CN109935808A - A method of silicon-carbon cathode material is prepared based on micron silicon wafer - Google Patents

A method of silicon-carbon cathode material is prepared based on micron silicon wafer Download PDF

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Publication number
CN109935808A
CN109935808A CN201910146041.4A CN201910146041A CN109935808A CN 109935808 A CN109935808 A CN 109935808A CN 201910146041 A CN201910146041 A CN 201910146041A CN 109935808 A CN109935808 A CN 109935808A
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China
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silicon
silicon wafer
cathode material
carbon cathode
micron
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CN201910146041.4A
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叶圣杰
赵东辉
周鹏伟
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Fujian Xfh Battery Material Co Ltd
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Fujian Xfh Battery Material Co Ltd
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Priority to CN201910146041.4A priority Critical patent/CN109935808A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

The present invention discloses a kind of method for preparing silicon-carbon cathode material based on micron silicon wafer, includes following steps: (1) being prepared for silicon wafer powder using electron beam evaporation method, the silicon thin film of 90-110nm thickness is deposited on the sheet metal of polymer-coated;(2) silicon thin film is removed from sheet metal, is ground into the microplate shape silicon wafer powder that lateral dimension is 3-5mm;(3) silicon wafer powder, pitch are added in the deionized water containing 0.5-5 wt% water soluble dispersing agent and are stirred dispersion, obtain slurry;(4) slurry is spray-dried, the solid after drying is warming up to 600-1500 DEG C, obtains silicon-carbon cathode material after high temperature cabonization 10-30h.Pass through the embedding lithium capacity high using silicon materials, so that the negative electrode material being prepared has biggish discharge capacity and higher first charge-discharge efficiency when being used to prepare half-cell, micron flakes silicon powder is closely combined using agraphitic carbon, disperse silicon micron chip and reduce itself and electrolyte interface, improves the stability and battery performance of silicon-carbon cathode material.

Description

A method of silicon-carbon cathode material is prepared based on micron silicon wafer
Technical field
The present invention relates to negative electrode material field technology, refer in particular to a kind of prepare silicon-carbon cathode material based on micron silicon wafer Method.
Background technique
The raising that lithium ion battery with high energy density is required with power battery automobile and large-scale fixed energy storage device.By In high gravimetric and volume capacity (3578 mAh/g and 2194 mAh/g, Li15Si4), and relatively low discharge potential (0.4V vs Li/Li+), silicon materials are expected to become the negative electrode material of next-generation lithium ion battery with high energy density.
However, silicium cathode has a serious problem, i.e., capacity retention ratio is poor in repeated charge-discharge cycles.Silicium cathode difference Cycle performance is to cause material cracked since silicon active material volume dilation is excessive in charge and discharge process and crush.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide one kind to be based on micron silicon The method that piece prepares silicon-carbon cathode material, with good long circulating performance.
To achieve the above object, the present invention is using following technical solution:
A method of silicon-carbon cathode material is prepared based on micron silicon wafer, includes following steps:
(1) silicon wafer powder is prepared for using electron beam evaporation method, 90-110nm thickness is deposited on the sheet metal of polymer-coated Silicon thin film;
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5mm, and passes through X-ray Diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder;
(3) silicon wafer powder, pitch are added in the deionized water containing 0.5-5 wt% water soluble dispersing agent and are stirred dispersion, obtained To slurry;
(4) slurry is spray-dried, the solid after drying is warming up to 600-1500 DEG C, is obtained after high temperature cabonization 10-30h Silicon-carbon cathode material.
As a preferred embodiment, the pitch partial size is≤50 μm.
As a preferred embodiment, the water soluble dispersing agent is one of acrylic compounds, maleic acid anhydride or a variety of.
As a preferred embodiment, the atmosphere that the high temperature cabonization uses is nitrogen, argon gas, nitrogen hydrogen mixed gas, argon One of gas hydrogen mixed gas.
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically, by above-mentioned technical proposal Known to:
By the embedding lithium capacity high using silicon materials, so that with larger when the negative electrode material being prepared is used to prepare half-cell Discharge capacity and higher first charge-discharge efficiency, and micron flakes silicon powder is closely combined using agraphitic carbon, is made Silicon micron chip disperses and reduces itself and electrolyte interface, improves the stability and battery performance of silicon-carbon cathode material, And 500 times circulation volume conservation rate effectively improves.
Detailed description of the invention
Fig. 1 is the SEM figure of the silicon-carbon cathode material of embodiments of the present invention 1.
Specific embodiment
Present invention discloses a kind of methods for preparing silicon-carbon cathode material based on micron silicon wafer, include following steps:
(1) silicon wafer powder is prepared for using electron beam evaporation method, 90-110nm thickness is deposited on the sheet metal of polymer-coated Silicon thin film.
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5mm, and passes through X X ray diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder.
(3) silicon wafer powder, pitch are added in the deionized water containing 0.5-5 wt% water soluble dispersing agent and are stirred point It dissipates, obtains slurry.The pitch partial size is≤50 μm, and the water soluble dispersing agent is acrylic compounds, one in maleic acid anhydride Kind is a variety of.
(4) slurry is spray-dried, the solid after drying is warming up to 600-1500 DEG C, after high temperature cabonization 10-30h Obtain silicon-carbon cathode material.The atmosphere that the high temperature cabonization uses is mixed for nitrogen, argon gas, nitrogen hydrogen mixed gas, argon gas hydrogen Close one of gas.
With multiple embodiments, invention is further described in detail below:
Embodiment 1:
A method of silicon-carbon cathode material being prepared based on micron silicon wafer, step includes:
(1) silicon wafer powder is prepared for using electron beam evaporation method, the silicon of 100 nm thickness is deposited on the sheet metal of polymer-coated Film.
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5 mm, and passes through X-ray diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder.
(3) 3 wt% silicon wafer powder, 3 wt% pitches, 1 wt% polyacrylamide are stirred dispersion in deionized water, obtained To slurry.
(4) slurry is spray-dried, the solid after drying is warming up to 1500 DEG C, obtains silicon after high temperature cabonization 12h Carbon negative pole material.
Embodiment 2:
A method of silicon-carbon cathode material being prepared based on micron silicon wafer, step includes:
(1) silicon wafer powder is prepared for using electron beam evaporation method, the silicon that 90nm thickness is deposited on the sheet metal of polymer-coated is thin Film.
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5 mm, and passes through X-ray diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder.
(3) 7 wt% silicon wafer powder, 0.7 wt% pitch, 3 wt% polyacrylamides are stirred dispersion in deionized water, Obtain slurry.
(4) slurry is spray-dried, the solid after drying is warming up to 1300 DEG C, obtains silicon after high temperature cabonization 10h Carbon negative pole material.
Embodiment 3:
A method of silicon-carbon cathode material being prepared based on micron silicon wafer, step includes:
(1) silicon wafer powder is prepared for using electron beam evaporation method, the silicon of 110 nm thickness is deposited on the sheet metal of polymer-coated Film.
(2) silicon fiml is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5 mm, and passes through X X ray diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder.
(3) 4 wt% silicon wafer powder, 2 wt% pitches, 2 wt% polyacrylamides are stirred dispersion in deionized water, are obtained To slurry.
(4) slurry is spray-dried, the solid after drying is warming up to 600 DEG C, obtains silicon-carbon after high temperature cabonization 30h Negative electrode material.
Comparative example 1:
Difference with embodiment 1 is: being not added with water soluble dispersing agent.
A method of lithium ion silicon-carbon cathode material being prepared, step includes:
(1) silicon wafer powder is prepared for using electron beam evaporation method, the silicon of 100 nm thickness is deposited on the sheet metal of polymer-coated Film.
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5 mm, and passes through X-ray diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder.
(3) 3 wt% silicon wafer powder, 3 wt% pitches are stirred dispersion in deionized water, obtain slurry.
(4) slurry is spray-dried, the solid after drying is warming up to 1500 DEG C, obtains silicon after high temperature cabonization 12h Carbon negative pole material.
Performance characterization:
Discharge capacity and charge and discharge for the first time are carried out to the negative electrode material in embodiment and comparative example using half-cell test method As a result the test of electrical efficiency is listed in table 1.Half-cell test method are as follows: use above-mentioned negative electrode material, while simulated battery is assemblied in Carried out in the glove box of inflated with nitrogen, electrolyte is 1M LiPF6+EC+DEC+DMC=1:1:1(volume ratio), metal lithium sheet is to electricity Pole, electrochemical property test carry out on blue electrical testing cabinet, and charging/discharging voltage range is 0.05 to 5.0V, and charge-discharge velocity is 0.1C。
Table 1
Discharge capacity (mAh/g) First charge-discharge efficiency (%) 500 circulation volume conservation rates (%)
Embodiment 1 1797 95 97
Embodiment 2 1542 94 96
Embodiment 3 1623 92 96
Comparative example 1 1508 83 84
As it can be seen from table 1 half-cell prepared by the cathode pole piece of embodiment 1-3 has biggish discharge capacity and higher head Secondary efficiency for charge-discharge, this is mainly due to the high embedding lithium capacity of silicon materials.And 500 circulation volume conservation rates are compared with comparative example Height is mainly closely combined micron flakes silicon powder due to agraphitic carbon, is dispersed silicon micron chip and is reduced itself and electrolysis Matter contact surface improves the stability and battery performance of silicon based anode material.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention, Therefore any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention, still Belong in the range of technical solution of the present invention.

Claims (4)

1. a kind of method for preparing silicon-carbon cathode material based on micron silicon wafer, it is characterised in that: include following steps:
(1) silicon wafer powder is prepared for using electron beam evaporation method, 90-110nm thickness is deposited on the sheet metal of polymer-coated Silicon thin film;
(2) silicon thin film is removed from sheet metal, is ground into lateral dimension and is the microplate shape silicon wafer powder of 3-5mm, and passes through X-ray Diffraction and Raman spectrum confirm the non crystalline structure of silicon wafer powder;
(3) silicon wafer powder, pitch are added in the deionized water containing 0.5-5 wt% water soluble dispersing agent and are stirred dispersion, obtained To slurry;
(4) slurry is spray-dried, the solid after drying is warming up to 600-1500 DEG C, is obtained after high temperature cabonization 10-30h Silicon-carbon cathode material.
2. a kind of method for preparing silicon-carbon cathode material based on micron silicon wafer according to claim 1, it is characterised in that: institute Stating pitch partial size is≤50 μm.
3. a kind of method for preparing silicon-carbon cathode material based on micron silicon wafer according to claim 1, it is characterised in that: institute Stating water soluble dispersing agent is one of acrylic compounds, maleic acid anhydride or a variety of.
4. a kind of method for preparing silicon-carbon cathode material based on micron silicon wafer according to claim 1, it is characterised in that: institute The atmosphere that high temperature cabonization uses is stated as one of nitrogen, argon gas, nitrogen hydrogen mixed gas, argon gas hydrogen mixed gas.
CN201910146041.4A 2019-02-27 2019-02-27 A method of silicon-carbon cathode material is prepared based on micron silicon wafer Pending CN109935808A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112234178A (en) * 2020-10-20 2021-01-15 陕西煤业化工技术研究院有限责任公司 Superfine nano silicon/carbon composite material and preparation method and application thereof

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CN101847708A (en) * 2009-03-27 2010-09-29 比亚迪股份有限公司 Cathode for lithium-ion secondary battery, method for producing same and lithium-ion secondary battery using same
JP2011065983A (en) * 2009-08-21 2011-03-31 Oike Ind Co Ltd Scale-like thin film fine powder dispersion liquid or scale-like thin film fine powder, and paste using the same, electrode for battery, and lithium secondary battery
CN102244240A (en) * 2011-06-15 2011-11-16 中南大学 Lithium ion battery composite anode material and preparation method thereof
CN105247704A (en) * 2011-11-22 2016-01-13 国际商业机器公司 Composite anode structure for high energy density lithium-ion batteries
CN105680013A (en) * 2016-01-26 2016-06-15 湖南有色金属研究院 Preparation method for silicon/graphite/carbon composite negative electrode material of lithium ion battery
CN107221579A (en) * 2017-06-09 2017-09-29 常州比太科技有限公司 Solar cell film plating process and solar cell
CN107416839A (en) * 2017-09-11 2017-12-01 商永辉 A kind of method for preparing lithium ion battery negative material using the discarded silica flour slurry of Buddha's warrior attendant wire cutting
CN107615528A (en) * 2015-06-22 2018-01-19 株式会社日立制作所 Lithium ion secondary battery cathode active material and lithium rechargeable battery

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Publication number Priority date Publication date Assignee Title
CN101847708A (en) * 2009-03-27 2010-09-29 比亚迪股份有限公司 Cathode for lithium-ion secondary battery, method for producing same and lithium-ion secondary battery using same
JP2011065983A (en) * 2009-08-21 2011-03-31 Oike Ind Co Ltd Scale-like thin film fine powder dispersion liquid or scale-like thin film fine powder, and paste using the same, electrode for battery, and lithium secondary battery
CN101800305A (en) * 2010-03-09 2010-08-11 福建师范大学 Method for depositing silicon film at surface of lithium titanate cathode of lithium ion battery
CN102244240A (en) * 2011-06-15 2011-11-16 中南大学 Lithium ion battery composite anode material and preparation method thereof
CN105247704A (en) * 2011-11-22 2016-01-13 国际商业机器公司 Composite anode structure for high energy density lithium-ion batteries
CN107615528A (en) * 2015-06-22 2018-01-19 株式会社日立制作所 Lithium ion secondary battery cathode active material and lithium rechargeable battery
CN105680013A (en) * 2016-01-26 2016-06-15 湖南有色金属研究院 Preparation method for silicon/graphite/carbon composite negative electrode material of lithium ion battery
CN107221579A (en) * 2017-06-09 2017-09-29 常州比太科技有限公司 Solar cell film plating process and solar cell
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112234178A (en) * 2020-10-20 2021-01-15 陕西煤业化工技术研究院有限责任公司 Superfine nano silicon/carbon composite material and preparation method and application thereof
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Application publication date: 20190625