CN103274480A - Precursor of polynary positive electrode material for lithium ion battery, and preparation method thereof - Google Patents
Precursor of polynary positive electrode material for lithium ion battery, and preparation method thereof Download PDFInfo
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- CN103274480A CN103274480A CN2013102229612A CN201310222961A CN103274480A CN 103274480 A CN103274480 A CN 103274480A CN 2013102229612 A CN2013102229612 A CN 2013102229612A CN 201310222961 A CN201310222961 A CN 201310222961A CN 103274480 A CN103274480 A CN 103274480A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a precursor of a polynary positive electrode material for a lithium ion battery, and a preparation method thereof. The precursor comprises NixCo(1-x-y-z)MnyWz(OH)2 (0<x<0.3,0<y<0.3,0<z<0.1), wherein W represents one of Al , Mg, Ti, Sr, Zr and W. The preparation method comprises the following steps of preparing a mixed salt solution A according to proportions, parallel-flowing the salt solution A and ammonium sulfate according to a certain proportion into a reactor with pure water by using sodium hydroxide and ammonium sulfate as a complexing agent; stirring the solution in the reactor continuously; controlling temperature and pH value of the reaction; introducing slurry in the reactor into another container through an overflow port for ageing; filtering precipitate and drying. The precursor has high density, high sphericility and complete crystal structure. The precursor has simple synthesis process, low cost and controllable granularity, and can be industrialized easily.
Description
Technical field
The present invention relates to a kind of lithium-ion technology field, be specifically related to a kind of lithium ion battery polynary system positive electrode material presoma and preparation method thereof.
Background technology
Lithium ion battery has many good characteristics because of it, now has been widely used in the portable electric appts such as notebook computer, mobile telephone, digital camera, has expanded to fields such as electromobile, satellite space flight and has used; At present the battery that uses because of the cost height, big for environment pollution, capacity is low, security is not high and work-ing life is not long, is difficult to satisfy people's daily use.
Summary of the invention
Goal of the invention: the objective of the invention is in order to remedy the deficiencies in the prior art, high lithium ion battery polynary system positive electrode material presoma of a kind of voltage high security and preparation method thereof is provided.
Technical scheme: a kind of lithium ion battery polynary system positive electrode material presoma, described component is NixCo(1-x-y-z) MnyWz(OH)
2(0＜x＜0.3,0＜y＜0.3,0＜z＜0.1), wherein W is a kind of in Al, Mg, Ti, Sr, Zr or the W element.
As optimization, described additive is one or more the mixture in vitriol, nitrate or the muriate of Al, Mg, Ti, Sr, Zr, W.
As optimization, a kind of lithium ion battery polynary system positive electrode material presoma and preparation method thereof: may further comprise the steps:
(a). Ni:Co:Mn:W=x:(1-x-y-z in molar ratio): y:z is mixed with mixing salt solution A, makes that concentration of metal ions is 0.4 ~ 2mol/L in this salts solution;
(b). be complexing agent with sodium hydroxide and ammonium sulfate, concentration of sodium hydroxide solution is 6 ~ 12mol/L, and ammonium sulfate is 10% aqueous solution;
(c). with salts solution A, ammonium sulfate by a certain percentage and flow in the reactor that fills pure water, solution constantly stirs in the reactor, fixing salts solution flow velocity, the control temperature of reaction is 40 ~ 50 ℃, the solution pH value is the add-on of 10.0 ~ 12.0 control sodium hydroxide in the reactor by controlling, slurry flows in another container by overflow port in the reactor, and ageing got final product in 4 ~ 10 hours;
(d). filter c item precipitation, and with 4 ~ 10 times of pure water washing leaching cakes of filter cake 3 ~ 6 times, instruct the wash water specific conductivity to get final product less than 200 μ S/cm, filtration then, filter cake dried by the fire in 80 ~ 120 ℃ baking oven 3 ~ 10 hours, can dry.
As optimization, described Ni, Co, Mn, W salt are one or several in muriate, vitriol, the nitrate.
As optimization, described complexing agent is one or several in ammonium sulfate, EDTA, the citric acid.
As optimization, described alkaline precipitating agent is one or several in sodium hydroxide, the potassium hydroxide.
Beneficial effect: presoma of the present invention is that a kind of high-density, high sphericity, crystalline structure are complete, and this presoma synthesis technique is simple, cost is low, granularity can be controlled, and industrialization easily.
Embodiment
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1:
A kind of lithium ion battery polynary system positive electrode material presoma and preparation method thereof: may further comprise the steps: Ni:Co:Mn:Al=0.1:0.75:0.1:0.05 is mixed with mixing salt solution A in molar ratio, makes that concentration of metal ions is 0.4mol/L in this salts solution; Be complexing agent with sodium hydroxide and ammonium sulfate, concentration of sodium hydroxide solution is 6mol/L, and ammonium sulfate is 10% aqueous solution; With salts solution A, ammonium sulfate by a certain percentage and flow in the reactor that fills pure water, solution constantly stirs in the reactor, fixing salts solution flow velocity, the control temperature of reaction is 40 ℃, the solution pH value is the add-on of 10.0 control sodium hydroxide in the reactor by controlling, slurry flows in another container by overflow port in the reactor, and ageing got final product in 4 hours; Filtering-depositing, and with 4 times of pure water washing leaching cakes of filter cake 3 times, instruct the wash water specific conductivity to get final product less than 200 μ S/cm, filtering then, filter cake dried by the fire 3 hours in 80 ℃ baking oven, can dry.
Embodiment 2:
A kind of lithium ion battery polynary system positive electrode material presoma and preparation method thereof: may further comprise the steps: Ni:Co:Mn:Al=0.2:0.55:0.2:0.05 is mixed with mixing salt solution A in molar ratio, makes that concentration of metal ions is 1.2mol/L in this salts solution; Be complexing agent with sodium hydroxide and ammonium sulfate, concentration of sodium hydroxide solution is 8mol/L, and ammonium sulfate is 10% aqueous solution; With salts solution A, ammonium sulfate by a certain percentage and flow in the reactor that fills pure water, solution constantly stirs in the reactor, fixing salts solution flow velocity, the control temperature of reaction is 45 ℃, the solution pH value is the add-on of 11.0 control sodium hydroxide in the reactor by controlling, slurry flows in another container by overflow port in the reactor, and ageing got final product in 8 hours; Filter c item precipitation, and with 7 times of pure water washing leaching cakes of filter cake 5 times, instruct the wash water specific conductivity to get final product less than 200 μ S/cm, filtration then, filter cake dried by the fire 6 hours in 100 ℃ baking oven, can dry.
Embodiment 3:
A kind of lithium ion battery polynary system positive electrode material presoma and preparation method thereof: may further comprise the steps: Ni:Co:Mn:Al=0.25:0.45:0.25:0.05 is mixed with mixing salt solution A in molar ratio, makes that concentration of metal ions is 2mol/L in this salts solution; Be complexing agent with sodium hydroxide and ammonium sulfate, concentration of sodium hydroxide solution is 12mol/L, and ammonium sulfate is 10% aqueous solution; With salts solution A, ammonium sulfate by a certain percentage and flow in the reactor that fills pure water, solution constantly stirs in the reactor, fixing salts solution flow velocity, the control temperature of reaction is 50 ℃, the solution pH value is the add-on of 12.0 control sodium hydroxide in the reactor by controlling, slurry flows in another container by overflow port in the reactor, and ageing got final product in 10 hours; Filter c item precipitation, and with 10 times of pure water washing leaching cakes of filter cake 6 times, instruct the wash water specific conductivity to get final product less than 200 μ S/cm, filtration then, filter cake dried by the fire 10 hours in 120 ℃ baking oven, can dry.
Claims (6)
1. lithium ion battery polynary system positive electrode material presoma, it is characterized in that: described component is NixCo(1-x-y-z) MnyWz(OH)
2(0＜x＜0.3,0＜y＜0.3,0＜z＜0.1), wherein W is a kind of in Al, Mg, Ti, Sr, Zr or the W element.
2. a kind of lithium ion battery polynary system positive electrode material presoma according to claim 1 is characterized in that: described additive is one or more the mixture in vitriol, nitrate or the muriate of Al, Mg, Ti, Sr, Zr, W.
3. a kind of lithium ion battery polynary system positive electrode material presoma according to claim 1 and preparation method thereof: it is characterized in that: may further comprise the steps:
(a). Ni:Co:Mn:W=x:(1-x-y-z in molar ratio): y:z is mixed with mixing salt solution A, makes that concentration of metal ions is 0.4 ~ 2mol/L in this salts solution;
(b). be complexing agent with sodium hydroxide and ammonium sulfate, concentration of sodium hydroxide solution is 6 ~ 12mol/L, and ammonium sulfate is 10% aqueous solution;
(c). with salts solution A, ammonium sulfate by a certain percentage and flow in the reactor that fills pure water, solution constantly stirs in the reactor, fixing salts solution flow velocity, the control temperature of reaction is 40 ~ 50 ℃, the pH value of solution value is the add-on of 10.0 ~ 12.0 control sodium hydroxide in the reactor by controlling, slurry flows in another container by overflow port in the reactor, and ageing got final product in 4 ~ 10 hours;
(d). filter c item precipitation, and with 4 ~ 10 times of pure water washing leaching cakes of filter cake 3 ~ 6 times, instruct the wash water specific conductivity to get final product less than 200 μ S/cm, filtration then, filter cake dried by the fire in 80 ~ 120 ℃ baking oven 3 ~ 10 hours, can dry.
4. a kind of lithium ion battery polynary system positive electrode material presoma according to claim 3 and preparation method thereof, it is characterized in that: described Ni, Co, Mn, W salt are one or several in muriate, vitriol, the nitrate.
5. a kind of lithium ion battery polynary system positive electrode material presoma according to claim 3 and preparation method thereof, it is characterized in that: described complexing agent is one or several in ammonium sulfate, EDTA, the citric acid.
6. a kind of lithium ion battery polynary system positive electrode material presoma according to claim 3 and preparation method thereof, it is characterized in that: described alkaline precipitating agent is one or several in sodium hydroxide, the potassium hydroxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109449435A (en) * | 2018-11-01 | 2019-03-08 | 广东佳纳能源科技有限公司 | The preparation method of semidefinite form positive electrode material precursor and positive electrode material precursor obtained, positive electrode, lithium ion battery and application |
| CN109950535A (en) * | 2019-03-20 | 2019-06-28 | 兰州金川新材料科技股份有限公司 | A method of filtrate secondary crystallization, which is worn, using hydroxide washing continuously synthesizes presoma |
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| CN101284683A (en) * | 2008-05-29 | 2008-10-15 | 金川集团有限公司 | Preparing method for precursor of lithium ionic cell positive material |
| CN101285197A (en) * | 2008-05-29 | 2008-10-15 | 金川集团有限公司 | Preparing method for precursor of lithium ionic cell positive material |
| CN101434417A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Dry preparation of battery grade spherical cobaltosic oxide particle |
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| CN102969505A (en) * | 2012-12-12 | 2013-03-13 | 南京大学 | LiFePO4 precursor hollow sphere and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109449435A (en) * | 2018-11-01 | 2019-03-08 | 广东佳纳能源科技有限公司 | The preparation method of semidefinite form positive electrode material precursor and positive electrode material precursor obtained, positive electrode, lithium ion battery and application |
| CN109950535A (en) * | 2019-03-20 | 2019-06-28 | 兰州金川新材料科技股份有限公司 | A method of filtrate secondary crystallization, which is worn, using hydroxide washing continuously synthesizes presoma |
| CN109950535B (en) * | 2019-03-20 | 2022-04-29 | 兰州金川新材料科技股份有限公司 | Method for continuously synthesizing precursor by washing filter material with hydroxide and secondary crystallization |
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Application publication date: 20130904 |