CN108400177A - A kind of battery electrode metallization class graphite film layer and preparation method thereof - Google Patents
A kind of battery electrode metallization class graphite film layer and preparation method thereof Download PDFInfo
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- CN108400177A CN108400177A CN201810209709.0A CN201810209709A CN108400177A CN 108400177 A CN108400177 A CN 108400177A CN 201810209709 A CN201810209709 A CN 201810209709A CN 108400177 A CN108400177 A CN 108400177A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 94
- 239000010439 graphite Substances 0.000 title claims abstract description 94
- 238000001465 metallisation Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 239000000470 constituent Substances 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 66
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 66
- 239000007789 gas Substances 0.000 claims description 34
- 229910052786 argon Inorganic materials 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 32
- 238000004544 sputter deposition Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 29
- 239000011521 glass Substances 0.000 claims description 17
- 238000000151 deposition Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 150000001721 carbon Chemical group 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000005240 physical vapour deposition Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910034327 TiC 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
- 238000005255 carburizing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000032258 transport Effects 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 kind of battery electrode metallization class graphite film layer and preparation method thereof, the percentage of each constituent for the class graphite film layer that metallizes are:Ti 3.5 ~ 8.0%, N 2.0 ~ 3.0%, impurity content≤0.05%, surplus C.The present invention prepares metallization class graphite film layer using graphite, Ti target cosputterings, and carbon atom is mainly with sp2Hybridized orbit bonding can overcome the defect that the big disadvantage of diamond-like resistivity, reduce carbon atom with sp3The mode of hybridized orbit bonding.The sheet resistance for the class graphite film layer that metallizes meets industrialized production requirement in 100m Ω/ ~ 3 Ω/.
Description
Technical field
The present invention relates to battery technology fields, and in particular to a kind of battery electrode metallization class graphite film layer and its preparation
Method.
Background technology
Solar cell is the novel industry to grow up the 1990s, has cleaning, new energy, pollution-free, section
The high feature of skill content.The electrode of battery is the main composition part of battery, it is primarily involved in the collection of electronics and transports journey.And
The electrode of solar cell is usually made of the electro-conductive glass for being loaded with platinum catalyst, and platinum cost is higher, and therefore, people attempt other
Method substitutes platinum.
Carbon material has the natural good characteristic as solar cell, and Carbon Materials catalytic activity is high, good conductivity, performance
Stablize, and at low cost;Meanwhile graphite-like film can be widely used as the electrode of sensor in electrochemistry related field
Into.Carbon with existing for variform the reason is that:Since carbon atom usually has 3 kinds of hybridized orbit bonding forms, i.e. sp3、sp2With
sp1.When carbon atom is with sp3When hybridized orbit bonding, the form of expression is diamond;With sp2When hybridized orbit bonding, performance
Form is graphite-structure.Diamond lattic structure intensity, hardness are big, and electric conductivity is small, and the DLC film resistance prepared is with million Ω
For unit.On the contrary, graphite-structure intensity, hardness are small, electric conductivity is strong, and film resistor is as unit of Ω or milli Ω, resistivity phase
Poor 106~109。
The electrode of battery requires good conductivity, the deposition method of electrode conductive film to be broadly divided into two classes:Chemical vapor deposition
Product and physical vapour deposition (PVD).Chemical vapor deposition is mainly with carbonaceous gas, such as methane, acetylene are carbon source, using plasma
Learn vapour deposition process;Physical vapour deposition (PVD) prepares film layer mainly using high purity graphite as target, using sputter coating mode.However,
Among the process for the electrode for preparing battery, sp2Hybridized orbit bonding form is difficult to be formed, and the resistivity prepared is big, far
Far above the resistivity of target graphite.The prior art has the film prepared using magnetron sputtering mode, and sheet resistance is 20 ~ 30
The technology requirement of bulk industrial production is also not achieved in Ω/.
Invention content
An object of the present invention is to provide a kind of battery electrode metallization class graphite film layer;The second object of the present invention
It is to provide a kind of preparation method of battery electrode metallization class graphite film layer.Metallization class graphite film layer prepared by the present invention,
Sheet resistance is 100m Ω/ ~ 3 Ω/;Among the process for the electrode for preparing battery, C-C is with sp2Hybridized orbit bonding.
The present invention is that technical solution used by realizing the first purpose is:A kind of battery electrode metallization class graphite film
Layer, the percentage of each constituent for the class graphite film layer that metallizes is:Ti 3.5 ~ 8.0%, N 2.0 ~ 3.0%, impurity content≤
0.05%, surplus C.
The present invention is that technical solution used by realizing the second purpose is:
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using 5 ~ 20min of ultrasonic cleaning Si matrixes;
Step 2: being passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, metallization class graphite film layer is made;
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 800 ~ 900 DEG C in blackbody furnace, is protected
2 ~ 3h of temperature.
Wherein, in step 2, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 800 ~ 1000 DEG C, is passed through argon gas and nitrogen, and the flow for adjusting the two makes the cavity of magnetic control co-sputtering filming equipment
Pressure is 0.2 ~ 0.5 Pa.
In the present invention, the flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 30 ~ 40sccm;Graphite target
The current density of material is 10 ~ 15 W/cm2, the current density of Ti targets is 0.5 ~ 1 W/cm2。
Wherein, the vacuum degree of the magnetic control co-sputtering filming equipment<1×10-4 Pa。
The present invention uses low pressure(0.2~0.5Pa), high base material temperature(800~1000℃), magnetron sputtering DC power supply
Using high-power mode(600~800W), target high current density(10~15W/cm2), atom is in substrate surface fast filming, original
Son is active, is not easy to form diamond-like carbon film layer, generates carburizing reagent at high temperature, part diamond-like is changed into class graphite.
In the membrane-film preparation process of the present invention, the elements such as incorporation Ti, N, Ti members are known as good electric conductivity, part Ti members
Element forms TiC, TiN with C, N, and TiC, TiN are also conductive, in Ti and TiC, TiN disperse and class graphite linings, the middle reaches of film layer
From electron concentration increase, improve the electric conductivity of film, required conductive class graphite film layer be made, class graphite film layer is corrosion-resistant
Property is strong, and rub resistance is strong, and intensity hardness is big, can meet the harsh environment in field.
Ti metallic conductivities are good, meanwhile, Ti element activities are strong so that film layer binding force is strong, does not allow to fall off, meets device
The service life of part.The TiN that the present invention adulterates has higher electric conductivity and superconductivity, can be applied to high-temperature structural material and surpasses
Lead material.
Advantageous effect:The present invention prepares metallization class graphite film layer using graphite, Ti target cosputterings, and carbon atom is main
With sp2Hybridized orbit bonding can overcome the defect that the big disadvantage of diamond-like resistivity, reduce carbon atom with sp3Hybridized orbit at
The mode of key.The sheet resistance for the class graphite film layer that metallizes meets industrialized production requirement in 100m Ω/ ~ 3 Ω/.
The doping of the elements such as Ti/N increases the conductivity of film, wear-resisting property and hardness.Ti elements make film layer knot
Resultant force is strong, does not allow to fall off, can meet the harsh environment in field, increases the service life of device.
With very strong Covalent bonding together between the TiC atoms that the present invention adulterates, several characteristics with metalloid are such as high
Fusing point, boiling point and hardness, hardness is only second to diamond, there is good heat conduction and electric conductivity.
Specific implementation mode
The present invention is further explained in the light of specific embodiments, so that those skilled in the art can be better
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions;It is raw materials used
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase;The present invention percentage, be
Mass percent.
A kind of battery electrode metallization class graphite film layer, the percentage of each constituent for the class graphite film layer that metallizes
For:Ti 3.5 ~ 8.0%, N 2.0 ~ 3.0%, impurity content≤0.05%, surplus C.
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using 5 ~ 20min of ultrasonic cleaning Si matrixes;
Step 2: being passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, metallization class graphite film layer is made;
Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, using graphite and T materials as cosputtering
Target raw material, using magnetic control co-sputtering filming equipment in FTO deposition on glass class graphite film layers;Wherein, base material is heated to 800
The flow for ~ 1000 DEG C, being passed through argon gas and nitrogen, and both adjusting make the chamber pressure of magnetic control co-sputtering filming equipment be 0.2 ~
0.5 Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 30 ~ 40sccm;The electric current of graphite target is close
Degree is 10 ~ 15 W/cm2, the current density of Ti targets is 0.5 ~ 1 W/cm2;The vacuum degree of magnetic control co-sputtering filming equipment<1×
10-4 Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 800 ~ 900 in blackbody furnace
DEG C, keep the temperature 2 ~ 3h.
Embodiment 1
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using ultrasonic cleaning Si matrixes 5min;
Step 2: physical vapor deposition coating film:It is passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, is made
Metallize class graphite film layer;Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 800 DEG C, is passed through argon gas and nitrogen, and the flow both adjusted makes the chamber pressure of magnetic control co-sputtering filming equipment be
0.5Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 30sccm;The current density of graphite target is
10W/cm2, the current density of Ti targets is 0.5W/cm2;Time is 2h;The vacuum degree of magnetic control co-sputtering filming equipment<1×10-4
Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 800 DEG C in blackbody furnace, is protected
Warm 3h carries out heat treatment process.
The thickness for the metallization class graphite film layer prepared is 4 μm.
Embodiment 2
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using ultrasonic cleaning Si matrixes 8min;
Step 2: physical vapor deposition coating film:It is passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, is made
Metallize class graphite film layer;Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 850 DEG C, is passed through argon gas and nitrogen, and the flow both adjusted makes the chamber pressure of magnetic control co-sputtering filming equipment be
0.35Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 40sccm;The current density of graphite target
For 15W/cm2, the current density of Ti targets is 1.0W/cm2;Time is 2h;The vacuum degree of magnetic control co-sputtering filming equipment<1×
10-4 Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 850 DEG C in blackbody furnace, is protected
Warm 2.5h carries out heat treatment process.
The thickness for the metallization class graphite film layer prepared is 5 μm.
Embodiment 3
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using ultrasonic cleaning Si matrixes 10min;
Step 2: physical vapor deposition coating film:It is passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, is made
Metallize class graphite film layer;Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 860 DEG C, is passed through argon gas and nitrogen, and the flow both adjusted makes the chamber pressure of magnetic control co-sputtering filming equipment be
0.40Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 35sccm;The current density of graphite target
For 12W/cm2, the current density of Ti targets is 0.5W/cm2;Time is 5h;The vacuum degree of magnetic control co-sputtering filming equipment<1×
10-4 Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 880 DEG C in blackbody furnace, is protected
Warm 3h carries out heat treatment process.
The thickness for the metallization class graphite film layer prepared is 8 μm.
Embodiment 4
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using ultrasonic cleaning Si matrixes 10min;
Step 2: physical vapor deposition coating film:It is passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, is made
Metallize class graphite film layer;Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 1000 DEG C, is passed through argon gas and nitrogen, and the flow for adjusting the two makes the chamber pressure of magnetic control co-sputtering filming equipment
For 0.25Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 33sccm;The electric current of graphite target is close
Degree is 14W/cm2, the current density of Ti targets is 0.8W/cm2;Time is 3h;The vacuum degree of magnetic control co-sputtering filming equipment<1×
10-4 Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 900 DEG C in blackbody furnace, is protected
Warm 2h carries out heat treatment process.
The thickness for the metallization class graphite film layer prepared is 5 μm.
Embodiment 5
A kind of battery electrode preparation method of metallization class graphite film layer, includes the following steps:
Step 1: using ultrasonic cleaning Si matrixes 10min;
Step 2: physical vapor deposition coating film:It is passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, is made
Metallize class graphite film layer;Wherein, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, with graphite
Target raw material with T materials as cosputtering, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, by base
Material is heated to 900 DEG C, is passed through argon gas and nitrogen, and the flow both adjusted makes the chamber pressure of magnetic control co-sputtering filming equipment be
0.20Pa;The flow-rate ratio of argon gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 38sccm;The current density of graphite target
For 13W/cm2, the current density of Ti targets is 0.7W/cm2;Time is 4h;The vacuum degree of magnetic control co-sputtering filming equipment<1×
10-4 Pa。
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 820 DEG C in blackbody furnace, is protected
Warm 2.2h carries out heat treatment process.
The thickness for the metallization class graphite film layer prepared is 6 μm.
The percentage composition of each component is as shown in table 1 below in the embodiment of the present invention 1 to embodiment 5.
The content of each component in 1 embodiment 1-5 of table
MSP-300B coating machines prepared by model Beijing Chuangshi Weina Technology Co., Ltd. of filming equipment of the present invention.
The equipment that heat treatment process of the present invention uses is that high temperature spectrum prepared by Beijing Chuangshi Weina Technology Co., Ltd. is true
Cavity body blackbody furnace.
In the present invention, the base material of sputtering selects sheet glass, can also replace with conventionally known sputtering substrate;Base material is clear
Wash, dry after be fixed on magnetic control co-sputtering filming equipment vacuum chamber chip bench on, startup power supply vacuumizes, vacuum degree<1×
10-4Pa;It needs to heat base material according to experiment, base material is heated to 800 ~ 1000 DEG C, be passed through argon gas and nitrogen, and adjust two
The flow of person makes the chamber pressure of magnetic control co-sputtering filming equipment be 0.2 ~ 0.5 Pa;Shielding power supply is opened, sputtering voltage is adjusted
And electric current, plated film is carried out after pre-sputtering.It is needed to control sputtering time according to experiment.
Graphite-like film produced by the present invention by changing the power of power supply, and then changes the current density of target, or
Change the length of plated film time to control the thickness of graphite-like film, the thickness of graphite-like film is controllable, versatile.
By class graphite electrode film made from comparative example and embodiment 1 to embodiment 5, determines each sheet resistance and be shown in Table 2.
The tester that the present invention measures class graphite film sheet resistance is four probe test of M-3 types hand-held of Suzhou Jingge Electronic Co., Ltd.
Instrument.It is found that class graphite electrode film prepared by the present invention, sheet resistance is small compared with the resistance of the conductive film of the prior art, and electric conductivity increases
By force.
The sheet resistance of film made from 2 embodiment 1-5 of table
Above example is in order to illustrate technical scheme of the present invention, and the purpose is to be that those skilled in the art is enable to understand
Present disclosure is simultaneously practiced, but is not limited the scope of the invention with this.In every essence according to the present invention
Hold the equivalent changes or modifications made, should all cover within the scope of the present invention.
Claims (5)
1. a kind of battery electrode metallization class graphite film layer, it is characterised in that:Each constituent for the class graphite film layer that metallizes
Percentage be:Ti 3.5 ~ 8.0%, N 2.0 ~ 3.0%, impurity content≤0.05%, surplus C.
2. the method for preparing a kind of battery electrode metallization class graphite film layer as described in claim 1, which is characterized in that packet
Include following steps:
Step 1: using 5 ~ 20min of ultrasonic cleaning Si matrixes;
Step 2: being passed through argon gas and nitrogen, using Ti, graphite target cosputtering method plated film, metallization class graphite film layer is made;
Step 3: metallization class graphite film layer obtained is heated in blackbody furnace, temperature is 800 ~ 900 DEG C in blackbody furnace, is protected
2 ~ 3h of temperature.
3. preparing a kind of method of battery electrode metallization class graphite film layer as claimed in claim 2, it is characterised in that:Step
In rapid two, Ti, graphite target cosputtering film plating process are:Using FTO electro-conductive glass as base material, using graphite and T materials as cosputtering
Target raw material, using magnetic control co-sputtering filming equipment in FTO deposition on glass carbon films;Wherein, base material is heated to 800 ~
The flow for 1000 DEG C, being passed through argon gas and nitrogen, and both adjusting make the chamber pressure of magnetic control co-sputtering filming equipment be 0.2 ~
0.5 Pa。
4. preparing a kind of method of battery electrode metallization class graphite film layer as claimed in claim 3, it is characterised in that:Argon
The flow-rate ratio of gas and nitrogen is 3:1;The total flow of argon gas and nitrogen is 30 ~ 40sccm;The current density of graphite target is 10 ~ 15
W/cm2, the current density of Ti targets is 0.5 ~ 1 W/cm2。
5. preparing a kind of method of battery electrode metallization class graphite film layer as claimed in claim 4, it is characterised in that:Institute
State the vacuum degree of magnetic control co-sputtering filming equipment<1×10-4 Pa。
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CN103147040A (en) * | 2013-03-12 | 2013-06-12 | 浙江大学 | Carbon-titanium composite coating and preparation method of coating |
CN103820761A (en) * | 2014-02-12 | 2014-05-28 | 西安金唐材料应用科技有限公司 | Preparation method for metal carbide coating |
CN105154833A (en) * | 2015-10-30 | 2015-12-16 | 攀枝花学院 | Method for preparing Ti-TiC-graphite composite material |
CN105374562A (en) * | 2015-11-03 | 2016-03-02 | 渤海大学 | Graphite phase C3N4/conductive black carbon composite counter electrode preparation method |
CN105761939A (en) * | 2016-04-25 | 2016-07-13 | 辽宁鑫金铂科技有限公司 | High specific capacitance capacitor cathode foil and film coating apparatus manufacturing the same |
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WO2022242732A1 (en) * | 2021-05-21 | 2022-11-24 | 华为技术有限公司 | Ecg electrode and preparation method therefor, and electronic device |
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