CN101777643A - Preparation method of anode material of Al2O3-cladding manganese-based laminated lithium battery - Google Patents
Preparation method of anode material of Al2O3-cladding manganese-based laminated lithium battery Download PDFInfo
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- CN101777643A CN101777643A CN201010018331A CN201010018331A CN101777643A CN 101777643 A CN101777643 A CN 101777643A CN 201010018331 A CN201010018331 A CN 201010018331A CN 201010018331 A CN201010018331 A CN 201010018331A CN 101777643 A CN101777643 A CN 101777643A
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Abstract
The invention relates to preparation of an anode material of a lithium battery, in particular to a preparation method of the anode material of an Al2O3-cladding manganese-based laminated lithium battery. The preparation method comprises the following steps of: preparing (Ni0.166Co0.166Mn0.688)(OH)2 precursor particles; preparing Li(Li0.20Ni0.133Co0.534)O2 with a laminated crystal structure by a high-temperature solid phase method; and enhancing the performance of a Li(Li0.20Ni0.133Co0.534)O2 particle product by Al2O3 cladding. The invention has the advantages of larger energy ratio of the product thereof than lithium cobaltoxide, low cost, good safety when the product is used as the anode material, long service life of the product, and higher charging/discharging specific capacity and cycle life as well as better safety of the particles of the Al2O3-cladding manganese-based laminated crystal structure.
Description
Technical field
The present invention relates to the preparation of the positive electrode of lithium battery, specifically is a kind of Al
2O
3The preparation method of cladding manganese-based laminated lithium battery positive electrode.
Background technology
Existing lithium battery, its positive electrode mainly contain LiFePO4, cobalt acid lithium etc.LiFePO4 is as anode material of lithium battery, and fail safe is good, but its energy is poor, can not satisfy the instructions for use of high-capacity lithium battery; Cobalt acid lithium is as anode material of lithium battery, has higher energy ratio, but because the cobalt element chemical property is active in the material, charging and discharging currents is excessive in its use, easily cause interior material structure to change and cause positive electrode puncture, and then cause short circuit, blast, thereby its fail safe is relatively poor.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of energy than big, cost is low, fail safe good, the Al of long service life
2O
3The preparation method of cladding manganese-based laminated lithium battery positive electrode.
Al of the present invention
2O
3The preparation method of cladding manganese-based laminated lithium battery positive electrode may further comprise the steps:
A. with NiSO4, CoSO4, MnSO4 example in molar ratio are made into the aqueous solution, cation molar concentration rate Ni: Co: Mn=0.133: 0.133: 0.534, the concentration summation of final all positive ions was 2.0 mol;
B. the metal ion solution that step a is obtained adds in the stirred reactor of nitrogen atmosphere, stirs and heating, and the control temperature is at 60 ℃;
C. the NaOH solution that with concentration is 2.0 mol splashes in the above-mentioned stirred reactor slowly, to produce (Ni
0.166Co
0.166Mn
0.688) (OH)
2The precipitation of particle splashes into speed 2～6 ml/min; When splashing into the NaOH aqueous solution, slowly splash into the ammoniacal liquor that concentration is 4.0 mol; Splash in NaOH solution and the ammoniacal liquor process, in the control stirred reactor pH value of reaction solution 11.0, NH
3+Concentration value in 0.36 mol.
D. with (Ni
0.166Co
0.166Mn
0.668) (OH)
2Granular product filters out and 100～150 ℃ of dryings, obtains graininess (Ni
0.166Co
0.166Mn
0.668) (OH)
2Presoma;
E. with graininess (Ni
0.166Co
0.166Mn
0.668) (OH)
2Presoma and LiOHH
2The O powder evenly mixes, and the mixing molar ratio is Li
+: other metal ion summations=1.3: 0.8;
F. the mixed-powder that step e is obtained places the sintering furnace of air atmosphere, earlier 450-520 ℃ of heating 4-7 hour, is warming up to 800-1000 ℃ then and can obtains layered crystal structure Li[Li in sintering 10-20 hour in air
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product;
G. with the resulting Li[Li in front
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product suspends and places the concentration in the stirred reactor is the Al (NO of 0.1 mol
3)
3Stir Al (NO in the solution
3)
3The total amount of solution is with last Al
2O
3Quality 3% the ratio that accounts for gross product calculate;
H. the ammoniacal liquor that with concentration is 0.2 mol slowly splashes in the stirred reactor, with the Al in the solution
3+Ion is all with Al (OH)
3Form be precipitated out;
I. the sediment of previous step filter out and in air 300 ℃ of heating, dryings can obtain Al
2O
3The Li[Li that coats
0.20Ni
0.133Co
0.133Mn
0.534] O
2The particle end product.
Positive electrode of the present invention is compared with traditional anode material of lithium battery and had the following advantages: 1, its energy compares greater than cobalt acid lithium, and owing to do not use cobalt material, its cost to reduce greatly; 2, fail safe is good, through experimental verification, does not have blast situation on fire under 100C rate charge-discharge electric current; 3, long service life, after testing, it is at first discharge capacity 220mAh/g, and 1000 times charge and discharge cycles is also possessed more than 90% of first capacity later on; 4, through Al
2O
3The particle of the manganese-base layered crystal structure that coats is compared with the material that does not coat, and it shows higher charging and discharging capacity and cycle life; In addition, dilation is better with the performance that prevents the material puncture in its charge and discharge process, and fail safe is better.
Embodiment
Positive electrode of the present invention obtains by the step of following examples:
One, (Ni
0.166Co
0.166Mn
0.688) (OH)
2The preparation of granular precursor.
1). with NiSO4, CoSO4, MnSO4 example in molar ratio are made into the aqueous solution, cation molar concentration rate Ni: Co: Mn=0.133: 0.133: 0.534, the concentration summation of final all positive ions was 2.0 mol.
2). NaOH is made into the aqueous solution of 2.0 mol
3). compound concentration is the ammoniacal liquor (NH of 4.0 mol
4OH)
4). get in the stirred reactor of the 2.0 liters of metal ion solutions that disposed adding nitrogen atmospheres, the blender mixing speed is 1000rpm, and heating and temperature are controlled at 60 ℃.
5). with total amount is that the NaOH solution that 4.2 liters of concentration are 2.0 mol splashes in the blender slowly, to produce (Ni
0.166Co
0.166Mn
0.688) (OH)
2The precipitation of particle, whole splashing into the about 12-40 of process need hour; When splashing into the NaOH aqueous solution, slowly splash into the ammoniacal liquor that concentration is 4.0 mol, because ammoniacal liquor just is used for doing chelating agent, not consumptive raw material, so the speed that ammoniacal liquor splashes into is slow more originally because of this.
6). splash into NaOH solution and ammoniacal liquor and control with pH meter and ammonium ion densimeter, in entire reaction course, the pH value of reaction solution is controlled at 11.0, NH in the blender
3+Concentration be controlled at 0.36 mol.
8). after reaction finishes, the total amount that precipitates is about 4.0 moles (Ni
0.166Co
0.166Mn
0.668) (OH)
2Granular product filters out and is dry about 110 ℃, the graininess (Ni that obtains
0.166Co
0.166Mn
0.668) (OH)
2The about 5 μ m of presoma diameter.
Two, high temperature solid-state method prepares layered crystal structure Li[Li
0.20Ni
0.133Co
0.133Mn
0.534] O
2
1). with front resulting granules shape (Ni
0.166Co
0.166Mn
0.668) (OH)
2Presoma and LiOHH
2The O powder evenly mixes, and the mixing molar ratio is Li
+: other metal ion summations=1.3: 0.8.Attention the ratio here is greater than Li[Li
0.20Ni
0.133Co
0.133Mn
0.534] O
2In theoretical value (1.2: 0.8).Using excessive lithium, is because the sub-fraction lithium can vapor away in sintering process.
2). top mixed-powder is placed the sintering furnace of air atmosphere, earlier 480 ℃ of heating 5 hours, be warming up to then 950 ℃ in air sintering can obtain having the Li[Li of layered crystal structure in 15 hours
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product.
Three, pass through Al
2O
3Coating increases Li[Li
0.20Ni
0.133Co
0.133Mn
0.534] O
2The performance of granular product
1). with the resulting Li[Li in front
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product is suspended in the Al (NO that the concentration that places stirred reactor is 0.1 mol
3)
3In the solution, mixing speed is 1000rpm.Al (NO
3)
3The total amount of solution need be used last Al
2O
3Quality 3% the ratio that accounts for gross product calculate.
2). with concentration is that the ammoniacal liquor of 0.2 mol slowly splashes in (process was above 5 hours) stirred reactor, with the Al in the solution
3+Ion is all with Al (OH)
3Form be precipitated out.
3). top mixed sediment filtered out and in air 300 ℃ of heating can obtain Al in 4 hours
2O
3The Li[Li that coats
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product.Final Al
2O
3Quality account for about 3% of gross product.
Claims (1)
1. Al
2O
3The preparation method of cladding manganese-based laminated lithium battery positive electrode is characterized in that: may further comprise the steps,
A. with NiSO4, CoSO4, MnSO4 example in molar ratio are made into the aqueous solution, cation molar concentration rate Ni: Co: Mn=0.133: 0.133: 0.534, the concentration summation of final all positive ions was 2.0 mol;
B. the metal ion solution that step a is obtained adds in the stirred reactor of nitrogen atmosphere, stirs and heating, and the control temperature is at 60 ℃;
C. the Na0H solution that with concentration is 2.0 mol splashes in the above-mentioned stirred reactor slowly, to produce (Ni
0.166Co
0.166Mn
0.688) (OH)
2The precipitation of particle splashes into speed 2～6 ml/min; When splashing into the NaOH aqueous solution, slowly splash into the ammoniacal liquor that concentration is 4.0 mol; Splash in NaOH solution and the ammoniacal liquor process, in the control stirred reactor pH value of reaction solution 11.0, NH
3+Concentration value in 0.36 mol.
D. with (Ni
0.166Co
0.166Mn
0.668) (OH)
2Granular product filters out and 100～150 ℃ of dryings, obtains graininess (Ni
0.166Co
0.166Mn
0.668) (OH)
2Presoma;
E. with graininess (Ni
0.166Co
0.166Mn
0.668) (OH)
2Presoma and LiOHH
2The O powder evenly mixes, and the mixing molar ratio is Li
+: other metal ion summations=1.3: 0.8;
F. the mixed-powder that step e is obtained places the sintering furnace of air atmosphere, earlier 450-520 ℃ of heating 4-7 hour, is warming up to 800-1000 ℃ then and can obtains layered crystal structure Li[Li in sintering 10-20 hour in air
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product;
G. with the resulting Li[Li in front
0.20Ni
0.133Co
0.133Mn
0.534] O
2Granular product suspends and places the concentration in the stirred reactor is the Al (NO of 0.1 mol
3)
3Stir Al (NO in the solution
3)
3The total amount of solution is with last Al
2O
3Quality 3% the ratio that accounts for gross product calculate;
H. the ammoniacal liquor that with concentration is 0.2 mol slowly splashes in the stirred reactor, with the Al in the solution
3+Ion is all with Al (OH)
3Form be precipitated out;
I. the sediment of previous step filter out and in air 300 ℃ of heating, dryings can obtain Al
2O
3The Li[Li that coats
0.20Ni
0.133Co
0.133Mn
0.534] O
2The particle end product.
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|---|---|---|---|
| CN201010018331A CN101777643A (en) | 2010-01-14 | 2010-01-14 | Preparation method of anode material of Al2O3-cladding manganese-based laminated lithium battery |
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|---|---|---|---|
| CN201010018331A CN101777643A (en) | 2010-01-14 | 2010-01-14 | Preparation method of anode material of Al2O3-cladding manganese-based laminated lithium battery |
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|---|---|
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Family
ID=42514032
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102169982A (en) * | 2011-04-02 | 2011-08-31 | 江苏科捷锂电池有限公司 | Preparation method of positive electrode material of lithium battery with manganese-based layered crystal structure |
| CN102169981A (en) * | 2011-04-02 | 2011-08-31 | 江苏科捷锂电池有限公司 | Lithium cell cathode material with manganese-based laminated crystal structure and preparation method thereof |
| CN102324514A (en) * | 2011-09-21 | 2012-01-18 | 江西博能新材料有限公司 | A kind of lithium ion battery tertiary cathode material is with the preparation method of presoma |
| CN102364725A (en) * | 2011-10-17 | 2012-02-29 | 江苏科捷锂电池有限公司 | Method for preparing manganese-based layered crystal structure positive electrode material of lithium battery |
| CN102810674A (en) * | 2012-08-14 | 2012-12-05 | 安徽亚兰德新能源材料股份有限公司 | Preparation method of Al-coated nickel-cobalt binary material |
| CN102983323A (en) * | 2012-12-19 | 2013-03-20 | 苏州大学 | Positive pole material of lithium ion secondary battery and preparation method of material |
| CN103107337A (en) * | 2012-04-01 | 2013-05-15 | 湖南大学 | Method for improving cycling stability of lithium ion battery anode material |
| CN103137962A (en) * | 2013-03-11 | 2013-06-05 | 佛山市邦普循环科技有限公司 | Method for preparing nickel-cobalt-manganese hydroxide |
| CN103274437A (en) * | 2013-06-21 | 2013-09-04 | 北京化工大学 | Three-dimensional flower-like layered double hydroxide and preparation method thereof |
| CN104577128A (en) * | 2013-10-10 | 2015-04-29 | 无锡星波能源科技有限公司 | Alumina coating method of lithium ion battery positive electrode material |
| CN104953172A (en) * | 2015-07-24 | 2015-09-30 | 上海中聚佳华电池科技有限公司 | Sodium-ion battery cathode materials, preparation method of sodium-ion battery cathode materials, and sodium-ion batteries |
| CN105870402A (en) * | 2015-01-22 | 2016-08-17 | 辅仁大学学校财团法人辅仁大学 | Metal gradient doped lithium battery positive electrode material |
| CN106252730A (en) * | 2016-08-04 | 2016-12-21 | 陈永林 | A kind of preparation method of energy-density lithium ion battery |
| CN106277074A (en) * | 2016-08-15 | 2017-01-04 | 北方奥钛纳米技术有限公司 | A kind of preparation method of high pressure ternary material |
| CN107768627A (en) * | 2017-10-03 | 2018-03-06 | 长沙仲善新能源科技有限公司 | A kind of high-temperature stability nickle cobalt lithium manganate combination electrode and preparation method and application |
| CN109167055A (en) * | 2018-08-06 | 2019-01-08 | 西北大学 | The method and system that a kind of pair of ternary material is coated |
| CN109807692A (en) * | 2017-11-21 | 2019-05-28 | 中芯国际集成电路制造(上海)有限公司 | A kind of lapping liquid, the method and chemical and mechanical grinding method for preparing lapping liquid |
| CN113677627A (en) * | 2019-04-12 | 2021-11-19 | 住友化学株式会社 | Lithium composite metal oxide powder and positive electrode active material for lithium secondary battery |
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Cited By (23)
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| CN102169981A (en) * | 2011-04-02 | 2011-08-31 | 江苏科捷锂电池有限公司 | Lithium cell cathode material with manganese-based laminated crystal structure and preparation method thereof |
| CN102169981B (en) * | 2011-04-02 | 2013-04-10 | 江苏科捷锂电池有限公司 | Lithium cell cathode material with manganese-based laminated crystal structure and preparation method thereof |
| CN102169982B (en) * | 2011-04-02 | 2013-04-24 | 江苏科捷锂电池有限公司 | Preparation method of positive electrode material of lithium battery with manganese-based layered crystal structure |
| CN102169982A (en) * | 2011-04-02 | 2011-08-31 | 江苏科捷锂电池有限公司 | Preparation method of positive electrode material of lithium battery with manganese-based layered crystal structure |
| CN102324514A (en) * | 2011-09-21 | 2012-01-18 | 江西博能新材料有限公司 | A kind of lithium ion battery tertiary cathode material is with the preparation method of presoma |
| CN102324514B (en) * | 2011-09-21 | 2013-09-25 | 江西博能新材料有限公司 | Preparation method of precursor for ternary anode material of lithium ion battery |
| CN102364725A (en) * | 2011-10-17 | 2012-02-29 | 江苏科捷锂电池有限公司 | Method for preparing manganese-based layered crystal structure positive electrode material of lithium battery |
| CN103107337A (en) * | 2012-04-01 | 2013-05-15 | 湖南大学 | Method for improving cycling stability of lithium ion battery anode material |
| CN102810674A (en) * | 2012-08-14 | 2012-12-05 | 安徽亚兰德新能源材料股份有限公司 | Preparation method of Al-coated nickel-cobalt binary material |
| CN102983323B (en) * | 2012-12-19 | 2016-08-03 | 苏州大学 | Lithium ion secondary battery anode material and preparation method thereof |
| CN102983323A (en) * | 2012-12-19 | 2013-03-20 | 苏州大学 | Positive pole material of lithium ion secondary battery and preparation method of material |
| CN103137962A (en) * | 2013-03-11 | 2013-06-05 | 佛山市邦普循环科技有限公司 | Method for preparing nickel-cobalt-manganese hydroxide |
| CN103274437A (en) * | 2013-06-21 | 2013-09-04 | 北京化工大学 | Three-dimensional flower-like layered double hydroxide and preparation method thereof |
| CN104577128A (en) * | 2013-10-10 | 2015-04-29 | 无锡星波能源科技有限公司 | Alumina coating method of lithium ion battery positive electrode material |
| CN105870402A (en) * | 2015-01-22 | 2016-08-17 | 辅仁大学学校财团法人辅仁大学 | Metal gradient doped lithium battery positive electrode material |
| CN104953172A (en) * | 2015-07-24 | 2015-09-30 | 上海中聚佳华电池科技有限公司 | Sodium-ion battery cathode materials, preparation method of sodium-ion battery cathode materials, and sodium-ion batteries |
| CN106252730A (en) * | 2016-08-04 | 2016-12-21 | 陈永林 | A kind of preparation method of energy-density lithium ion battery |
| CN106277074A (en) * | 2016-08-15 | 2017-01-04 | 北方奥钛纳米技术有限公司 | A kind of preparation method of high pressure ternary material |
| CN107768627A (en) * | 2017-10-03 | 2018-03-06 | 长沙仲善新能源科技有限公司 | A kind of high-temperature stability nickle cobalt lithium manganate combination electrode and preparation method and application |
| CN109807692A (en) * | 2017-11-21 | 2019-05-28 | 中芯国际集成电路制造(上海)有限公司 | A kind of lapping liquid, the method and chemical and mechanical grinding method for preparing lapping liquid |
| CN109167055A (en) * | 2018-08-06 | 2019-01-08 | 西北大学 | The method and system that a kind of pair of ternary material is coated |
| CN113677627A (en) * | 2019-04-12 | 2021-11-19 | 住友化学株式会社 | Lithium composite metal oxide powder and positive electrode active material for lithium secondary battery |
| CN113677627B (en) * | 2019-04-12 | 2023-11-14 | 住友化学株式会社 | Lithium composite metal oxide powder and positive electrode active material for lithium secondary battery |
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Application publication date: 20100714 |