CN103227323B - Preparation method of positive pole material (spinel type lithium nickel manganese oxide) of high-voltage lithium ion battery - Google Patents
Preparation method of positive pole material (spinel type lithium nickel manganese oxide) of high-voltage lithium ion battery Download PDFInfo
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Abstract
The invention relates to a preparation method of a positive pole material (spinel type lithium nickel manganese oxide) of a high-voltage lithium ion battery, which comprises the following steps: simultaneously dissolving a lithium-containing compound, a manganese-containing compound and a nickel-containing compound instead of adding a lithium source afterwards, and ensuring that the lithium compound, the nickel compound and the manganese compound are evenly mixed; and adding precipitant to generate manganese-containing precipitate, wherein the generated manganese-containing precipitate provides crystal nuclei for further precipitation in the hydrothermal process, particles having different sizes can be obtained by controlling hydrothermal conditions, the particle sizes of the products can be increased by decreasing the concentrations of the metal salts, increasing the hydrothermal temperature and prolonging the hydrothermal time, and materials having different shapes can be obtained or porous materials can be prepared by adding different additives. The method omits the steps of filtration and water washing; and the synthesis process is economic and environment-friendly. The lithium nickel manganese oxide material prepared by the invention is in a spinel structure, and is high in crystallinity and excellent in electrochemical performance; and the specific capacity can be up to 130-142mAh/g, 120-135mAh/g and 105-120mAh/g in case of 1C, 2C and 5C rate discharge.
Description
Technical field
The invention belongs to field of material technology, relate to a kind of preparation method of anode material for lithium-ion batteries, particularly relate to a kind of preparation method of anode material for lithium-ion batteries spinel-type nickel ion doped.
Background technology
For tackling global energy crisis, national governments actively promote the development of the new-energy automobile based on electric automobile.Electrokinetic cell is the important component part of electric automobile. directly affect electric automobile performance.Lithium ion battery has the remarkable advantage that operating voltage is high, memory-less effect, self-discharge rate are little, energy density is large and have extended cycle life, and as electrokinetic cell, has wide practical use.
In the positive electrode of current several main flows, LiFePO 4 cannot meet the needs of electrokinetic cell due to cryogenic property and lot stability, and the fail safe (high nickel content) of the high-temperature behavior that LiMn2O4 is poor and ternary material also cannot separately as the positive electrode of electrokinetic cell.In positive electrode, spinel-type positive electrode LiNi
0.5mn
1.5o
4there is higher discharge platform (4.7V) and higher capacity (theoretical specific capacity 146.7 mAh/g), and the structural stability of excellence, rich in natural resources, cheap cost and advantages of environment protection.And the cyclical stability under high temperature has also had the lifting of matter than LiMn2O4, and can improve battery safety by the higher negative material of compatible operations voltage, therefore it is with a wide range of applications as power battery material.
LiNi
0.5mn
1.5o
4there are two kinds of space groups, are respectively P4
332 to Fd3m, and wherein space group is the LiNi of Fd3m
0.5mn
1.5o
4-xhave better chemical property, particularly under high magnification, circulation time has low impedance and high discharge capacity.The structure, impurity content, degree of crystallinity, microscopic appearance, particle size, domain size distribution etc. of preparation method to material have a significant impact, thus affect its performance.Current LiNi
0.5mn
1.5o
4preparation method mainly contain solid phase method and liquid phase method etc.Solid phase method technique is simple, is preparation LiNi
0.5mn
1.5o
4common method, preparation technology is simple, by the lithium source of a certain proportion of solid, nickel source and the mixing of manganese source ball milling, then calcines, but material heterogeneity prepared by the method, and particle size is large.High sintering temperature can cause as NiO or Li
xni
1 xthe appearance of O impurity, and turn down temperature the degree of crystallinity of product can be made low.Liquid phase method comprises coprecipitation, sol-gal process and molten salt growth method etc., raw material can be mixed homogeneous, the LiNi that preparation particle size is little
0.5mn
1.5o
4material, but the method complex process, particle size is little makes it have large specific area, serious with electrolyte side reaction.
Summary of the invention
The object of this invention is to provide a kind of preparation method of anode material for lithium-ion batteries spinel-type nickel ion doped, mixed by the liquid phase of lithium nickel manganese, realize material homogeneous, by controlling water-heat process, obtain the granular precursor of suitable size, pattern, sintering obtains nickel ion doped material.
The present invention prepares anode material for lithium-ion batteries spinel-type nickel ion doped in accordance with the following steps:
One, Li:Ni:Mn=1 ~ 1.1:0.5:1.5 claims lithium source, nickel source and manganese source in molar ratio, is dissolved in deionized water, stirs and obtain solution A;
Two, add in solution A
entera certain amount of additive, lithium salts and additive mol ratio are 0.1 ~ 1, stir and obtain solution B;
Three, under room temperature, while stirring, slowly drip a certain amount of precipitation reagent in solution B, lithium salts and precipitation reagent mol ratio are 0.1 ~ 0.4, obtain mixture C;
Four, transfer in hydrothermal reaction kettle by mixture C, at 120 ~ 240 DEG C, react 5 ~ 15 h, then at 60 ~ 80 DEG C, stir evaporation, drying obtains presoma;
Five, presoma is put into Muffle furnace air atmosphere, pre-burning 3 ~ 8 h at 300 ~ 500 DEG C, be then warming up to 700 ~ 1000 DEG C of calcining 8 ~ 20 h, with the cooling of the speed of 0.5 ~ 1 DEG C/min, obtain nickel ion doped material.
In above-mentioned preparation method, described lithium source is one or more the mixture in lithium acetate, lithium nitrate, lithium ethoxide, lithium formate, lithium carbonate.
In above-mentioned preparation method, described nickel source is one or both the mixture in nickel acetate, carbonyl nickel, nickel formate and nickel nitrate.
In above-mentioned preparation method, described manganese source is one or both the mixture in manganese acetate, formic acid manganese and manganese nitrate.
In above-mentioned preparation method, described additive is one or both the mixture in ethanol, polyethylene glycol, oxalic acid, polyacrylic acid, 2-ethyl acetic acid, ethylenediamine tetra-acetic acid, 1,2,4-1H-triazole and resorcinol.
In above-mentioned preparation method, described precipitation reagent is one or both the mixture in carbonic hydroammonium, ammonium carbonate, urea and ammonium oxalate.
The present invention is by lithium-containing compound, and containing manganese compound, nickel compound containing dissolves simultaneously, instead of after add lithium source, make lithium nickel manganese three kinds of compound even, and accurately can control material rate; After adding precipitation reagent, being precipitated as in water-heat process further precipitation containing manganese and providing nucleus of generation; Control the particle that hydrothermal condition can obtain different size, reduce metal salt concentrations, improve hydrothermal temperature and extend the hydro-thermal time, product particle size can be made to increase; Adopt different additives, the material of different-shape can be obtained, or prepare porous material; This method without filtration, water-washing step, synthesis technique economical environment-protective.
Nickel ion doped material granule prepared by the present invention is even, for spinel structure, degree of crystallinity is high, electrochemical performance, voltage platform is about 4.7,130 ~ 142mAh/g, 120 ~ 135 mAh/g and 105 ~ 120mAh/g can be reached with specific capacity during 1C, 2C and 5C multiplying power discharging, there is good high rate performance and cycle performance.
Accompanying drawing explanation
Fig. 1 is LiNi prepared by the present invention
0.5mn
1.5o
4the SEM figure of material.
Fig. 2 is LiNi prepared by the present invention
0.5mn
1.5o
4charging and discharging curve under the different multiplying of material.
Fig. 3 is LiNi prepared by the present invention
0.5mn
1.5o
4cycle performance curve under the different multiplying of material.
Embodiment
Embodiment one: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol Li (CH
3cOO), 0.01mol Ni (CH
3cOO)
2with 0.03mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Then add 10ml absolute ethyl alcohol, stir; While stirring, slowly drip the ammonium bicarbonate soln of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then with the cooling of the speed of 0.5 DEG C/min, obtains nickel ion doped material.
As Figure 1-3, nickel ion doped material granule size prepared by present embodiment is about 1 μm, when discharging with 0.2C, 1C, 5C and 15C, specific capacity can reach 140.1mAh/g, 138.2mAh/g, 118.4mAh/g and 96.8mAh/g, has good high rate performance and cycle performance.
Embodiment two: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol Li (CH
3cOO), 0.01mol Ni (CH
3cOO)
2, 0.03mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Then add 10ml absolute ethyl alcohol, stir; While stirring, slowly drip the ammonium bicarbonate soln of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 160 DEG C, reacts 3h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 3h at 400 DEG C, calcines 12h at 800 DEG C, and then lower the temperature with 0.5 DEG C/min, obtain nickel ion doped material, material granule size is about 0.5 μm.When discharging with 1C and 5C, specific capacity can reach 142mAh/g and 120mAh/g, has good high rate performance and cycle performance.
Embodiment three: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.01mol Li (CH
3cOO), 0.005mol Ni (CH
3cOO)
2, 0.015mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Add 10ml absolute ethyl alcohol, stir; While stirring, slowly drip the ammonium bicarbonate soln of 50ml 1mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, and then lower the temperature with 0.5 DEG C/min, obtain nickel ion doped material, material granule size is about 2 μm.When discharging with 1C and 5C, specific capacity can reach 135mAh/g and 105.5mAh/g, has good high rate performance and cycle performance.
Embodiment four: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol Li (CH
3cOO), 0.01mol Ni (CH
3cOO)
2, 0.03mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Add 5ml polyethylene glycol and 0.5g oxalic acid, stir; While stirring, slowly drip the ammonium bicarbonate soln of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains nickel ion doped material, and granule-morphology is octahedra.When discharging with 1C and 5C, specific capacity can reach 138mAh/g and 115.5mAh/g, has good high rate performance and cycle performance.
Embodiment five: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol Li (CH
3cOO), 0.01mol Ni (CH
3cOO)
2, 0.03mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Add 0.02mol 1,2,4-1H-triazole, stir; Stir, slowly drip the ammonium bicarbonate soln of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains nickel ion doped material, and granule-morphology is cube.When discharging with 1C and 5C, specific capacity can reach 138.2mAh/g and 110.5mAh/g, has good high rate performance and cycle performance.
Embodiment six: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol Li (CH
3cOO), 0.01mol Ni (CH
3cOO)
2, 0.03mol Mn (CH
3cOO)
2, be dissolved in 50ml deionized water, stir; Add 0.1mol resorcinol, stir; While stirring, slowly drip the ammonium bicarbonate soln of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains the nickel ion doped material of porous.When discharging with 1C and 5C, specific capacity can reach 141mAh/g and 119.5mAh/g, has good high rate performance and cycle performance.
Embodiment seven: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol lithium nitrate, 0.01mol nickel nitrate, 0.03mol manganese acetate, be dissolved in 50ml deionized water, stir; Add 5ml polyethylene glycol and 0.5g oxalic acid, stir; While stirring, slowly drip the ammonium bicarbonate soln of 25ml 1mol/L and the sal volatile of 25ml 1mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains nickel ion doped material, and granule-morphology is octahedra.When discharging with 1C and 5C, specific capacity can reach 139mAh/g and 116mAh/g, has good high rate performance and cycle performance.
Embodiment eight: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.021mol lithium carbonate, 0.01mol nickel acetate, 0.03mol manganese nitrate, be dissolved in 50ml deionized water, stir; Add 5ml polyethylene glycol and 0.5g oxalic acid, stir; While stirring, slowly drip the sal volatile of 50ml 2mol/L.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains nickel ion doped material, and granule-morphology is octahedra.When discharging with 1C and 5C, specific capacity can reach 136mAh/g and 108mAh/g, has good high rate performance and cycle performance.
Embodiment nine: present embodiment prepares nickel ion doped material in accordance with the following steps:
Take 0.01mol lithium carbonate and 0.01mol lithium formate, 0.01mol nickel acetate, 0.02mol manganese nitrate and 0.01mol manganese acetate, be dissolved in 50ml deionized water, stir; Add 5ml polyethylene glycol and 0.5g oxalic acid, stir; While stirring, add 0.05mol urea.
Above mixture is transferred to 200ml hydrothermal reaction kettle, at 180 DEG C, reacts 5h, then at 80 DEG C, stir evaporation, dry, obtain presoma.
Above presoma is placed in Muffle furnace, and pre-burning 4h at 400 DEG C, calcines 10h at 800 DEG C, then lowers the temperature with 0.5 DEG C/min, obtains nickel ion doped material, and granule-morphology is octahedra.When discharging with 1C and 5C, specific capacity can reach 136mAh/g and 108mAh/g, has good high rate performance and cycle performance.
Claims (6)
1. the preparation method of anode material for high-voltage lithium ion spinel-type nickel ion doped, is characterized in that described method step is as follows:
One, Li:Ni:Mn=1 ~ 1.1:0.5:1.5 claims lithium source, nickel source and manganese source in molar ratio, is dissolved in deionized water, stirs and obtain solution A;
Two, add in solution A
entera certain amount of additive, lithium salts and additive mol ratio are 0.1 ~ 1, stir and obtain solution B, and described additive is ethanol, polyethylene glycol, oxalic acid, polyacrylic acid, 2-ethyl acetic acid, ethylenediamine tetra-acetic acid, 1, one or both mixture in 2,4-1H-triazole and resorcinol;
Three, under room temperature, in solution B, slowly a certain amount of precipitation reagent is dripped while stirring, lithium salts and precipitation reagent mol ratio are 0.1 ~ 0.4, obtain mixture C, and described precipitation reagent is one or both the mixture in carbonic hydroammonium, ammonium carbonate, urea, ammonium oxalate;
Four, transfer in hydrothermal reaction kettle by mixture C, at 120 ~ 240 DEG C, react 5 ~ 15 h, then at 60 ~ 80 DEG C, stir evaporation, drying obtains presoma;
Five, presoma is put into Muffle furnace air atmosphere, pre-burning 3 ~ 8 h at 300 ~ 500 DEG C, be then warming up to 700 ~ 1000 DEG C of calcining 8 ~ 20 h, with the cooling of the speed of 0.5 ~ 1 DEG C/min, obtain nickel ion doped material.
2. the preparation method of anode material for high-voltage lithium ion spinel-type nickel ion doped according to claim 1, is characterized in that described lithium source, the mol ratio in nickel source and manganese source is Li:Ni:Mn=1.1:0.5:1.5.
3. the preparation method of anode material for high-voltage lithium ion spinel-type nickel ion doped according to claim 1, is characterized in that described lithium source, the mol ratio in nickel source and manganese source is Li:Ni:Mn=1:0.5:1.5.
4. the preparation method of the anode material for high-voltage lithium ion spinel-type nickel ion doped according to claim 1,2 or 3, is characterized in that described lithium source is one or more the mixture in lithium acetate, lithium nitrate, lithium ethoxide, lithium formate, lithium carbonate.
5. the preparation method of the anode material for high-voltage lithium ion spinel-type nickel ion doped according to claim 1,2 or 3, is characterized in that described nickel source is one or both the mixture in nickel acetate, carbonyl nickel, nickel formate and nickel nitrate.
6. the preparation method of anode material for high-voltage lithium ion spinel-type nickel ion doped according to claim 1, is characterized in that described manganese source is one or both the mixture in manganese acetate, formic acid manganese and manganese nitrate.
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| CN105280915B (en) * | 2015-09-23 | 2017-06-16 | 苏州大学 | A kind of preparation method of anode material of lithium battery nickel ion doped |
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| CN107017405A (en) * | 2017-06-16 | 2017-08-04 | 湖南师范大学 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN108281604B (en) * | 2017-12-12 | 2020-08-25 | 昆明理工大学 | Solvothermal synthesis method of lithium ion battery anode material |
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| CN109065852A (en) * | 2018-07-04 | 2018-12-21 | 上海电气集团股份有限公司 | A kind of positive electrode and preparation method thereof |
| CN108862407B (en) * | 2018-07-12 | 2021-01-08 | 青岛华冠恒远锂电科技有限公司 | Preparation method of lithium nickel manganese oxide positive electrode material and precursor |
| CN109292826B (en) * | 2018-07-26 | 2020-12-22 | 华南理工大学 | Porous lithium manganate material with high charge-discharge capacity, and preparation method and application thereof |
| CN110335995B (en) * | 2019-05-20 | 2021-03-05 | 大连理工大学 | Doped Al3+Preparation method of regular octahedral lithium nickel manganese oxide material |
| CN112652764B (en) * | 2019-10-10 | 2022-09-06 | 中国石油化工股份有限公司 | Battery positive electrode material precursor, battery positive electrode material, preparation method and application thereof |
| CN111769286A (en) * | 2020-07-16 | 2020-10-13 | 凤凰新能源(惠州)有限公司 | High-voltage lithium nickel manganese oxide positive electrode material and preparation method thereof |
| CN116093304B (en) * | 2023-01-13 | 2023-09-08 | 安徽博石高科新材料股份有限公司 | High-voltage lithium nickel manganese oxide positive electrode material and preparation method and application thereof |
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