CN108400177B - Preparation method of metallized graphite film layer for battery electrode - Google Patents
Preparation method of metallized graphite film layer for battery electrode Download PDFInfo
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- CN108400177B CN108400177B CN201810209709.0A CN201810209709A CN108400177B CN 108400177 B CN108400177 B CN 108400177B CN 201810209709 A CN201810209709 A CN 201810209709A CN 108400177 B CN108400177 B CN 108400177B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000010439 graphite Substances 0.000 title claims abstract description 78
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004544 sputter deposition Methods 0.000 claims abstract description 51
- 239000013077 target material Substances 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 82
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 82
- 238000000576 coating method Methods 0.000 claims description 51
- 229910052757 nitrogen Inorganic materials 0.000 claims description 45
- 239000011248 coating agent Substances 0.000 claims description 43
- 229910052786 argon Inorganic materials 0.000 claims description 41
- 239000000758 substrate Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 63
- 238000005240 physical vapour deposition Methods 0.000 description 7
- 238000005477 sputtering target Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 101100167360 Drosophila melanogaster chb gene Proteins 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- -1 high melting point Chemical class 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02697—Forming conducting materials on a substrate
Abstract
A preparation method of a metallized graphite film layer for a battery electrode comprises the following components in percentage: 3.5 to 8.0 percent of Ti,2.0-3.0% of N, less than or equal to 0.05% of impurity content and the balance of C. The invention adopts graphite and Ti target materials to prepare the metallized graphite film layer by co-sputtering, and carbon atoms are mainly sp2The hybridized orbital forms bonds, can overcome the defect of large resistivity of diamond-like carbon, and reduce sp of carbon atoms3The mode of hybrid orbital bonding. The sheet resistance of the metallized graphite film layer is 100m omega/□ -3 omega/□, and the industrial production requirement is met.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method of a metallized graphite film layer for a battery electrode.
Background
The solar cell is a novel industry developed in the 90 s of the 20 th century, and has the characteristics of cleanness, new energy, no pollution and high technological content. The electrodes of the battery are the main constituents of the battery, which mainly participate in the collection and transport of electrons. However, since electrodes of solar cells are generally made of conductive glass carrying a platinum catalyst, the cost of platinum is high, and therefore, other methods have been attempted to replace the platinum metal.
The carbon material has the natural excellent characteristics of being used as a solar battery, and has high catalytic activity, good conductivity, stable performance and low cost; meanwhile, the graphite-like film can be used as an electrode of a sensor and is widely applied in the related field of electrochemistry. The reason why carbon exists in various forms is: since carbon atoms generally have 3 hybrid orbital bonding forms, i.e. sp3、sp2And sp1. When the carbon atom is in sp3When the hybrid orbit is bonded, the hybrid orbit is expressed in the form of diamond; in sp2When the hybrid orbitals are bonded, they behave as graphitic structures. The diamond structure has high strength and hardness and low conductivity, and the prepared diamond-like carbon film has resistance in megaohm as a unit. On the contrary, the graphite structure has small strength and hardness and strong conductivity, the sheet resistance is in omega or milliomega unit, and the resistivity difference is 106~109。
The electrode of the battery requires good conductivity, and the deposition of the conductive film of the electrodeThe method is mainly divided into two types: chemical vapor deposition and physical vapor deposition. The chemical vapor deposition mainly uses carbon-containing gas, such as methane, acetylene and the like as a carbon source and adopts a plasma chemical vapor deposition method; the physical vapor deposition mainly takes high-purity graphite as a target material and adopts a sputtering coating mode to prepare a film layer. However, in the process of preparing the electrode of the battery, sp2The hybrid orbit is difficult to form in a bonding form, and the prepared resistivity is large and far higher than that of the target graphite. The prior art has a film prepared by a magnetron sputtering mode, the sheet resistance of the film is 20-30 omega/□, and the technical requirement of batch industrial production cannot be met.
Disclosure of Invention
One of the purposes of the invention is to provide a metallized graphite film layer for a battery electrode; the second purpose of the invention is to provide a preparation method of a metallized graphite film layer for a battery electrode. The metallized graphite film layer prepared by the invention has the sheet resistance of 100m omega/□ -3 omega/□; during the process of preparing the electrode of the battery, C-C is sp2The hybrid orbital forms a bond.
The technical scheme adopted by the invention for realizing one of the purposes is as follows: a metallized graphite film layer for a battery electrode comprises the following components in percentage: 3.5 to 8.0 percent of Ti, 2.0 to 3.0 percent of N, less than or equal to 0.05 percent of impurity content and the balance of C.
The second technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 5-20 min by using ultrasonic waves;
step two, introducing argon and nitrogen, and coating a film by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer;
and step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 800-900 ℃, and preserving heat for 2-3 hours.
In the second step, the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein, the substrate is heated to 800-1000 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.2-0.5 Pa.
In the invention, the flow ratio of argon to nitrogen is 3: 1; the total flow of the argon and the nitrogen is 30-40 sccm; the current density of the graphite target is 10-15W/cm2The current density of the Ti target material is 0.5-1W/cm2。
Wherein, the vacuum degree of the magnetron co-sputtering coating equipment<1×10-4Pa。
The invention adopts low air pressure (0.2-0.5 Pa), high substrate temperature (800-1000 ℃), high power mode (600-800W) for magnetron sputtering DC power supply, and high current density (10-15W/cm) for target material2) Atoms form a film on the surface of the base material quickly, the atoms are active, a diamond-like film layer is not easy to form, a carbonization reaction is generated at high temperature, and part of diamond-like is converted into graphite-like.
In the preparation process of the film, elements such as Ti, N and the like are doped, the Ti element has good electric conductivity, part of the Ti element and C, N form TiC and TiN, the TiC and the TiN also have electric conductivity, the free electron concentration in the film layer is increased in the dispersion of the Ti, the TiC and the TiN and the graphite-like layer, the electric conductivity of the film is improved, the required conductive graphite-like film layer is prepared, and the graphite-like film layer has strong corrosion resistance, strong friction resistance and high strength and hardness, and can meet the harsh environment in the field.
The Ti metal has good conductivity, and meanwhile, the Ti element has strong activity, so that the thin film layer has strong binding force and is not easy to fall off, and the service life of the device is met. The doped TiN has higher conductivity and superconductivity, and can be applied to high-temperature structural materials and superconducting materials.
Has the advantages that: the invention adopts graphite and Ti target materials to prepare the metallized graphite film layer by co-sputtering, and carbon atoms are mainly sp2The hybridized orbital forms bonds, can overcome the defect of large resistivity of diamond-like carbon, and reduce sp of carbon atoms3The mode of hybrid orbital bonding. The sheet resistance of the metallized graphite-like film layer is 100m omega/□ -3 omega/□And the industrial production requirement is met.
The doping of elements such as Ti/N and the like increases the conductivity, the wear resistance and the hardness of the film. Ti element makes the film layer have strong binding force and is not easy to fall off, which can meet the harsh environment of the field and prolong the service life of the device.
The TiC atoms doped in the invention are combined by strong covalent bonds, have a plurality of characteristics similar to metals, such as high melting point, boiling point and hardness, the hardness is second to that of diamond, and the TiC alloy has good heat conduction and electric conductivity.
Detailed Description
The present invention is further described with reference to specific examples to enable those skilled in the art to better understand the present invention and to practice the same, but the examples are not intended to limit the present invention.
Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the raw materials or instruments used are not indicated by manufacturers, and are all conventional products which can be purchased and obtained on the market; the percentages of the invention are mass percentages.
A metallized graphite film layer for a battery electrode comprises the following components in percentage: 3.5 to 8.0 percent of Ti, 2.0 to 3.0 percent of N, less than or equal to 0.05 percent of impurity content and the balance of C.
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 5-20 min by using ultrasonic waves;
step two, introducing argon and nitrogen, and coating a film by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: the method comprises the following steps of (1) depositing a graphite-like film layer on FTO (fluorine-doped tin oxide) glass by using the FTO conductive glass as a base material and graphite and a T material as co-sputtered target raw materials by using magnetron co-sputtering coating equipment; heating the substrate to 800-1000 ℃, introducing argon and nitrogen, and adjusting the flow of the argon and the nitrogen to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.2-0.5 Pa; the flow ratio of argon to nitrogen was 3: 1; total flow of argon and nitrogenThe amount is 30-40 sccm; the current density of the graphite target is 10-15W/cm2The current density of the Ti target material is 0.5-1W/cm2(ii) a Vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 800-900 ℃, and preserving heat for 2-3 hours.
Example 1
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 5min by using ultrasonic waves;
step two, physical vapor deposition coating: introducing argon and nitrogen, and coating by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein, the substrate is heated to 800 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.5 Pa; the flow ratio of argon to nitrogen was 3: 1; the total flow of argon and nitrogen is 30 sccm; the current density of the graphite target material is 10W/cm2The current density of the Ti target material is 0.5W/cm2(ii) a The time is 2 h; vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 800 ℃, and preserving heat for 3 hours to carry out a heat treatment process.
The thickness of the prepared metallized graphite film layer is 4 mu m.
Example 2
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 8min by using ultrasonic waves;
step two, physical vapor deposition coating: introducing argon and nitrogen, and coating by using a Ti and graphite target co-sputtering method to prepare the metallized graphite filmA layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein, the substrate is heated to 850 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.35 Pa; the flow ratio of argon to nitrogen was 3: 1; the total flow of argon and nitrogen is 40 sccm; the current density of the graphite target material is 15W/cm2The current density of the Ti target material is 1.0W/cm2(ii) a The time is 2 h; vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 850 ℃, and preserving heat for 2.5 hours to carry out a heat treatment process.
The thickness of the prepared metallized graphite film layer is 5 mu m.
Example 3
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 10min by using ultrasonic waves;
step two, physical vapor deposition coating: introducing argon and nitrogen, and coating by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein, the substrate is heated to 860 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.40 Pa; the flow ratio of argon to nitrogen was 3: 1; the total flow of argon and nitrogen was 35 sccm; the current density of the graphite target material is 12W/cm2The current density of the Ti target material is 0.5W/cm2(ii) a The time is 5 h; vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 880 ℃, and preserving heat for 3 hours to carry out a heat treatment process.
The thickness of the prepared metallized graphite film layer is 8 mu m.
Example 4
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 10min by using ultrasonic waves;
step two, physical vapor deposition coating: introducing argon and nitrogen, and coating by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein, the substrate is heated to 1000 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.25 Pa; the flow ratio of argon to nitrogen was 3: 1; the total flow of argon and nitrogen was 33 sccm; the current density of the graphite target material is 14W/cm2The current density of the Ti target material is 0.8W/cm2(ii) a The time is 3 h; vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 900 ℃, and preserving heat for 2 hours to carry out a heat treatment process.
The thickness of the prepared metallized graphite film layer is 5 mu m.
Example 5
A preparation method of a metallized graphite film layer for a battery electrode comprises the following steps:
step one, cleaning a Si substrate for 10min by using ultrasonic waves;
step two, physical vapor deposition coating: introducing argon and nitrogen, and coating by using a Ti and graphite target co-sputtering method to prepare a metallized graphite film layer; the co-sputtering coating method of the Ti and graphite target comprises the following steps: using FTO conductive glass as a base material, using graphite and a T material as co-sputtering target raw materials, and depositing a carbon film on the FTO conductive glass by using magnetron co-sputtering coating equipment; wherein the substrate is heated to 900 ℃ and argon is introducedGas and nitrogen, and the flow of the gas and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.20 Pa; the flow ratio of argon to nitrogen was 3: 1; the total flow rate of argon and nitrogen is 38 sccm; the current density of the graphite target material is 13W/cm2The current density of the Ti target material is 0.7W/cm2(ii) a The time is 4 h; vacuum degree of magnetron co-sputtering coating equipment<1×10-4Pa。
And step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 820 ℃, and preserving heat for 2.2 hours to carry out a heat treatment process.
The thickness of the prepared metallized graphite film layer is 6 mu m.
The percentage of each component in examples 1 to 5 of the present invention is shown in table 1 below.
TABLE 1 contents of components in examples 1 to 5
The type of the coating equipment is an MSP-300B coating machine prepared by Wei Nake technology of Beijing Chuangshi.
The heat treatment process adopts equipment which is a high-temperature spectrum vacuum cavity black body furnace prepared by Weinake technology of Beijing Chuangshi.
In the invention, the base material for sputtering is a glass sheet, and can be replaced by the existing known sputtering substrate; cleaning and drying the substrate, fixing the substrate on a substrate table of a vacuum chamber of a magnetron co-sputtering coating device, starting a power supply to vacuumize, and vacuumizing<1×10-4Pa; heating the substrate according to experimental needs, heating the substrate to 800-1000 ℃, introducing argon and nitrogen, and adjusting the flow of the argon and the nitrogen to enable the pressure of a cavity of the magnetron co-sputtering coating equipment to be 0.2-0.5 Pa; and (4) turning on a sputtering power supply, adjusting sputtering voltage and current, and performing film coating after pre-sputtering. The sputtering time was controlled according to experimental requirements.
The graphite-like thin film prepared by the invention has the advantages that the current density of the target material is changed by changing the power of the power supply, or the thickness of the graphite-like thin film is controlled by changing the coating time, the thickness of the graphite-like thin film is controllable, and the universality is strong.
The sheet resistances of the graphite-like electrode films obtained in comparative example and examples 1 to 5 were measured and are shown in table 2. The invention relates to a tester for measuring the sheet resistance of a graphite-like film, which is an M-3 type handheld four-probe tester of Suzhou crystal lattice electronics Limited. Therefore, the sheet resistance of the graphite-like electrode film prepared by the method is lower than that of the conductive film in the prior art, and the conductivity is enhanced.
TABLE 2 sheet resistance of films obtained in examples 1 to 5
The above examples are intended to illustrate the technical solutions of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, but not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. A preparation method of a metallized graphite film layer for a battery electrode is characterized by comprising the following steps: the percentage of each component of the metallized graphite film layer is as follows: 3.5-8.0% of Ti, 2.0-3.0% of N, less than or equal to 0.05% of impurity content and the balance of C; the preparation method comprises the following steps:
step one, cleaning a Si substrate for 5-20 min by using ultrasonic waves;
secondly, introducing argon and nitrogen, and coating a film by using a Ti and graphite target co-sputtering method, wherein the metalized graphite film layer is prepared by using FTO conductive glass as a substrate and using graphite and a Ti material as co-sputtered target raw materials;
and step three, heating the prepared metallized graphite film layer in a black body furnace, wherein the temperature in the black body furnace is 800-900 ℃, and preserving heat for 2-3 hours.
2. The method for preparing the metallized graphite-like film layer for the battery electrode according to claim 1, wherein the method comprises the following steps: in the second step, the co-sputtering coating method of the Ti and graphite target comprises the following steps: depositing a carbon film on the FTO glass by utilizing magnetron co-sputtering coating equipment; wherein, the substrate is heated to 800-1000 ℃, argon and nitrogen are introduced, and the flow of the argon and the nitrogen is adjusted to ensure that the pressure of a cavity of the magnetron co-sputtering coating equipment is 0.2-0.5 Pa.
3. The method for preparing the metallized graphite-like film layer for the battery electrode according to claim 2, wherein: the flow ratio of argon to nitrogen was 3: 1; the total flow of the argon and the nitrogen is 30-40 sccm; the current density of the graphite target is 10-15W/cm2The current density of the Ti target material is 0.5-1W/cm2。
4. The method for preparing the metallized graphite-like film layer for the battery electrode according to claim 3, wherein the method comprises the following steps: the vacuum degree of the magnetron co-sputtering coating equipment<1×10-4Pa。
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