CN102751477A - Preparation method for silicon-silver composite negative electrode material of lithium ion battery - Google Patents
Preparation method for silicon-silver composite negative electrode material of lithium ion battery Download PDFInfo
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- CN102751477A CN102751477A CN2012102292378A CN201210229237A CN102751477A CN 102751477 A CN102751477 A CN 102751477A CN 2012102292378 A CN2012102292378 A CN 2012102292378A CN 201210229237 A CN201210229237 A CN 201210229237A CN 102751477 A CN102751477 A CN 102751477A
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- ion battery
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- 239000002131 composite material Substances 0.000 title claims abstract description 27
- XNRNVYYTHRPBDD-UHFFFAOYSA-N [Si][Ag] Chemical compound [Si][Ag] XNRNVYYTHRPBDD-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 26
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007773 negative electrode material Substances 0.000 title abstract 6
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 5
- 238000013019 agitation Methods 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 10
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 10
- 239000010703 silicon Substances 0.000 abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 abstract description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 abstract description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 5
- 238000006253 efflorescence Methods 0.000 abstract description 3
- 206010037844 rash Diseases 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract 3
- 238000007599 discharging Methods 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 239000011856 silicon-based particle Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention especially relates to a preparation method for a silicon-silver composite negative electrode material of a lithium ion battery, which belongs to the technical field of preparation methods for chemical materials. According to the method, polyvinylpyrrolidone (PVP) is used as a surfactant, ammonia water is used as a complexing agent, sodium borohydride is used as a reducing agent, AgNO3 is reduced to prepare nanometer silver particles with uniformly distributed particle sizes, and the nanometer silver particles are allowed to uniformly adhere onto the surface of nanometer silicon particles with an average particle size of 30 nm to 500 nm so as to prepare the silicon-silver composite negative electrode material. The preparation method is simple, does not use any complicated equipment, allows reactions to be carried out at normal temperature under normal pressure and can easily realize industrial production. The silicon-silver composite material prepared in the invention has a high density, can improve conductivity of silicon by using good conductivity and ductility of silver metal and alleviates and inhibits efflorescence of silicon in the process of charging and discharging, so the performance of a Si-based negative electrode material is improved; meanwhile, the conductivity of a silicon negative electrode material can also be improved, which allows heavy current charging and discharging of the silicon-silver composite negative electrode material to be realized.
Description
Technical field
The invention belongs to chemical materials preparation method technical field, particularly a kind of preparation method of lithium ion battery silicon silver composite negative pole material.
Background technology
Since Sony Corporation in 1991 commercially produced lithium ion battery, lithium ion battery had become the indispensable part of portable electric appts.Simultaneously, receive the pressure of global petroleum reserves and environment, hybrid vehicle and pure electric automobile are all competitively being developed in countries in the world in recent years, to replace traditional fuel-engined vehicle.Therefore, society has promoted deepening continuously of Study on Li-ion batteries using to the demand of lithium ion battery.
At present, business-like lithium ion battery adopts graphite as negative material, and its source is abundant, stable operating voltage, but theoretical capacity only has 372 mAh/g.Be improving the specific capacity of negative material, have the highest theoretical specific capacity (4212 mAh/g) as the Si of lithium ion battery negative material, is the element that reserves are only second to oxygen in the earth's crust.But the conductivity of silicon is lower, and in charge and discharge process, has the volumetric expansion up to 300 %.This causes the efflorescence of particle, and then separates with conductive agent, peels off from collector, has reduced the cycle performance of Si base negative material, has therefore restricted the commercial applications of Si base negative material.
The method of taking for problems such as solution silicium cathode material efflorescence and electric conductivity differences at present is mainly makes one dimension silicon nanowires or two-dimentional silicon nano thin-film, and this all need utilize large-scale, expensive equipment, and manufacture craft is numerous and diverse, is difficult to realize commercial application.
Summary of the invention
To the prior art deficiency, the invention provides a kind of preparation method of lithium-ions battery silicon silver composite negative pole material.
A kind of preparation method of lithium ion battery silicon silver composite negative pole material is characterized in that the concrete steps of this method are following:
(1) pre-treatment: silicon powder particle is joined in the acetone soln; Supersound washing 20 to 40 minutes; The sodium hydroxide solution or the concentration that add concentration then and be 0.1 mol/L ~ 1.0 mol/L are the hydrofluoric acid solution of 0.1 mol/L ~ 1.0 mol/L; Magnetic agitation 1 h ~ 2 hours, suction filtration then, wash to solution for neutral;
(2) take by weighing the AgNO of respective quality in proportion
3And PVP, wherein AgNO
3The quality of middle Ag is 20% ~ 200% of a silicon powder particle quality, and the quality of polyvinylpyrrolidone (PVP) is 20% ~ 100% of a silicon powder particle quality, and being dissolved in concentration jointly is that magnetic agitation to solution is clarified in the ammonia spirit of 0.5 mol/L ~ 2 mol/L;
(3) the configuration quality mark is 1% ~ 20% sodium borohydride solution;
(4) distilled water and ammoniacal liquor are configured to mother liquor, the concentration of mother liquor is 0.5 mol/L ~ 2 mol/L, places agitated reactor, and the control temperature of reaction kettle is 10 ℃ ~ 30 ℃, under ultrasound condition, carries out powerful mechanical agitation;
(5) resulting solution in step (2) and the step (3) slowly is added drop-wise in the step (4) in the resulting mother liquor simultaneously, after being added dropwise to complete, the control temperature of reaction kettle is 10 ℃ ~ 30 ℃, continues reaction 1 h ~ 3 hours;
(6) after reaction finishes, reaction products resulting in the step (5) is centrifugal with centrifuge, take out lower sediment, thin up, suction filtration and washing are clarified until solution; Again deposition is put into oven drying, obtain a kind of lithium ion battery silicon silver composite negative pole material.
The particle diameter of said silicon powder particle is 30 nm ~ 500 nm.
Mixing speed is 600 r/min ~ 1000 r/min in the said step (4).
Rate of addition is 0.1 ml/min ~ 10 ml/min in the said step (5).
Centrifuge speed is 3000 r/min ~ 5000 r/min in the said step (6).
Centrifugation time is 5 minutes ~ 10 minutes in the said step (6).
Oven temperature is 80 ℃ ~ 120 ℃ in the said step (6).
Be 12 h ~ 16 hours drying time in the said step (6).
Beneficial effect of the present invention is:
Production technology of the present invention is simple, does not use any complex device, and reaction all is to carry out at normal temperatures and pressures, easy realization of industrial production.
The present invention can solve the conductivity of Si low with charge and discharge process in pulverizing problem, the present invention reduces silicon grain particle diameter to nanoscale and evenly adheres to nano-Ag particles to process the silicon silver composite material at silicon face.Wherein, prepared silicon silver composite material can utilize the conductivity of silver metal good electrical conductivity and ductility raising silicon, in charge and discharge process, alleviates and suppress the pulverizing problem of silicon, improves the performance of Si base negative material.
Can improve the silicium cathode conductivity of electrolyte materials through adhering to nano-Ag particles simultaneously, make nano-silicon silver composite negative pole material realize high current charge-discharge; Also can improve the density of this material through methods such as refinement particle, preparation sphere materials.
Description of drawings
Fig. 1 is the silicon nanoparticle electromicroscopic photograph of surface attachment nano-Ag particles.
Fig. 2 is the XRD figure of the prepared silicon silver composite negative pole material of embodiment 2.
Fig. 3 is the prepared cycle performance figure of silicon silver composite negative pole material in lithium ion battery.
Embodiment
The invention provides a kind of preparation method of lithium ion battery silicon silver composite negative pole material, the present invention is further specified below in conjunction with accompanying drawing and embodiment.
Embodiment 1
(1) pre-treatment: getting particle diameter is silicon powder particle 1 gram of 50 nm, joins in the acetone soln, washed 20 minutes, and suction filtration, adding concentration then is the HF solution 50ml of 0.2 mol/L, magnetic agitation 2 hours, filtering and washing is neutral until solution;
(2) take by weighing 2 g AgNO
3, take by weighing 0.5 g PVP, being dissolved in concentration jointly is that magnetic agitation to solution is clarified in the 1 mol/L ammoniacal liquor;
(3) the configuration quality mark is 3% sodium borohydride solution 200 ml;
(4) distilled water and ammoniacal liquor being configured to 1 L concentration is the mother liquor of 1 mol/L, places agitated reactor, and the control temperature of reaction kettle is 10 ℃, and under ultrasound condition, adds powerful mechanical agitation;
(5) solution of gained in step (2) and the step (3) slowly is added drop-wise in the step (4) in the resulting mother liquor simultaneously, dripping speed is 0.5 ml/min, and after dripping off, the control temperature of reaction kettle is 10 ℃, continues reaction 1 hour;
(6) after reaction finishes, the product of gained in the step (5) with centrifuge with the rotating speed of 5000 r/min centrifugal 5 minutes, is taken out lower sediment, thin up, suction filtration also washs, and clarifies until solution.Again deposition is put into 120 ℃ of oven dryings 12 hours, obtain a kind of lithium ion battery silicon silver composite negative pole material.
Embodiment 2
(1) pre-treatment: getting particle diameter is silicon powder particle 1 g of 200 nm, joins in the acetone soln, washed 40 minutes, and suction filtration, adding concentration then is NaOH solution 100 ml of 0.5 mol/L, magnetic agitation 1.5 hours, filtering and washing is neutral until solution;
(2) take by weighing 1 g AgNO
3, take by weighing 1 g PVP, being dissolved in concentration jointly is that magnetic agitation to solution is clarified in the 2 mol/L ammoniacal liquor;
(3) the configuration quality mark is 5% sodium borohydride solution 200 ml;
(4) distilled water and ammoniacal liquor being configured to 1 L concentration is the mother liquor of 2 mol/L, and the control temperature of reaction kettle is 25 ℃, and under ultrasound condition, adds powerful mechanical agitation;
(5) solution of gained in step (2) and the step (3) slowly is added drop-wise in the step (4) in the resulting mother liquor simultaneously, dripping speed is 3 ml/min, and after dripping off, the control temperature of reaction kettle is 25 ℃, continues reaction 1.5 hours;
(6) after reaction finishes, the product of gained in the step (5) with centrifuge with the rotating speed of 4000 r/min centrifugal 10 minutes, is taken out lower sediment, thin up, suction filtration also washs, and clarifies until solution.Again deposition is put into 80 ℃ of oven dryings 16 hours, obtain a kind of lithium ion battery silicon silver composite negative pole material.
Claims (8)
1. the preparation method of lithium ion battery silicon silver composite negative pole material is characterized in that the concrete steps of this method are following:
(1) pre-treatment: silicon powder particle is joined in the acetone soln; Supersound washing 20 to 40 minutes; The sodium hydroxide solution or the concentration that add concentration then and be 0.1 mol/L ~ 1.0 mol/L are the hydrofluoric acid solution of 0.1 mol/L ~ 1.0 mol/L; Magnetic agitation 1 h ~ 2 hours, suction filtration then, wash to solution for neutral;
(2) take by weighing the AgNO of respective quality in proportion
3And PVP, wherein AgNO
3The quality of middle Ag is 20% ~ 200% of a silicon powder particle quality, and the quality of PVP is 20% ~ 100% of a silicon powder particle quality, and being dissolved in concentration jointly is that magnetic agitation to solution is clarified in the ammonia spirit of 0.5 mol/L ~ 2 mol/L;
(3) the configuration quality mark is 1% ~ 20% sodium borohydride solution;
(4) distilled water and ammoniacal liquor are configured to mother liquor, the concentration of mother liquor is 0.5 mol/L ~ 2 mol/L, places agitated reactor, and the control temperature of reaction kettle is 10 ℃ ~ 30 ℃, under ultrasound condition, carries out powerful mechanical agitation;
(5) resulting solution in step (2) and the step (3) slowly is added drop-wise in the step (4) in the resulting mother liquor simultaneously, after being added dropwise to complete, the control temperature of reaction kettle is 10 ℃ ~ 30 ℃, continues reaction 1 h ~ 3 hours;
(6) after reaction finishes, reaction products resulting in the step (5) is centrifugal with centrifuge, take out lower sediment, thin up, suction filtration and washing are clarified until solution; Again deposition is put into oven drying, obtain a kind of lithium ion battery silicon silver composite negative pole material.
2. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: the particle diameter of said silicon powder particle is 30 nm ~ 500 nm.
3. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: mixing speed is 600 r/min ~ 1000 r/min in the said step (4).
4. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: rate of addition is 0.1 ml/min ~ 10 ml/min in the said step (5).
5. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: centrifuge speed is 3000 r/min ~ 5000 r/min in the said step (6).
6. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: centrifugation time is 5 minutes ~ 10 minutes in the said step (6).
7. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: oven temperature is 80 ℃ ~ 120 ℃ in the said step (6).
8. the preparation method of a kind of lithium ion battery silicon silver composite negative pole material according to claim 1, it is characterized in that: be 12 h ~ 16 hours drying time in the said step (6).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102969489A (en) * | 2012-12-05 | 2013-03-13 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material, preparation method of silicon-carbon composite material, and lithium ion battery containing silicon-carbon composite material |
| CN103151504A (en) * | 2013-04-08 | 2013-06-12 | 廖小玉 | Preparation method of silver doped carbon-silicon composite negative electrode material |
| CN105226244A (en) * | 2015-08-27 | 2016-01-06 | 西北师范大学 | Three-dimensional porous silicon-nano silver composite material and preparation thereof and the application as lithium ion battery negative material |
| CN106299276A (en) * | 2016-08-25 | 2017-01-04 | 合肥国轩电池材料有限公司 | A kind of preparation method of ion cathode material lithium silver surface modified lithium titanate |
| CN112271297A (en) * | 2020-10-20 | 2021-01-26 | 西安工程大学 | Grid type laminated structure material synthesis and molding integrated silicon cathode and preparation method thereof |
| CN115084478A (en) * | 2022-07-11 | 2022-09-20 | 成都佰思格科技有限公司 | Hard carbon silver composite negative electrode material, preparation method thereof and lithium ion battery |
| CN115863660A (en) * | 2022-12-09 | 2023-03-28 | 江苏正力新能电池技术有限公司 | Negative current collector of negative-electrode-free lithium battery and preparation method and application thereof |
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2012
- 2012-07-03 CN CN2012102292378A patent/CN102751477A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102969489A (en) * | 2012-12-05 | 2013-03-13 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material, preparation method of silicon-carbon composite material, and lithium ion battery containing silicon-carbon composite material |
| CN103151504A (en) * | 2013-04-08 | 2013-06-12 | 廖小玉 | Preparation method of silver doped carbon-silicon composite negative electrode material |
| CN103151504B (en) * | 2013-04-08 | 2015-10-28 | 廖小玉 | A kind of preparation method of Ag doping carbon-silicon composite cathode material |
| CN105226244A (en) * | 2015-08-27 | 2016-01-06 | 西北师范大学 | Three-dimensional porous silicon-nano silver composite material and preparation thereof and the application as lithium ion battery negative material |
| CN106299276A (en) * | 2016-08-25 | 2017-01-04 | 合肥国轩电池材料有限公司 | A kind of preparation method of ion cathode material lithium silver surface modified lithium titanate |
| CN112271297A (en) * | 2020-10-20 | 2021-01-26 | 西安工程大学 | Grid type laminated structure material synthesis and molding integrated silicon cathode and preparation method thereof |
| CN112271297B (en) * | 2020-10-20 | 2022-09-06 | 西安工程大学 | Grid type laminated structure material synthesis and molding integrated silicon cathode and preparation method thereof |
| CN115084478A (en) * | 2022-07-11 | 2022-09-20 | 成都佰思格科技有限公司 | Hard carbon silver composite negative electrode material, preparation method thereof and lithium ion battery |
| CN115084478B (en) * | 2022-07-11 | 2023-03-07 | 成都佰思格科技有限公司 | Hard carbon-silver composite negative electrode material, preparation method thereof and lithium ion battery |
| CN115863660A (en) * | 2022-12-09 | 2023-03-28 | 江苏正力新能电池技术有限公司 | Negative current collector of negative-electrode-free lithium battery and preparation method and application thereof |
| CN115863660B (en) * | 2022-12-09 | 2024-05-17 | 江苏正力新能电池技术有限公司 | Negative electrode current collector of non-negative electrode lithium battery and preparation method and application thereof |
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Application publication date: 20121024 |