpm, and the time is 30-240 minutes.
Further, in the step (2), the atmosphere in the tube furnace is nitrogen or argon inert atmosphere, and the heating time is 1-10 hours.
Further, in the step (3), the organic solvent may be N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide.
Further, in the step (3), the mass ratio of the added hydrogen fluoride to the mixed metal salt is 5: 1-1: 1.
further, in the step (3), the ultrasonic time is 60-240 minutes.
Further, in the step (3), the rotation speed of the centrifugation is 800-.
Further, in the step (3), the temperature of vacuum drying is 60-80 ℃, and the drying time is 12-24 hours.
The invention has the following advantages:
the synthesis method has the advantages of low requirement on equipment, simple process, strong operability and easy amplification, the fluorine content of the product fluorinated graphene can be adjusted by adjusting the reaction time, the thickness of the synthesized fluorinated graphene is about 3.6nm, the yield reaches 10g level, and the method has wide application prospects in the fields of lithium batteries, anticorrosive coatings and the like.
[ description of the drawings ]
The invention will be further described with reference to the following examples with reference to the accompanying drawings.
FIG. 1 is a thermogravimetric analysis of graphite fluoride used in the present invention.
Fig. 2 is an atomic force microscope image of fluorinated graphene synthesized in example 1 of the present invention.
Fig. 3 is a thickness analysis diagram of an atomic force microscope of fluorinated graphene synthesized in example 1 of the present invention.
Fig. 4 shows fluorine contents of fluorinated graphene corresponding to different reaction times in example 2 of the present invention.
Fig. 5 is an atomic force microscope image of fluorinated graphene synthesized in example 4 of the present invention.
Fig. 6 is a thickness analysis diagram of an atomic force microscope of fluorinated graphene synthesized in example 4 of the present invention.
[ detailed description ] embodiments
The invention relates to a preparation method of a fluorinated graphene material with adjustable fluorine content, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) uniformly mixing the mixed metal salt and graphite fluoride, wherein the mixing method can be grinding or ball milling;
(2) placing the mixed product in a tube furnace to react for a period of time at 550 ℃;
(3) and (3) ultrasonically stripping the reaction product in a mixed solution of an organic solvent and hydrogen fluoride, centrifugally separating out an upper layer solution, performing suction filtration and washing, and performing vacuum drying to obtain the fluorinated graphene.
The mixed metal salt in the step (1) is NaCl and CaCl2、LiCl、BaCl2And ZnCl2Of said mixed metal salt has a melting point below 550 ℃. The mass ratio of the mixed metal salt to the graphite fluoride is 4: 1-1: 1. in the step (1), if the mixing method is grinding, the grinding time is 30-120 minutes; if the mixing method is ball milling, the rotation speed of the ball milling is 200 and 600rpm, and the time is 30-240 minutes.
In the step (2), the atmosphere in the tubular furnace is nitrogen or argon inert atmosphere, and the heating time is 1-10 hours.
In the step (3), the organic solvent may be N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide. The mass ratio of the added hydrogen fluoride to the mixed metal salt is 5: 1-1: 1; the ultrasonic time is 60-240 minutes; the rotation speed of centrifugation is 800-1200rpm, and the time is 10-30 minutes; the temperature of vacuum drying is 60-80 ℃, and the drying time is 12-24 hours.
The technical scheme of the invention is further explained by combining specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Graphite fluoride was purchased from Shanghai Fubang chemical Co., Ltd.
Oil sealed planetary ball mills are available from long-sand ice cream instruments ltd.
The single temperature zone tube furnace is purchased from combined fertilizer and crystal material technology ltd.
Example 1
1.169g of sodium chloride, 2.415g of anhydrous calcium chloride (molar ratio of the two is 1: 1.088) and 1.792g of graphite fluoride are weighed, mixed together and ground for 60 minutes by a mortar. The ground solid was placed in a tube furnace and heated to 550 ℃ at a rate of 10 degrees per minute for 2 hours.
After the reaction, the solid was taken out, dispersed in 100ml of N-methylpyrrolidone, and then 5g of a hydrogen fluoride solution was added thereto, followed by ultrasonic exfoliation for 120 minutes. The resulting solution was centrifuged at 1000rpm for 10 minutes and the supernatant was collected. And (3) carrying out suction filtration on the supernatant, washing the supernatant with N-methyl pyrrolidone, absolute ethyl alcohol and water for three times respectively, collecting a solid product, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain a final sample, namely 1.428g of fluorinated graphene.
Example 2
1.272g of lithium chloride, 1.793g of anhydrous calcium chloride (the molar ratio of the two is 1.857: 1) and 1.184g of graphite fluoride are weighed and mixed together, and ball-milled for 60 minutes at the rotating speed of 500rpm by adopting an oil-sealed planetary ball mill. And putting the ball-milled solid into a tube furnace, heating to 550 ℃ at the speed of 10 ℃ per minute, and heating for 1, 2, 5 and 10 hours respectively.
After the reaction, the solid was taken out, dispersed in 100ml of N-methylpyrrolidone, and then 10g of a hydrogen fluoride solution was added thereto, followed by ultrasonic exfoliation for 180 minutes. The resulting solution was centrifuged at 1000rpm for 10 minutes and the supernatant was collected. And (3) carrying out suction filtration on the supernatant, washing the supernatant with N-methyl pyrrolidone, absolute ethyl alcohol and water for three times respectively, collecting a solid product, and carrying out vacuum drying at 70 ℃ for 12 hours, wherein the heating time is 1, 2, 5 and 10 hours, so that the final samples of the fluorinated graphene are 1.480g, 1.256g, 1.086g and 0.992g respectively.
Example 3
0.654g of sodium chloride, 1.435g of anhydrous calcium chloride, 1.224g of anhydrous barium chloride (the molar ratio of the three is 0.373: 0.432: 0.196), and 1.657g of graphite fluoride are weighed, mixed together, and ground for 90 minutes by using a mortar. The ground solid was placed in a tube furnace and heated to 550 ℃ at a rate of 10 degrees per minute for 5 hours.
After the reaction, the solid was taken out, dispersed in 100ml of N-dimethylformamide, and 8g of a hydrogen fluoride solution was added thereto, and ultrasonically peeled off for 240 minutes. The resulting solution was centrifuged at 1000rpm for 10 minutes and the supernatant was collected. And (3) carrying out suction filtration on the supernatant, washing the supernatant with N, N-dimethylformamide, absolute ethyl alcohol and water for three times respectively, collecting a solid product, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain a final sample of 1.438 g.
Example 4
11.69g of sodium chloride, 24.15g of anhydrous calcium chloride (the molar ratio of the sodium chloride to the anhydrous calcium chloride is 1: 1.088) and 17.92g of graphite fluoride are weighed and mixed together, and ball-milled for 120 minutes at the rotating speed of 500rpm by adopting an oil-sealed planetary ball mill. The ground solid was placed in a tube furnace and heated to 550 ℃ at a rate of 10 degrees per minute for 2 hours.
After the reaction, the solid was taken out, dispersed in 500ml of N-methylpyrrolidone, and then 60g of a hydrogen fluoride solution was added thereto, followed by ultrasonic exfoliation for 180 minutes. The resulting solution was centrifuged at 1000rpm for 10 minutes and the supernatant was collected. The supernatant was filtered by suction, washed three times with N-methylpyrrolidone, absolute ethanol and water, respectively, the solid product was collected and vacuum dried at 60 ℃ for 24 hours to obtain 15.689g of the final sample. Further, FIG. 1 is a thermogravimetric analysis of the graphite fluoride used in the present invention, and it can be seen from the graph that the temperature at which the graphite fluoride starts to decompose is 550 ℃ or higher, and therefore the heating temperature of the present invention does not exceed 550 ℃.
FIG. 2 is an atomic force microscope image of the fluorinated graphene synthesized in this example 1, and it can be seen that the synthesized fluorinated graphene has a lamellar structure
Fig. 3 is a thickness analysis chart of the atomic force microscope of the fluorinated graphene synthesized in example 1 of the present invention, and it can be seen that the thickness of the fluorinated graphene synthesized in this example is 3.6 nm.
Fig. 4 shows the fluorine content of the fluorinated graphene corresponding to different reaction times in example 2 of the present invention, and it can be seen from the figure that the reaction time is 1 hour, and the fluorine content of the fluorinated graphene as a reaction product is 52.1%; the reaction time is 2 hours, and the fluorine content in the reaction product fluorinated graphene is 43.2%; the reaction time is 5 hours, and the fluorine content in the reaction product fluorinated graphene is 20.8 percent; the reaction time is 10 hours, and the fluorine content in the reaction product fluorinated graphene is 6.6 percent; it is demonstrated that the fluorine content in the fluorinated graphene gradually decreases with the increase of the reaction time.
FIG. 5 is an atomic force microscope image of the fluorinated graphene synthesized in this example 4, from which it can be seen that the synthesized fluorinated graphene has a lamellar structure
Fig. 6 is a thickness analysis chart of the atomic force microscope of the fluorinated graphene synthesized in example 4 of the present invention, and it can be seen that the thickness of the fluorinated graphene synthesized in this example is 3.5 nm.
In conclusion, the synthesis method disclosed by the invention has the advantages of low equipment requirement, simple process, strong operability and easiness in amplification, the fluorine content of the product fluorinated graphene can be adjusted by adjusting the reaction time, the thickness of the synthesized fluorinated graphene is about 3.6nm, the yield reaches the level of 10g, and the method has a wide application prospect in the fields of lithium batteries, anticorrosive coatings and the like.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.
Claims (10)
1. A preparation method of a fluorinated graphene material with adjustable fluorine content is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly mixing the mixed metal salt and graphite fluoride, wherein the mixing method can be grinding or ball milling;
(2) placing the mixed product in a tube furnace to react for a period of time at 550 ℃;
(3) and (3) ultrasonically stripping the reaction product in a mixed solution of an organic solvent and hydrogen fluoride, centrifugally separating out an upper layer solution, performing suction filtration and washing, and performing vacuum drying to obtain the fluorinated graphene.
2. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: the mixed metal salt in the step (1) is NaCl and CaCl2、LiCl、BaCl2And ZnCl2Of said mixed metal salt has a melting point below 550 ℃.
3. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: the mass ratio of the mixed metal salt to the graphite fluoride is 4: 1-1: 1.
4. the method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (1), if the mixing method is grinding, the grinding time is 30-120 minutes; if the mixing method is ball milling, the rotation speed of the ball milling is 200 and 600rpm, and the time is 30-240 minutes.
5. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (2), the atmosphere in the tubular furnace is nitrogen or argon inert atmosphere, and the heating time is 1-10 hours.
6. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (3), the organic solvent may be N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide.
7. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (3), the mass ratio of the added hydrogen fluoride to the mixed metal salt is 5: 1-1: 1.
8. the method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (3), the ultrasonic time is 60-240 minutes.
9. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (3), the rotation speed of the centrifugation is 800-1200rpm, and the time is 10-30 minutes.
10. The method for preparing fluorinated graphene material with adjustable fluorine content according to claim 1, wherein the method comprises the following steps: in the step (3), the temperature of vacuum drying is 60-80 ℃, and the drying time is 12-24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010344637.8A CN111620326B (en) | 2020-04-27 | 2020-04-27 | Preparation method of fluorinated graphene material with adjustable fluorine content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010344637.8A CN111620326B (en) | 2020-04-27 | 2020-04-27 | Preparation method of fluorinated graphene material with adjustable fluorine content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111620326A true CN111620326A (en) | 2020-09-04 |
| CN111620326B CN111620326B (en) | 2022-09-02 |
Family
ID=72268004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010344637.8A Active CN111620326B (en) | 2020-04-27 | 2020-04-27 | Preparation method of fluorinated graphene material with adjustable fluorine content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111620326B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661146A (en) * | 2020-12-23 | 2021-04-16 | 湘潭大学 | Preparation method of laminated fluorinated graphene for positive electrode of lithium battery |
| CN112786822A (en) * | 2020-12-30 | 2021-05-11 | 惠州亿纬锂能股份有限公司 | Lithium-carbon fluoride battery positive pole piece, preparation method thereof and lithium-carbon fluoride battery |
| CN113871615A (en) * | 2021-08-31 | 2021-12-31 | 兰州大学 | Fluorinated graphene electrode active material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588195A (en) * | 2013-11-01 | 2014-02-19 | 天津大学 | Preparation method of graphene |
| CN104724700A (en) * | 2015-03-19 | 2015-06-24 | 岳红军 | Method for efficiently preparing fluorinated graphene |
| CN104944402A (en) * | 2014-03-24 | 2015-09-30 | 中国科学院兰州化学物理研究所 | Method for quickly and efficiently preparing adjustable-fluorine-content fluoridized graphene |
| CN109231188A (en) * | 2018-11-26 | 2019-01-18 | 上海应用技术大学 | A method of nitrating fluorinated graphene is prepared using fluorographite |
| CN110950331A (en) * | 2019-12-02 | 2020-04-03 | 陕西科技大学 | Method for preparing fluorinated graphene dispersion liquid on large scale |
-
2020
- 2020-04-27 CN CN202010344637.8A patent/CN111620326B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588195A (en) * | 2013-11-01 | 2014-02-19 | 天津大学 | Preparation method of graphene |
| CN104944402A (en) * | 2014-03-24 | 2015-09-30 | 中国科学院兰州化学物理研究所 | Method for quickly and efficiently preparing adjustable-fluorine-content fluoridized graphene |
| CN104724700A (en) * | 2015-03-19 | 2015-06-24 | 岳红军 | Method for efficiently preparing fluorinated graphene |
| CN109231188A (en) * | 2018-11-26 | 2019-01-18 | 上海应用技术大学 | A method of nitrating fluorinated graphene is prepared using fluorographite |
| CN110950331A (en) * | 2019-12-02 | 2020-04-03 | 陕西科技大学 | Method for preparing fluorinated graphene dispersion liquid on large scale |
Non-Patent Citations (2)
| Title |
|---|
| SHUFEN WANG ET AL: ""Towards understanding the salt-intercalation exfoliation of graphite into graphene"", 《RSC ADVANCES》 * |
| 高天明等: "中国天然石墨未来需求与发展展望", 《资源科学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661146A (en) * | 2020-12-23 | 2021-04-16 | 湘潭大学 | Preparation method of laminated fluorinated graphene for positive electrode of lithium battery |
| CN112661146B (en) * | 2020-12-23 | 2022-07-05 | 湘潭大学 | Preparation method of laminated fluorinated graphene for positive electrode of lithium battery |
| CN112786822A (en) * | 2020-12-30 | 2021-05-11 | 惠州亿纬锂能股份有限公司 | Lithium-carbon fluoride battery positive pole piece, preparation method thereof and lithium-carbon fluoride battery |
| CN113871615A (en) * | 2021-08-31 | 2021-12-31 | 兰州大学 | Fluorinated graphene electrode active material and preparation method and application thereof |
| CN113871615B (en) * | 2021-08-31 | 2024-03-15 | 兰州大学 | Fluorinated graphene electrode active material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111620326B (en) | 2022-09-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111620326B (en) | Preparation method of fluorinated graphene material with adjustable fluorine content | |
| CN107204445B (en) | A kind of lithium ion battery three-dimensional porous silicon-carbon cathode material and preparation method thereof | |
| CN102760866B (en) | Preparation method of nitrogen-doped graphene | |
| CN104495935B (en) | A kind of strip preparation method of molybdenum disulfide nano sheet layer | |
| CN109830661B (en) | Selenium-doped MXene composite nano material and preparation method and application thereof | |
| CN109817382B (en) | Preparation method of high-stability graphene conductive paste | |
| CN104319012B (en) | A kind of flexible electrode preparation method based on graphene | |
| CN104817075B (en) | Preparation method of highly dispersed graphene oxide nanobelt solution | |
| US20120256121A1 (en) | Method for producing graphene solutions, graphene alkali metal salts, and graphene composite materials | |
| CN108483432B (en) | Electrochemical preparation method of fluorinated graphene material | |
| CN108336310B (en) | Composite material based on self-supporting reduced graphene oxide roll and preparation method | |
| JP2014504248A (en) | Graphene fluoride oxide and preparation method thereof | |
| CN110451482B (en) | Preparation method of nitrogen and sulfur co-doped carbon nanosheet material | |
| CN102153074A (en) | Method for preparing graphene with high specific surface area through low-temperature pyrolysis and expansion | |
| CN102698774A (en) | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material | |
| CN112591732B (en) | Preparation method of fluorinated graphene and fluorinated carbon nanotube with controllable fluorine content | |
| CN107500275A (en) | A kind of method for producing different Oil repellent fluorinated graphenes in enormous quantities | |
| CN109003826A (en) | N and S codope graphene-graphene nanobelt aeroge preparation method | |
| CN108831757A (en) | A kind of preparation method of N and S codope graphene/carbon nano-tube aeroge | |
| CN105789628B (en) | A kind of azepine graphene and manganese dioxide hybrid aerogel and its preparation method and application | |
| US11254574B2 (en) | Graphene material prepared from waste tire and preparation method thereof | |
| CN103022468A (en) | Environment-friendly preparation method for high-specific-capacitance Mn3O4/graphene composite material for poles | |
| CN106587020B (en) | A kind of fast preparation method of high conductivity sulfur doping graphene | |
| CN107610838A (en) | It is a kind of to prepare the method with superconductivity energy graphene composite material | |
| CN108314022B (en) | Method for preparing graphene by directly stripping ionic liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |