CN102881884A - Manufacturing process for Al-clad spherical nickel-cobalt-manganese ternary material - Google Patents
Manufacturing process for Al-clad spherical nickel-cobalt-manganese ternary material Download PDFInfo
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- CN102881884A CN102881884A CN2012103449742A CN201210344974A CN102881884A CN 102881884 A CN102881884 A CN 102881884A CN 2012103449742 A CN2012103449742 A CN 2012103449742A CN 201210344974 A CN201210344974 A CN 201210344974A CN 102881884 A CN102881884 A CN 102881884A
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Abstract
The invention relates to the field of the lithium-ion battery materials, and particularly relates to a manufacturing process for an Al-clad spherical nickel-cobalt-manganese ternary material. The process comprises the following steps: an Aluminum source is dissolved in an organic solvent; the organic solvent is sprayed into a spherical nickel-cobalt-manganese ternary material in a mixer; the spherical nickel-cobalt-manganese ternary material is sufficiently wetted and stirred uniformly under a stirring state, and is dried in a vacuum drying machine; and the spherical nickel is processed after being clad with the Al, and then is calcined again to obtain the Al-clad spherical nickel-cobalt-manganese ternary material. According to the manufacturing process for the Al-clad spherical nickel-cobalt-manganese ternary material, provided by the invention, the process flow is relatively simple, the cladding effect is more excellent, the tap density is higher, the material performance is excellent, and the stability and the consistency are better.
Description
Technical field
The present invention relates to the lithium ion battery material field, particularly the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al.
Background technology
The nickel-cobalt-manganese ternary material, to use comparatively general a kind of material in the anode material for lithium-ion batteries, prior art mainly coats the Al processing technology by dry method, the nickel-cobalt-manganese ternary material of the bag Al of this technique preparation, not only technique is comparatively loaded down with trivial details, A1 skewness in the while product, the product cycle performance is relatively poor and unstable, and tap density is lower.
Summary of the invention
In order to solve the technical problem that exists in the prior art, the object of the present invention is to provide the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al.
The technical solution used in the present invention is as follows:
The production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al is characterized in that, comprises the steps:
1., spherical nickel-cobalt manganese hydroxide preparation
Take pure water as end liquid, temperature rises to 40～80 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree and pH value at 80～180r/min;
Nickel cobalt manganese mixing salt solution and sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid, precipitation reaction occurs at 40～80 ℃, the solids in pulp amount of control reaction system, and keep above-mentioned basicity and pH value, the reaction feed liquid flows out into aging reactor continuously by reactor top overfall, then dry through washing press washing and vacuum drier, obtain spherical nickel-cobalt manganese hydroxide;
2., spherical nickel-cobalt manganese ternary material preparation
Spherical nickel-cobalt manganese hydroxide obtains spherical nickel-cobalt manganese ternary material through joining the lithium calcining;
3., spherical nickel-cobalt manganese ternary material surface bag Al processes
The aluminium source is dissolved in the organic solvent, then sprays on the spherical nickel-cobalt manganese ternary material in mixer, with spherical nickel-cobalt manganese ternary material abundant wetting stirring under stirring, then in vacuum drier, carry out drying;
4., coat the preparation of the spherical nickel-cobalt manganese ternary material of Al
Spherical nickel-cobalt manganese ternary material after the bag Al processing is calcined again, namely got the spherical nickel-cobalt manganese ternary material that coats Al.
Preferably, described step 1. in nickel salt be nickelous sulfate, nickel chloride or nickel nitrate; Cobalt salt is cobaltous sulfate, cobalt chloride or cobalt nitrate; Manganese salt is manganese sulfate, manganese chloride or manganese nitrate.
Further, the described step 1. middle total concentration of metal ions of nickel cobalt manganese mixing salt solution is 60～120g/l, and the concentration of sodium hydroxide solution is 15～30%, and ammonia concn is 10～25%.
Further, described step 1. middle slurry solid content is controlled at 150～300g/l, and the basicity of reaction system is controlled at 25～45g/l, and pH is controlled at 10.5～12.5.
Further, described step 1. in washing adopt 50～80 ℃ hot deionized water wash to pH be 7.5～9.5, baking temperature is 80～120 ℃.
Preferably, described step 2. middle lithium source is battery-level lithium carbonate, and the proportioning of battery-level lithium carbonate and spherical nickel-cobalt manganese hydroxide is 1～1.08: 1.
Further, described step 3. middle aluminium source is aluminium isopropoxide, and organic solvent is acetone or alcohol.
Further, described step 3. in baking temperature be 90～110 ℃.
Further, described step 2. middle calcining heat is 450～900 ℃, and step 4. middle calcining heat is 500～1000 ℃.
Comparatively perfect is that the tap density of the spherical nickel-cobalt manganese ternary material of the coating Al of preparation is 2.6～3.2g/cm
3, granularity is 5～25um.
The production technology of spherical nickel-cobalt manganese ternary material outer cladding Al of the present invention, technological process is relatively simple, the better effects if of coating, tap density is higher, the excellent performance of material, stability and consistency are better.
Description of drawings
For the ease of it will be appreciated by those skilled in the art that the present invention is further illustrated below in conjunction with accompanying drawing.
Fig. 1 is the scanning electron microscope (SEM) photograph of the spherical nickel-cobalt manganese hydroxide of the embodiment of the invention 1 preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph of the spherical nickel-cobalt manganese ternary material of the embodiment of the invention 1 preparation.
Fig. 3 is the scanning electron microscope (SEM) photograph of spherical nickel-cobalt manganese ternary material of the coating Al of the embodiment of the invention 1 preparation.
Embodiment
Embodiment 1
1., spherical nickel-cobalt manganese hydroxide preparation
Take pure water as end liquid, temperature rises to 75～80 ℃, and the control speed of agitator is at 160～180r/min, and adding ammoniacal liquor adjusting end liquid caustic soda degree is 25g/l, and end liquid pH value is 10.5.
Nickel cobalt manganese mixing salt solution and sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid, and nickel salt is nickelous sulfate, and cobalt salt is cobaltous sulfate, and manganese salt is manganese sulfate.The total concentration of metal ions of nickel cobalt manganese mixing salt solution is 60g/l, and the concentration of sodium hydroxide solution is 30% (quality percentage composition, lower same), and ammonia concn is 18% (volumn concentration, lower same).
Precipitation reaction occurs at 75～80 ℃, the solids in pulp amount of control reaction system is 260～300g/l, and keep above-mentioned basicity and pH value, the reaction feed liquid flows out into aging reactor continuously by reactor top overfall, then dry through washing press washing and vacuum drier, washing adopt 50 ℃ hot deionized water wash to pH be 8.9～9.5, baking temperature is 80 ℃, and then obtains spherical nickel-cobalt manganese hydroxide.See also Fig. 1, the sphericity of sample is better, and particle diameter distributes more concentrated.
2., spherical nickel-cobalt manganese ternary material preparation
Spherical nickel-cobalt manganese hydroxide is through joining the lithium calcining, and the lithium source is battery-level lithium carbonate, and the proportioning of battery-level lithium carbonate and spherical nickel-cobalt manganese hydroxide is 1: 1, and calcining heat is 900 ℃, thereby obtains spherical nickel-cobalt manganese ternary material.See also Fig. 2, it is more even that lithium distributes in material, and the tap density of material is higher.
3., spherical nickel-cobalt manganese ternary material surface bag Al processes
Aluminium isopropoxide is dissolved in the acetone, then spray on the spherical nickel-cobalt manganese ternary material in mixer, with spherical nickel-cobalt manganese ternary material abundant wetting stirring under stirring, then in vacuum drier, carry out drying, baking temperature is 90 ℃, acetone is reclaimed, and aluminium isopropoxide then is coated on spherical nickel-cobalt manganese ternary material surface uniformly.
4., coat the preparation of the spherical nickel-cobalt manganese ternary material of Al
Spherical nickel-cobalt manganese ternary material after the bag Al processing is calcined again, and calcining heat is 1000 ℃, namely gets the spherical nickel-cobalt manganese ternary material that coats Al.See also Fig. 3, Al is coated on the surface of ternary material nucleus uniformly.The product tap density is 2.6g/cm
3, granularity is 8～15um.
Embodiment 2
1., spherical nickel-cobalt manganese hydroxide preparation
Take pure water as end liquid, temperature rises to 55～60 ℃, and the control speed of agitator is at 110～130r/min, and adding ammoniacal liquor adjusting end liquid caustic soda degree is 35g/l, and end liquid pH value is 11.5.
Nickel cobalt manganese mixing salt solution and sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid, and nickel salt is nickel chloride, and cobalt salt is cobaltous sulfate, and manganese salt is manganese nitrate.The total concentration of metal ions of nickel cobalt manganese mixing salt solution is 120g/l, and the concentration of sodium hydroxide solution is 25%, and ammonia concn is 10%.
Precipitation reaction occurs at 55～60 ℃, the solids in pulp amount of control reaction system is 190～220g/l, and keep above-mentioned basicity and pH value, the reaction feed liquid flows out into aging reactor continuously by reactor top overfall, then dry through washing press washing and vacuum drier, washing adopt 70 ℃ hot deionized water wash to pH be 7.5～8.0, baking temperature is 120 ℃, and then obtains spherical nickel-cobalt manganese hydroxide.
2., spherical nickel-cobalt manganese ternary material preparation
Spherical nickel-cobalt manganese hydroxide is through joining the lithium calcining, and the lithium source is battery-level lithium carbonate, and the proportioning of battery-level lithium carbonate and spherical nickel-cobalt manganese hydroxide is 1.05: 1, and calcining heat is 750 ℃, thereby obtains spherical nickel-cobalt manganese ternary material.
3., spherical nickel-cobalt manganese ternary material surface bag Al processes
Aluminium isopropoxide is dissolved in the ethanol, then spray on the spherical nickel-cobalt manganese ternary material in mixer, with spherical nickel-cobalt manganese ternary material abundant wetting stirring under stirring, then in vacuum drier, carry out drying, baking temperature is 110 ℃, ethanol is reclaimed, and aluminium isopropoxide then is coated on spherical nickel-cobalt manganese ternary material surface uniformly.
4., coat the preparation of the spherical nickel-cobalt manganese ternary material of Al
Spherical nickel-cobalt manganese ternary material after the bag Al processing is calcined again, and calcining heat is 800 ℃, namely gets the spherical nickel-cobalt manganese ternary material that coats Al.The product tap density is 3.2g/cm
3, granularity is 15～25um.
Embodiment 3
1., spherical nickel-cobalt manganese hydroxide preparation
Take pure water as end liquid, temperature rises to 40～45 ℃, and the control speed of agitator is at 80～95r/min, and adding ammoniacal liquor adjusting end liquid caustic soda degree is 45g/l, and end liquid pH value is 12.5.
Nickel cobalt manganese mixing salt solution and sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid, and nickel salt is nickel chloride, and cobalt salt is cobalt chloride, and manganese salt is manganese chloride.The total concentration of metal ions of nickel cobalt manganese mixing salt solution is 90g/l, and the concentration of sodium hydroxide solution is 15%, and ammonia concn is 25%.
Precipitation reaction occurs at 40～45 ℃, the solids in pulp amount of control reaction system is 150～180g/l, and keep above-mentioned basicity and pH value, the reaction feed liquid flows out into aging reactor continuously by reactor top overfall, then dry through washing press washing and vacuum drier, washing adopt 80 ℃ hot deionized water wash to pH be 8.5～9.0, baking temperature is 100 ℃, and then obtains spherical nickel-cobalt manganese hydroxide.
2., spherical nickel-cobalt manganese ternary material preparation
Spherical nickel-cobalt manganese hydroxide is through joining the lithium calcining, and the lithium source is battery-level lithium carbonate, and the proportioning of battery-level lithium carbonate and spherical nickel-cobalt manganese hydroxide is 1.08: 1, and calcining heat is 450 ℃, thereby obtains spherical nickel-cobalt manganese ternary material.
3., spherical nickel-cobalt manganese ternary material surface bag Al processes
Aluminium isopropoxide is dissolved in the acetone, then spray on the spherical nickel-cobalt manganese ternary material in mixer, with spherical nickel-cobalt manganese ternary material abundant wetting stirring under stirring, then in vacuum drier, carry out drying, baking temperature is 100 ℃, acetone is reclaimed, and aluminium isopropoxide then is coated on spherical nickel-cobalt manganese ternary material surface uniformly.
4., coat the preparation of the spherical nickel-cobalt manganese ternary material of Al
Spherical nickel-cobalt manganese ternary material after the bag Al processing is calcined again, and calcining heat is 500 ℃, namely gets the spherical nickel-cobalt manganese ternary material that coats Al.The product tap density is 3g/cm
3, granularity is 5～15um.
Above content only is to structure example of the present invention and explanation; under those skilled in the art described specific embodiment is made various modifications or replenish or adopt similar mode to substitute; only otherwise depart from the structure of invention or do not surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (10)
1. the production technology of a spherical nickel-cobalt manganese ternary material outer cladding Al is characterized in that, comprises the steps:
1., spherical nickel-cobalt manganese hydroxide preparation
Take pure water as end liquid, temperature rises to 40～80 ℃, and the control speed of agitator adds ammoniacal liquor and regulates end liquid caustic soda degree and pH value at 80～180r/min;
Nickel cobalt manganese mixing salt solution and sodium hydroxide solution, the continuous also stream of ammoniacal liquor are pumped in the end liquid, precipitation reaction occurs at 40～80 ℃, the solids in pulp amount of control reaction system, and keep above-mentioned basicity and pH value, the reaction feed liquid flows out into aging reactor continuously by reactor top overfall, then dry through washing press washing and vacuum drier, obtain spherical nickel-cobalt manganese hydroxide;
2., spherical nickel-cobalt manganese ternary material preparation
Spherical nickel-cobalt manganese hydroxide obtains spherical nickel-cobalt manganese ternary material through joining the lithium calcining;
3., spherical nickel-cobalt manganese ternary material surface bag Al processes
The aluminium source is dissolved in the organic solvent, then sprays on the spherical nickel-cobalt manganese ternary material in mixer, with spherical nickel-cobalt manganese ternary material abundant wetting stirring under stirring, then in vacuum drier, carry out drying;
4., coat the preparation of the spherical nickel-cobalt manganese ternary material of Al
Spherical nickel-cobalt manganese ternary material after the bag Al processing is calcined again, namely got the spherical nickel-cobalt manganese ternary material that coats Al.
2. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1 is characterized in that, described step 1. middle nickel salt is nickelous sulfate, nickel chloride or nickel nitrate; Cobalt salt is cobaltous sulfate, cobalt chloride or cobalt nitrate; Manganese salt is manganese sulfate, manganese chloride or manganese nitrate.
3. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1, it is characterized in that, the described step 1. middle total concentration of metal ions of nickel cobalt manganese mixing salt solution is 60～120g/l, and the concentration of sodium hydroxide solution is 15～30%, and ammonia concn is 10～25%.
4. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1, it is characterized in that, described step 1. middle slurry solid content is controlled at 150～300g/l, and the basicity of reaction system is controlled at 25～45g/l, and pH is controlled at 10.5～12.5.
5. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1 is characterized in that, described step 1. in washing adopt 50～80 ℃ hot deionized water wash to pH be 7.5～9.5, baking temperature is 80～120 ℃.
6. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1 is characterized in that, described step 2. middle lithium source is battery-level lithium carbonate, and the proportioning of battery-level lithium carbonate and spherical nickel-cobalt manganese hydroxide is 1～1.08: 1.
7. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1 is characterized in that, described step 3. middle aluminium source is aluminium isopropoxide, and organic solvent is acetone or alcohol.
8. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding Al according to claim 1 is characterized in that, described step 3. middle baking temperature is 90～110 ℃.
9. the production technology of a kind of spherical nickel-cobalt manganese ternary material outer cladding A1 according to claim 1 is characterized in that, described step 2. middle calcining heat is 450～900 ℃, and step 4. middle calcining heat is 500～1000 ℃.
10. the production technology of each described a kind of spherical nickel-cobalt manganese ternary material outer cladding Al is characterized in that according to claim 1～9, and the tap density of the spherical nickel-cobalt manganese ternary material of the coating Al of preparation is 2.6～3.2g/cm
3, granularity is 5～25um.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103165878A (en) * | 2013-03-25 | 2013-06-19 | 安徽亚兰德新能源材料股份有限公司 | Preparation method of spherical nickel-manganese binary material |
| CN103872331A (en) * | 2014-03-24 | 2014-06-18 | 宁德新能源科技有限公司 | Aluminum cladding method for lithium ion positive electrode material |
| CN104332622A (en) * | 2014-09-05 | 2015-02-04 | 金驰能源材料有限公司 | Spheroidic nickel-cobalt-manganese precursor material with high purity and high crystallinity, and preparation method thereof |
| CN106340642A (en) * | 2016-11-30 | 2017-01-18 | 烟台卓能电池材料股份有限公司 | Long-circulation and high-capacity lithium battery positive electrode material and preparing method |
| CN108365183A (en) * | 2018-01-02 | 2018-08-03 | 乳源东阳光磁性材料有限公司 | Ternary material with surface coated with aluminum oxide and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103165878A (en) * | 2013-03-25 | 2013-06-19 | 安徽亚兰德新能源材料股份有限公司 | Preparation method of spherical nickel-manganese binary material |
| CN103165878B (en) * | 2013-03-25 | 2016-03-30 | 安徽亚兰德新能源材料股份有限公司 | A kind of preparation method of spherical nickel-manganese binary material |
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| CN104332622A (en) * | 2014-09-05 | 2015-02-04 | 金驰能源材料有限公司 | Spheroidic nickel-cobalt-manganese precursor material with high purity and high crystallinity, and preparation method thereof |
| CN106340642A (en) * | 2016-11-30 | 2017-01-18 | 烟台卓能电池材料股份有限公司 | Long-circulation and high-capacity lithium battery positive electrode material and preparing method |
| CN108365183A (en) * | 2018-01-02 | 2018-08-03 | 乳源东阳光磁性材料有限公司 | Ternary material with surface coated with aluminum oxide and preparation method thereof |
| CN108365183B (en) * | 2018-01-02 | 2020-10-20 | 乳源东阳光磁性材料有限公司 | Ternary material with surface coated with aluminum oxide and preparation method thereof |
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