CN103236520B - Preparation method of lithium ion battery silicon oxide/carbon composite negative pole material - Google Patents
Preparation method of lithium ion battery silicon oxide/carbon composite negative pole material Download PDFInfo
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Abstract
The invention provides a preparation method of a silicon oxide/carbon negative pole composite material for lithium ion batteries, belonging to the fields of new materials and electrochemistry. The silicon oxide/carbon composite material provided by the invention uses a porous carbon material with a xerogel or aerogel structure as a matrix, and silicon oxide particles are uniformly dispersed in the carbon matrix. Resorcinol and formaldehyde are used as matrix raw materials, organosilicon is used as a silicon source, and a one-step sol-gel method in combination with a heat treatment technique is utilized to prepare the nano silicon oxide/carbon composite negative pole material. The invention has the advantages of simple technical process, controllable reaction and mild conditions, and is convenient for large-scale preparation. The silicon oxide/carbon composite negative pole material prepared by the method has higher specific capacity and favorable loop stability, is an ideal lithium ion battery negative pole material, and can be widely used in the fields of various portable electronic devices, electric automobiles, aerospace and the like.
Description
Technical field
The invention belongs to new material and electrochemical field, be specifically related to a kind of novel can the preparation method of charging-discharging lithium ion battery silicon oxide/carbon composite negative material.
Technical background
Along with the raising of the electrified demand of the industrial expansions such as electronics, communication, space flight, automobile and daily necessities, people are miniaturized to lithium ion battery, high-octane requirement is day by day urgent.Current business-like lithium ion battery negative material mainly graphite cathode material, through a large amount of improvements, the actual lithium storage content of current graphite more and more its theoretical capacity of convergence (graphite theoretical capacity is 372 mAh/g, 855 mAh/cm
3), be difficult to meet portable electric appts and electric automobile to the requirement of lithium ion battery high-energy-density, the lithium ion battery negative electrode material of Novel high-specific capacity flexible must be researched and developed.
The theoretical lithium storage content of silicon, up to 4200 mAh/g, is a kind of very rising height ratio capacity negative material, now one of focus becoming this area research.But silicon-based anode with huge change in volume, easily causes electrode to ftracture and efflorescence, causes electrode cycle degradation in charge and discharge process.And the electron conduction ability of silicon is poor, affect the performance of electrode active component capacity and the multiplying power property of electrode.For the above shortcoming of silicon, researchers conduct extensive research improving silicon-based anode.Preparing silica based composites is exactly a kind of wherein method effectively can improving silicium cathode cycle performance.Oxidation silicon based anode material can form active phase nano Si particle and nonactive phase Li in embedding lithium process first
2o and Li
4siO
4, active phase Si particle will be dispersed in nonactive mutually in.Nonactive phase can prevent the reunion of nano Si particle on the one hand, and all right effectively bulk effect of buffer Si in charge and discharge process, obtains good cycle performance simultaneously.Therefore silica based combined electrode material causes researchers' more and more concern.
At present in this field, the general commercialization SiO powder standby with high temperature evaporation legal system of researchers, for silicon source, carries out modification to it.As prepared SiO/C composite negative pole material by methods such as high-energy ball milling, chemical vapour deposition (CVD) or hydro-thermals.Chil-Hoon Doh seminar of electrician research institute of Korea S carries out high-energy ball milling process to commercialization silica powder and graphite mixing and prepares SiO/C composite material, with electrode prepared by this material, its first discharge specific capacity and charge specific capacity are respectively 1556 and 693 mAh/g(C.H. Doh, et al. Journal of Power Sources 179 (2008): 367-370), after 30 circulations, reversible capacity still has 688 mAh/g.Wu Naili seminar of chemical engineering institute of Univ Nat Taiwan carries out high-energy ball milling to commercialization SiO powder and chemical vapor deposition process prepares SiO/C composite material, material is made electrode, it discharges first and charging capacity is respectively 1056 and 675 mAh/g, 620 mAh/g(W. Liu are still kept, et al. Journal of Applied Electrochemistry 39 (2009): 1643-1649) after 50 circulations.This seminar take tetraethoxysilane as silicon source, silica/carbon composite is prepared in conjunction with heat treatment by st ber method, electrode cycle reversible capacity is about 800 mAh/g(J. Wang, et al. Journal of Power Sources 196 (2011): 4811-4815).
Adopt commercialization SiO powder to be silicon source preparation oxidation silicon based anode material, owing to adopting high temperature evaporation legal system complicated for commercialization SiO powder craft, cost is higher, is unfavorable for suitability for industrialized production, and the performance of material not easy-regulating.And the high-energy ball milling adopted, chemical vapour deposition (CVD) and hydro thermal method technique are comparatively complicated; productive rate is low; cost is high; be unfavorable for the scale preparation of silica based composites; therefore be necessary to study a kind of raw material relatively cheap; technique is simple and easy to manipulation, the preparation method of the oxidation silicon based anode material that output is larger.
Carbon aerogels is prepared with sol-gel process, freeze-drying and high temperature cabonization technique by Ma Zifeng seminar of chemical industry system of Shanghai Communications University, then carbon aerogels and silica powder are carried out ball-milling treatment prepares silica-carbon aerogels composite negative pole material.Material is made electrode, reversible capacity is 685 mAh/g first, after 30 circulations, capacity is still 539 mAh/g, and electrode has good high rate performance (Y. Chao, et al. Electrochimica Acta 53 (2008): 3468-3473).The porosity characteristic of carbon aerogels can the effective change in volume of buffer Si O material in charge and discharge process, and can increase the electronic conductance ability of material, improves cycle performance and the high rate performance of electrode.Carbon aerogels can also provide good electron propagation ducts simultaneously.But freeze drying and high temperature cabonization technique comparatively complicated, cost is higher, limits the possibility of its industrialization.If the preparation of nano silicon oxide and the preparation of carbon aerogels are combined as a whole, and adopt constant pressure and dry technique to prepare material, on the one hand by Simplified flowsheet, reduce costs, nano silicon oxide being uniformly distributed in carbon aerogels can be realized on the other hand, be conducive to the raising of electrode cycle stability.
Summary of the invention
First object of the present invention is to provide a kind of lithium ion battery silicon oxide/carbon composite negative material.This kind of silicon oxide/carbon composite negative material has higher specific discharge capacity, can meet the demand of growing Portable power source to height ratio capacity lithium ion battery.This negative material is made up of electro-chemical activity core material and matrix, electro-chemical activity core material is dispersed in basis material, described electro-chemical activity core material is silica, and described basis material is the porous carbon materials with xerogel or aerogel structure.
Another object of the present invention is the preparation method providing a kind of lithium ion battery silicon oxide/carbon composite negative material, with the relatively cheap organosilicon of price for silicon source, prepares silica/carbon composite by a step sol-gel process in conjunction with heat treatment.
The preparation method of the lithium ion battery negative material that the present invention adopts, it is characterized in that: adopt a step sol-gel process preparation to have the porous silica/carbon matrix precursor material of xerogel or aerogel structure, prepare nanoscale silicon/carbon compound cathode materials in conjunction with heat treatment.This preparation method is simple, cost is low, be convenient to scale preparation, and the material of synthesis possesses higher electrochemistry circulation volume and stable cycle performance.
Its concrete steps are:
(1) solution is configured: select resorcinol, take required quality, be dissolved in a certain amount of deionized water, then add a certain amount of formalin, stir formation solution, and this solution is designated as solution A;
Select organosilicon to be silicon source, measure volume required, be dissolved in a certain amount of absolute ethyl alcohol, then add a certain amount of deionized water, stir formation clear solution.Wherein the volume ratio of absolute ethyl alcohol and tetraethoxysilane controls: absolute ethyl alcohol/tetraethoxysilane=1 ~ 2, and the volume ratio of tetraethoxysilane and deionized water controls: tetraethoxysilane/deionized water=2 ~ 4, and this solution is designated as solution B;
(2) under agitation, in solution A, add a certain amount of gel catalyst, this solution is designated as solution C;
(3) under agitation, in solution B, add a certain amount of acidic catalyst, regulate the pH value of solution 1 ~ 5, this solution is designated as solution D;
(4) solution D is added drop-wise in solution C, Keep agitation 0.5 ~ 2 h, moves in water-bath and carry out isothermal holding, after leaving standstill, form gel;
(5) adding absolute ethyl alcohol in the gel formed to step (4) carries out aging, replaces absolute ethyl alcohols, repeat 1 ~ 3 time every 24 h;
(6) gel in step (5) is carried out constant pressure and dry, obtain precursor product;
(7), under nitrogen or argon atmosphere, the precursor product of step (6) gained is warming up to 800 ~ 1200
oc is incubated 1 ~ 4 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.
Step (1) select weight percentage be 37 ~ 40% formalin.In described solution A, the ratio of the amount of substance of formaldehyde and resorcinol controls: formaldehyde/resorcinol=1 ~ 4.
The addition of the deionized water described in step (1), makes the concentration of resorcinol in solution A control at 0.5 ~ 3 mol/100 ml.
The organosilicon that step (1) is selected is methyl silicate or tetraethoxysilane.
Gel catalyst described in step (2) is Na
2cO
3, K
2cO
3, NaHCO
3or KHCO
3.
Gel catalyst addition described in step (2), makes the ratio of the amount of substance of resorcinol and gel catalyst in solution C control: resorcinol/gel catalyst=50 ~ 100.
Acidic catalyst described in step (3) is hydrochloric acid, nitric acid or acetic acid.
Solution D addition described in step (4), makes tetraethoxysilane in mixed solution control with the ratio of the amount of substance of resorcinol: tetraethoxysilane/resorcinol=3 ~ 7.
Water bath heat preservation process described in step (4), bath temperature is 40 ~ 80
oc.
Constant pressure and dry described in step (6) is by oven drying, and baking oven set temperature is 80 ~ 120
oc.
Porous silica/carbon matrix precursor material that the present invention adopts a step sol-gel process first to prepare to possess xerogel or aerogel structure, synthesizes nanoscale silicon/carbon composite in conjunction with Technology for Heating Processing.The invention has the advantages that preparation process is simple, reaction condition is gentle, and cost is low, is convenient to large-scale production; The silica prepared in this approach/carbon composite particle is tiny, and particle diameter, distributed components have good electrical chemical property, is a kind of desirable lithium ion battery negative material.
Accompanying drawing explanation
Fig. 1 is the first charge-discharge curve chart of the silicon oxide/carbon composite negative material of embodiment 1.
Fig. 2 is the circulation volume figure of the silicon oxide/carbon composite negative material of embodiment 1.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but be not limited to protection scope of the present invention:
Embodiment 1:
Take 6.6 g resorcinols, be dissolved in 10 ml deionized waters, then add 4.4 ml formalins (weight percentage is 37 ~ 40%), stir formation solution, and this solution is designated as solution A; Measure 30 ml tetraethoxysilanes to be dissolved in 20 ml absolute ethyl alcohols, then add 10 ml deionized waters, stir formation clear solution, is designated as solution B; Under agitation, 0.128 g Na in solution A
2cO
3, this solution is designated as solution C; Under agitation, in solution B, drip hydrochloric acid, regulate the pH value of solution 3, this solution is designated as solution D; Solution D be added drop-wise in solution C, Keep agitation 1 h, move in water-bath and carry out isothermal holding, bath temperature is 60
oc, forms gel after leaving standstill; In gel, add absolute ethyl alcohol carries out aging, replaces absolute ethyl alcohol, repeat 2 times every 24 h; Gel is put into 80
ocarry out drying in C baking oven, obtain precursor product; Under nitrogen protection atmosphere, the precursor product of gained is warming up to 1000
oc is incubated 1 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.The PVdF of the obtained silica/carbon composite of 70 wt.%, the acetylene black of 15 wt.% and 15 wt.% is mixed, make slurry, be evenly coated on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electrode with lithium metal, 1 mol/L LiPF
6/ DMC+DEC+EC(volume ratio is 1:1:1) be electrolyte, Celgard 2400 is barrier film, composition test cell.Constant current charge-discharge test is carried out to battery, charging/discharging voltage scope is 0.01 ~ 2.5 V, result shows, it has good chemical property, under the current density of 0.1 A/g, first discharge specific capacity and charge specific capacity are respectively 1403.8 and 777.7 mAh/g, and the specific capacity of material after 100 times that circulates still has maintained 617.5 mAh/g, and material has good cyclical stability.
Embodiment 2:
Take 6.6 g resorcinols, be dissolved in 10 ml deionized waters, then add 4.4 ml formalins (weight percentage is 37 ~ 40%), stir formation solution, and this solution is designated as solution A; Measure 20 ml tetraethoxysilanes to be dissolved in 20 ml absolute ethyl alcohols, then add 10 ml deionized waters, stir formation clear solution, is designated as solution B; Under agitation, 0.256 g Na in solution A
2cO
3, this solution is designated as solution C; Under agitation, in solution B, drip hydrochloric acid, regulate the pH value of solution 4, this solution is designated as solution D; Solution D be added drop-wise in solution C, Keep agitation 1 h, move in water-bath and carry out isothermal holding, bath temperature is 60
oc, forms gel after leaving standstill; In gel, add absolute ethyl alcohol carries out aging, replaces absolute ethyl alcohol, repeat 2 times every 24 h; Gel is put into 80
ocarry out drying in C baking oven, obtain precursor product; Under nitrogen protection atmosphere, the precursor product of gained is warming up to 900
oc is incubated 1 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.The PVdF of the obtained silica/carbon composite of 70 wt.%, the acetylene black of 15 wt.% and 15 wt.% is mixed, make slurry, be evenly coated on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electrode with lithium metal, 1 mol/L LiPF
6/ DMC+DEC+EC(volume ratio is 1:1:1) be electrolyte, Celgard 2400 is barrier film, composition test cell.Constant current charge-discharge test is carried out to battery, charging/discharging voltage scope is 0.01 ~ 2.5 V, result shows, it has good chemical property, under the current density of 0.1 A/g, first discharge specific capacity and charge specific capacity are respectively 1269.8 and 703.5 mAh/g, and the specific capacity of material after 80 times that circulates is 650.7 mAh/g, and material has good cyclical stability.
Embodiment 3:
Take 6.6 g resorcinols, be dissolved in 10 ml deionized waters, then add 2.2 ml formalins (weight percentage is 37 ~ 40%), stir formation solution, and this solution is designated as solution A; Measure 15 ml tetraethoxysilanes to be dissolved in 20 ml absolute ethyl alcohols, then add 10 ml deionized waters, stir formation clear solution, is designated as solution B; Under agitation, 0.128 g Na in solution A
2cO
3, this solution is designated as solution C; Under agitation, in solution B, drip hydrochloric acid, regulate the pH value of solution 3, this solution is designated as solution D; Solution D be added drop-wise in solution C, Keep agitation 1 h, move in water-bath and carry out isothermal holding, bath temperature is 60
oc, forms gel after leaving standstill; In gel, add absolute ethyl alcohol carries out aging, replaces absolute ethyl alcohol, repeat 2 times every 24 h; Gel is put into 80
ocarry out drying in C baking oven, obtain precursor product; Under nitrogen protection atmosphere, the precursor product of gained is warming up to 1000
oc is incubated 1 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.The PVdF of the obtained silica/carbon composite of 70 wt.%, the acetylene black of 15 wt.% and 15 wt.% is mixed, make slurry, be evenly coated on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electrode with lithium metal, 1 mol/L LiPF
6/ DMC+DEC+EC(volume ratio is 1:1:1) be electrolyte, Celgard 2400 is barrier film, composition test cell.Carry out constant current charge-discharge test to battery, charging/discharging voltage scope is 0.01 ~ 2.5 V, and result shows, it has good chemical property, and under the current density of 0.1 A/g, first discharge specific capacity and charge specific capacity are respectively 1212.2 and 665.5 mAh/g.
Embodiment 4:
Take 6.6 g resorcinols, be dissolved in 10 ml deionized waters, then add 4.4 ml formalins (weight percentage is 37 ~ 40%), stir formation solution, and this solution is designated as solution A; Measure 20 ml tetraethoxysilanes to be dissolved in 40 ml absolute ethyl alcohols, then add 10 ml deionized waters, stir formation clear solution, is designated as solution B; Under agitation, 0.166 g K in solution A
2cO
3, this solution is designated as solution C; Under agitation, in solution B, drip hydrochloric acid, regulate the pH value of solution 4, this solution is designated as solution D; Solution D be added drop-wise in solution C, Keep agitation 1 h, move in water-bath and carry out isothermal holding, bath temperature is 40
oc, forms gel after leaving standstill; In gel, add absolute ethyl alcohol carries out aging, replaces absolute ethyl alcohol, repeat 1 time every 24 h; Gel is put into 80
ocarry out drying in C baking oven, obtain precursor product; Under nitrogen protection atmosphere, the precursor product of gained is warming up to 1100
oc is incubated 1 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.The PVdF of the obtained silica/carbon composite of 70 wt.%, the acetylene black of 15 wt.% and 15 wt.% is mixed, make slurry, be evenly coated on Copper Foil, after vacuum drying, be stamped into circular electrode pole piece, be to electrode with lithium metal, 1 mol/L LiPF
6/ DMC+DEC+EC(volume ratio is 1:1:1) be electrolyte, Celgard 2400 is barrier film, composition test cell.Carry out constant current charge-discharge test to battery, charging/discharging voltage scope is 0.01 ~ 2.5 V, and result shows, it has good chemical property, and under the current density of 0.1 A/g, first discharge specific capacity and charge specific capacity are respectively 1092.2 and 611.7 mAh/g.
Claims (10)
1. the preparation method of a lithium ion battery silicon oxide/carbon composite negative pole material, it is characterized in that first preparing by a step sol-gel process porous silica/carbon matrix precursor material possessing xerogel or aerogel structure, again in conjunction with Technology for Heating Processing, prepare nanoscale silicon/carbon compound cathode materials, concrete technology step is:
(1) solution is configured: select resorcinol, take required quality, be dissolved in a certain amount of deionized water, then add a certain amount of formalin, stir formation solution, and this solution is designated as solution A;
Select organosilicon to be silicon source, measure volume required, be dissolved in a certain amount of absolute ethyl alcohol, then add a certain amount of deionized water, stir formation clear solution; Wherein absolute ethyl alcohol and organosilyl volume ratio are: absolute ethyl alcohol/organosilicon=1 ~ 2, and the volume ratio of organosilicon and deionized water is: organosilicon/deionized water=2 ~ 4, and this solution is designated as solution B;
(2) under agitation, in solution A, add a certain amount of gel catalyst, this solution is designated as solution C;
(3) under agitation, in solution B, add a certain amount of acidic catalyst, regulate the pH value of solution 1 ~ 5, this solution is designated as solution D;
(4) solution D is added drop-wise in solution C, Keep agitation 0.5 ~ 2 h, moves in water-bath and carry out isothermal holding, after leaving standstill, form gel;
(5) adding absolute ethyl alcohol in the gel formed to step (4) carries out aging, replaces absolute ethyl alcohols, repeat 1 ~ 3 time every 24 h;
(6) gel after aging in step (5) is carried out constant pressure and dry, obtain precursor product;
(7), under nitrogen or argon atmosphere, the precursor product of step (6) gained is warming up to 800 ~ 1200
oc is incubated 1 ~ 4 h, cools to room temperature with the furnace and obtains nano silicon oxide/carbon compound cathode materials powder.
2. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: step (1) select weight percentage be 37 ~ 40% formalin; In solution A described in step (1), the ratio of the amount of substance of formaldehyde and resorcinol controls: formaldehyde/resorcinol=1 ~ 4.
3. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the addition of the deionized water described in step (1), and the concentration of resorcinol in solution A is controlled at 0.5 ~ 3 mol/100 ml.
4. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the organosilicon that step (1) is selected is methyl silicate or tetraethoxysilane.
5. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the gel catalyst described in step (2) is Na
2cO
3, K
2cO
3, NaHCO
3or KHCO
3.
6. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, it is characterized in that: the gel catalyst addition described in step (2), the ratio of the amount of substance of resorcinol and gel catalyst in solution C is controlled: resorcinol/gel catalyst=50 ~ 100.
7. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the acidic catalyst described in step (3) is hydrochloric acid, nitric acid or acetic acid.
8. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, it is characterized in that: the solution D addition described in step (4), organosilicon in mixed solution is controlled with the ratio of the amount of substance of resorcinol: organosilicon/resorcinol=3 ~ 7.
9. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the water bath heat preservation process described in step (4), and bath temperature is 40 ~ 80
oc.
10. the preparation method of lithium ion battery silicon oxide/carbon composite negative pole material according to claim 1, is characterized in that: the constant pressure and dry described in step (6) is oven drying, and baking oven set temperature is 80 ~ 120
oc.
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| EP3545569A4 (en) * | 2016-11-23 | 2020-07-15 | GRST International Limited | Method of preparing anode slurry for secondary battery |
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| CN104475074B (en) * | 2014-10-29 | 2016-10-12 | 东南大学 | The preparation of boron doping hollow carbon balls and the application in cathode in direct methanol fuel cells |
| CN105489891A (en) * | 2015-12-21 | 2016-04-13 | 宁波高新区锦众信息科技有限公司 | Preparation method for high-capacity silicon-based negative electrode material for lithium ion battery |
| SG11201912783XA (en) * | 2016-11-23 | 2020-01-30 | Grst Int Ltd | Anode slurry for secondary battery |
| CN111418095A (en) * | 2017-12-01 | 2020-07-14 | 大洲电子材料株式会社 | Negative active material for non-aqueous electrolyte secondary battery comprising silicon oxide composite and method for preparing same |
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| CN110931744B (en) * | 2019-11-29 | 2021-03-16 | 深圳技术大学 | Silicon-carbon negative electrode material and preparation method thereof |
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| CN111952558A (en) * | 2020-07-28 | 2020-11-17 | 华陆工程科技有限责任公司 | Preparation method of silicon-carbon negative electrode material of lithium ion battery |
| CN113659120B (en) * | 2021-07-30 | 2023-06-06 | 江苏泛亚微透科技股份有限公司 | Elastic aerogel derived high-capacity silicon oxygen carbon lithium battery negative electrode material and preparation method thereof |
| CN113921783A (en) * | 2021-09-27 | 2022-01-11 | 天津市捷威动力工业有限公司 | Long-cycle high-rate silicon-carbon negative electrode material and preparation method thereof |
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| CN103035917B (en) * | 2013-01-09 | 2014-08-13 | 北京科技大学 | Preparation method of silicon dioxide/ carbon composite negative electrode material for lithium ion battery |
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