CN101830451A - Microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate - Google Patents
Microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate Download PDFInfo
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- CN101830451A CN101830451A CN200910111252A CN200910111252A CN101830451A CN 101830451 A CN101830451 A CN 101830451A CN 200910111252 A CN200910111252 A CN 200910111252A CN 200910111252 A CN200910111252 A CN 200910111252A CN 101830451 A CN101830451 A CN 101830451A
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- phosphate
- lithium
- olivine
- ion battery
- aqueous solution
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title claims abstract description 10
- ILXAVRFGLBYNEJ-UHFFFAOYSA-K lithium;manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[O-]P([O-])([O-])=O ILXAVRFGLBYNEJ-UHFFFAOYSA-K 0.000 title claims abstract description 9
- 239000010450 olivine Substances 0.000 title claims description 8
- 229910052609 olivine Inorganic materials 0.000 title claims description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 42
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 11
- 239000010452 phosphate Substances 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 9
- 239000010405 anode material Substances 0.000 claims abstract description 8
- 150000002696 manganese Chemical class 0.000 claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- -1 phosphate anion Chemical class 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 4
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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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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- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明涉及一种橄榄石型锂离子电池正极材料磷酸锰锂的微波水热合成方法。该方法以氢氧化锂、锰盐、磷酸或磷酸盐为原料，配制一定浓度的溶液并通过控制氢氧化锂的量来调变溶液的pH，然后将配制的溶液进行微波水热，所得产物经过洗涤、过滤和干燥，得到橄榄石型LiMnPO4粉体。该方法工艺流程简单、反应条件温和、反应快速高效、制备成本低，同时所制备的材料纯度高，结构完善，结晶完好。
The invention relates to a microwave hydrothermal synthesis method of lithium manganese phosphate, an anode material of an olivine-type lithium ion battery. The method uses lithium hydroxide, manganese salt, phosphoric acid or phosphate as raw materials, prepares a solution with a certain concentration and adjusts the pH of the solution by controlling the amount of lithium hydroxide, and then microwaves the prepared solution. Wash, filter and dry to obtain olivine-type LiMnPO 4 powder. The method has the advantages of simple technological process, mild reaction conditions, fast and efficient reaction, low preparation cost, and meanwhile, the prepared material has high purity, perfect structure and intact crystallization.
Description
Technical field
The present invention relates to the synthetic method of lithium ion battery electrode material, especially microwave hydrothermal prepares the method for olivine type lithium ion battery positive pole material manganese lithium phosphate.
Background technology
Lithium ion battery have voltage height, specific energy big, have extended cycle life, self-discharge is little, memory-less effect, advantages of environment protection, therefore be widely used in handheld devices such as mobile phone, laptop computer, digital camera, in recent years, in fields such as electric vehicle and national defense industry, also demonstrate great application prospect.Stratiform lithium-containing transition metal oxide LiCoO
2Be most widely used positive electrode material in the present commercialization lithium ion battery, but the cobalt resource shortage, so LiCoO
2Cost an arm and a leg, finally make the price comparison height of lithium ion battery, it is imperative therefore to develop other cheap positive electrode materials.Olivine-type LiMnPO
4About voltage platform 4.1V, just in time with LiCoO
2Almost, and low price, therefore be the cheap beautiful positive electrode material of a kind of thing, be expected to be used for to substitute LiCoO
2At present, olivine-type LiMnPO
4The preparation method few, solid phase method, sol-gel method and traditional hydrothermal method are arranged.Solid phase method and sol-gel method all need high temperature sintering, and not only energy consumption is big, and particle size be not easy control, grow up easily under the high temperature, difficulty makes high electrochemical activity LiMnPO
4The tradition hydrothermal method can prepare complete crystallization and have the LiMnPO of electrochemical activity under very low temperature
4, but have slow, the shortcoming inhomogeneous, that the reaction times is long of being heated of rate of heating.Microwave-hydrothermal method is a kind of functional materials novel preparation method of developing in the world in recent years, compare with traditional hydrothermal method, the advantage that have that rate of heating is fast, reaction system is heated evenly, be quick on the draw, temperature of reaction is lower and the reaction times is shorter, the therefore controlled preparation of easier realization functional materials.
Summary of the invention
The present invention proposes a kind of microwave hydrothermal method for preparing olivine type lithium ion battery positive pole material manganese lithium phosphate.This method have reaction conditions gentleness, process simply rapidly and efficiently, characteristics that preparation cost is low.
The present invention relates to the microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate, detailed process is as follows:
1, under the room temperature, compound concentration is manganese salt and phosphoric acid or phosphatic mixed aqueous solution, the wherein mn ion of 0.1～2mol/L: phosphate anion (Mn: PO
4 3-) mol ratio be 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 0.1～3.5mol/L;
2, with lithium hydroxide aqueous solution and manganese salt and phosphoric acid or phosphatic aqueous solution, the pH value is controlled between 6～11;
3, above-mentioned mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 70～80%, temperature of reaction is 160～200 ℃, reaction times is 0.5～6 hour, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 5～12 hours at 100～150 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
Used manganese salt can be one or more in manganous nitrate, manganous sulfate, Manganous chloride tetrahydrate, the manganese acetate in the wherein above-mentioned preparation process; Phosphoric acid salt can be one or more in primary ammonium phosphate, ammonium hydrogen phosphate, ammonium phosphate, potassium primary phosphate, the SODIUM PHOSPHATE, MONOBASIC.
The present invention utilizes microwave hydrothermal to make reaction system be heated more fast evenly by control reactant concn, pH value of solution value and temperature of reaction and the time then, and the accelerated reaction process is with efficient production olivine-type anode material for lithium-ion batteries LiMnPO
4
Microwave-hydrothermal method of the present invention prepares olivine-type LiMnPO
4Has the advantage that technology is simple, reaction is quick, cost is low, simultaneously Zhi Bei olivine-type LiMnPO
4Structure is perfect, complete crystallization.
Description of drawings
Fig. 1 embodiment 1 prepared olivine-type LiMnPO
4XRD figure.
Fig. 2 embodiment 1 prepared olivine-type LiMnPO
4SEM figure.
Embodiment
Example 1: under the room temperature, compound concentration is manganous sulfate and primary ammonium phosphate mixed aqueous solution, the wherein mn ion of 0.5mol/L: phosphate anion (Mn: PO
4 3-) mol ratio be 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 1mol/L; Lithium hydroxide aqueous solution is joined in the mixed aqueous solution of manganous sulfate and primary ammonium phosphate, the pH of solution is～9; The gained mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 80%, temperature of reaction is 160 ℃, reaction times is 6 hours, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 12 hours at 150 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
Fig. 1 is prepared olivine-type LiMnPO
4XRD figure.Diagram shows that the material of preparation is single olivine-type LiMnPO
4, and have good degree of crystallinity.
Fig. 2 is prepared olivine-type LiMnPO
4SEM figure.Granular size is about 150～500 nanometers.
Example 2: under the room temperature, compound concentration is Manganous chloride tetrahydrate and phosphoric acid mixed aqueous solution, the wherein mn ion of 1mol/L: phosphate anion (Mn: PO
4 3-) mol ratio be 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 2mol/L; Lithium hydroxide aqueous solution is joined in the mixed aqueous solution of Manganous chloride tetrahydrate and phosphoric acid, the pH of solution is～10; The gained mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 80%, temperature of reaction is 180 ℃, reaction times is 6 hours, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 12 hours at 120 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
Example 3: under the room temperature, compound concentration is manganous sulfate and phosphoric acid mixed aqueous solution, the wherein mn ion of 1mol/L: phosphate anion (Mn: PO
4 3-) mol ratio be 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 3mol/L; Lithium hydroxide aqueous solution is joined in the mixed aqueous solution of manganous sulfate and phosphoric acid, the pH of solution is～10; The gained mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 75%, temperature of reaction is 200 ℃, reaction times is 3 hours, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 12 hours at 120 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
Example 4: under the room temperature, compound concentration is manganese acetate and potassium primary phosphate mixed aqueous solution, the wherein mn ion of 1mol/L: phosphate anion (Mn: PO
4 3-) mol ratio be 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 1.5mol/L; Lithium hydroxide aqueous solution is joined in the mixed aqueous solution of manganese acetate and potassium primary phosphate, the pH of solution is～9.5; The gained mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 75%, temperature of reaction is 200 ℃, reaction times is 5 hours, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 12 hours at 100 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
Claims (3)
1. the microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate, it is characterized in that: under the room temperature, compound concentration is manganese salt and phosphoric acid or phosphatic mixed aqueous solution, the wherein mn ion of 0.1～2mol/L: the mol ratio of phosphate anion is 1: 1; Compound concentration is the lithium hydroxide aqueous solution of 0.1～3.5mol/L; With lithium hydroxide aqueous solution and manganese salt and phosphoric acid or phosphatic aqueous solution, the pH value is controlled between 6～11; The gained mixed solution is carried out the microwave hydrothermal reaction, the compactedness of retort is 70～80%, temperature of reaction is 160～200 ℃, reaction times is 0.5～6 hour, with the reacted product water of microwave hydrothermal thorough washing, filtration, put into baking oven then and descended dry 5～12 hours at 100～150 ℃, gained then is olivine-type anode material for lithium-ion batteries LiMnPO
4
2. the microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate as claimed in claim 1, it is characterized in that: described manganese salt is one or more in manganous nitrate, manganous sulfate, Manganous chloride tetrahydrate or the manganese acetate.
3. the microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate as claimed in claim 1, it is characterized in that: described phosphoric acid salt can be one or more in primary ammonium phosphate, ammonium hydrogen phosphate, ammonium phosphate, potassium primary phosphate or the SODIUM PHOSPHATE, MONOBASIC.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102629687A (en) * | 2012-05-03 | 2012-08-08 | 哈尔滨工业大学 | A shape-controlled synthesis method of LiMnPO4 electrode material |
| CN103137969A (en) * | 2011-11-30 | 2013-06-05 | 现代自动车株式会社 | Cathode material for secondary battery and manufacturing method of the same |
| US20140056797A1 (en) * | 2011-04-28 | 2014-02-27 | Showa Denko K.K. | Method of producing cathode active material for lithium secondary battery |
| CN104167542A (en) * | 2014-08-06 | 2014-11-26 | 西南民族大学 | Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder |
| CN104393289A (en) * | 2014-10-21 | 2015-03-04 | 浙江大学 | Preparation method of lithium manganese phosphate nano-microsphere and product |
| CN104638262A (en) * | 2013-11-11 | 2015-05-20 | 新乡学院 | Novel preparation method of lithium-ion battery positive electrode material lithium manganese phosphate |
| CN105692578A (en) * | 2016-04-11 | 2016-06-22 | 福州大学 | Microwave hydrothermal synthesis method of olivine-type lithium ion battery anode material lithium manganese phosphate |
| CN106129403A (en) * | 2016-06-30 | 2016-11-16 | 贵州民族大学 | A kind of preparation method of LiFePO4 |
| WO2022089204A1 (en) * | 2020-10-26 | 2022-05-05 | 广东邦普循环科技有限公司 | Coated high nickel ternary material and preparation method therefor and use thereof |
| CN115448284A (en) * | 2022-09-30 | 2022-12-09 | 曲靖市德方纳米科技有限公司 | Method for preparing battery-grade lithium manganese phosphate composite material by using minerals and application thereof |
-
2009
- 2009-03-13 CN CN200910111252A patent/CN101830451A/en active Pending
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| A. VADIVEL MURUGAN ET AL.: "Dimensionally Modulated, Single-Crystalline LiMPO4 (M= Mn, Fe, Co, and Ni) with Nano-Thumblike Shapes for High-Power Energy Storage", 《INORGANIC CHEMISTRY》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140056797A1 (en) * | 2011-04-28 | 2014-02-27 | Showa Denko K.K. | Method of producing cathode active material for lithium secondary battery |
| US9745194B2 (en) * | 2011-04-28 | 2017-08-29 | Showa Denko K.K. | Method of producing cathode active material for lithium secondary battery |
| CN103137969A (en) * | 2011-11-30 | 2013-06-05 | 现代自动车株式会社 | Cathode material for secondary battery and manufacturing method of the same |
| CN103137969B (en) * | 2011-11-30 | 2017-07-18 | 现代自动车株式会社 | Cathode material for secondary battery and its manufacture method |
| CN102629687A (en) * | 2012-05-03 | 2012-08-08 | 哈尔滨工业大学 | A shape-controlled synthesis method of LiMnPO4 electrode material |
| CN102629687B (en) * | 2012-05-03 | 2014-06-11 | 哈尔滨工业大学 | A shape-controlled synthesis method of LiMnPO4 electrode material |
| CN104638262A (en) * | 2013-11-11 | 2015-05-20 | 新乡学院 | Novel preparation method of lithium-ion battery positive electrode material lithium manganese phosphate |
| CN104167542A (en) * | 2014-08-06 | 2014-11-26 | 西南民族大学 | Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder |
| CN104393289B (en) * | 2014-10-21 | 2016-08-24 | 浙江大学 | The preparation method of a kind of lithium manganese phosphate Nano microsphere and product |
| CN104393289A (en) * | 2014-10-21 | 2015-03-04 | 浙江大学 | Preparation method of lithium manganese phosphate nano-microsphere and product |
| CN105692578A (en) * | 2016-04-11 | 2016-06-22 | 福州大学 | Microwave hydrothermal synthesis method of olivine-type lithium ion battery anode material lithium manganese phosphate |
| CN106129403A (en) * | 2016-06-30 | 2016-11-16 | 贵州民族大学 | A kind of preparation method of LiFePO4 |
| WO2022089204A1 (en) * | 2020-10-26 | 2022-05-05 | 广东邦普循环科技有限公司 | Coated high nickel ternary material and preparation method therefor and use thereof |
| CN115448284A (en) * | 2022-09-30 | 2022-12-09 | 曲靖市德方纳米科技有限公司 | Method for preparing battery-grade lithium manganese phosphate composite material by using minerals and application thereof |
| CN115448284B (en) * | 2022-09-30 | 2024-01-30 | 曲靖市德方纳米科技有限公司 | Method for preparing battery-grade lithium manganese phosphate composite material by using minerals and application of battery-grade lithium manganese phosphate composite material |
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Application publication date: 20100915 |