CN103472401B - Lithium ion battery anode active material specific storage detection method after circulation - Google Patents
Lithium ion battery anode active material specific storage detection method after circulation Download PDFInfo
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Abstract
The invention provides the rear lithium ion battery anode active material specific storage detection method of a kind of circulation, comprising: electric discharge is carried out to the lithium ion battery after circulation and disassembles taking-up cathode pole piece; Organic solvent drip washing is soaked and is dried; Cathode pole piece after drying is placed in acid solution, and ultrasonic process makes cathode membrane drop in acid solution and dispersed, takes out collector; There is the solution of cathode membrane material to carry out Separation of Solid and Liquid to dispersed, obtain solid matter, with deionized water drip washing repeatedly, until the pH value of the filtrate formed is 6 ~ 7; Vacuum drying, under being placed in protective atmosphere protection, 350 ~ 450 DEG C of roasting 3h, grinding after cooling, screening obtain negative active core-shell material particle; Slurry is made in the mixing of negative active core-shell material particle, conductive agent, cementing agent and solvent; In drying shed, adopt compressed-air actuated gravity type spray gun to be applied on the Copper Foil of stationary installation by pulp spraying, vacuum drying, obtain specific storage detection cathode pole piece after colding pressing, measure after being assembled into button cell.
Description
Technical field
The present invention relates to a kind of lithium ion battery detection method, particularly relate to the rear lithium ion battery anode active material specific storage detection method of a kind of circulation.
Background technology
Along with greatly developing of lithium ion battery, also more and more deep to the research of lithium ion battery material in the industry.Negative material as the important component part of lithium ion battery, wield influence whole capacity of lithium ion battery and the cycle performance of its specific storage.Study thus lithium ion battery repeatedly circulate after the change of negative material specific storage be vital.
Specific capacity of negative electrode material of lithium ion battery detection method after the Chinese patent application publication number CN102610792A announced on April 1st, 2012 discloses a kind of circulation, the method obtains purer powdered graphite by adopting organic solvent drip washing and acid solution to soak, and then surveys its specific storage.But organic solvent drip washing and acid solution soak the cementing agent that all well cannot remove powdered graphite surface, thus affect the precision of specific storage detection.At present, the cathode pole piece for testing specific storage needs mechanical raking and scraper for coating, can cause a large amount of losses of material like this, thus adds the sample size needed for specific storage test.But the testing and analyzing of the chemical property of lithium ion battery negative material is not only confined to specific storage after circulation, the sample size that therefore can be used for carrying out specific storage test is limited.According to magnetic agitation and scraper for coating, adopt in test process and increase quantity of solvent to meet the demand of less sample size, easily occur so again too low the and cathode pole piece crawling of slurry viscosity, to such an extent as to specific storage test cannot be carried out or cannot accurately test.
Summary of the invention
In view of background technology Problems existing, the object of the present invention is to provide the rear lithium ion battery anode active material specific storage detection method of a kind of circulation, the accuracy that after it can improve circulation, lithium ion battery anode active material specific storage detects.
Another object of the present invention is to provide a kind of circulation rear lithium ion battery anode active material specific storage detection method, it can be reduced in the loss of material in the preparation process of the cathode pole piece that specific storage detects.
Another object of the present invention is to provide a kind of circulation rear lithium ion battery anode active material specific storage detection method, and it can realize carrying out detection specific storage by less sample size, realizes carrying out reliable specific storage test with a small amount of sample.
To achieve these goals, the invention provides the rear lithium ion battery anode active material specific storage detection method of a kind of circulation, it comprises step: discharge to the lithium ion battery after circulation, disassemble lithium ion battery and take out cathode pole piece; Cathode pole piece adopted organic solvent drip washing and soak, drying afterwards; Cathode pole piece after drying is placed in acid solution, and ultrasonic process makes the cathode membrane of cathode pole piece to drop in acid solution and the homogenize material of cathode membrane is disperseed, and takes out the collector of cathode pole piece; There is the solution of cathode membrane material to carry out Separation of Solid and Liquid to dispersed, obtain solid matter; With deionized water solid matter described in drip washing repeatedly, until the deionized water pH value of filtrate that solid matter described in drip washing is formed repeatedly is 6 ~ 7; Described solid matter after the drip washing of vacuum drying deionized water; Under dried described solid matter being placed in protective atmosphere protection, 350 ~ 450 DEG C of roasting 3h, grinding after cooling, screening obtain negative active core-shell material particle; Slurry is made in negative active core-shell material particle, conductive agent, cementing agent and the deionized water mixing as solvent; In drying shed, adopt compressed-air actuated gravity type spray gun to be applied on the Copper Foil of stationary installation by described pulp spraying, vacuum drying, after colding pressing, obtain specific storage detection cathode pole piece; And detection cathode pole piece and lithium sheet, barrier film are assembled into button cell and inject electrolytic solution, after leaving standstill, measure the specific storage of detection cathode pole piece.
Beneficial effect of the present invention is as follows:
Acid wash is combined with roasting method, effectively can removes cementing agent and the thickening agent of graphite surface, obtain clean and there is no destroyed negative active core-shell material, thus improving the accuracy of specific storage test;
Adopt compressed-air actuated gravity type lance ejection slurry to prepare cathode pole piece, not only considerably reduce the employing amount of sample, reduce cost, and improve controllability, the easily uniform detection cathode pole piece of acquisition coating of coating process, thus realize carrying out reliable specific storage test with a small amount of sample.
Accompanying drawing explanation
Fig. 1 adopts acid wash process graphite and the SEM comparison diagram in conjunction with acid wash and roasting method process graphite.
Fig. 2 is stationary installation schematic diagram:
Fig. 3 is the charging and discharging capacity test pattern of embodiment 1 and comparative example 1.
Wherein, description of reference numerals is as follows:
1 solid plexiglass base plate 2 Copper Foil
3 hollow organic-glass frames
Embodiment
The following detailed description of the embodiment of lithium ion battery anode active material specific storage detection method after circulation according to the present invention.
First illustrate according to lithium ion battery anode active material specific storage detection method after circulation of the present invention.
Step is comprised: the lithium ion battery after circulation is discharged, disassembles lithium ion battery and take out cathode pole piece according to lithium ion battery anode active material specific storage detection method after circulation of the present invention; Cathode pole piece adopted organic solvent drip washing and soak, drying afterwards; Cathode pole piece after drying is placed in acid solution, and ultrasonic process makes the cathode membrane of cathode pole piece to drop in acid solution and the homogenize material of cathode membrane is disperseed, and takes out the collector of cathode pole piece; There is the solution of cathode membrane material to carry out Separation of Solid and Liquid to dispersed, obtain solid matter; With deionized water solid matter described in drip washing repeatedly, until the deionized water pH value of filtrate that solid matter described in drip washing is formed repeatedly is 6 ~ 7; Described solid matter after the drip washing of vacuum drying deionized water; Under dried described solid matter being placed in protective atmosphere protection, 350 ~ 450 DEG C of roasting 3h, grinding after cooling, screening obtain negative active core-shell material particle; Slurry is made in negative active core-shell material particle, conductive agent, cementing agent and the deionized water mixing as solvent; In drying shed, adopt compressed-air actuated gravity type spray gun to be applied on the Copper Foil of stationary installation by described pulp spraying, vacuum drying, after colding pressing, obtain specific storage detection cathode pole piece; And detection cathode pole piece and lithium sheet, barrier film are assembled into button cell and inject electrolytic solution, after leaving standstill, measure the specific storage of detection cathode pole piece.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, first adopt organic solvent drip washing lithium ion battery negative electrode, effectively can remove the electrolytic solution on cathode pole piece and organic SEI film, prevent lithium salts to decompose the destruction of Louise acid to graphite of generation HF and strong polarity; Adopt acid solution ultrasonic cleaning negative active core-shell material again, effectively can remove a large amount of accessory substances produced in lithium ion battery circulation, reach the object of purification of graphite; Adopt graphite to the filtrate after deionized water drip washing acid solution purifying to be neutral, both ensure that the potential of hydrogen of graphite, clean again the CMC thickening agent in cathode size further; Because abovementioned steps all cannot remove the cementing agent SBR of graphite surface effectively, therefore adopt the high-temperature roasting under protective atmosphere condition, purer negative active core-shell material can be obtained.If but do not adopt acid solution ultrasonic cleaning, and directly adopt the cathode pole piece after the drip washing of high-temperature roasting organic solvent, because CMC has more residual volume after high-temperature roasting, to such an extent as to cannot purifying negative active core-shell material.Therefore the present invention adopts the processing mode that acid wash is combined with high-temperature roasting method, obtains pure negative active core-shell material, thus is conducive to the accuracy improving specific storage detection.Adopt compressed-air actuated gravity type lance ejection cathode size to prepare cathode pole piece, significantly reduce the use amount of negative active core-shell material, improve the controllability of coating process, thus obtain being coated with uniform lithium ion battery negative electrode, thus realize carrying out reliable specific storage test with a small amount of sample; The employing of gravity type spray gun makes the coating of small size more even; Compared with nitrogen and inert gas, pressurized air significantly reduces cost.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described organic solvent can be dimethyl carbonate (DMC) or ethyl acetate (EA).
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described acid solution can be sulfuric acid or hydrochloric acid, and concentration can be 0.1 ~ 1mol/L.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described Separation of Solid and Liquid can adopt suction filtration.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, the temperature of the described solid matter after the drip washing of vacuum drying deionized water can be 60 ~ 100 DEG C, is preferably 85 DEG C.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described protective atmosphere can be nitrogen or argon gas.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described screening can adopt double-deck screening, wherein ground floor screening employing 150 mesh sieve, second layer screening employing 200 mesh sieve.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, when making slurry: the conductive carbon as conductive agent joins in beaker jointly with sodium carboxymethyl cellulose (CMC) solution as thickening agent, ultrasonic process, add negative active core-shell material particle and the deionized water as solvent afterwards, stir and ultrasonic process; After continuing to add the carboxymethylcellulose sodium solution as thickening agent in whipping process again, and then styrene-butadiene rubber (SBR) emulsion added as cementing agent, finally obtain described slurry, wherein, the mass ratio of negative active core-shell material: conductive carbon: CMC:SBR is 94.5:1.5:1.5:2.5, and the solid content in slurry is 50%.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, the both sides up and down of described stationary installation are respectively solid plexiglass base plate and hollow organic-glass frame, middle layer is Copper Foil, and the hair side of Copper Foil is relative with hollow organic-glass frame.
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, described solid plexiglass base plate is identical with the housing size of hollow organic-glass frame, is 10 × 15cm
2; The size of the inside casing of hollow organic-glass frame is (2 ~ 8cm) × (5 ~ 12cm).
After according to circulation of the present invention in lithium ion battery anode active material specific storage detection method, the relative humidity in described drying shed is lower than 2%.
Embodiment according to lithium ion battery anode active material specific storage detection method after circulation of the present invention, comparative example and test result are finally described.
Embodiment 1
Circulation after lithium ion battery negative active core-shell material extract: by using H type graphite as negative active core-shell material, circulate 1 week after 506971 lithium ion batteries be discharged to voltage lower than 2V with 0.1C, to disassemble in hothouse and after taking out cathode pole piece, use dimethyl carbonate (DMC) drip washing immediately and soak, take out afterwards and dry; Cathode pole piece after drying is put into 0.1mol/L hydrochloric acid solution, ultrasonic process 0.5h, now the cathode membrane of cathode pole piece drops to hydrochloric acid solution and the homogenize material of cathode membrane is distributed in hydrochloric acid solution, and takes out the collector of cathode pole piece; Suction filtration, makes Separation of Solid and Liquid, obtains solid matter; With deionized water drip washing solid matter repeatedly, until the deionized water PH of filtrate that drip washing is formed repeatedly is 6.8 by the vacuum drying at 85 DEG C of the solid matter after deionized water drip washing; Then under the protection of nitrogen atmosphere, by dried solid matter at 400 DEG C of roasting 3h, grinding after cooling, double-deck screening, ground floor screening employing 150 mesh sieve, second layer screening employing 200 mesh sieve, obtains negative active core-shell material particle.
Prepare cathode size: join in the beaker of 20ml by conductive carbon and 1.5wt.% carboxymethylcellulose sodium solution (CMC), ultrasonic 10min; Add 2g negative active core-shell material particle and deionized water, stir 0.5h, ultrasonic 0.5h; 45wt.% SBR emulsion (SBR) is added in continuation whipping process, uniform cathode size is obtained after continuing to stir 0.5h, the mass ratio that feeds intake of wherein negative active core-shell material: conductive carbon: CMC:SBR is 94.5:1.5:1.5:2.5, and solid content is 50%.
Prepare cathode pole piece: in relative humidity (RH) value lower than in the drying shed of 2%, on the Copper Foil hair side adopting compressed-air actuated gravity type spray gun to be sprayed to by the cathode size of preparation to be fixed in stationary installation, vacuum drying at 60 DEG C, cold pressing after obtain cathode pole piece, the size of the organic glass frame wherein in stationary installation is 6cm × 10cm;
Specific storage detects: the cathode pole piece of preparation is die-cut into sequin and is assembled into button cell with lithium sheet, barrier film and electrolytic solution, after leaving standstill 2h, use 0.05mA current discharge to 5mV after adopting 0.05C current discharge to 5mV again, 2V is charged to afterwards with 0.1C, the capacity filled is the specific storage first of negative active core-shell material, wherein, the content of electrolytic solution lithium salts is the LiPF of 1mol/L
6, solvent quality is than the potpourri of DEC, EC and the PC for 1:1:1.
Comparative example 1
Except directly adopting the former powder of H type graphite as except the negative active core-shell material particle in embodiment 1 in the negative active core-shell material leaching process of lithium ion battery after cycling, all the other are with embodiment 1.
Comparative example 2
Except in the negative active core-shell material leaching process of lithium ion battery after cycling, dried solid matter is without except 400 DEG C of roasting 3h, and all the other are with embodiment 1.
Comparative example 3
Adopt scraper for coating to replace the compressed-air actuated gravity type spray gun prepared in cathode pole piece process, all the other are with embodiment 1.
Embodiment 2
After circulation, the negative active core-shell material of lithium ion battery extracts: 506971 lithium ion batteries after being negative active core-shell material with H type graphite, circulating 600 weeks are discharged to voltage lower than 2V with 0.1C, to disassemble in hothouse and after taking out cathode pole piece, use ethyl acetate (EA) drip washing immediately and soak, take out afterwards and dry; Cathode pole piece after drying is put into 0.5mol/L sulfuric acid solution, ultrasonic process 0.5h, now the cathode membrane of cathode pole piece drops to sulfuric acid solution and the homogenize material of cathode membrane is distributed in sulfuric acid solution, and takes out the collector of cathode pole piece; Suction filtration, makes Separation of Solid and Liquid, obtains solid matter; With deionized water drip washing solid matter repeatedly, until the deionized water pH value of filtrate that drip washing is formed repeatedly is 6.5; By the vacuum drying at 85 DEG C of the solid matter after deionized water drip washing; Then under the protection of argon gas atmosphere, by dried solid matter at 400 DEG C of roasting 3h, grinding after cooling, double-deck screening, ground floor screening employing 150 mesh sieve, second layer screening employing 200 mesh sieve, obtains negative active core-shell material particle.
Prepare cathode size: join in 20ml beaker by conductive carbon and 1.5wt.% carboxymethylcellulose sodium solution (CMC), ultrasonic 8min; Add 1.5g negative active core-shell material particle and deionized water, stir 0.5h, ultrasonic 0.5h; 45wt.% SBR emulsion (SBR) is added in continuation whipping process, uniform cathode size is obtained after continuing to stir 0.5h, wherein, the rate of charge of negative active core-shell material: conductive carbon: CMC:SBR is 94.5:1.5:1.5:2.5, and solid content is 50%.
Prepare cathode pole piece: in relative humidity (RH) value lower than in the drying shed of 2%, on the Copper Foil hair side adopting compressed-air actuated gravity type spray gun to be sprayed to by the cathode size of preparation to be fixed in stationary installation, vacuum drying at 60 DEG C, obtain cathode pole piece after colding pressing, the size of the organic glass frame wherein in stationary installation is 3cm × 9cm;
Specific storage detects: the cathode pole piece of preparation is die-cut into sequin and is assembled into button cell with lithium sheet, barrier film and electrolytic solution, after leaving standstill 2h, use 0.05mA current discharge to 5mV after adopting 0.05C current discharge to 5mV again, 2V is charged to afterwards with 0.1C, the capacity filled is the specific storage first of negative active core-shell material, wherein, the content of electrolytic solution lithium salts is the LiPF of 1mol/L
6, solvent quality is than the potpourri of DEC, EC and the PC for 1:1:1.
Comparative example 4
Carry out except circulation 600 weeks the button cell of comparative example 1 except in specific storage testing process, all the other are all with comparative example 1.
Embodiment 3
Circulation after lithium ion battery negative active core-shell material extract: by using H type graphite as negative active core-shell material, circulate 800 weeks after 506971 lithium ion batteries be discharged to voltage lower than 2V with 0.1C, to disassemble in hothouse and after taking out cathode pole piece, use dimethyl carbonate (DMC) drip washing immediately and soak, take out afterwards and dry; Cathode pole piece after drying is put into 0.2mol/L hydrochloric acid solution, ultrasonic process 0.5h, now the cathode membrane of cathode pole piece drops to hydrochloric acid solution and the homogenize material of cathode membrane is distributed in hydrochloric acid solution, and takes out the collector of cathode pole piece; Suction filtration, makes Separation of Solid and Liquid, obtains solid matter; With deionized water drip washing solid matter repeatedly, until the deionized water pH value of filtrate that drip washing is formed repeatedly is 7; By the vacuum drying at 85 DEG C of the solid matter after deionized water drip washing; Then under the protection of nitrogen atmosphere, by dried solid matter at 400 DEG C of roasting 3h, grinding after cooling, double-deck screening, ground floor screening employing 150 mesh sieve, second layer screening employing 200 mesh sieve, obtains negative active core-shell material particle.
Prepare cathode size: join in 20ml beaker by conductive carbon and 1.5wt.% carboxymethylcellulose sodium solution (CMC), ultrasonic 5min; Add 1g negative active core-shell material and deionized water, stir 0.5h, ultrasonic 0.5h; In continuation whipping process, add 45wt.% SBR emulsion (SBR), obtain uniform cathode size after continuing to stir 0.5h, the rate of charge of wherein negative active core-shell material: conductive carbon: CMC:SBR is 94.5:1.5:1.5:2.5, and solid content is 50%.
Prepare cathode pole piece: in relative humidity (RH) value lower than in the drying shed of 2%, on the Copper Foil hair side adopting compressed-air actuated gravity type spray gun to be sprayed to by the cathode size of preparation to be fixed in stationary installation, vacuum drying at 60 DEG C, obtains cathode pole piece after colding pressing.The size of the organic glass frame wherein in stationary installation is 3cm × 6cm;
Specific storage detects: the cathode pole piece of preparation is die-cut into sequin and is assembled into button cell with lithium sheet, barrier film and electrolytic solution, after leaving standstill 2h, use 0.05mA current discharge to 5mV after adopting 0.05C current discharge to 5mV again, 2V is charged to afterwards with 0.1C, the capacity filled is the specific storage first of negative active core-shell material, wherein, the content of electrolytic solution lithium salts is the LiPF of 1mol/L
6, solvent quality is than the potpourri of DEC, EC and the PC for 1:1:1.
Comparative example 5
Carry out except circulation 800 weeks the button cell of comparative example 1 except in specific storage testing process, all the other are all with comparative example 1.
Finally provide the lithium ion battery anode active material specific storage testing result of embodiment 1-3 and comparative example 1-5.
Table 1 adopts the negative active core-shell material specific storage testing result of embodiment 1-3 and comparative example 1-5
As can be seen from Table 1, only with acid wash purify the H type graphite (comparative example 2) obtained specific storage relative to the former powder of H type graphite (comparative example 1) deviation comparatively greatly, and embodiment 1 processes the specific storage of specific storage closer to the former powder of H type graphite (comparative example 1) of the H type graphite obtained; In addition, as can be seen from Figure 3, the H type graphite that extracts of embodiment 1 and the H type graphite former powder specific storage of comparative example 1 close.
As can be seen from Table 1, adopted by cathode size the mode of scraper for coating (comparative example 3) to spray, because sample size is very few and successfully cannot prepare cathode pole piece, therefore cannot testing result be obtained.
As can be seen from Table 1, the discharge capacity of the H type graphite after the circulation that purifying obtains 600 weeks (embodiments 2) and circulation 800 weeks (embodiment 3), be 99.94% and 99.63% with the ratio of the discharge capacity of comparative example 4 and comparative example 5 respectively, can measure more accurately the specific storage of the negative material after circulation.
As can be seen from Figure 1, the H type graphite after the method purified lithium ion battery that embodiment 1 adopts acid wash to be combined with roasting method circulates, its surface treating adhesive can be removed.
In sum, the present invention is by carrying out organic solvent cleaning, acidification and high-temperature roasting under protective atmosphere to lithium ion battery anode active material, the lithium salts and aqueous additive (such as CMC thickening agent) that generate in the electrolytic solution on cathode pole piece, cyclic process are washed away, burn the cementing agent of graphite surface, activate the activity of negative active core-shell material, thus improve the accuracy of specific storage test; And use gunite to prepare cathode pole piece, greatly reduce the use amount of sample, improve the controllability of coating process, easily obtain the uniform cathode pole piece of coating.Therefore the method can reduce the requirement of the amount of sample and the accuracy of the specific storage measurement of lithium ion battery anode active material after improving circulation.
Claims (12)
1. a lithium ion battery anode active material specific storage detection method after circulation, is characterized in that, comprise step:
Lithium ion battery after circulation is discharged, disassembles lithium ion battery and take out cathode pole piece;
Cathode pole piece adopted organic solvent drip washing and soak, drying afterwards;
Cathode pole piece after drying is placed in acid solution, and ultrasonic process makes the cathode membrane of cathode pole piece to drop in acid solution and the homogenize material of cathode membrane is disperseed, and takes out the collector of cathode pole piece;
There is the solution of cathode membrane material to carry out Separation of Solid and Liquid to dispersed, obtain solid matter;
With deionized water solid matter described in drip washing repeatedly, until the deionized water pH value of filtrate that solid matter described in drip washing is formed repeatedly is 6 ~ 7;
Described solid matter after the drip washing of vacuum drying deionized water;
Under dried described solid matter being placed in protective atmosphere protection, 350 ~ 450 DEG C of roasting 3h, grinding after cooling, screening obtain negative active core-shell material particle;
Slurry is made in negative active core-shell material particle, conductive agent, cementing agent and the deionized water mixing as solvent;
In drying shed, adopt compressed-air actuated gravity type spray gun to be applied on the Copper Foil of stationary installation by described pulp spraying, vacuum drying, after colding pressing, obtain specific storage detection cathode pole piece; And
Detection cathode pole piece and lithium sheet, barrier film are assembled into button cell and inject electrolytic solution, after leaving standstill, measures the specific storage of detection cathode pole piece.
2. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, described organic solvent is dimethyl carbonate (DMC) or ethyl acetate (EA).
3. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, described acid solution is sulfuric acid or hydrochloric acid, and concentration is 0.1 ~ 1mol/L.
4. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, described Separation of Solid and Liquid adopts suction filtration.
5. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, the temperature of the described solid matter after the drip washing of vacuum drying deionized water is 60 ~ 100 DEG C.
6. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, the temperature of the described solid matter after the drip washing of vacuum drying deionized water is 85 DEG C.
7. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, described protective atmosphere is nitrogen or argon gas.
8. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, is characterized in that, described screening adopts double-deck screening, wherein ground floor screening employing 150 mesh sieve, second layer screening employing 200 mesh sieve.
9. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, it is characterized in that, when making slurry: the conductive carbon as conductive agent joins in beaker jointly with sodium carboxymethyl cellulose (CMC) solution as thickening agent, ultrasonic process, add negative active core-shell material particle and the deionized water as solvent afterwards, stir and ultrasonic process; After continuing to add the carboxymethylcellulose sodium solution as thickening agent in whipping process again, and then styrene-butadiene rubber (SBR) emulsion added as cementing agent, finally obtain described slurry, wherein, the mass ratio of negative active core-shell material: conductive carbon: CMC:SBR is 94.5:1.5:1.5:2.5, and the solid content in slurry is 50%.
10. lithium ion battery anode active material specific storage detection method after circulation according to claim 1, it is characterized in that, the both sides up and down of described stationary installation are respectively solid plexiglass base plate and hollow organic-glass frame, middle layer is Copper Foil, and the hair side of Copper Foil is relative with hollow organic-glass frame.
After 11. circulations according to claim 10, lithium ion battery anode active material specific storage detection method, is characterized in that, described solid plexiglass base plate is identical with the housing size of hollow organic-glass frame, is 10 × 15cm
2; The size of the inside casing of hollow organic-glass frame is (2 ~ 8cm) × (5 ~ 12cm).
After 12. circulations according to claim 1, lithium ion battery anode active material specific storage detection method, is characterized in that, the relative humidity in described drying shed is lower than 2%.
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| CN107045106A (en) * | 2016-12-20 | 2017-08-15 | 赣州市瑞富特科技有限公司 | Carbon negative pole material specific capacity and first coulombic efficiency method of testing |
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| JP2011096470A (en) * | 2009-10-29 | 2011-05-12 | National Institute Of Advanced Industrial Science & Technology | Negative electrode material in all solid lithium ion secondary battery, and manufacturing method of all solid lithium ion secondary battery |
| JP2011124028A (en) * | 2009-12-09 | 2011-06-23 | Hitachi Zosen Corp | Manufacturing method of all solid lithium ion secondary battery |
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| CN102082262A (en) * | 2010-12-31 | 2011-06-01 | 上海交通大学 | Method for preparing nano-carbon coated lithium battery anode material |
| CN103022435A (en) * | 2011-09-20 | 2013-04-03 | 宁波杉杉新材料科技有限公司 | Lithium ion battery silicon-carbon composite negative electrode material and preparation method thereof |
| CN102332572A (en) * | 2011-09-21 | 2012-01-25 | 广东达之邦新能源技术有限公司 | Anode material and manufacturing method thereof as well as lithium ion battery and negative plate thereof |
| CN102610792A (en) * | 2012-04-01 | 2012-07-25 | 东莞新能源科技有限公司 | Detecting method of specific capacity of negative electrode material of lithium ion battery after circulation |
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