CN105633348A - Preparation method for multi-layer composite positive electrode material of lithium ion battery - Google Patents
Preparation method for multi-layer composite positive electrode material of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method for a multi-layer composite positive electrode material of a lithium ion battery. The preparation method comprises the following steps of 1) preparing a mixed solution of solutions of Ni<2+>, Co<2+> and Mn<2+> compounds, allowing the mixed solution to react with a complexing agent and hydroxide to obtain a precursor, adding an aluminum salt and a magnesium salt to a precursor mixture solution, carrying out suction filtration after a reaction, and drying the obtained material to obtain a multi-layer spherical multi-element precursor; 2) uniformly mixing the obtained precursor and a lithium source compound according to a mole ratio of (0.9-1.30):1, placing the mixture in a high-temperature furnace for sintering, and carrying out calcination at 300-1,000 DEG C to obtain the positive electrode material of the lithium ion battery; and 3) making the positive electrode material of the lithium ion battery into slurry, uniformly mixing a lithium salt and iron phosphate according to a mole ratio of (1-1.05):1 through multi-pump circulation, and drying and roasting the mixture to obtain the multi-layer composite positive electrode material of the lithium ion battery. In the multi-layer composite positive electrode material of the lithium ion battery, prepared according to the preparation method, the inner-layer material is spherical, elements such as Al and Mg are added into the intermediate layer, the surface is coated with a layer of lithium iron phosphate material, and thus, the multi-layer composite positive electrode material is high in volume capacity density and high in product purity.
Description
Technical field
The invention belongs to lithium battery material field, the preparation method being specifically related to a kind of MULTILAYER COMPOSITE anode material for lithium-ion batteries.
Background technology
In recent years, lithium ion battery is swift and violent as current widely used power source development, and its positive electrode also becomes the focus of research and receives much attention. Main several anode material for lithium-ion batteries such as LiNi1/3Co1/3Mn1/3O2��LiNi0.5Mn1.5O4��LiMn2O4, owing to nickel, two kinds of elements of manganese dissolve and Ni in the electrolytic solution4+Be there is more side reaction in the strong oxidation of electrolyte, cause that they all also exist cycle performance under the high temperature conditions and decline. In order to solve this problem, majority all adopts the method for cladding to solve. But single cladding can increase the internal resistance of battery, and can not form uniform surface layer.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of MULTILAYER COMPOSITE anode material for lithium-ion batteries, it adopts spherical high density presoma, intermediate layer is added the elements such as Al, Mg and is made anode material for lithium-ion batteries, then, and one layer of LiFePO 4 material of Surface coating.
The preparation method of a kind of MULTILAYER COMPOSITE anode material for lithium-ion batteries of the present invention comprises the following steps:
1) Ni is prepared respectively2+��Co2+��Mn2+The solution of compound, wherein Ni2+��Co2+��Mn2+Molar concentration range for 0 < C (Ni2+)��0.10,0 < C (Co2+)��0.40,0 < C (Mn2+)��0.10;
2) by step 1) mixing of gained solution, mixed solution, chelating agent, hydroxide are continuously inputted in reactor with pump respectively, Ni2+��Co2+��Mn2+The mol ratio of solution is (4-8): (1-2): (1-4), and reacting liquid pH value controls at 10.0-11.0, obtains hydroxide co-precipitation precursor through stirring, precipitate, separate, drying;
3) by step 2) hydroxide co-precipitation precursor and sodium bicarbonate solution join in reactor and be stirred, at 50-55 DEG C, stir 1-8h with the speed of 200r/min-900r/min;
4) aluminium salt, magnesium salt solution are joined step 3 with the rate of addition of 0.05L/min-0.15L/min) in the mixed solution of gained, making aluminium salt, magnesium salt solution and step 3) mol ratio of the mixed solution of gained is: 0.02-1, stirring, the pH value being simultaneously introduced ammonia adjustment solution is 9.5-13;
5) by step 4) solution stand 80min-120min, then be filtered, wash, be 6.5-7.0 to cleaning mixture pH;
6) by step 5) material of gained carries out sucking filtration, and then dry 3-9h when 80 DEG C-100 DEG C, obtain the polynary presoma of Multi-layer spherical;
7) by step 6) gained presoma and Li source compound (0.9-1.30) in molar ratio: 1 mix homogeneously after, put in high temperature furnace and be sintered, under air or oxygen atmospheric condition, 300-1000 DEG C of calcining 4-48h, cooled, pulverize, obtain anode material for lithium-ion batteries after classification and screening;
8) by step 7) resulting materials is dispersed in pure water, stirs into slurry, and solid content is 50-70%;
9) by lithium salts and iron phosphate (1-1.05) in molar ratio: 1 joins in pure water, is made into slurry, and solid content is 50-60%;
10) by step 8) and 9) gained slurry mix homogeneously, gained mixture after drying, is calcined 9 hours for 850-900 DEG C under oxygen-free atmosphere, cools down, pulverizes, sieving obtains MULTILAYER COMPOSITE anode material for lithium-ion batteries.
Wherein, step 10) in hybrid mode be: by step 8) and 9) gained slurry pumps into from agitator top with the speed of 0.3L/min-0.5L/min respectively, from agitator bottom, this mixed slurry is pumped simultaneously, again pump into same agitator from top, be circulated stirring to step 8) and 9) gained slurry carries complete.
The volume capacity density of the MULTILAYER COMPOSITE anode material for lithium-ion batteries that preparation method of the present invention prepares is high, and electrochemistry side reaction is few, and charge and discharge platform is many, and high voltage capability is good, and product purity is high, less costly.
Detailed description of the invention
By the following examples the detailed process of the present invention is described further.
Embodiment 1
1) NiSO is prepared respectively4��CoSO4��MnSO4Solution, wherein C (Ni2+)=0.08mol/L, C (Co2+)=0.01mol/L, C (Mn2+)=0.01mol/L;
2) by step 1) gained solution mix homogeneously, mixed solution, 2.0mol/L ammonia, 8.0mol/L sodium hydroxide are continuously inputted in reactor with pump respectively, the mol ratio of input is: Ni:Co:Mn=8:1:1, reacting liquid pH value controls at 10.0-11.0, obtains hydroxide co-precipitation precursor Ni through stirring, precipitate, separate, drying0.8Co0.1Mn0.1(OH)2;
3) by step 2) the sodium bicarbonate solution that hydroxide co-precipitation precursor 100g and 200mL concentration are 0.5mol/L join in reactor and be stirred, at 50-55 DEG C, stir 3h with the speed of 300r/min;
4) 0.02mol/L aluminium salt, 0.02mol/L magnesium salt solution are joined step 3 with the rate of addition of 0.05L/min) in gained mixed solution, making aluminium salt, magnesium salt solution and step 3) mol ratio of gained mixed solution is: 0.02-1, stirring, the pH value being simultaneously introduced ammonia adjustment solution is 10.5-11.0;
5) by step 4) solution stand 80min-120min, then be filtered, wash, be 6.5-7.0 to cleaning mixture pH;
6) by step 5) washing after material carry out sucking filtration, then when 95 DEG C-100 DEG C dry 6h, obtain the polynary presoma of Multi-layer spherical;
7) by step 6) gained presoma and Li source compound be after 0.9:1 is mixed homogeneously in molar ratio, put in high temperature furnace and be sintered, under air or oxygen atmospheric condition, calcine 10h at 1000 DEG C, cooled, pulverize, obtain anode material for lithium-ion batteries after classification and screening;
8) by step 7) resulting materials is dispersed in pure water, stirs into slurry, and solid content is 60-70%;
9) joining in pure water by lithium salts with iron phosphate 1:1 in molar ratio, be made into slurry, solid content is at 50-55%;
10) by step 8) and 9) gained slurry pumps into from agitator top with the speed of 0.3L/min-0.5L/min respectively, from agitator bottom, this mixed slurry is pumped simultaneously, again pump into same agitator from top, be circulated stirring to step 8) and 9) gained slurry carries complete;
11) by step 10) gained mixture after drying, under oxygen-free atmosphere 850-900 DEG C calcine 9 hours, cooling, pulverize, sieve and obtain MULTILAYER COMPOSITE anode material for lithium-ion batteries.
The MULTILAYER COMPOSITE anode material for lithium-ion batteries prepared is made CR2016 battery and is then carried out charge-discharge performance contrast test. It is 81% that the battery of common material 1C at 55 DEG C circulates 100 capability retentions, and it is 96% that the battery of MULTILAYER COMPOSITE anode material for lithium-ion batteries 1C at 55 DEG C circulates 100 capability retentions.
Embodiment 2
1) Ni (NO is prepared respectively3)2��Co(NO3)2��Mn(NO3)2Solution, wherein C (Ni2+)=0.04mol/L, C (Co2+)=0.02mol/L, C (Mn2+)=0.01mol/L;
2) by step 1) mixing of gained solution, mixed solution, 2.0mol/L ammonia, 8.0mol/L sodium hydroxide are continuously inputted in reactor with pump respectively, the mol ratio of input is Ni:Co:Mn=4:2:2, reacting liquid pH value controls at 10.0-11.0, to obtain hydroxide co-precipitation precursor Ni through stirring, precipitate, separate, drying0.4Co0.2Mn0.2(OH)2;
3) by step 2) the sodium bicarbonate solution that hydroxide co-precipitation precursor 100g and 300mL concentration are 0.5mol/L join in reactor and be stirred, at 50-55 DEG C, stir 3h with the speed of 300r/min;
4) 0.02mol/L aluminium salt, 0.02mol/L magnesium salt solution are added step 3 with the rate of addition of 0.05L/min) in the mixed solution of gained, making aluminium salt, magnesium salt solution and step 3) mol ratio of the mixed solution of gained is: 0.02-1, stirring, the pH value being simultaneously introduced ammonia adjustment solution is 10.5-11.0;
5) by step 4) solution stand 80min-120min, then be filtered, wash, be 6.5-7.0 to cleaning mixture pH;
6) by step 5) material of gained carries out sucking filtration, and then dry 6h when 95 DEG C-100 DEG C, obtain the polynary presoma of Multi-layer spherical;
7) by step 6) gained presoma is for Li source compound after 1:1 is mixed homogeneously in molar ratio, put in high temperature furnace and be sintered, under air or oxygen atmospheric condition, 300 DEG C of calcining 10h, cooled, pulverize, obtain anode material for lithium-ion batteries after classification and screening;
8) by step 7) resulting materials is dispersed in pure water, stirs into slurry, and solid content is 60-70%;
9) joining in pure water by lithium salts with iron phosphate 1.05:1 in molar ratio, be made into slurry, solid content is at 50-55%;
10) by step 8) and 9) gained slurry pumps into from agitator top with the speed of 0.3L/min-0.5L/min respectively, from agitator bottom, this mixed slurry is pumped simultaneously, again pump into same agitator from top, be circulated stirring to step 8) and 9) gained slurry carries complete;
11) by step 10) gained mixture after drying, under oxygen-free atmosphere 850-900 DEG C calcine 9 hours, cooling, pulverize, sieve and obtain MULTILAYER COMPOSITE anode material for lithium-ion batteries.
The MULTILAYER COMPOSITE anode material for lithium-ion batteries prepared is made CR2016 battery and is then carried out charge-discharge performance contrast test. It is 81% that the battery of common material 1C at 55 DEG C circulates 100 capability retentions, and it is 98% that the battery of MULTILAYER COMPOSITE anode material for lithium-ion batteries 1C at 55 DEG C circulates 100 capability retentions.
Embodiment 3
1) NiSO is prepared respectively4��CoSO4��MnSO4Solution, wherein C (Ni2+)=0.10mol/L, C (Co2+)=0.04mol/L, C (Mn2+)=0.01mol/L;
2) by step 1) gained solution mix homogeneously, mixed solution, 2.0mol/L ammonia, 8.0mol/L sodium hydroxide are continuously inputted in reactor with pump respectively, the mol ratio of input is: Ni:Co:Mn=8:1:1, reacting liquid pH value controls at 10.0-11.0, obtains hydroxide co-precipitation precursor Ni through stirring, precipitate, separate, drying0.8Co0.1Mn0.1(OH)2;
3) by step 2) the sodium bicarbonate solution that hydroxide co-precipitation precursor 100g and 500mL concentration are 0.5mol/L join in reactor and be stirred, at 50-55 DEG C, stir 3h with the speed of 300r/min;
4) 0.02mol/L aluminium salt, 0.02mol/L magnesium salt solution are added step 3 with the rate of addition of 0.05L/min) in the mixed solution of gained, making aluminium salt, magnesium salt solution and step 3) mol ratio of the mixed solution of gained is: 0.02-1, stirring, the pH value being simultaneously introduced ammonia adjustment solution is 10.5-11.0;
5) by step 4) solution stand 80min-120min, then be filtered, wash, be 6.5-7.0 to cleaning mixture pH;
6) by step 5) resulting materials carries out sucking filtration, and then dry 6h when 95 DEG C-100 DEG C, obtain the polynary presoma of Multi-layer spherical;
7) by step 6) gained presoma and Li source compound be after 1.3:1 is mixed homogeneously in molar ratio, put in high temperature furnace and be sintered, under air or oxygen atmospheric condition, calcine 10h at 800 DEG C, cooled, pulverize, obtain anode material for lithium-ion batteries after classification and screening;
8) by step 7) resulting materials is dispersed in pure water, stirs into slurry, and solid content is 60-70%;
9) joining in pure water by lithium salts with iron phosphate 1.02:1 in molar ratio, be made into slurry, solid content is at 50-60%;
10) by step 8) and 9) gained slurry pumps into from agitator top with the speed of 0.3L/min-0.5L/min respectively, from agitator bottom, this mixed slurry is pumped simultaneously, again pump into same agitator from top, be circulated stirring to step 8) and 9) gained slurry carries complete;
11) by step 10) gained mixture after drying, under oxygen-free atmosphere 850-900 DEG C calcine 9 hours, cooling, pulverize, sieve and obtain MULTILAYER COMPOSITE anode material for lithium-ion batteries.
The MULTILAYER COMPOSITE anode material for lithium-ion batteries prepared is made CR2016 battery and is then carried out charge-discharge performance contrast test. It is 81% that the battery of common material 1C at 55 DEG C circulates 100 capability retentions, and it is 97.6% that the battery of MULTILAYER COMPOSITE anode material for lithium-ion batteries 1C at 55 DEG C circulates 100 capability retentions.
Claims (2)
1. the preparation method of a MULTILAYER COMPOSITE anode material for lithium-ion batteries, it is characterised in that comprise the following steps:
1) Ni is prepared respectively2+��Co2+��Mn2+The solution of compound, wherein Ni2+��Co2+��Mn2+Molar concentration range for 0 < C (Ni2+)��0.10,0 < C (Co2+)��0.40,0 < C (Mn2+)��0.10;
2) by step 1) mixing of gained solution, mixed solution, chelating agent, hydroxide are continuously inputted in reactor with pump respectively, Ni2+��Co2+��Mn2+The mol ratio of solution is (4-8): (1-2): (1-4), and reacting liquid pH value controls at 10.0-11.0, obtains hydroxide co-precipitation precursor through stirring, precipitate, separate, drying;
3) by step 2) hydroxide co-precipitation precursor and sodium bicarbonate solution join in reactor and be stirred, at 50-55 DEG C, stir 1-8h with the speed of 200r/min-900r/min;
4) aluminium salt, magnesium salt solution are joined step 3 with the rate of addition of 0.05L/min-0.15L/min) in the mixed solution of gained, making aluminium salt, magnesium salt solution and step 3) mol ratio of gained mixed solution is: 0.02-1, stirring, the pH value being simultaneously introduced ammonia adjustment solution is 9.5-13;
5) by step 4) solution stand 80min-120min, then be filtered, wash, be 6.5-7.0 to cleaning mixture pH;
6) by step 5) material of gained carries out sucking filtration, and then dry 3-9h when 80 DEG C-100 DEG C, obtain the polynary presoma of Multi-layer spherical;
7) by step 6) gained presoma and Li source compound (0.9-1.30) in molar ratio: 1 mix homogeneously after, put in high temperature furnace and be sintered, under air or oxygen atmospheric condition, 300-1000 DEG C of calcining 4-48h, cooled, pulverize, obtain anode material for lithium-ion batteries after classification and screening;
8) by step 7) resulting materials is dispersed in pure water, stirs into slurry, and solid content is 50-70%;
9) by lithium salts and iron phosphate (1-1.05) in molar ratio: 1 joins in pure water, is made into slurry, and solid content is 50-60%;
10) by step 8) and 9) gained slurry mix homogeneously, gained mixture after drying, is calcined 9 hours for 850-900 DEG C under oxygen-free atmosphere, cools down, pulverizes, sieving obtains MULTILAYER COMPOSITE anode material for lithium-ion batteries.
2. the preparation method of MULTILAYER COMPOSITE anode material for lithium-ion batteries according to claim 1, it is characterized in that: step 10) in hybrid mode be: by step 8) and 9) gained slurry pumps into from agitator top with the speed of 0.3L/min-0.5L/min respectively, from agitator bottom, this mixed slurry is pumped simultaneously, again pump into same agitator from top, be circulated and stir to step 8) and 9) slurry of gained carries complete.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109273683A (en) * | 2018-09-07 | 2019-01-25 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN109449378A (en) * | 2018-09-07 | 2019-03-08 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
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| CN103178258A (en) * | 2013-01-21 | 2013-06-26 | 宁德新能源科技有限公司 | Method for preparing aluminum oxide coated modified lithium nickel cobalt manganese oxygen cathode material |
| CN103208623A (en) * | 2012-01-17 | 2013-07-17 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery and rechargeable lithium battery including the same |
| CN103474625A (en) * | 2013-08-05 | 2013-12-25 | 合肥国轩高科动力能源股份公司 | Coating method for core-shell novel positive electrode material for lithium ion battery |
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| CN103208623A (en) * | 2012-01-17 | 2013-07-17 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery and rechargeable lithium battery including the same |
| CN103178258A (en) * | 2013-01-21 | 2013-06-26 | 宁德新能源科技有限公司 | Method for preparing aluminum oxide coated modified lithium nickel cobalt manganese oxygen cathode material |
| CN103474625A (en) * | 2013-08-05 | 2013-12-25 | 合肥国轩高科动力能源股份公司 | Coating method for core-shell novel positive electrode material for lithium ion battery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109273683A (en) * | 2018-09-07 | 2019-01-25 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN109449378A (en) * | 2018-09-07 | 2019-03-08 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN109273683B (en) * | 2018-09-07 | 2021-05-25 | 北京泰丰先行新能源科技有限公司 | Composite positive electrode material of lithium ion battery and preparation method thereof |
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Application publication date: 20160601 |