CN1268015C - A modified bamboocarbon lithium-ion battery cathode material and method for making same - Google Patents
A modified bamboocarbon lithium-ion battery cathode material and method for making same Download PDFInfo
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- CN1268015C CN1268015C CNB2004100183969A CN200410018396A CN1268015C CN 1268015 C CN1268015 C CN 1268015C CN B2004100183969 A CNB2004100183969 A CN B2004100183969A CN 200410018396 A CN200410018396 A CN 200410018396A CN 1268015 C CN1268015 C CN 1268015C
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- bamboo carbon
- lithium
- bamboo
- ion battery
- carbon
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title abstract description 19
- 239000010406 cathode material Substances 0.000 title abstract description 5
- 238000000034 method Methods 0.000 title description 6
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 60
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 60
- 241001330002 Bambuseae Species 0.000 claims abstract description 60
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 60
- 239000011425 bamboo Substances 0.000 claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 52
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011574 phosphorus Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000012986 modification Methods 0.000 claims description 18
- 230000004048 modification Effects 0.000 claims description 18
- 229910052796 boron Inorganic materials 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- YZSKZXUDGLALTQ-UHFFFAOYSA-N [Li][C] Chemical compound [Li][C] YZSKZXUDGLALTQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007773 negative electrode material Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 21
- 239000000203 mixture Substances 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 16
- 230000002441 reversible effect Effects 0.000 description 8
- 239000010703 silicon Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 230000005518 electrochemistry Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- BCNBMSZKALBQEF-UHFFFAOYSA-N 1,3-dimethylpyrrolidin-2-one Chemical compound CC1CCN(C)C1=O BCNBMSZKALBQEF-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000002194 amorphous carbon material Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 150000002641 lithium Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002931 mesocarbon microbead Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002006 petroleum coke Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000002916 wood waste Substances 0.000 description 1
Classifications
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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 present invention relates to a modified bamboo carbon lithium-ion battery cathode material which comprises the components of the following weight percentage: 0.5 to 6.0 wt% of Si, 0.2 to 4.0 wt% of B, 0.12 to 3.0 wt% of P and the balance of bamboo carbon in which moisture and ash content are eliminated. The cathode material has a preparation method that the bamboo carbon which is burnt from natural bamboo is pulverized by a machine to be sieved to 50 meshes to 300 meshes, the bamboo carbon powder is put in water, nitric acid is added, the mixture is stirred and filtrated at 60 DEG C to 80 DEG C, the mixture is washed repeatedly by deionized water, then the mixture is dried, the bamboo carbon, silicon powder, boron powder and phosphorus powder are uniformly mixed mechanically in proportion, and then, the mixture is ground or milled in a ball milling mode. The modified bamboo carbon lithium-ion battery cathode material of the present invention has the characteristics of high electrochemical capacity, good circulation performance, safety, no pollution, wide material source, etc.
Description
Technical field
The present invention relates to lithium ion battery cathode material and its preparation method.
Background technology
Risen since the nineties in 20th century " bamboo carbon heat ", it is bamboo wood and the industrial wood waste product through high temperature pyrolysis, and the production of bamboo carbon and research mainly are Japan abroad, also have Korea S, India, countries such as Indonesia.China is the distribution center of world's bamboo, and bamboo resource is very abundant, and from nineteen ninety-five, China begins to fire bamboo carbon, has had suitable scale at present.Bamboo is short as a kind of growth cycle, and it is fast to become a useful person, and upgrades easily, and the forest reserves that power of regeneration is strong are easy to sustainable operation, are subject to people's attention day by day.Bamboo carbon is as the important products of bamboo; be mainly used in aspects such as fuel, environmental protection, food fresh keeping, agricultural production; the lot of domestic and international experts and scholars have carried out number of research projects to bamboo carbon processing and utilization at present, and hope can be developed many new applications.
Sony corporation of Japan in 1991 are with the material with carbon element substituted metal cathode of lithium of graphite-structure, developed lithium ion battery after, started the upsurge of the research and the industrialization of lithium ion battery in the world wide.In recent years, because developing rapidly of portable electronics, and the potential advantages that on electric automobile (EV), have of lithium ion battery, the whole world is increasing to the demand of lithium ion battery at present, performance requirement is also more and more higher, and material with carbon element is as the most frequently used negative material of lithium ion battery, and development prospect is boundless.At present, the carbon negative pole material of commercialization lithium ion battery employing mainly is graphite, petroleum coke, mesophase pitch base carbosphere (MCMB), carbon fiber and RESEARCH OF PYROCARBON etc.Wherein native graphite, petroleum coke, MCMB etc. are first resources, and are non-renewable.And the heat treatment temperature of most of material with carbon elements is higher than 2000 ℃, technology controlling and process difficulty relatively in the production.Bamboo carbon is as a kind of low temperature pyrolyzer amorphous carbon material, phosphorus content height.But the cycle performance of general amorphous carbon is all undesirable, the reversible lithium storage capacity generally with decaying of circulation than very fast.There is hysteresis in voltage in addition, when lithium inserts, mainly is to carry out below 0.3V, and when deviating from, a sizable part is then arranged more than 0.8V.And in general, the primary efficiency for charge-discharge of low temperature amorphous carbon material is lower, and reversible capacity is not high.
Summary of the invention
The purpose of this invention is to provide a kind of electrochemistry capacitance height that has, good cycle, safety non-pollution, the modification bamboo carbon lithium ion cell negative electrode material and preparation method thereof widely of drawing materials.
The present invention is the negative material that the bamboo carbon that modification is handled is used as a kind of lithium ion battery.Modification bamboo carbon lithium ion cell negative electrode material provided by the invention contains (by weight): 0.5～6.0%Si, 0.2～4.0%B, and 0.12～3.0%P, surplus for removing the bamboo carbon of moisture and ash content.
The preparation method of modification bamboo carbon lithium ion cell negative electrode material of the present invention, step is as follows: after natural bamboo is fired the bamboo carbon mechanical crushing that forms and crossed 50～300 mesh sieves, put into water, add nitric acid, stir down at 60～80 ℃, filter, use the deionized water cyclic washing, oven dry then, remove moisture and ash content in the bamboo carbon, machinery is mixed even in proportion with silica flour, boron powder, phosphorus powder with bamboo carbon, grinds then or ball milling, products therefrom is the lithium ion battery negative material of bamboo carbon after silicon, boron, phosphorus modification.
With prepared modification bamboo carbon as electrode active material and acetylene black and be dissolved in Kynoar (PVDF) solution of dimethyl pyrrolidone (NMP) mixed in certain proportion evenly after, be coated on the Copper Foil of certain size, dry 4h in drying box, on twin rollers, be pressed into the thin slice of 0.05～0.15mm then, and in vacuum drying chamber in 120 ℃ of dry 12h, make electrode slice.
Handle the bamboo carbon made as lithium ion battery negative material with of the present invention by mixing silicon, boron, phosphorus modification, in the charge and discharge process, silicon can with lithium atom generation reversible action, in repeatedly still not decay of its electrochemistry capacitance of circulation back.Owing to the adding of boron, increased the binding energy of lithium and material with carbon element, can improve the reversible capacity of bamboo carbon.Mix phosphorus the interlamellar spacing of material with carbon element is increased, help the insertion of lithium and deviate from.In bamboo carbon, mix silicon, boron, P elements simultaneously, bamboo carbon is improved as the reversible embedding lithium capacity and the charge-discharge performance of lithium ion battery negative material.Material of the present invention has the electrochemistry capacitance height, good cycle, safety non-pollution, characteristics such as draw materials extensively.
Embodiment
Embodiment:
Modification bamboo carbon lithium ion cell negative electrode material contains (by weight): 1.4%Si, 0.53%B, and 0.32%P, surplus for removing the bamboo carbon of moisture and ash content.
The preparation method may further comprise the steps: natural bamboo is fired well-thought-out plan carbon, and bamboo carbon contains (by weight): 85% carbon, and 4% ash, all the other are moisture; After bamboo carbon mechanical crushing crossed 100 mesh sieves, put into water, add nitric acid, stir down, filter, use the deionized water cyclic washing, oven dry then, moisture and ash content in the removal bamboo carbon at 60 ℃; Bamboo carbon and silica flour, boron powder, phosphorus powder are mixed evenly by above-mentioned weight content ratio machinery, and ball milling 15h obtains product then.
With prepared modification bamboo carbon product as electrode active material and acetylene black and Kynoar (PVDF) solution that is dissolved in dimethyl pyrrolidone (NMP) with the ratio of 85: 7.5: 7.5 (weight ratio) mixed evenly after, be coated on the Copper Foil that diameter is 14mm, dry 4h in drying box, on twin rollers, be pressed into the thin slice of 0.05～0.15mm then, and in vacuum drying chamber in 120 ℃ of dry 12h, make electrode slice.
The electrode slice of making is formed bipolar electrode formula simulated battery as lithium ion battery negative and to electrode.To electrode is metal lithium sheet (purity is greater than 99.9%), and the lithium electrode consumption is excessive.Electrolyte is to contain 1mol/L LiPF
6DEC+EC (weight ratio DEC: EC=1: 1), barrier film polypropylene Celgard2400.The simulated battery assembling process is finished in relative humidity is lower than 1% dry glove box.The simulated battery that assembles adopts constant current charge-discharge (current density 1mA/cm after placing 12h
2) mode, charging/discharging voltage is 0.005～3V.The reversible embedding lithium capacity of the electrode slice that the measurement lithium ion battery negative material of the present invention that circulates is repeatedly at normal temperatures made and the variation of charge-discharge performance.
The bamboo carbon of removing moisture and ash content is through after mixing silicon, boron, phosphorus modification and handling, in charge and discharge process silicon can with lithium atom generation reversible action, especially between 0.1～0.6V, the still not decay after circulation repeatedly of its capacity.The sub-property of the short of electricity of boron increases the binding energy of lithium and material with carbon element, can improve the reversible capacity of bamboo carbon.And the adding of phosphorus increases the interlamellar spacing of material with carbon element, helps the insertion of lithium and deviates from.After silicon, boron, phosphorus joined bamboo carbon, greatly improved the chemical property of bamboo carbon.
Test result shows that the bamboo carbon modification lithium-ion battery negative material that makes has the following advantages:
1) electrochemistry capacitance height. Bamboo carbon after this example modification, the first embedding lithium capacity of electrode material has had Very big raising. Discharge capacity after the first charge-discharge circulation reaches 403mAh/g, after repeatedly circulating The efficient of doff lithium still remains on very high level, and has obviously improved showing of voltage delay in the removal lithium embedded process Resemble. And the first embedding lithium capacity of bamboo carbon that does not pass through any processing is less than 200mAh/g, first irreversible capacity Greatly, doff lithium efficient is less than 50%.
2) charge-discharge performance is good. At charging and discharging currents density 1mA/cm2, simulated battery voltage range be 0.005 under～3.0V the condition, compare the present invention with the chemical property of the bamboo carbon that did not carry out any processing Bamboo carbon modification lithium-ion battery negative material cycle performance has had obvious improvement, after the first charge-discharge circulation, holds Amount is not repeatedly still decaying after the circulation substantially. And bamboo carbon modification lithium-ion battery negative material of the present invention is greatly It is good that electric current discharges and recharges under the condition cycle performance.
Claims (3)
1. a modification bamboo carbon lithium ion cell negative electrode material is characterized in that containing: 0.5～6.0%Si, 0.2～4.0%B, 0.12～3.0%P, surplus bamboo carbon for removal moisture and ash content.
2. modification bamboo carbon lithium ion cell negative electrode material according to claim 1 is characterized in that containing: 1.4%Si, and 0.53%B, 0.32%P, surplus for removing the bamboo carbon of moisture and ash content.
3. the preparation method of modification bamboo carbon lithium ion cell negative electrode material according to claim 1 and 2, after it is characterized in that natural bamboo fired the bamboo carbon mechanical crushing that forms and cross 50～300 mesh sieves, put into water, add nitric acid, under 60～80 ℃, stir, filter, use the deionized water cyclic washing, then oven dry, machinery is evenly mixed in proportion with bamboo carbon and silica flour, boron powder, phosphorus powder, grinds then or ball milling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100183969A CN1268015C (en) | 2004-05-12 | 2004-05-12 | A modified bamboocarbon lithium-ion battery cathode material and method for making same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100183969A CN1268015C (en) | 2004-05-12 | 2004-05-12 | A modified bamboocarbon lithium-ion battery cathode material and method for making same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1571196A CN1571196A (en) | 2005-01-26 |
| CN1268015C true CN1268015C (en) | 2006-08-02 |
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| CNB2004100183969A Expired - Fee Related CN1268015C (en) | 2004-05-12 | 2004-05-12 | A modified bamboocarbon lithium-ion battery cathode material and method for making same |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315207C (en) * | 2005-06-22 | 2007-05-09 | 浙江大学 | Composite negative pole material of Li-ion battery and its preparing process |
| CN100422112C (en) * | 2005-07-08 | 2008-10-01 | 中国科学院物理研究所 | Carbon-silicon composite material with spherical nucleocapsid, and its preparing method and use |
| CN102263230B (en) * | 2010-05-28 | 2013-09-25 | 荣炭科技股份有限公司 | Lithium ion secondary battery anode material and preparation method |
| CN103633306B (en) * | 2012-08-28 | 2016-01-20 | 华为技术有限公司 | A kind of silicon-carbon composite cathode material and preparation method thereof and lithium ion battery |
| JP6583806B2 (en) * | 2016-09-12 | 2019-10-02 | パナソニックＩｐマネジメント株式会社 | Lithium battery |
| CN107275587B (en) * | 2017-05-11 | 2018-12-18 | 华南农业大学 | A kind of lithium ion silicon-carbon composite cathode material and preparation method thereof |
| CN107275588B (en) * | 2017-05-11 | 2019-01-11 | 华南农业大学 | A kind of lithium ion battery bamboo charcoal/molybdenum sulfide composite negative pole material and preparation method thereof |
| CN107619033A (en) * | 2017-09-08 | 2018-01-23 | 绵阳梨坪科技有限公司 | Bamboo charcoal material for lithium ion battery cathode prepared by a kind of natural products |
| CN107623115A (en) * | 2017-09-18 | 2018-01-23 | 浙江大学 | A kind of hollow pearl nano-silicone wire/carbon composite material and its preparation method and application |
| CN110649239B (en) * | 2019-09-27 | 2020-10-23 | 东北大学 | Si-B-C negative electrode material, preparation method and application thereof, and negative electrode material, electrode plate and lithium ion battery containing Si-B-C negative electrode material |
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2004
- 2004-05-12 CN CNB2004100183969A patent/CN1268015C/en not_active Expired - Fee Related
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| CN1571196A (en) | 2005-01-26 |
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