CN102195038B - Lithium ion battery as well as negative material and preparation method thereof - Google Patents
Lithium ion battery as well as negative material and preparation method thereof Download PDFInfo
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- CN102195038B CN102195038B CN201010118185.8A CN201010118185A CN102195038B CN 102195038 B CN102195038 B CN 102195038B CN 201010118185 A CN201010118185 A CN 201010118185A CN 102195038 B CN102195038 B CN 102195038B
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- 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
Abstract
The invention relates to a negative material of a lithium ion battery and a preparation method thereof. The preparation method comprises the following steps: (1) evenly mixing conductive carbon with polysiloxane, cracking and carbonizing in the presence of inert gas, grinding, and sieving so as to obtain a mixture I; and (2) mixing the mixture I with a lithium-containing compound so as to obtain a mixture II, heating and decomposing the lithium-containing compound in the mixture II, cooling, grinding, and sieving. According to the invention, the defects that the promotion spaces of the specific capacity and charge-discharge property of the battery using a graphite negative material are small and the traditional silicon-based negative material can generate a volume effect are overcome, and a novel negative material which is capable of effectively reducing a silicon volume effect and well improving the specific capacity of the lithium ion battery and has the advantages of good circulation property, rate discharge property and long service life and a lithium ion battery with the same is provided.
Description
Technical field
The present invention relates to electrochemical field, particularly relate to negative material of a kind of lithium ion battery and preparation method thereof, the invention still further relates to a kind of lithium ion battery containing this negative material.
Background technology
Lithium ion battery is the secondary chemical sources of electric energy of the repeated discharge and recharge most with prospects of people's accreditation up to now, it has than Cd-Ni secondary battery and the much higher energy density of lead-acid battery, and there is less energy density per unit volume, inside battery is not containing element environment to severe contamination, be one of chemical power source system of current people's most study, have good development prospect.Present lithium ion battery has been widely applied to small portable electrical equipment, as fields such as mobile phone, palmtop PC, CD players.Along with the develop rapidly of science and technology, the new power consumption equipment constantly occurred and people to improving constantly of requiring of power supply unit cause people require lithium ion battery towards less, gentlier, the future development of higher, the longer service life of energy density.In order to meet these requirements, people are finding the active material with more high-energy-density and better cycle life.
The lithium ion battery negative material of current trend mostly adopts graphited material with carbon element, the theoretical capacity of this material is 372mAh/g, the capacity (340-360mAh/g) that present reality uses is close to this numerical value, therefore, in order to improve the specific capacity of battery further, finding new negative material has become everybody common task.At present, the material with carbon element that people have a new structure except research is for except lithium ion battery, and non-carbon based material is also the focus that everybody studies.In Al, Sn, Si of existing research and alloy thereof and lithium titanate, silicon based anode material and tin base cathode get more and more people's extensive concerning because having very high reversible lithium storage amount (the reversible lithium storage amount as monocrystalline silicon is 4200mAh/g).But existing research shows, silica-base material and tin-based material all have larger irreversible capacity first, and in removal lithium embedded process, they all exist serious bulk effect, and these shortcomings cause their practicality to be restricted.In order to improve the shortcoming of these negative materials, people attempt adopting various ways to carry out modification to reducing its irreversible capacity, raising cycle life first to it.As CN1913200A proposes silica flour to be broken into small-particle, then use the organic method of cracking carbon coated outside, to improve the specific capacity of negative material and to reduce the bulk effect of silicon.Be greater than 85% by cycle efficieny first can be obtained after coated process, first capacity be greater than the silicon-carbon composite cathode material of 450mAh/g.The raising of its negative pole performance, has benefited from the bulk effect that surface coated carbon inhibits silicon to a great extent.In like manner, in order to suppress the bulk effect of tin base cathode material, propose a kind of method in patent CN 1585160, the method is by solution reaction synthesis of nano ~ micron-sized Sn
3o
2(OH)
2or Sn
6o
4(OH)
4particle or particle cluster.When this material is as active material, metallic tin can be produced in the electro-reduction process of first week, in the accessory substance that metallic tin produces after being dispersed in electrochemical reduction as the active material of electrode, metallic tin particle can surround and isolate by the existence of these accessory substances effectively, thus effectively prevents the bulk effect of tin.Except above-mentioned two patents, much similar method is also had to be used for the silica-based or tin base cathode material of process to improve its combination property.
Summary of the invention
Technical problem to be solved by this invention be to overcome in existing lithium ion battery due to use graphite as negative material make the specific capacity of battery and charge-discharge performance room for promotion little, and traditional silicon based anode material in use can produce the defects such as bulk effect, provide a kind of new lithium ion battery cathode material and its preparation method.Negative material of the present invention effectively can reduce the bulk effect of silicon, improves the specific capacity of lithium ion battery well, makes it have excellent cycle performance and multiplying power discharging property and longer useful life.Present invention also offers a kind of new lithium ion battery, it contains negative material of the present invention thus has high power capacity and long-life.
The invention provides a kind of preparation method of lithium ion battery negative material, it comprises the steps:
(1) conductive carbon mixed with polysiloxanes, cracking carbonization under inert gas shielding, grinding, after sieving, obtains mixture I;
(2) mixture I is mixed with lithium-containing compound, obtain mixtures II; Under inert gas shielding, the lithium-containing compound in mixtures II described in heat resolve, cooling, grinding, sieves, obtains lithium ion battery negative material.
In step (1), described polysiloxanes is used for providing silicon-oxygen-carbon glass ceramics to negative material, therefore polysiloxanes of the present invention can select the polysiloxanes of any routine, as one or more in silicone oil, silicon rubber and silicones etc., as long as its with Si-O repetitive for main chain, and simultaneously containing silicon, oxygen and carbon.Described conductive carbon can select the conventional all kinds of conductive carbon used in this area, as one or more in graphitized carbon, Delanium, native graphite, conductive carbon black and carbon nano-tube.As long as the particle size range of described conductive carbon can meet the custom requirements of anticathode material particle size in this area.Described conductive carbon and the mixed proportion of polysiloxanes are preferably weight ratio 2: 8 ~ 6: 4.Described cracking temperature can be selected according to the cracking temperature of the polysiloxanes of routine, is preferably 800 ~ 1400 DEG C.For reaching good lytic effect in the present invention, make the mixture I obtained more be conducive to the preparation of negative material, described pyrolysis time is preferably 1 ~ 10 hour, and better is 1 ~ 8 hour.Described inert gas is preferably argon gas.Described grinding and to sieve be requirement in order to make the particle diameter of mixture I meet lithium cell cathode material, the size of sieve aperture is preferably more than 400 orders.
In step (2), described lithium-containing compound can select the conventional various lithium-containing compounds used in field of lithium ion battery, comprises one or more in lithium salts, lithia and lithium hydroxide etc.Described lithium salts can be organic lithium salt and/or inorganic lithium salt, the lithium-containing compound in the present invention be preferably in organic lithium salt one or more.Described organic lithium salt is preferably one or more in lithium acetate, tert-butyl alcohol lithium, lithium methoxide, acetoacetate lithium and trimethylsilanylethyn lithium; Described inorganic lithium salt is preferably one or more in lithium carbonate, lithium fluoride, lithium chloride and lithium nitrate.In step (2), described lithium-containing compound can directly mix with mixture I, mixes after also this lithium-containing compound can being dissolved in solvent with mixture I.When using solvent, described solvent is the solvent for dissolving lithium-containing compound that this area routine uses, as oxolane.No matter adopt any one in above-mentioned two kinds of modes, as long as mixed with mixture I by this lithium-containing compound.Wherein, for coordinating with silicon-oxygen-carbon glass ceramics, make the chemical property that negative material reaches best, in lithium-containing compound, elemental lithium accounts for 0.05 ~ 10% of mixture I and elemental lithium total weight.
In step (2), described heat resolve temperature is the temperature of the decomposition lithium-containing compound of this area routine, is preferably 300 ~ 900 DEG C.For reaching good discomposing effect in the present invention, the described heat resolve time is preferably 0.5 ~ 10 hour, and better is 1 ~ 8 hour.Described cooling is preferably for being cooled to room temperature.Described inert gas is preferably nitrogen.Described grinding and to sieve be requirement in order to make the particle diameter of the negative material obtained meet lithium battery, the size of sieve aperture is preferably more than 400 orders.
Present invention also offers a kind of lithium ion battery negative material obtained by the preparation method of above-mentioned lithium ion battery negative material.Containing silicon-oxygen-carbon glass ceramics in this negative material, it has higher reversible lithium-inserting amount.Wherein, silicon is present in negative material with atom or molecular dimension, is significantly less than silicon particle size of the prior art, can be scattered in negative material well, effectively reduce bulk effect.The existence of conductive carbon can improve the conductivity of negative material.In negative material, the existence of lithium can form one deck solid film on the surface of negative material, reduces electrolytical decomposition.The cooperative effect of above-mentioned triple factor effectively can reduce the change in volume that repetition discharge and recharge causes, and makes this negative material have higher Reversible lithium insertion capacity and higher cycle life.
Present invention also offers a kind of new lithium ion battery, it comprises lithium ion battery negative material of the present invention.Lithium ion battery of the present invention can adopt the method for this area routine to be prepared.
Room temperature described in the present invention is 20 ~ 40 DEG C.
In the present invention, above-mentioned optimum condition can combination in any on the basis meeting this area general knowledge, obtains the preferred embodiments of the invention.
The present invention's raw material used, reagent are all commercially.
Positive progressive effect of the present invention is: the invention provides a kind of new lithium ion battery, lithium ion battery cathode material and its preparation method.In lithium ion battery negative material of the present invention, silicon is scattered in negative material with atom or molecular forms, makes negative material in use can not produce bulk effect; Contain silicon-oxygen-carbon glass ceramics in this negative material simultaneously, reversible lithium-inserting amount can be significantly improved, thus the specific capacity of lithium ion battery can be improved well, make it have excellent cycle performance and multiplying power discharging property.Lithium ion battery of the present invention and lithium ion battery negative material all have higher capacity and useful life.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern of embodiment 1 gained negative material;
Fig. 2 is the cycle life curve of embodiment 2 gained negative material, and wherein curve 1 and 2 is cycle charge discharge curve, and 1 is discharge curve, and 2 is charging curve.Curve 3 is efficiency for charge-discharge-cycle-index line.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but the present invention is not limited.
Polyphenyl methyl siloxane in following embodiment and dimethyl silicone polymer are purchased from DOW CORNING chemical company.
Embodiment 1
One, the preparation of lithium ion battery negative material:
(1) 100mg conductive carbon black and 400mg polyphenyl methyl siloxane (weight ratio 2: 8) are mixed, be placed in argon gas atmosphere in 1100 DEG C of cracking 1 hour, pulverize, cross 400 mesh sieves, obtain mixture I;
(2) get mixture I 150mg, add the tetrahydrofuran solution (elemental lithium accounts for 7.4% of mixture I and elemental lithium total weight) of 3.4mL 0.5mol/L trimethylsilanylethyn lithium, fully mixing infiltrates to obtain mixtures II; Under nitrogen protection in 400 DEG C of roastings 2 hours, be cooled to room temperature, grinding, cross 400 mesh sieves and get final product.
Two, the test of lithium ion battery negative material:
(1) structural behaviour:
Fig. 1 is the XRD collection of illustrative plates of this negative material.As can be seen from collection of illustrative plates, in the negative material of gained, there is an obvious graphite diffraction maximum.In addition, there is not obvious diffraction maximum.Illustrate thus, the negative material of gained belongs to the complex that amorphous silicon-oxygen-carbon glass ceramic material and graphite coexist, and the decomposition of lithium-containing compound leaves obvious crystalline state species on the surface of material.
(2) chemical property:
Adopt conventional battery performance method of testing, the product obtained is made Electrode, in button cell, carries out performance test.During test, temperature is room temperature, and adopt constant current charge-discharge, current density is 50mA/g, and control reference voltage is 0.005-2.0V.
The preparation method of Electrode is as follows: by gained negative material by 9: 1 weight ratio mix with Kynoar solution after, with scraper by slurry uniform application on the Copper Foil cleaned through acetone, vacuumize 12 hours at 120 DEG C, then through compressing tablet, cutting, obtained Electrode.
The assembling mode of button cell is as follows: using lithium sheet as to electrode, and Celgard 2300 is as barrier film, and electrolyte adopts containing 1M LiPF
6eC-DMC (1: 1) solution.
Electrochemical results shows, and the embedding first lithium capacity of gained negative material is 713mAh/g, and reversible de-lithium capacity is 534mAh/g, and initial coulomb efficiency is 75%.After 20 circulations, reversible de-lithium capacity is 443mAh/g, and capacity is 83% of capacity first.Reversible capacity is higher than graphitic carbon material (372mAh/g), and cycle life is much higher than the carbon-silicon-pre-ceramic material of oxygen glass (see comparative example) of Direct Resolution polysiloxanes gained.
Embodiment 2
One, the preparation of lithium ion battery negative material:
(1) 150mg graphous graphite powder and 350mg polyphenyl methyl siloxane (weight ratio 3: 7) are mixed, be then placed in argon gas atmosphere in 1100 DEG C of cracking 2 hours, pulverize, cross 400 mesh sieves, obtain mixture I;
(2) get mixture I 150mg, add the tetrahydrofuran solution (elemental lithium accounts for 7.4% of mixture I and elemental lithium total weight) of 3.4mL 0.5mol/L trimethylsilanylethyn lithium, fully mixing infiltrates to obtain mixtures II; Under nitrogen protection in 400 DEG C of roastings 2 hours, be cooled to room temperature, grinding, cross 400 mesh sieves and get final product.
Two, the test of lithium ion battery negative material:
(1) structural behaviour:
The XRD collection of illustrative plates of this negative material, with embodiment 1, shows that gained negative material has the crystal phase structure identical with embodiment 1.
(2) chemical property:
The battery performance method of testing of embodiment 1 is adopted to test.The embedding first lithium capacity of test result display gained negative material is 670mAh/g, and reversible de-lithium capacity is 545mAh/g, and initial coulomb efficiency is 81.3%.After 20 circulations, reversible de-lithium capacity is 512mAh/g, and capacity is 93.9% of capacity first, and efficiency for charge-discharge is close to 100%.The reversible capacity of material is much higher than graphitic carbon material (372mAh/g), and the cycle life of material have also been obtained further raising.Fig. 2 is the cycle charge discharge curve of this material.
Embodiment 3
One, the preparation of lithium ion battery negative material:
(1) 300mg graphous graphite powder and 200mg dimethyl silicone polymer (weight ratio 6: 4) are mixed, be then placed in argon gas atmosphere in 800 DEG C of cracking 10 hours, pulverize, cross 400 mesh sieves, obtain mixture I;
(2) get mixture I 150mg, add 100mg lithium hydroxide (elemental lithium accounts for 10% of mixture I and elemental lithium total weight, fully mixing infiltrates to obtain mixtures II; Under nitrogen protection in 900 DEG C of roastings 10 hours, be cooled to room temperature, grinding, cross 400 mesh sieves and get final product.
Two, the test of lithium ion battery negative material:
(1) structural behaviour:
The XRD collection of illustrative plates of this negative material, with embodiment 1, shows that gained negative material has the crystal phase structure identical with embodiment 1.
(2) chemical property:
The battery performance method of testing of embodiment 1 is adopted to test.The embedding first lithium capacity of test result display gained negative material is 698mAh/g, and reversible de-lithium capacity is 583mAh/g, and initial coulomb efficiency is 83.5%.After 20 circulations, reversible de-lithium capacity is 554mAh/g, and capacity is 95.1% of capacity first, and efficiency for charge-discharge is close to 100%.The reversible capacity of material is much higher than graphitic carbon material (372mAh/g), and the cycle life of material have also been obtained further raising.
Embodiment 4
One, the preparation of lithium ion battery negative material:
(1) 300mg graphous graphite powder and 300mg dimethyl silicone polymer (weight ratio 5: 5) are mixed, be then placed in argon gas atmosphere in 1400 DEG C of cracking 1 hour, pulverize, cross 400 mesh sieves, obtain mixture I;
(2) get mixture I 150mg, add 1.1mg bis-acetate hydrate lithium (elemental lithium accounts for 0.05% of mixture I and elemental lithium total weight, fully mixing infiltrates to obtain mixtures II; Under nitrogen protection in 300 DEG C of roastings 1 hour, be cooled to room temperature, grinding, cross 400 mesh sieves and get final product.
Two, the test of lithium ion battery negative material:
(1) structural behaviour:
The XRD collection of illustrative plates of this negative material, with embodiment 1, shows that gained negative material has the crystal phase structure identical with embodiment 1.
(2) chemical property:
The battery performance method of testing of embodiment 1 is adopted to test.The embedding first lithium capacity of test result display gained negative material is 628mAh/g, and reversible de-lithium capacity is 490mAh/g, and initial coulomb efficiency is 78%.After 20 circulations, reversible de-lithium capacity is 425mAh/g, and capacity is 86.7% of capacity first, and efficiency for charge-discharge is close to 100%.The reversible capacity of material is much higher than graphitic carbon material (372mAh/g), and the cycle life of material have also been obtained further raising.
Comparative example
One, the preparation of lithium ion battery negative material: polyphenyl methyl siloxane is directly placed in argon gas atmosphere in 1100 DEG C of cracking 2 hours.Product after cracking, through pulverizing, crossing 400 mesh sieves, obtains negative material.
XRD analysis shows that this product has amorphous structure.
Two, the electrochemical property test of lithium ion battery negative material:
Battery performance method of testing is with embodiment 1.
Difference is that Electrode obtains as follows: by gained negative material by 7: 2: 1 weight ratio mix with conductive carbon black and Kynoar binding agent, with scraper by slurry uniform application on the Copper Foil cleaned through acetone, vacuumize 12 hours at 120 DEG C, then through compressing tablet, cutting, obtained Electrode.
After tested, the embedding first lithium capacity of this negative material is 1382mAh/g, and reversible de-lithium capacity is 769mAh/g, and initial coulomb efficiency is 55.6%.After 20 circulations, reversible de-lithium capacity is 453mAh/g, and capacity only has 58.9% of capacity first.
Claims (8)
1. a preparation method for lithium ion battery negative material, is characterized in that: it comprises the steps:
(1) conductive carbon mixed with polysiloxanes, cracking carbonization under inert gas shielding, grinding, after sieving, obtains mixture I;
(2) mixture I is mixed with lithium-containing compound, obtain mixtures II; Under inert gas shielding, the lithium-containing compound in mixtures II described in heat resolve, cooling, grinding, sieves;
In step (2), described lithium-containing compound is one or more in lithium salts, lithia and lithium hydroxide; Described lithium salts is organic lithium salt and/or inorganic lithium salt; Described organic lithium salt is one or more in lithium acetate, tert-butyl alcohol lithium, lithium methoxide, acetoacetate lithium and trimethylsilanylethyn lithium; Described inorganic lithium salt is one or more in lithium carbonate, lithium fluoride, lithium chloride and lithium nitrate.
2. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: in step (1), and described conductive carbon is one or more in graphitized carbon, Delanium, native graphite, conductive carbon black and carbon nano-tube.
3. the preparation method of lithium ion battery negative material as claimed in claim 1 or 2, it is characterized in that: in step (1), described conductive carbon and the mixing ratio of polysiloxanes are weight ratio 2:8 ~ 6:4.
4. the preparation method of lithium ion battery negative material as claimed in claim 1 or 2, it is characterized in that: in step (1), described cracking temperature is 800 ~ 1400 DEG C; Described pyrolysis time is 1 ~ 10 hour.
5. the preparation method of lithium ion battery negative material as claimed in claim 1 or 2, it is characterized in that: in step (2), in described lithium-containing compound, the content of elemental lithium is 0.05 ~ 10% of mixture I and elemental lithium total weight.
6. the preparation method of lithium ion battery negative material as claimed in claim 1 or 2, it is characterized in that: in step (2), described heat resolve temperature is 300 ~ 900 DEG C; The heat resolve time is 0.5 ~ 10 hour.
7. the lithium ion battery negative material prepared by the method according to any one of claim 1 ~ 6.
8. a lithium ion battery, is characterized in that: it contains lithium ion battery negative material according to claim 7.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103165870B (en) * | 2011-12-13 | 2016-03-16 | 上海杉杉科技有限公司 | A kind of silicon based composite material, lithium ion battery and its preparation method and application |
| CN104332608B (en) * | 2014-08-19 | 2017-06-06 | 新乡市远东电子科技股份有限公司 | A kind of lithium ion battery silicon composite cathode material and preparation method thereof |
| CN106299314B (en) * | 2016-10-14 | 2019-10-11 | 焦作聚能能源科技有限公司 | A kind of lithium ion battery negative material and preparation method thereof, lithium ion battery |
| CN107994225B (en) * | 2017-12-11 | 2020-09-25 | 徐军红 | Porous silicon-carbon composite negative electrode material, preparation method thereof and lithium ion battery |
| CN112652755B (en) * | 2019-10-09 | 2022-07-12 | 中国石油化工股份有限公司 | Silicon-carbon negative electrode material, preparation method and application thereof, and lithium ion battery |
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| CN1913200A (en) * | 2006-08-22 | 2007-02-14 | 深圳市贝特瑞电子材料有限公司 | Silicon carbone compound negative polar material of lithium ion battery and its preparation method |
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| EP2065955A1 (en) * | 2007-11-27 | 2009-06-03 | Samsung SDI Co., Ltd. | Negative active materiel, method of preparing same, and rechargeable lithium battery including the same |
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| CN1913200A (en) * | 2006-08-22 | 2007-02-14 | 深圳市贝特瑞电子材料有限公司 | Silicon carbone compound negative polar material of lithium ion battery and its preparation method |
| EP2065955A1 (en) * | 2007-11-27 | 2009-06-03 | Samsung SDI Co., Ltd. | Negative active materiel, method of preparing same, and rechargeable lithium battery including the same |
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Denomination of invention: A lithium ion battery and its cathode material and preparation method Effective date of registration: 20220701 Granted publication date: 20150415 Pledgee: Baotou Branch of Inner Mongolia Hohhot Jingu Rural Commercial Bank Co.,Ltd. Pledgor: INNER MONGOLIA SHANSHAN TECHNOLOGY Co.,Ltd. Registration number: Y2022150000063 |