CN103808860A - Lithium defect detection method for lithium ion anode material - Google Patents
Lithium defect detection method for lithium ion anode material Download PDFInfo
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- CN103808860A CN103808860A CN201410060993.1A CN201410060993A CN103808860A CN 103808860 A CN103808860 A CN 103808860A CN 201410060993 A CN201410060993 A CN 201410060993A CN 103808860 A CN103808860 A CN 103808860A
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- lithium
- anode material
- iodide
- lithium ion
- ion anode
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- Y—GENERAL 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
- 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 discloses a lithium defect detection method for a lithium ion anode material. The detection method comprises the following steps of dispersing a lithium ion anode material into an acetonitrile solvent, adding lithium iodide serving as a detection agent to perform lithiation reaction by controlling the reaction temperature and the time, then washing and centrifugating a reaction solution, testing the iodide ion content through supernate to obtain the consumption of the lithium iodide, and finally calculating a lithium defect condition and a lithium defect amount of the lithium ion anode material. The lithium defect detection method has an important guiding significance for improvement of the performance of the lithium ion anode material; furthermore, the detection method is simple and is easy to operate.
Description
Technical field
The present invention relates to a kind of lithium ion anode material lithium defect inspection method.
Background technology
There is the advantages such as high-energy, long-life and high voltage due to lithium ion battery, shown wide application prospect in the various fields such as portable electric appts and electric automobile, and become an important directions of China's New Energy Industry.At present, the synthetic main flow route of lithium ion anode material is high temperature solid-state method, due to reasons such as lithium source volatilizations under hot conditions, causes positive electrode to occur lithium room phenomenon, is referred to as lithium defect, finally can affect the chemical property of material.Therefore, to the lithium defect of material carry out simply, accurately detect assessment most important.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithium ion anode material lithium defect inspection method.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of lithium ion anode material lithium defect inspection method, comprises the following steps:
(1) utilize iodide standard solution to draw iodide calibration curve;
(2) by lithium ion anode material sample dispersion in acetonitrile solvent, obtain solution A;
(3) detection agent lithium iodide solution is added in described solution A, make the mol ratio of lithium iodide and lithium ion anode material be: 0.01～2:1, the lithiation 1～10h that refluxes at 80 ℃, obtains solution B;
(4) described solution B is carried out to high speed centrifugation, and use organic solvent supersound washing, leave and take supernatant cleansing solution;
(5) described supernatant cleansing solution dilution is carried out to iodide ion analysis, utilize iodide calibration curve, draw the amount of substance of iodide ion, calculate the iodide ion amount consuming, obtain lithium ion anode material lithium defect condition and defect level.
As preferably, the lithium ion anode material described in step (2) is: LiFePO
4, LiFePO
4/ C, LiMFePO
4(M=II A, III A, IV A, V A, VI A, III B, V B, VI B, VI B, VII B, VIII), LiCoO
2, LiMCoO
2(M=II A, III A, IV A, V A, VI A, III B, V B, VI B, VI B, VII B, VIII), LiNiO
2, LiMnO
2, LiMn
2o
4, Li (Ni
xco
ymn
1-x-y) O
2(x < 1, y < 1, x+y < 1), Li (Ni
xco
yal
1-x-y) O
2at least one in the compound clad material of (x < 1, y < 1, x+y < 1) and above-mentioned material, comprises nucleocapsid structure, sandwich construction and mixed structure that multiple material forms; Described compound is: Al
2o
3, Al (OH)
3, ZrO
2, TiO
2, SiO
2, MgO, ZnO, SnO
2.
As preferably, the lithiation mechanism described in step (3) is:
Lithium ion anode material Li
1-x+ LiI → lithium ion anode material Li+LiI
3
As preferably, the organic solvent described in step (4) is: at least one in toluene, benzene, ethanol, methyl alcohol, ether, acetone, acetonitrile, chloroform.
As preferably, anode material of lithium defect level and ratio of defects utilize iodide ion analytical approach described in iodide calibration curve described in step (1) and step (5) to calculate, and formula is as follows:
Lithium defect level=n × (n
1-n
2)
Wherein, the molecular weight that M is lithium ion anode material, the quality that m is lithium ion anode material, n is step (5) supernatant cleansing solution extension rate, n
1for the amount of substance of lithium iodide step (3) Suo Shu, n
2the amount of substance of the iodide ion obtaining for step (5).
The invention has the beneficial effects as follows:
Workable, not only lithium defect can be detected but also lithium defect can be repaired, be applicable to various lithium ion anode material lithium defects detection and correct assessment.
Embodiment
Embodiment 1:
(1) utilize iodide standard solution to draw iodide calibration curve;
(2) by the theoretical 0.1580g lithium 1%(mol ratio that lacks) ion positive electrode LiFePO
4be scattered in acetonitrile solvent;
(3) detection agent lithium iodide solution is added in step (2) solution, make the mol ratio of lithium iodide and lithium ion anode material be: 0.01:1, back flow reaction 1h at 80 ℃;
(4) step (3) solution is carried out to high speed centrifugation, and use organic solvent supersound washing, leave and take supernatant cleansing solution;
(5) 100 times of step (4) supernatant cleansing solution dilutions are carried out to iodide ion analysis, utilize iodide calibration curve, draw the amount of substance of iodide ion, calculate the iodide ion amount consuming, obtain lithium ion anode material lithium defect condition and defect level, adopt following formula:
Lithium defect level=n × (n
1-n
2)
Wherein, the molecular weight that M is lithium ion anode material, the quality that m is lithium ion anode material, n is step (5) supernatant cleansing solution extension rate, n
1for the amount of substance of lithium iodide step (3) Suo Shu, n
2the amount of substance of the iodide ion obtaining for step (5).
LiFePO
4synthetic method is with reference to CN1652999A, and after tested, lithium ratio of defects is 1.003%, suitable with theoretical value, illustrates that method of testing of the present invention is workable, lithium defect condition that can accurate evaluation lithium ion anode material.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any modification of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in claim protection domain of the present invention.
Claims (5)
1. a lithium ion anode material lithium defect inspection method, is characterized in that comprising the following steps:
(1) utilize iodide standard solution to draw iodide calibration curve;
(2) by lithium ion anode material sample dispersion in acetonitrile solvent, obtain solution A;
(3) detection agent lithium iodide solution is added in described solution A, make the mol ratio of lithium iodide and lithium ion anode material be: 0.01～2:1, lithiation 1～10 h that refluxes at 80 ℃, obtains solution B;
(4) described solution B is carried out to high speed centrifugation, and use organic solvent supersound washing, leave and take supernatant cleansing solution;
(5) described supernatant cleansing solution dilution is carried out to iodide ion analysis, utilize iodide calibration curve, draw the amount of substance of iodide ion, calculate the iodide ion amount consuming, obtain lithium ion anode material lithium defect condition and defect level.
2. lithium ion anode material lithium defect inspection method as claimed in claim 1, is characterized in that: the lithium ion anode material described in step (2) is: LiFePO
4, LiFePO
4/ C, LiMFePO
4(M=II A, III A, IV A, V A, VI A, III B, V B, VI B, VI B, VII B, VIII), LiCoO
2, LiMCoO
2(M=II A, III A, IV A, V A, VI A, III B, V B, VI B, VI B, VII B, VIII), LiNiO
2, LiMnO
2, LiMn
2o
4, Li (Ni
xco
ymn
1-x-y) O
2(x < 1, y < 1, x+y < 1), Li (Ni
xco
yal
1-x-y) O
2at least one in the compound clad material of (x < 1, y < 1, x+y < 1) and above-mentioned material, comprises nucleocapsid structure, sandwich construction and mixed structure that multiple material forms; Described compound is: Al
2o
3, Al (OH)
3, ZrO
2, TiO
2, SiO
2, MgO, ZnO, SnO
2.
3. lithium ion anode material lithium defect inspection method as claimed in claim 1, is characterized in that: the lithiation mechanism described in step (3) is:
Lithium ion anode material Li
1-x+ LiI → lithium ion anode material Li+LiI
3.
4. lithium ion anode material lithium defect inspection method as claimed in claim 1, is characterized in that: the organic solvent described in step (4) is: at least one in toluene, benzene, ethanol, methyl alcohol, ether, acetone, acetonitrile, chloroform.
5. lithium ion anode material lithium defect inspection method as claimed in claim 1, it is characterized in that: anode material of lithium defect level and ratio of defects utilize iodide ion analytical approach described in iodide calibration curve described in step (1) and step (5) to calculate, and formula is as follows:
Lithium defect level=
Lithium ratio of defects (%)=
Wherein,
mfor the molecular weight of lithium ion anode material, the quality that m is lithium ion anode material, n is step (5) supernatant cleansing solution extension rate, n
1for the amount of substance of lithium iodide step (3) Suo Shu, n
2the amount of substance of the iodide ion obtaining for step (5).
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|---|---|---|---|
| CN201410060993.1A CN103808860B (en) | 2014-02-21 | 2014-02-21 | A kind of lithium ion anode material lithium defect inspection method |
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|---|---|---|---|
| CN201410060993.1A CN103808860B (en) | 2014-02-21 | 2014-02-21 | A kind of lithium ion anode material lithium defect inspection method |
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| Publication Number | Publication Date |
|---|---|
| CN103808860A true CN103808860A (en) | 2014-05-21 |
| CN103808860B CN103808860B (en) | 2015-07-29 |
Family
ID=50705936
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124675A (en) * | 2016-06-13 | 2016-11-16 | 合肥国轩高科动力能源有限公司 | A kind of method of lithium battery electrolytes chromatograph test pre-treatment |
Citations (3)
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|---|---|---|---|---|
| JPS5713670A (en) * | 1980-06-26 | 1982-01-23 | Japan Storage Battery Co Ltd | Solid electrolyte battery |
| CN1461065A (en) * | 2003-06-05 | 2003-12-10 | 福建师范大学 | Preparation of material for modifying lighium vanadium oxide electrode and its application in cell |
| CN102709542A (en) * | 2012-05-25 | 2012-10-03 | 青岛乾运高科新材料股份有限公司 | Method for repairing oxygen defect in preparation process of spinel lithium manganate as lithium-ion cathode material |
-
2014
- 2014-02-21 CN CN201410060993.1A patent/CN103808860B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5713670A (en) * | 1980-06-26 | 1982-01-23 | Japan Storage Battery Co Ltd | Solid electrolyte battery |
| CN1461065A (en) * | 2003-06-05 | 2003-12-10 | 福建师范大学 | Preparation of material for modifying lighium vanadium oxide electrode and its application in cell |
| CN102709542A (en) * | 2012-05-25 | 2012-10-03 | 青岛乾运高科新材料股份有限公司 | Method for repairing oxygen defect in preparation process of spinel lithium manganate as lithium-ion cathode material |
Non-Patent Citations (2)
| Title |
|---|
| LIMEI YANG等: "Effect of consumption amount of lithium salt on the properties of LiFeP04/C cathode materials", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 496, 12 February 2010 (2010-02-12) * |
| 卢侠等: "锂电池基础科学问题(II)—电池材料缺陷化学", 《储能科学与技术》, vol. 2, no. 2, 31 March 2013 (2013-03-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124675A (en) * | 2016-06-13 | 2016-11-16 | 合肥国轩高科动力能源有限公司 | A kind of method of lithium battery electrolytes chromatograph test pre-treatment |
| CN106124675B (en) * | 2016-06-13 | 2019-07-19 | 合肥国轩高科动力能源有限公司 | A kind of method of lithium battery electrolytes chromatography test pre-treatment |
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|---|---|
| CN103808860B (en) | 2015-07-29 |
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Address after: 230000 Yaohai Industrial Zone, Hefei New District, Anhui, No. D weft Road, No. 7 Patentee after: Hefei Guoxuan High-Tech Power Energy Co., Ltd. Address before: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Patentee before: Hefei Guoxuan High-Tech Power Energy Co., Ltd. |