CN102496703A - Multiple doped carbon cathode active material and negative electrode used for lithium battery as well as preparation method thereof - Google Patents
Multiple doped carbon cathode active material and negative electrode used for lithium battery as well as preparation method thereof Download PDFInfo
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- CN102496703A CN102496703A CN2011104564550A CN201110456455A CN102496703A CN 102496703 A CN102496703 A CN 102496703A CN 2011104564550 A CN2011104564550 A CN 2011104564550A CN 201110456455 A CN201110456455 A CN 201110456455A CN 102496703 A CN102496703 A CN 102496703A
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Abstract
The invention relates to a multiple doped carbon cathode active material and a negative electrode used for a lithium battery as well as a preparation method thereof. The multiple doped carbon cathode active material comprises the following ingredients by weight percentage: 5-30% of nano porous carbon aerogel, 50-90% of graphite, 1-5% of superconductive carbon black and 3-10% of binder polyvinylidene fluoride. According to the invention, the multiple doped carbon cathode active material is capable of placing a traditional graphite-base cathode material and can be practically used on the lithium ion battery cathode, the advantages of the traditional graphite-base cathode and nano porous charcoal electrode are combined, so that the problems of low energy density and poor circulation performance of a traditional lithium battery can be solved, and high energy density and a good voltage flat can be provided; the traditional lithium ion battery cathode preparation technology is employed, the production process is simple and easy to operate; the raw materials of the carbon doped cathode active material are easy to acquire, so that the method of the invention is in favor of industrial production.
Description
Technical field
The invention belongs to technical field of lithium ion, especially a kind of lithium battery is with multi-element doping carbon negative active core-shell material, negative electrode and preparation method thereof.
Background technology
The demand of electronic information epoch to portable power source increases fast.Since lithium ion battery have high voltage, high power capacity and have extended cycle life, characteristics such as security performance is good; It is had broad application prospects in many-sides such as portable electric appts, electric automobile, space technology, national defense industry, become the research focus of widely paying close attention in recent years.Though use the small rechargeable lithium ion battery commercialization of carbon electrode, and be used widely,, still the assistant officer is to be solved for problem such as how further to improve specific energy, specific power (discharging current), cycle life, reduce cost.And nearest global environmental protection declaration requires the extended-life lithium ion battery of high-energy, high power, high security to be applied to fields such as large-scale storage battery and electric automobile in the near future more, and this has proposed requirements at the higher level to li-ion electrode materials undoubtedly.
The lithium ion battery performance depends on electrode material, particularly negative material consumingly, and research work at present mainly concentrates on material with carbon element and other metal oxide with special construction.Graphite, soft carbon, middle phase carbosphere have more R and D at home and abroad, and multiple nanostructured carbon material such as hard carbon, CNT, bucky-ball C60 are studied (J.Power Sources 2004,136,334.).The researcher thinks that research from now on will more focus mostly in the embedding lithium micro-structural of littler nanoscale.The graphite-based carbon material is widely used in GND at present, but there is following unavoidable shortcoming in this material: complex process, low energy densities and cycle performance are not good etc.And preparation high-purity and regular micro-structural carbon negative pole material are important directions of development; The resin that will have special cross-linked structure at high temperature decomposes the hard carbon that obtains; The reversible capacitance amount is higher than graphitic carbon, can reach 1170mAh/g like the M J Matthews of U.S. MIT report PPP-700 (a kind of thermal decomposition product of poly-phenylene vinylene (ppv)) lithium storage content.But it is bigger that the structure of this material with carbon element is influenced by raw material; But general document thinks that the nanometer micropore in these carbon structures has considerable influence to its embedding lithium capacity; Its research is mainly concentrated on the high polymer that utilizes special molecular structure to prepare and contains the more carbon (Nat.Mater.2005 of Donna meter level micropore; 4,366).
Carbon aerogels (Carbon Aerogel) is the novel nano porous network structure material that a kind of porosity is high, specific area is big, structure artificial is controlled; For the injection of ion provides smooth and easy passage with withdrawing from; And greatly improved the capacity of lithium ion, also help making lithium ion battery to more more miniaturization development of lightweight.In addition; The carbon network backbone of carbon aerogels is amorphous carbon and the graphite mixed structure of microcrystalline carbon mutually normally, and this structure can be embedded in the micro crystal graphite structure lithium ion, and position such as carbon nano-structured layer, limit end, surface; Increased embedding lithium capacity; Abundant simultaneously hole can make electrolyte osmosis in aeroge nanoporous network, fully contacts with carbon aerogels nanometer skeleton, improves contact area; The performances such as energy density, quick charge of lithium ion battery be can significantly improve, thereby the development and the exploitation of the devices such as quick charge lithium ion battery that high-performance, big capacity, circulation are durable are expected to promote.But unbodied carbon aerogels discharges and recharges does not have tangible platform, and higher irreversible capacity is arranged, and therefore, also is difficult at present carbon aerogels is used for lithium ion battery electrode material.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; Provide a kind of lithium battery with multi-element doping carbon negative active core-shell material, negative electrode and preparation method thereof; Use multi-element doping carbon negative active core-shell material to replace traditional graphite-based negative material, solved problems such as low energy densities, the cycle performance of traditional lithium battery be not good.
The present invention solves its technical problem and takes following technical scheme to realize:
A kind of lithium battery is with multi-element doping carbon negative active core-shell material, and it constitutes component and weight percentages of components is: nanoporous carbon aerogels 5%～30%, graphite 50%～90%, superconduction carbon black 1%～5%, binding agent Kynoar 3%～10%.
And described nanoporous carbon aerogels is to be precursor reagent with resorcinol and formaldehyde, and sodium carbonate liquor is a catalyst, through Temperature Treatment, solvent replacing, constant pressure and dry, high temperature carbonization, gas activation and make.
And the mol ratio of described resorcinol and sodium carbonate liquor is 100～2000, and the mass fraction of catalyst solution is 10%～60%.
And the aperture of described nanoporous carbon aerogels is 2nm～200nm, and specific area is 400m
2/ g～3500m
2/ g, resistivity is less than or equal to 0.3 Ω cm.
A kind of negative electrodes for lithium batteries that uses multi-element doping carbon negative active core-shell material; Comprise active material collector, active material, barrier film, electrolyte, organic solvent and reference electrode, described active material is each described multi-element doping carbon negative active core-shell material of claim 1 to 4, and the active material collector is a copper sheet; Barrier film is the Celgard2500 micro-pore septum; Electrolyte is a lithium hexafluoro phosphate, and organic solvent is EC: EMC=1: 1 (volume ratio), reference electrode are metal lithium sheet.
A kind of preparation method who uses the negative electrodes for lithium batteries of multi-element doping carbon negative active core-shell material; Comprise: multi-element doping carbon negative active core-shell material is milled into powder and uses 200 mesh to filter; With powder and binding agent polyvinylidene fluoride mixed by 90: 10; Join mixing and stirring in the solvent 1-Methyl-2-Pyrrolidone, evenly spread upon on the copper sheet, promptly obtain negative electrodes for lithium batteries after the drying.
Advantage of the present invention and good effect are:
The present invention adopts multi-element doping carbon negative active core-shell material to replace traditional graphite-based negative material and this material is applied to lithium ion battery negative; In conjunction with the advantage of conventional graphite base carbon negative pole and nanoporous carbon electrode; Solved problems such as low energy densities, the cycle performance of traditional lithium battery be not good, also had simultaneously: high energy density and voltage platform preferably; Adopt the preparation technology of traditional lithium ion battery negative, the simple and easy operating of production technology; The employed raw material of doping carbon negative active core-shell material are prone to obtain, and help industrialization production.
Description of drawings
Fig. 1 is the SEM figure (multiplication factor is 10000 times) of multi-element doping carbon negative active core-shell material of the present invention;
Fig. 2 is the SEM figure (10000 times of multiplication factors) of nanoporous carbon aerogels of the present invention.
Embodiment
Below in conjunction with instance the present invention is done and to further describe.
A kind of lithium battery is with multi-element doping carbon negative active core-shell material; It constitutes component and weight percentages of components is: nanoporous carbon aerogels 5%～30%, graphite 50%～90%, superconduction carbon black 1%～5%; Binding agent Kynoar 3%～10%, the summation of each component are 100%.
In said components; The nanoporous carbon aerogels is to be precursor reagent with resorcinol (R) and formaldehyde (F); Sodium carbonate (C) solution is catalyst; Through certain Temperature Treatment, solvent replacing, constant pressure and dry, high temperature carbonization, gas activation and make, the carbon aerogels aperture of finally preparing is 2nm～200nm, and specific area is 400m
2/ g～3500m
2/ g, resistivity is not higher than 0.3 Ω cm.Wherein, reactant resorcinol (R) is 100～2000 with the mol ratio of catalyst carbonic acid sodium (C), and the mass fraction of catalyst solution is 10%～60%.
A kind of negative electrodes for lithium batteries that adopts multi-element doping carbon negative active core-shell material; Comprise active material collector, multi-element doping carbon negative active core-shell material, barrier film, electrolyte, organic solvent and reference electrode; This active material collector is a copper sheet, and barrier film is the Celgard2500 micro-pore septum, and electrolyte is a lithium hexafluoro phosphate; Organic solvent is EC: EMC=1: 1 (volume ratio), reference electrode are metal lithium sheet.This negative electrodes for lithium batteries preparation method is: multi-element doping carbon negative active core-shell material is milled into powder and uses 200 mesh to filter; With powder and binding agent polyvinylidene fluoride mixed by 90: 10; Join mixing and stirring in the solvent 1-Methyl-2-Pyrrolidone; Evenly spread upon on the copper sheet, promptly obtain negative electrodes for lithium batteries after the drying.
Embodiment 1
With resorcinol and formaldehyde is reactant, with resorcinol and the formaldehyde mixed in molar ratio with 1: 2, is catalyst with the sodium carbonate liquor of 0.05mol/L; The mol ratio of resorcinol and sodium carbonate is 1500, and deionization water as solvent, liquid quality fraction are 30%; Stir; Sealing is placed in the baking oven, handles 1 day, 2 days and 3 days at 30 ℃, 50 ℃ and 90 ℃ respectively, generates the organic wet gel of RF at last.Sample is immersed in carried out solvent replacing in the acetone 72 hours, every therebetween at a distance from acetone of replacing in 24 hours.After treating that acetone volatilizees fully naturally, promptly get organic aerogel (RF).Under nitrogen protection, carry out carbonization according to certain carbonization curve afterwards, obtain the carbon aerogels material (CRF) of nano-porous structure.The carbon aerogels material aperture that obtains is 28nm, and specific area is 761m
2/ g, resistivity is 0.185 Ω cm, and is this carbon aerogels material carries out 10000 times under electron microscope after, as shown in Figure 2.
The porous carbon aeroge of preparing, graphite, superconduction carbon black, binding agent Kynoar are prepared lithium battery with multi-element doping carbon negative active core-shell material according to existing negative electrode active material material manufacturing technique.This lithium battery with multi-element doping carbon negative active core-shell material after carrying out 10000 times under the electron microscope, as shown in Figure 1.
A kind of preparation method who adopts the negative electrodes for lithium batteries of multi-element doping carbon negative active core-shell material: multi-element doping carbon negative active core-shell material is milled into powder and uses 200 mesh to filter; Mix (CRF: PVDF=90: 10) to powder and polyvinylidene fluoride (PVDF) by a certain percentage; Add the solvent 1-Methyl-2-Pyrrolidone and mix well, evenly spread upon on the Copper Foil to certain viscosity.Air dry is at room temperature put into vacuum desiccator then in 150 ℃ of following vacuumizes 12 hours (taking out moisture and other organic solvents fully).
Embodiment 2
With resorcinol and formaldehyde is reactant; With resorcinol and formaldehyde mixed in molar ratio with 1: 2, be catalyst with the sodium carbonate liquor of 0.05mol/L, the mol ratio of resorcinol and sodium carbonate is 1000; The deionization water as solvent; Liquid quality fraction is 50%, repeats the step among the embodiment 2, obtains the carbon aerogels (CRF) of nano-porous structure.The carbon aerogels material aperture that obtains is 8.2nm, and specific area is 571m
2/ g, resistivity is 0.157 Ω cm.
The porous carbon aeroge of preparing, graphite, superconduction carbon black, binding agent Kynoar are prepared lithium battery with multi-element doping carbon negative active core-shell material according to existing negative electrode active material material manufacturing technique.
A kind of preparation of adopting the negative electrodes for lithium batteries of multi-element doping carbon negative active core-shell material: multi-element doping carbon negative active core-shell material is milled into powder and uses 200 mesh to filter; Mix (CRF: PVDF=90: 10) to powder and polyvinylidene fluoride (PVDF) by a certain percentage; Add the solvent 1-Methyl-2-Pyrrolidone and mix well, evenly spread upon on the Copper Foil to certain viscosity.Air dry is at room temperature put into vacuum desiccator then in 150 ℃ of following vacuumizes 12 hours (taking out moisture and other organic solvents fully).
It is emphasized that; Embodiment of the present invention is illustrative; Rather than it is determinate; Therefore the present invention is not limited to the embodiment described in the embodiment, and every other execution modes that drawn by those skilled in the art's technical scheme according to the present invention belong to the scope that the present invention protects equally.
Claims (6)
1. a lithium battery is with multi-element doping carbon negative active core-shell material; It is characterized in that: it constitutes component and weight percentages of components is: nanoporous carbon aerogels 5%～30%; Graphite 50%～90%, superconduction carbon black 1%～5%, binding agent Kynoar 3%～10%.
2. lithium battery according to claim 1 is with multi-element doping carbon negative active core-shell material; It is characterized in that: described nanoporous carbon aerogels is to be precursor reagent with resorcinol and formaldehyde; Sodium carbonate liquor is a catalyst, through Temperature Treatment, solvent replacing, constant pressure and dry, high temperature carbonization, gas activation and make.
3. lithium battery according to claim 2 is characterized in that with multi-element doping carbon negative active core-shell material: the mol ratio of described resorcinol and sodium carbonate liquor is 100～2000, and the mass fraction of catalyst solution is 10%～60%.
4. lithium battery according to claim 2 is characterized in that with multi-element doping carbon negative active core-shell material: the aperture of described nanoporous carbon aerogels is 2nm～200nm, and specific area is 400m
2/ g～3500m
2/ g, resistivity is less than or equal to 0.3 Ω cm.
5. negative electrodes for lithium batteries that uses multi-element doping carbon negative active core-shell material; Comprise active material collector, active material, barrier film, electrolyte, organic solvent and reference electrode; It is characterized in that: described active material is each described multi-element doping carbon negative active core-shell material of claim 1 to 4; The active material collector is a copper sheet, and barrier film is the Celgard2500 micro-pore septum, and electrolyte is a lithium hexafluoro phosphate; Organic solvent is EC: EMC=1: 1 (volume ratio), reference electrode are metal lithium sheet.
6. the preparation method of a negative electrodes for lithium batteries as claimed in claim 5; It is characterized in that: comprising: multi-element doping carbon negative active core-shell material is milled into powder and uses 200 mesh to filter; With powder and binding agent polyvinylidene fluoride mixed by 90: 10; Join mixing and stirring in the solvent 1-Methyl-2-Pyrrolidone, evenly spread upon on the copper sheet, promptly obtain negative electrodes for lithium batteries after the drying.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721645A (en) * | 2013-12-23 | 2014-04-16 | 河北省科学院能源研究所 | Carbon aerogel for electric adsorption electrode and preparation method for carbon aerogel |
| CN106531981A (en) * | 2015-12-08 | 2017-03-22 | 宁波杉杉新材料科技有限公司 | Negative electrode material for high-rate and low-expansion lithium ion battery and preparation method of negative electrode material |
| CN107416788A (en) * | 2017-06-26 | 2017-12-01 | 中国电力科学研究院 | A kind of porous charcoal-aero gel of rich phosphorus and preparation method thereof |
| CN108807922A (en) * | 2018-06-21 | 2018-11-13 | 黄媛容 | A kind of negative electrode active material of lithium battery and preparation method thereof |
| CN109075309A (en) * | 2016-11-23 | 2018-12-21 | 皓智环球有限公司(中国香港) | Method of the preparation for the anode slurry of secondary cell |
| US10770720B2 (en) | 2014-04-29 | 2020-09-08 | Huawei Technologies Co., Ltd. | Composite negative electrode material and method for preparing composite negative electrode material, negative electrode plate of lithium ion secondary battery, and lithium ion secondary battery |
| CN116314624A (en) * | 2023-03-17 | 2023-06-23 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of miniature flexible lithium ion battery based on carbon aerogel |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721645A (en) * | 2013-12-23 | 2014-04-16 | 河北省科学院能源研究所 | Carbon aerogel for electric adsorption electrode and preparation method for carbon aerogel |
| CN103721645B (en) * | 2013-12-23 | 2016-04-20 | 河北省科学院能源研究所 | A kind of carbon aerogels for electric adsorption electrode and preparation method thereof |
| US10770720B2 (en) | 2014-04-29 | 2020-09-08 | Huawei Technologies Co., Ltd. | Composite negative electrode material and method for preparing composite negative electrode material, negative electrode plate of lithium ion secondary battery, and lithium ion secondary battery |
| CN106531981A (en) * | 2015-12-08 | 2017-03-22 | 宁波杉杉新材料科技有限公司 | Negative electrode material for high-rate and low-expansion lithium ion battery and preparation method of negative electrode material |
| CN109075309A (en) * | 2016-11-23 | 2018-12-21 | 皓智环球有限公司(中国香港) | Method of the preparation for the anode slurry of secondary cell |
| CN107416788A (en) * | 2017-06-26 | 2017-12-01 | 中国电力科学研究院 | A kind of porous charcoal-aero gel of rich phosphorus and preparation method thereof |
| CN107416788B (en) * | 2017-06-26 | 2021-10-01 | 中国电力科学研究院 | Phosphorus-rich porous carbon aerogel and preparation method thereof |
| CN108807922A (en) * | 2018-06-21 | 2018-11-13 | 黄媛容 | A kind of negative electrode active material of lithium battery and preparation method thereof |
| CN116314624A (en) * | 2023-03-17 | 2023-06-23 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of miniature flexible lithium ion battery based on carbon aerogel |
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Application publication date: 20120613 |