CN102867951A - Preparation method of cell positive electrode material LiNi0.5Mn1.5O4 - Google Patents
Preparation method of cell positive electrode material LiNi0.5Mn1.5O4 Download PDFInfo
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- CN102867951A CN102867951A CN2012103745619A CN201210374561A CN102867951A CN 102867951 A CN102867951 A CN 102867951A CN 2012103745619 A CN2012103745619 A CN 2012103745619A CN 201210374561 A CN201210374561 A CN 201210374561A CN 102867951 A CN102867951 A CN 102867951A
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- nickel
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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
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Abstract
The invention discloses a preparation method of a cell positive electrode material LiNi0.5Mn1.5O4. The preparation method includes following steps: a, dissolving nickel nitrate, manganese nitrate and lithium nitrate into deionized water to form solution according to a mole ratio of 0.5:1.5:1.05-1.2, adding moderate NH4NO3 into the solution, and stirring the solution uniformly; b, ultrasonically spraying and pyrolyzing the solution prepared in the step a with an ultrasonic frequency of 1.8-2 MHz (megahertz) and a pyrolysis temperature of 950-990 DEG C to obtain powder; and c, calcining the powder obtained in the step b for 5-12 hours under the condition of 700-900 DEG C to obtain a finished product. Nitrates of nickel, manganese and lithium serve as raw materials and the deionized water serves as solvent, so that the raw materials are mixed completely in a molecular state, and can be mixed more uniformly by ultrasound spray pyrolysis, and preparation steps are simplified. The preparation method of the cell positive electrode material LiNi0.5Mn1.5O4 is simple, and the raw materials are uniform in mixing.
Description
Technical field
The invention belongs to the battery material field, be specifically related to cell positive material LiNi
0.5Mn
1.5O
4The preparation method.
Background technology
The nickel LiMn2O4 is mainly spinel-type nickel LiMn2O4, and chemical formula can be expressed as LiNi
0.5Mn
1.5O
4Although, have now much about preparation LiNi
0.5Mn
1.5O
4Method, but these researchs mostly are in laboratory stage, also do not have in the market the formal production on the essential meaning.Main cause is that the nickel LiMn2O4 belongs to the composite oxides of three kinds of metallic elements (lithium, nickel, manganese), is difficult to realize the even mixing of each material composition on synthesizing with conventional method.
Application number is that 201110186663.3 Chinese patent discloses a kind of synthetic high-tap density spinel LiNi
0.5Mn
1.5O
4Method, it adopts lithium salts, nickel salt, manganese salt, the auxiliary agent of special ratios to be dissolved in the deionized water, stir and heat and make it to form collosol intermixture, colloidal sol is being obtained Primary product under the specified temp after the special time pre-burning, Primary product obtaining final products under the specified temp after the formal calcining of special time high temperature, is needed to add a large amount of auxiliary agents in the method, particularly when auxiliary agent is selected urea, because the carbon component that induced one, the chemical property of material is had a negative impact.
Summary of the invention
The purpose of this invention is to provide a kind of cell positive material LiNi
0.5Mn
1.5O
4The preparation method, the method can not introduced carbon component, solves the mixed uniformly problem that existing preparation method is difficult to realize raw material.
Technical scheme of the present invention is: cell positive material LiNi
0.5Mn
1.5O
4The preparation method, it is characterized in that: step is as follows:
A, be that 0.5 ︰, 1.5 ︰ 1.05～1.1 are dissolved into and form solution in the deionized water with nickel nitrate, manganese nitrate, lithium nitrate according to mol ratio, in solution, add an amount of NH
4NO
3, stir;
B, the solution that step a is prepared carry out ultrasonic spray pyrolysis, supersonic frequency 1.8～2MHz, and 950～990 ℃ of pyrolysis temperatures obtain powder;
C, the powder that step b is obtained are calcined under 700～900 ℃ of conditions and were got product in 5～12 hours.
Preferably, among the preparation method of battery anode material nickel LiMn2O4 of the present invention, the NH that adds among the step a
4NO
3With the mol ratio of nickel nitrate be 0.005～0.05 ︰ 1.
Preferably, among the preparation method of battery anode material nickel LiMn2O4 of the present invention, the supersonic frequency described in the step b is 1.9MHz, and pyrolysis temperature is 980 ℃.
Preferably, among the preparation method of battery anode material nickel LiMn2O4 of the present invention, the calcining heat described in the step c is 890 ℃, and calcination time is 8 hours.
The present invention compared with prior art has following advantage:
1, to adopt the nitrate of nickel, manganese, lithium be raw material in the present invention, take deionized water as solvent, thereby raw material mixed with molecular state, and it is more even that ultrasonic spray pyrolysis is mixed to get raw material, and simplified preparation process.
2, the mol ratio of lithium nitrate is slightly larger than 1 in the raw material, can compensate the loss of lithium salts in the high-temperature sintering process.
3, in solution, add an amount of NH
4NO
3, carbonaceous component not in the raw material; Because NH
4 +Existence, in the drop thermal decomposition process, easier formation nucleation crystal seed.
4, the present invention has that raw material mixes, the simple characteristics of preparation method.
Embodiment
Embodiment 1
Cell positive material LiNi
0.5Mn
1.5O
4Preparation,
A, be that 0.5 ︰, 1.5 ︰ 1.05 are dissolved into and form solution in the deionized water with nickel nitrate, manganese nitrate, lithium nitrate according to mol ratio, in solution, add NH
4NO
3, NH
4NO
3With the mol ratio of nickel nitrate be 0.005 ︰ 1, stir;
B, the solution that step a is prepared carry out ultrasonic spray pyrolysis, supersonic frequency 1.8MHz, and 950 ℃ of pyrolysis temperatures obtain powder;
C, the powder that step b is obtained are calcined under 700 ℃ of conditions and were got product in 12 hours.
Embodiment 2
Cell positive material LiNi
0.5Mn
1.5O
4The preparation method,
A, be that 0.5 ︰, 1.5 ︰ 1.2 are dissolved into and form solution in the deionized water with nickel nitrate, manganese nitrate, lithium nitrate according to mol ratio, in solution, add NH
4NO
3, NH
4NO
3With the mol ratio of nickel nitrate be 0.05 ︰ 1, stir;
B, the solution that step a is prepared carry out ultrasonic spray pyrolysis, supersonic frequency 2MHz, and 990 ℃ of pyrolysis temperatures obtain powder;
C, the powder that step b is obtained are calcined under 900 ℃ of conditions and were got product in 5 hours.
Embodiment 3
Cell positive material LiNi
0.5Mn
1.5O
4The preparation method,
A, be that 0.5 ︰, 1.5 ︰ 1.1 are dissolved into and form solution in the deionized water with nickel nitrate, manganese nitrate, lithium nitrate according to mol ratio, in solution, add NH
4NO
3, NH
4NO
3With the mol ratio of nickel nitrate be 0.025 ︰ 1, stir;
B, the solution that step a is prepared carry out ultrasonic spray pyrolysis, supersonic frequency 1.9MHz, and 980 ℃ of pyrolysis temperatures obtain powder;
C, the powder that step b is obtained are calcined under 890 ℃ of conditions and were got product in 8 hours.
Performance Detection
LiNi of the present invention
0.5Mn
1.5O
4After testing, actual capacity reaches 132mAh/g, apparently higher than the LiNi of existing additive method preparation
0.5Mn
1.5O
4, can be widely used in the manufacturing electrokinetic cell.
Claims (4)
1. cell positive material LiNi
0.5Mn
1.5O
4The preparation method, it is characterized in that: step is as follows:
A, be that 0.5 ︰, 1.5 ︰ 1.05～1.1 are dissolved into and form solution in the deionized water with nickel nitrate, manganese nitrate, lithium nitrate according to mol ratio, in solution, add an amount of NH
4NO
3, stir;
B, the solution that step a is prepared carry out ultrasonic spray pyrolysis, supersonic frequency 1.8～2MHz, and 950～990 ℃ of pyrolysis temperatures obtain powder;
C, the powder that step b is obtained are calcined under 700～900 ℃ of conditions and were got product in 5～12 hours.
2. cell positive material LiNi according to claim 1
0.5Mn
1.5O
4The preparation method, it is characterized in that: the NH that adds among the step a
4NO
3With the mol ratio of nickel nitrate be 0.005～0.05 ︰ 1.
3. cell positive material LiNi according to claim 2
0.5Mn
1.5O
4The preparation method, it is characterized in that: the supersonic frequency described in the step b is 1.9MHz, pyrolysis temperature is 980 ℃.
4. cell positive material LiNi according to claim 3
0.5Mn
1.5O
4The preparation method, it is characterized in that: the calcining heat described in the step c is 890 ℃, calcination time is 8 hours.
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|---|---|---|---|
| CN2012103745619A CN102867951A (en) | 2012-10-08 | 2012-10-08 | Preparation method of cell positive electrode material LiNi0.5Mn1.5O4 |
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|---|---|---|---|
| CN2012103745619A CN102867951A (en) | 2012-10-08 | 2012-10-08 | Preparation method of cell positive electrode material LiNi0.5Mn1.5O4 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105932269A (en) * | 2016-05-24 | 2016-09-07 | 浙江美达瑞新材料科技有限公司 | Method for preparing positive electrode material for lithium ion cell by spraying, combusting and pyrolyzing |
| CN106328924A (en) * | 2015-07-03 | 2017-01-11 | 北京化工大学 | Carbon-coated lithium nickel manganese oxide positive electrode material with high potential and preparation method of positive electrode material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102709544A (en) * | 2012-06-06 | 2012-10-03 | 中南大学 | Nickel cobalt lithium manganate composite cathode material and preparation method of nickel cobalt lithium manganate composite cathode material |
-
2012
- 2012-10-08 CN CN2012103745619A patent/CN102867951A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102709544A (en) * | 2012-06-06 | 2012-10-03 | 中南大学 | Nickel cobalt lithium manganate composite cathode material and preparation method of nickel cobalt lithium manganate composite cathode material |
Non-Patent Citations (3)
| Title |
|---|
| S.-H.PARK，ET AL.: "Effects of synthesis condition on LiNi1/2Mn3/2O4 cathode material for prepared by ultrasonic spray pyrolysis method", 《SOLID STATE IONICS》, vol. 176, 31 December 2005 (2005-12-31), pages 481 - 486 * |
| 刘智敏等: "超声喷雾热分解制备锂离子电池正极材料LiNi1/3Co1/3Mn1/3O2及表征", 《无机材料学报》, vol. 22, no. 4, 31 July 2007 (2007-07-31), pages 637 - 641 * |
| 宋植彦等: "高电压镍锰酸锂动力电池正极材料研究进展", 《电源技术》, vol. 36, no. 9, 30 September 2012 (2012-09-30), pages 1405 - 1409 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328924A (en) * | 2015-07-03 | 2017-01-11 | 北京化工大学 | Carbon-coated lithium nickel manganese oxide positive electrode material with high potential and preparation method of positive electrode material |
| CN105932269A (en) * | 2016-05-24 | 2016-09-07 | 浙江美达瑞新材料科技有限公司 | Method for preparing positive electrode material for lithium ion cell by spraying, combusting and pyrolyzing |
| CN105932269B (en) * | 2016-05-24 | 2019-04-30 | 浙江美达瑞新材料科技有限公司 | The method that spray burning pyrolysis prepares anode material for lithium-ion batteries |
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