CN103794792B - A kind of preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material - Google Patents
A kind of preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material Download PDFInfo
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- CN103794792B CN103794792B CN201410072173.4A CN201410072173A CN103794792B CN 103794792 B CN103794792 B CN 103794792B CN 201410072173 A CN201410072173 A CN 201410072173A CN 103794792 B CN103794792 B CN 103794792B
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- 239000004005 microsphere Substances 0.000 title claims abstract description 57
- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 38
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 25
- 239000010439 graphite Substances 0.000 claims abstract description 25
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000009825 accumulation Methods 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000000527 sonication Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 5
- 238000001241 arc-discharge method Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 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
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
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- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation method for used as negative electrode of Li-ion battery nano carbon microsphere material.Employing high purity graphite is anode, inert metal plate is negative electrode, Direct Electrolysis in mellitic acid, adding the non-toxic base material easily decomposing volatilization makes nano carbon microsphere particle precipitate rapidly, after drying precipitate, namely obtain diameter has nano-porous structure nano carbon microsphere material between the used as negative electrode of Li-ion battery of 10-1000nm scope.Electrolysis divides two stages to carry out electrolysis, and first stage electrolysis time is not less than 1 day, and initial voltage is not more than 200V, and electric current is not more than 3A; Second stage initial voltage is not more than 36V, and Current Control is between 3-30A.The hydro thermal method of relatively-high temperature high pressure of the present invention, the arc discharge method of vacuum condition, its technique is simple, convenient operation.
Description
Technical field
The present invention relates to a kind of nano carbon microsphere material preparation method with nano-porous structure, particularly a kind of for lithium ion battery negative pole carbon material preparation method, belong to field of nano material preparation.
Background technology
Relatively other traditional secondary cells, lithium ion battery have high working voltage, high-energy-density, operating temperature range wide, have extended cycle life, the advantage such as memory-less effect, in industry and life, have extensive application demand.The performance of negative material on battery of lithium ion battery has vital impact.Current commercial lithium cell negative electrode material is mainly the material with carbon element such as native graphite and the micro-carbon ball of mesophase spherule.Native graphite theoretical capacity less (372mAh/g), and solvent molecule easily occurs embed graphite flake layer altogether with lithium ion and cause the phenomenon that graphite " peels off ", brings out structural damage thus causes the rapid degradation of electrode cycle performance.Relative to Delanium, there is a large amount of microcellular structures in mesocarbon ball, has higher lithium memory capacity, and not easily occur that lamella " peels off " phenomenon.But its particle size is mainly micron order.As by further for carbon micron-spheres fine, its Electronic Structure and crystal structure will change, and have higher specific area and activity, be conducive to the performance improving lithium ion battery further.
The method preparing nano carbon microsphere material at present has multiple, the methods such as such as chemical oxidizing agent graphite oxide method, plasma discharge oxidizing process, electronbeam irradiation method, arc discharge evaporation.Above-mentioned various method all directly can not obtain high-purity, active, the nano carbon microsphere of stable uniform, also needs much to assist modification process and equipment, prepares with said method, equipment is too complicated, and technique is too loaded down with trivial details, and output is not high, some technique uses heavy metal substance in a large number, is unfavorable for environmental protection.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material is provided.
In order to solve the problems of the technologies described above, the technical scheme that the present invention takes is: a kind of preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material, high purity graphite electrolysis in mellitic acid solution is adopted to obtain used as negative electrode of Li-ion battery nano carbon microsphere material, anode electrode plate adopts thickness to be 50-80mm, the high purity graphite plate of length 300-700mm, width 300-700mm; Cathode electrode plate adopts thickness to be 2-10mm, length 300-700mm, the inert metal plate of width 300-700mm;
After switching on power, point two stages carry out electrolysis, and first stage electrolysis time is not less than 1 day, and initial voltage is not more than 200V, and electric current is not more than 3A; Second stage initial voltage is not more than 36V, and Current Control is between 3-30A; Preparing every 1-3h in nano carbon microsphere process, open processor for ultrasonic wave circular treatment once, circular flow is 5-30L/min, single treatment time 10min-30min, odd-numbered day accumulation sonication treatment time 2-3h; Preparation electrolysis is stopped when nano carbon microsphere domain size distribution D50 is in 10-1000 nm;
After obtaining qualified nano carbon microsphere liquid, add the alkaline matter easily decomposing volatilization, make pH value close to 7 in electrolyte, nano carbon microsphere precipitates, and repeatedly wash deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
The pH value of the mellitic acid solution described in above-mentioned steps is 2-5.
Between the preferred 150-200V of initial voltage of the first stage electrolysis described in above-mentioned steps, the preferred 2A-3A of electric current, the preferred 1-2 days of electrolysis time.
The power of the processor for ultrasonic wave described in above-mentioned steps is 1000-3000W, and ultrasonic frequency is 10KHz-40KHz.
Alkaline matter described in above-mentioned steps is (NH
4)
2cO
3or NH
4hCO
3.
The nano carbon microsphere scantling obtained in above-mentioned steps is between 10-1000 nm, and its inside has nano-porous structure.
Prior art is compared, and the present invention has following beneficial effect:
Technique is simple, convenient operation.This technique adopts high purity graphite, mellitic acid is raw material, nano-lithium ion cell negative pole nano carbon microsphere material is directly obtained by electrolysis mode, carbon ball has significant nano-porous structure, and when making lithium-ion negative pole and using, battery charging and discharging capacity can reach 370-1000 mAh/g.The hydro thermal method of relatively-high temperature high pressure of the present invention, the arc discharge method of vacuum condition, its technique is simple, convenient operation.
Accompanying drawing explanation
Fig. 1 is the SEM photo figure (a is low power, and b is high power) under the embodiment of the present invention 1 used as negative electrode of Li-ion battery nano carbon microsphere material different multiples.
Embodiment
Before description material of the present invention, method, be to be understood that this disclosure is not limited to described concrete grammar and material, because these can change.Will also be understood that the object of term as used in this specification just in order to describe these specific forms or embodiment, instead of be intended to limit this scope.Unless otherwise defined, as used herein all technology or the term of science there is the identical implication usually understood with those of ordinary skill in the art.
Employing high purity graphite is anode, and inert metal plate is negative electrode, and in mellitic acid, Direct Electrolysis obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
Anode electrode plate adopts thickness to be 50-80mm, length 300-700mm, the high purity graphite plate of width 300-700mm; Cathode electrode plate adopts thickness to be 2-10mm, length 300-700mm, the inert metal plate of width 300-700mm.Described inert metal plate is titanium plate, corrosion resistant plate, nickel plate or have metallic oxide coating electrode plate.
After switching on power, first stage initial voltage controls between 150-200V, and Current Control is between 2-3A, and the time is about 1-2 days; Second stage Current Control is between 3-30A; Preparing in nano carbon microsphere liquid process every 1-3h, open processor for ultrasonic wave circular treatment once, circular flow is 5-30L/min, single treatment time 10min-30min, odd-numbered day accumulation sonication treatment time 2-3h, hyperacoustic power is 1000-3000W, and ultrasonic frequency is 10KHz-40KHz; Stop preparation when nano carbon microsphere particle diameter D50 is at 10-1000 nm, obtain required product.
If described power supply selects commutating DC stabilized voltage power supply, first stage selection specification is 3A/1500V high voltage low current stabilized voltage power supply, and second stage selects specification to be the stabilized voltage power supply of 50A/50V.
If described power supply selects pulse voltage unstable state power supply, pulse repetition frequency controls between 5-50Hz, and the cycle is 0.2 second-0.02 second.
After obtaining qualified nano carbon microsphere solution, in solution, add (the NH easily decomposing volatilization
4)
2cO
3or NH
4hCO
3alkaline matter, change pH value close to 7, nano carbon microsphere is precipitated, repeatedly washes deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
Provide three specific embodiments utilizing preparation method of the present invention to prepare used as negative electrode of Li-ion battery nano carbon microsphere material below.
embodiment 1
Anode electrode plate adopts thickness to be 60mm, length 500mm, the high purity graphite plate of width 500mm, purity >=99.99% of high purity graphite plate, ash≤50ppm, bulk density >=1.85g/cm3, rupture strength >=60Mpa, granularity < 300 order; Cathode electrode plate adopts thickness to be 5mm, length 500mm, the titanium plate of width 500; Spacing between adjacent high purity graphite plate and titanium plate is 3mm.Power supply selects commutating DC stabilized voltage power supply.The pH value of mellitic acid solution is about 2.
After switching on power, first stage adopts 3A/1500V high voltage low current stabilized voltage power supply, initial voltage is 200V, along with the prolongation of electroxidation time, start in electrolyte water to occur graphite carbon granules, conductivity strengthens gradually, electric current starts to rise, by regulation voltage, control electric current at about 3A, electrolysis 1 day; Second stage adopts specification to be the stabilized voltage power supply of 50A/50V, and initial voltage is 10V, and Current Control is at about 15A; Preparing every 1h in charcoal glue process, open processor for ultrasonic wave circular treatment once, circular flow is 30L/min, single treatment time 30min, odd-numbered day accumulation sonication treatment time 3h, and hyperacoustic power is 3000W, and ultrasonic frequency is 40KHz; Electrolysis is stopped when nano carbon microsphere particle diameter D50 is at 50-100 nm.
After obtaining qualified nano carbon microsphere solution, in solution, add (NH
4)
2cO
3, change pH value close to 7, nano carbon microsphere is precipitated, repeatedly washes deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
Institute's nano carbon microsphere material that obtains is as negative pole, and specific capacity is 700 mAh/g, and relative commercially available prod (370 mAh/g) has better specific capacity.
Can find out that from the SEM figure of Fig. 1 this nano carbon microsphere material has significant nano-porous structure.
embodiment 2
Anode electrode plate adopts thickness to be 50mm, length 300mm, the high purity graphite plate of width 300mm, purity >=99.99% of high purity graphite plate, ash≤50ppm, bulk density >=1.85g/cm3, rupture strength >=60Mpa, granularity < 300 order; Cathode electrode plate adopts thickness to be 2mm, length 300mm, the titanium plate of width 300mm; Spacing between adjacent high purity graphite plate and titanium plate is 5mm.Power supply selects pulse voltage unstable state power supply.The pH value of mellitic acid solution is about 5.
After switching on power, the pulse repetition frequency in the whole cycle controls at 5Hz, and the cycle is 0.2 second.First stage initial voltage controls at about 150V, and along with the prolongation of electroxidation time, start in electrolyte water to occur graphite carbon granules, conductivity strengthens gradually, and electric current starts to rise, and by regulation voltage, control electric current at about 2A, electrolysis time is 2 days; Second stage initial voltage controls at 3V, and Current Control is between 3A; Preparing every 2h in charcoal glue process, open processor for ultrasonic wave circular treatment once, circular flow is 20L/min, single treatment time 20min, odd-numbered day accumulation sonication treatment time 2h, and hyperacoustic power is 2000W, and ultrasonic frequency is 30KHz; Stop preparation when nano carbon microsphere particle diameter D50 is at 15-20 nm, stop electrolysis.
After obtaining qualified nano carbon microsphere solution, in solution, add NH
4hCO
3, change pH value close to 7, nano carbon microsphere is precipitated, repeatedly washes deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
Institute's nano carbon microsphere material that obtains is as negative pole, and specific capacity is 600 mAh/g, and relative commercially available prod (370 mAh/g) has better specific capacity.
embodiment 3
Anode electrode plate adopts thickness to be 80mm, length 700mm, the high purity graphite plate of width 700mm, purity >=99.99% of high purity graphite plate, ash≤50ppm, bulk density >=1.85g/cm3, rupture strength >=60Mpa, granularity < 300 order; Cathode electrode plate adopts thickness to be 10mm, length 700mm, the titanium plate of width 700mm; Spacing between adjacent high purity graphite plate and titanium plate is 10mm.Power supply selects pulse voltage unstable state power supply.The pH value of mellitic acid solution is about 3.5.
After switching on power, the pulse repetition frequency in the whole cycle controls at 50Hz, and the cycle is 0.02 second.First stage initial voltage controls at about 180V, and along with the prolongation of electroxidation time, start in electrolyte water to occur graphite carbon granules, conductivity strengthens gradually, and electric current starts to rise, and by regulation voltage, control electric current at about 2.5A, electrolysis time is 1.5 days; Second stage initial voltage controls at 36V, and Current Control is at about 30A; Preparing every 3h in charcoal glue process, open processor for ultrasonic wave circular treatment once, circular flow is 5L/min, single treatment time 10min, and hyperacoustic power is 1000W, and ultrasonic frequency is 10KHz; Electrolysis is stopped when D50 is at 500-1000nm.
After obtaining qualified nano carbon microsphere solution, in solution, add NH
4hCO
3, change pH value close to 7, nano carbon microsphere is precipitated, repeatedly washes deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
The nano carbon microsphere material specific capacity that obtains is 420mAh/g, and relative commercially available prod (370mAh/g) has better specific capacity.
Claims (9)
1. the preparation method of a used as negative electrode of Li-ion battery nano carbon microsphere material, it is characterized in that described nano carbon microsphere material obtains by adopting high purity graphite electrolysis in mellitic acid solution, anode electrode plate adopts thickness to be 50-80mm, the high purity graphite plate of length 300-700mm, width 300-700mm; Cathode electrode plate adopts thickness to be 2-10mm, length 300-700mm, the inert metal plate of width 300-700mm;
After switching on power, point two stages carry out electrolysis, and first stage electrolysis time is not less than 1 day, and initial voltage is not more than 200V, and electric current is not more than 3A; Second stage initial voltage is not more than 36V, and Current Control is between 3-30A; Preparing every 1-3h in nano carbon microsphere process, open processor for ultrasonic wave circular treatment once, circular flow is 5-30L/min, single treatment time 10min-30min, odd-numbered day accumulation sonication treatment time 2-3h; Electrolysis is stopped when nano carbon microsphere domain size distribution D50 is in 10-1000nm;
After obtaining nano carbon microsphere liquid, add alkaline matter, make pH value close to 7 in electrolyte, nano carbon microsphere precipitates, and repeatedly wash deposit, under 100 degrees celsius, namely drying obtains used as negative electrode of Li-ion battery nano carbon microsphere material.
2. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, is characterized in that the pH value of described mellitic acid solution is 2-5.
3. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, is characterized in that described power supply selects commutating DC stabilized voltage power supply or pulse voltage unstable state power supply.
4. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 3, it is characterized in that first stage selection specification is 3A/1500V high voltage low current commutating DC stabilized voltage power supply, second stage selection specification is the commutating DC stabilized voltage power supply of 50A/50V.
5. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 3, it is characterized in that described its pulse repetition frequency of pulse voltage unstable state power supply controls between 5-50Hz, the cycle is 0.2 second-0.02 second.
6. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, it is characterized in that the initial voltage of described first stage electrolysis is 150-200V, electric current is 2A-3A, and electrolysis time is 1-2 days.
7. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, it is characterized in that the power of described processor for ultrasonic wave is 1000-3000W, ultrasonic frequency is 10KHz-40KHz.
8. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, is characterized in that described alkaline matter is (NH
4)
2cO
3or NH
4hCO
3.
9. the preparation method of used as negative electrode of Li-ion battery nano carbon microsphere material according to claim 1, it is characterized in that the dry rear nano carbon microsphere scantling obtained is between 10-1000nm, its inside has nano-porous structure.
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| CN104831307B (en) * | 2015-05-13 | 2017-06-16 | 东南大学 | A kind of preparation method of micro-nano graphene film |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
| CN110698683B (en) * | 2019-09-27 | 2021-08-24 | 广西师范大学 | One-dimensional dysprosium polymer and preparation method thereof |
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| CN1853764A (en) * | 2005-04-20 | 2006-11-01 | 北京天中树科技发展有限公司 | Production and producer for nanometer carbon liquid |
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| JP2000086220A (en) * | 1998-09-14 | 2000-03-28 | Kenichi Fujita | Ultrafine carbon particle |
| WO2006022100A1 (en) * | 2004-08-27 | 2006-03-02 | Jfe Chemical Corporation | Graphite material, method for producing same, negative electrode material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1579932A (en) * | 2003-08-12 | 2005-02-16 | 刘键 | Preparation of nano graphite carbon colloidal SOL by pulse electrode process |
| CN1853764A (en) * | 2005-04-20 | 2006-11-01 | 北京天中树科技发展有限公司 | Production and producer for nanometer carbon liquid |
| CN103373722A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | Preparation of nano-graphite carbon sol |
| CN103395777A (en) * | 2013-08-07 | 2013-11-20 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
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