CN112897521A - Preparation method of graphite film composite material - Google Patents
Preparation method of graphite film composite material Download PDFInfo
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- CN112897521A CN112897521A CN202110053991.XA CN202110053991A CN112897521A CN 112897521 A CN112897521 A CN 112897521A CN 202110053991 A CN202110053991 A CN 202110053991A CN 112897521 A CN112897521 A CN 112897521A
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- graphite
- germanium
- graphite film
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- magnetron sputtering
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 81
- 239000010439 graphite Substances 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 84
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 33
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229920001721 polyimide Polymers 0.000 claims abstract description 27
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 23
- 230000001105 regulatory effect Effects 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000004642 Polyimide Substances 0.000 claims abstract description 12
- 230000009471 action Effects 0.000 claims abstract description 6
- 230000001276 controlling effect Effects 0.000 claims abstract description 6
- 239000011258 core-shell material Substances 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- 238000005087 graphitization Methods 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 150000003949 imides Chemical class 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052744 lithium Inorganic materials 0.000 abstract description 7
- 238000003860 storage Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 32
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
- 239000010406 cathode material Substances 0.000 description 8
- 239000007773 negative electrode material Substances 0.000 description 6
- 239000007770 graphite material Substances 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- 239000011149 active material Substances 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910013458 LiC6 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- 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
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
Abstract
The invention relates to the technical field of energy storage, in particular to a preparation method of a graphite film composite material, which comprises the following steps: selecting a polyimide graphite film as a substrate material, and alternately growing a bonding material and a germanium material on the substrate material in sequence; regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument; under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed. The composite material has good heat-conducting property and electric conductivity; meanwhile, the volume change of the germanium material can be relieved, the lithium storage performance of the germanium can be effectively exerted, and the working cycle life is longer.
Description
Technical Field
The invention relates to the technical field of energy storage, in particular to a preparation method of a graphite film composite material.
Background
The cathode material of commercial lithium ion batteries is generally a graphite material which is still the main force in the field of cathode materials at present. The graphite material is a wide variety of materials, including natural crystalline flake graphite, artificial graphite, fibrous carbon material (having a graphite structure), and the like. The non-renewable natural crystalline flake graphite has a natural graphite structure degree, and can be directly used as a lithium ion battery cathode material after high-temperature treatment. The artificial graphite is generally prepared by using natural crystalline flake graphite as an aggregate and combining other materials through a hot pressing process. After long-time circulation, the lithium storage capacity of natural crystalline flake graphite and artificial graphite is generally maintained at 320 mAh/g; the lithium storage capacity of the modified graphite material can be brought to some extent close to the theoretical capacity level (372 mAh/g; LiC6) in a short period of time. Fibrous carbon materials have potential advantages over graphite materials. The carbon fiber is a fibrous carbon material, and the carbon element content in the chemical composition of the carbon fiber is more than 90 percent. The carbon fiber has the advantages of higher specific modulus, high heat conduction/electric rate, corrosion resistance, creep resistance, low thermal expansion coefficient and the like, can be used as a structural material and a functional material, and is widely applied to the fields of automobile manufacturing, bridge construction, cultural and sports entertainment products and the like.
With the development of science and technology, the specific capacity provided by the conventional graphite cathode material cannot meet the requirements of power sources, electronic products and the like, and the cathode material with high specific capacity is urgently needed. In the cathode material, materials such as silicon, germanium, tin, metal oxide and the like also have higher theoretical lithium storage capacity. Germanium has higher theoretical specific capacity (1600 mAh.g < -1 >) and lower working voltage, and is considered to be an ideal choice for the negative electrode material of the lithium ion battery
And selecting one. Compared with a silicon-based cathode material, the germanium has small forbidden band width, higher conductivity and lithium ion diffusion coefficient, is more suitable for being applied to high-power and high-current equipment, and has better potential application in the direction of a power automobile. However, as an alloy type negative electrode material, germanium has a large volume change in the lithium intercalation-deintercalation process, generates a large mechanical stress between active material particles, reduces electrical contact between active materials and between the active materials and a current collector, and leads the cracked/pulverized electrode material not to participate in electrochemical reaction any more, so that the battery capacity attenuation is serious.
Disclosure of Invention
The invention aims to solve the problem that the germanium material in the prior art is generally powder, and is mixed with a conductive agent and a binder to be used as a negative electrode material to prepare a lithium ion battery. Germanium material in powder form will increase the interfacial resistance and is not good for ion transport. The disadvantages of the prior art are that the preparation method of the graphite film composite material is provided.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphite film composite material is designed, and comprises the following steps:
selecting a polyimide graphite film as a substrate material, and alternately growing a bonding material and a germanium material on the substrate material in sequence;
regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument;
under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed.
The invention also provides a preparation method of the polyimide graphite film, which comprises the following steps:
s1: selecting a polyimide film and flexible graphite paper, and alternately stacking the polyimide film and the flexible graphite paper to enable the polyimide film to be in an interlayer of the flexible graphite paper;
s2: placing the raw material treated in the step S1 in a heating furnace, placing a square graphite block on the uppermost flexible graphite paper, and pressing the square graphite block on the whole imide film/flexible graphite paper stack;
s3: firstly, raising the temperature in a heating furnace to 1273K at a heating rate of 5-10K/min, using argon as protective gas in the process, carrying out graphitization treatment under the protection of high-purity argon, wherein the graphitization treatment temperature is 2000K-3273K at a heating rate of 5-10K/min, and keeping the constant temperature for 0.5h when the temperature is raised to a preset temperature;
s4: and preparing a graphite film blank after graphitization treatment, and flattening the surface of the graphite film blank by rolling of a roll press.
Preferably, the bonding material is a nickel material, a cobalt material or a titanium material, and the nickel material is preferred.
Preferably, when the power parameter of the magnetron sputtering instrument is regulated, the power of the bonding material is 10-20W; the power of the germanium material is 10-20W.
Preferably, the working air pressure of the magnetron sputtering instrument is regulated and controlled to be 1.5-4 Pa.
The preparation method of the graphite film composite material has the beneficial effects that:
1. the germanium material has wide source and is rich in the earth crust. The cost of raw materials is low, the preparation method is relatively mature, and the low-cost production of products is favorably realized.
2. The graphite film is prepared by using polyimide as a raw material and carrying out processes such as graphitization and the like. The film has the characteristics of good electrical conductivity, thermal conductivity, acid resistance, alkali resistance and corrosion resistance. Can be used as a conductive reinforcing material and can also be applied as a structural material.
3. The germanium-based composite material is prepared by combining germanium, a bonding material and a high-conductivity graphite film substrate material by adopting a magnetron sputtering technology.
4. The novel germanium-based composite material has excellent conductivity, can relieve the volume change effect of a germanium material by structural design, can effectively store/release lithium ions, is used as a lithium ion negative electrode material, and can be used for preparing a high-performance lithium ion battery.
Drawings
FIG. 1 is a schematic view of the morphology of a graphite thin film composite material.
Fig. 2 is a schematic diagram of the electrochemical performance of the graphite thin film composite material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
Referring to fig. 1, a method for preparing a graphite film composite material includes the following steps:
selecting a polyimide graphite film as a substrate material, and alternately growing a nickel material and a germanium material on the substrate material in sequence;
regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument, wherein the power of the nickel material is 10W when the power parameter of the magnetron sputtering instrument is regulated and controlled; the power of the germanium material is 10W, and the working air pressure of the magnetron sputtering instrument is regulated and controlled to be 1.5 Pa;
under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed.
The invention also provides a preparation method of the polyimide graphite film, which comprises the following steps:
s1: selecting a polyimide film and flexible graphite paper, and alternately stacking the polyimide film and the flexible graphite paper to enable the polyimide film to be in an interlayer of the flexible graphite paper;
s2: placing the raw material treated in the step S1 in a heating furnace, placing a square graphite block on the uppermost flexible graphite paper, and pressing the square graphite block on the whole imide film/flexible graphite paper stack;
s3: firstly, raising the temperature in a heating furnace to 1273K at a heating rate of 5-10K/min, using argon as protective gas in the process, carrying out graphitization treatment under the protection of high-purity argon, wherein the graphitization treatment temperature is 2000K-3273K at a heating rate of 5-10K/min, and keeping the constant temperature for 0.5h when the temperature is raised to a preset temperature;
s4: and preparing a graphite film blank after graphitization treatment, and flattening the surface of the graphite film blank by rolling of a roll press.
Example 2
Referring to fig. 1, a method for preparing a graphite film composite material includes the following steps:
selecting a polyimide graphite film as a substrate material, and alternately growing a cobalt material and a germanium material on the substrate material in sequence
Regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument, wherein the power of the cobalt material is 15W when the power parameter of the magnetron sputtering instrument is regulated and controlled; the power of the germanium material is 15W, and the working air pressure of the magnetron sputtering instrument is regulated and controlled to be 2.5 Pa;
under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed.
The invention also provides a preparation method of the polyimide graphite film, which comprises the following steps:
s1: selecting a polyimide film and flexible graphite paper, and alternately stacking the polyimide film and the flexible graphite paper to enable the polyimide film to be in an interlayer of the flexible graphite paper;
s2: placing the raw material treated in the step S1 in a heating furnace, placing a square graphite block on the uppermost flexible graphite paper, and pressing the square graphite block on the whole imide film/flexible graphite paper stack;
s3: firstly, raising the temperature in a heating furnace to 1273K at a heating rate of 5-10K/min, using argon as protective gas in the process, carrying out graphitization treatment under the protection of high-purity argon, wherein the graphitization treatment temperature is 2000K-3273K at a heating rate of 5-10K/min, and keeping the constant temperature for 0.5h when the temperature is raised to a preset temperature;
s4: and preparing a graphite film blank after graphitization treatment, and flattening the surface of the graphite film blank by rolling of a roll press.
Example 3
Referring to fig. 1, a method for preparing a graphite film composite material includes the following steps:
selecting a polyimide graphite film as a substrate material, and alternately growing a titanium material and a germanium material on the substrate material in sequence;
regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument, wherein the power of the titanium material is 20W when the power parameter of the magnetron sputtering instrument is regulated and controlled; the power of the germanium material is 20W, and the working air pressure of the magnetron sputtering instrument is regulated and controlled to be 4 Pa;
under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed.
The invention also provides a preparation method of the polyimide graphite film, which comprises the following steps:
s1: selecting a polyimide film and flexible graphite paper, and alternately stacking the polyimide film and the flexible graphite paper to enable the polyimide film to be in an interlayer of the flexible graphite paper;
s2: placing the raw material treated in the step S1 in a heating furnace, placing a square graphite block on the uppermost flexible graphite paper, and pressing the square graphite block on the whole imide film/flexible graphite paper stack;
s3: firstly, raising the temperature in a heating furnace to 1273K at a heating rate of 5-10K/min, using argon as protective gas in the process, carrying out graphitization treatment under the protection of high-purity argon, wherein the graphitization treatment temperature is 2000K-3273K at a heating rate of 5-10K/min, and keeping the constant temperature for 0.5h when the temperature is raised to a preset temperature;
s4: and preparing a graphite film blank after graphitization treatment, and flattening the surface of the graphite film blank by rolling of a roll press.
The electrochemical performance analysis of the graphite film composite material comprises the following steps:
1. assembling the battery:
negative electrode material/electrolyte/metallic lithium positive electrode, the charging of the cell was carried out in a glove box and under argon protection.
2. And (3) detecting the battery performance: the electrochemical performance was examined by cycling at a current density of 50-1000 mA/g. One series of materials are selected as the negative electrode material to carry out electrochemical performance test.
As shown in FIG. 2, when the current is circulated under the current density of 0.05A/g, the first reversible capacity can reach 1000 mAh/g; after 30 times of circulation, the average reversible specific capacity in the whole process is still maintained at 900mA h/g, the coulombic efficiency in the circulation process is very stable, and the excellent circulation performance is shown. The composite material has good heat-conducting property and electric conductivity; meanwhile, the volume change of the germanium material can be relieved, the lithium storage performance of the germanium can be effectively exerted, the working cycle life is long, and the germanium material can be used as a high-performance lithium ion battery cathode material to prepare a lithium ion battery.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The preparation method of the graphite film composite material is characterized by comprising the following steps:
selecting a polyimide graphite film as a substrate material, and alternately growing a bonding material and a germanium material on the substrate material in sequence;
regulating and controlling the power parameter and working gas pressure of a magnetron sputtering instrument;
under the action of a magnetron sputtering instrument, a germanium material is positioned in a three-dimensional layered wrapping structure of a bonding material, the material is cut into pole pieces, the bonding material is grown on the surface of the pole pieces to serve as an outer shell layer, and finally a core-shell structure is formed.
2. The method for preparing the polyimide graphite film according to claim 1, comprising the following steps:
s1: selecting a polyimide film and flexible graphite paper, and alternately stacking the polyimide film and the flexible graphite paper to enable the polyimide film to be in an interlayer of the flexible graphite paper;
s2: placing the raw material treated in the step S1 in a heating furnace, placing a square graphite block on the uppermost flexible graphite paper, and pressing the square graphite block on the whole imide film/flexible graphite paper stack;
s3: firstly, raising the temperature in a heating furnace to 1273K at a heating rate of 5-10K/min, using argon as protective gas in the process, carrying out graphitization treatment under the protection of high-purity argon, wherein the graphitization treatment temperature is 2000K-3273K at a heating rate of 5-10K/min, and keeping the constant temperature for 0.5h when the temperature is raised to a preset temperature;
s4: and preparing a graphite film blank after graphitization treatment, and flattening the surface of the graphite film blank by rolling of a roll press.
3. The method for preparing the graphite film composite material as claimed in claim 1, wherein the binding material is a nickel material, a cobalt material or a titanium material, preferably a nickel material.
4. The method for preparing the graphite film composite material as claimed in claim 1, wherein the power of the binding material is 10-20W when the power parameter of the magnetron sputtering instrument is regulated; the power of the germanium material is 10-20W.
5. The method for preparing the graphite film composite material as claimed in claim 1, wherein the working pressure of the magnetron sputtering apparatus is controlled to be 1.5-4 Pa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6212057B1 (en) * | 1998-12-22 | 2001-04-03 | Matsushita Electric Industrial Co., Ltd. | Flexible thin film capacitor having an adhesive film |
| CN103011141A (en) * | 2012-12-20 | 2013-04-03 | 宁波今山新材料有限公司 | Method for manufacturing high thermal conductivity graphite film |
| CN104495798A (en) * | 2014-11-28 | 2015-04-08 | 苏州格优碳素新材料有限公司 | Manufacturing method of graphite heat-conduction membrane |
-
2021
- 2021-01-15 CN CN202110053991.XA patent/CN112897521A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6212057B1 (en) * | 1998-12-22 | 2001-04-03 | Matsushita Electric Industrial Co., Ltd. | Flexible thin film capacitor having an adhesive film |
| CN103011141A (en) * | 2012-12-20 | 2013-04-03 | 宁波今山新材料有限公司 | Method for manufacturing high thermal conductivity graphite film |
| CN104495798A (en) * | 2014-11-28 | 2015-04-08 | 苏州格优碳素新材料有限公司 | Manufacturing method of graphite heat-conduction membrane |
Non-Patent Citations (1)
| Title |
|---|
| IBRAHIM, A.S.等: "《Ge/TiO2 composite thin films prepared by RF magnetron sputtering for Photovoltaic Applications》", 《3RD IET INTERNATIONAL CONFERENCE ON CLEAN ENERGY AND TECHNOLOGY (CEAT) 2014》 * |
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Application publication date: 20210604 |