CN100583512C - Spherical aluminum-doped nickel cobalt lithium for lithium ion battery and its making method - Google Patents
Spherical aluminum-doped nickel cobalt lithium for lithium ion battery and its making method Download PDFInfo
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Abstract
The invention discloses a preparation method of a spherical doped Al-Ni lithium cobalt oxide for lithium-ion battery. The preparation steps are that: first, sulfate, nitrate or chlorate of Al-Ni-Co react with strong alkali that is added with complex agent in liquid phase; the pH value, the temperature and the feeding speed of the reaction solution are controlled so as to produce a spherical precursor of Al-Ni-Co hydroxide; then the spherical precursor of Al-Ni-Co hydroxide is dried and evenly mixed with lithium hydroxide, lithium nitrate or lithium carbonate and dried; the obtained mixture is roasted into a spherical doped Al-Ni lithium cobalt oxide. The spherical doped Al-Ni lithium cobalt oxide has comparatively high tap density and remarkable cycle stability in the process of high-rate charge/discharge cycle, which improves over charge performance of Ni-Co substance and first obviously enhances charge/discharge efficiency; in addition, the preparation method of the spherical doped Al-Ni lithium cobalt oxide has the advantages of being simple, controllable and suitable for industrialized production with low energy consumption, high efficiency, short reaction time and low cost.
Description
Technical field:
The present invention relates to the secondary cell field, particularly relate to a kind of preparation method of anode material for lithium ion battery spherical aluminum-doped nickel cobalt acid lithium.
Background technology:
Lithium ion battery has been widely used in various mobile electronic electrical equipment at present, as mobile phone, camera, notebook computer etc., for adapting to the fast development of these equipment, the supporting manufacturer of each battery is less for size, weight lithium rechargeable battery demand light, that capacity is bigger constantly increases.LiNiO
2The positive electrode of doping Co element has had LiNiO simultaneously
2The specific discharge capacity that material is higher has been stablized the layer structure of material again, has strengthened the cyclical stability of material.But also there is relatively poor, the more high defective of irreversible capacity of discharging first of overcharging resisting ability, thermal stability in this material.For overcoming the above problems, make nickel cobalt material can be applied to the commercialization field as early as possible, Chinese scholars has been carried out a large amount of doping tests, to improve the chemical property of material.Wherein the doping of aluminium can be stablized nickel cobalt material structure, increases the diffusion coefficient of lithium ion, obviously suppresses the anti-thermal response in the charge and discharge process, so the cycle performance of material and overcharging resisting performance obviously improve.But because aluminium ion is+3 valencys, be difficult to form single layer structure, can't form the high density spherical nickel-cobalt material with the nickel cobalt element, and the loaded down with trivial details difficulty of its preparation method, need of industrial production can not be adapted to.
Summary of the invention:
In order to address the above problem, the object of the present invention is to provide a kind ofly have higher density, be easy to prepare and the lithium ion battery of function admirable with the preparation method of spherical aluminum-doped nickel cobalt acid lithium.
The objective of the invention is to realize by the following technical programs:
A kind of lithium ion battery preparation method of spherical aluminum-doped nickel cobalt acid lithium may further comprise the steps:
(1) preparation of ball-shape nickel hydroxide cobalt aluminium presoma: a) with mol ratio be the salting liquid that 80: 15: 5 nickel, cobalt, aluminium salt is hybridly prepared into 1.5～2.5M, NaOH is mixed with the aqueous slkali of 5.5～6.5M and adds the complexing agent of 0.5～1M, the volume ratio of salting liquid and aqueous slkali is 25: 1～4: 1; Two kinds of solution that b) will prepare add simultaneously by peristaltic pump and contain in the 10L reactor that 1.5-2.5L concentration is the 0.25-0.75M carbonate aqueous solution, the mixing salt solution charging rate is 20ml/min, the charging rate of the aqueous slkali that makes in regulating a) with the pH value of control reaction system between 9～13, stirring also is heated to 20～80 ℃, reaction is carried out between 20～30h, the presoma granularity reaches 8～15 o'clock reinforced end, isolates ball-shape nickel hydroxide cobalt aluminium presoma then; C) with the oven dry after deionized water wash filters of ball-shape nickel hydroxide cobalt aluminium presoma, make ball-shape nickel hydroxide cobalt aluminium presoma;
(2) preparation of spherical aluminum-doped nickel cobalt acid lithium: a) lithium source and the ball-shape nickel hydroxide cobalt aluminium presoma that makes are mixed; B) with mixture 700～900 ℃ roasting temperature 20～30 hours, cool off after the roasting and broken classification, obtain spherical aluminum-doped nickel cobalt acid lithium.
Above-mentioned nickel, cobalt, aluminium salt are its sulfate, nitrate or chlorate.
Above-mentioned complexing agent is a kind of or wherein several mixture in ammoniacal liquor, carbonic hydroammonium, citric acid and the oxalic acid.
Above-mentioned carbonate is a kind of or wherein several mixture in sodium carbonate, sodium acid carbonate and the carbonic hydroammonium.
Above-mentioned lithium source is a kind of or wherein several mixture in LITHIUM BATTERY lithium hydroxide, lithium nitrate and the lithium carbonate.
Preferably, above-mentioned sintering temperature is 700～800 ℃.
Preferably, above-mentioned roasting time is 20～24 hours.
In the preparation method of spherical aluminum-doped nickel cobalt acid lithium of the present invention; the doped junction of the formation of presoma and aluminium element is lumped together; having reached the nickel cobalt element mixes with the atom level of aluminium element; obtain spherical and the spherical co-precipitation presoma of class; synthetic nickel cobalt material granule has kept the spherical morphology of presoma basically; this makes material have the good flowability of material, helps that positive electrode is applied on the anode pole piece uniformly in the manufacturing engineering of battery.In the positive electrode that roasting obtains, nickel cobalt aluminium ion is staggered between lattice regularly, can significantly improve the charge and discharge cycles stability of material.By in material, introducing the two-dimensional layer crystal structure that aluminium element can be stablized nickel cobalt material, the stable circulation performance that significantly the improves material simultaneously diffusion impedance of electric charge carrier is less, the diffusion coefficient of lithium ion increases, exothermic reaction in the charge and discharge process is simultaneously obviously suppressed, and has improved the chemical property of material under room temperature and higher temperature.The spherical aluminum-doped nickel cobalt prepared among the present invention acid lithium material positive electrode has particle size and distributes controlledly with pattern, and advantage such as height ratio capacity, production process are simple, and product price is low has significantly improved the cycle performance and the security performance of battery simultaneously.
Description of drawings:
Fig. 1 spherical aluminum-doped nickel cobalt acid of the present invention lithium preparation method's flow chart;
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of spherical aluminum-doped nickel cobalt acid lithium of the present invention;
Fig. 3 is the stereoscan photograph of spherical aluminum-doped nickel hydroxide cobalt among the present invention;
Fig. 4 is the stereoscan photograph of spherical aluminum-doped nickel cobalt acid lithium of the present invention;
Fig. 5 is the charging and discharging curve figure of spherical aluminum-doped nickel cobalt acid lithium of the present invention;
Fig. 6 is the electrode cycle performance curve of spherical aluminum-doped nickel cobalt acid lithium of the present invention.
Embodiment:
Below in conjunction with the drawings and specific embodiments the preparation method of lithium ion battery of the present invention with spherical aluminum-doped nickel cobalt acid lithium is described further.
Example 1:
At first nickel nitrate, cobalt nitrate and aluminum nitrate were hybridly prepared into the aqueous solution of 2M in 0.8: 0.15: 0.05 in molar ratio, NaOH are formulated as the solution 2L of 6M and add the ammoniacal liquor of 0.4L 1M.Then the salting liquid that the prepares flow velocity with 0.5L/h is added in the 10L reactor of the aqueous sodium carbonate that fills 2000ml 0.5M, stirring also is heated to 25 ℃, the charging rate of the aqueous slkali that adjusting makes with control reaction system the pH value between 10.0～10.2, through 24h, the presoma granularity reaches 12.077 in the solidliquid mixture, the reinforced end isolated spherical aluminum-doped nickel cobalt acid lithium presoma, and its electromicroscopic photograph as shown in Figure 3.Again the presoma of preparing after filtering, deionized water wash is dried 24h under 120 ℃ of temperature.Lithium hydroxide and presoma are even with 1.05: 1 mixed, mixture are placed the stove roasting again, and 700 ℃ of following roastings 24 hours, the cooling broken classification in back obtained spherical aluminum-doped nickel cobalt acid lithium material, and its electromicroscopic photograph as shown in Figure 4.
Through check, this aluminum-doped nickel cobalt acid lithium tap density is 2.02g/cm3, and particle mean size is 11.023 μ m.As shown in Figure 2, its X-ray diffraction (XRD) collection of illustrative plates is consistent with lithium nickel cobalt dioxide, and its pattern is illustrated in figure 4 as sphere, and initial capacity is 185mAh/g, and first charge-discharge efficiency is 89% as shown in Figure 5; 100 circulation volume conservation rates are 86% as shown in Figure 6.
Example 2:
Prepare by the method for example 1 and to mix aluminium nickel hydroxide cobalt precursor and mix the back temperature with lithium salts and be controlled at 750 ℃, the time is 24h, and the broken classification in cooling back obtains spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density is 2.12g/cm3, and granularity is 9.421 μ m, initial capacity 181mAh/g, and 100 times the circulation volume conservation rate is 84%, first charge-discharge efficiency is 91%.
Example 3:
Prepare by the method for example 1 and to mix aluminium nickel hydroxide cobalt precursor and mix the back temperature with lithium salts and be controlled at 800 ℃, the time is 24h, and the broken classification in cooling back obtains spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density 2.21g/cm3, granularity 10.215 μ m, initial capacity 171mAh/g, 100 times the circulation volume conservation rate is 83%, first charge-discharge efficiency is 84%.
Example 4:
Nickel nitrate, cobalt nitrate and aluminum nitrate were hybridly prepared into the aqueous solution of 2M in 0.8: 0.17: 0.03 in molar ratio, NaOH are formulated as the solution 2L of 6M and add the ammonium bicarbonate soln 0.5L of 1M.Then the salting liquid that the prepares flow velocity with 0.5L/h is added in the 10L reactor of the aqueous sodium carbonate that fills 1500ml 0.75M, stirring also is heated to 25 ℃, regulate and control the pH value of reaction system between 10.4～10.6 with the aqueous slkali that makes, through 24h, the presoma granularity reaches 13.211 in the solidliquid mixture, the reinforced end isolated spherical aluminum-doped nickel cobalt acid lithium presoma.Again the presoma of preparing after filtering, deionized water wash is dried 24h under 120 ℃ of temperature.Lithium hydroxide and presoma are even with 1.05: 1 mixed, mixture are placed the stove roasting again, and 700 ℃ of following roastings 24 hours, the cooling broken classification in back obtained spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density is 2.13g/cm3, and particle mean size is 12.011 μ m, and initial capacity is 189mAh/g, and 100 times the circulation volume conservation rate is 82%, and first charge-discharge efficiency is 84%.
Example 5:
Prepare by the method for example 4 and to mix aluminium nickel hydroxide cobalt precursor and mix the back temperature with lithium salts and be controlled at 800 ℃, the time is 24h, and the broken classification in cooling back obtains spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density 2.26g/cm
3, granularity 11.985 μ m, initial capacity 173mAh/g, 100 times the circulation volume conservation rate is 83%, first charge-discharge efficiency is 81%.
Example 6:
Nickel nitrate, cobalt nitrate and aluminum nitrate were hybridly prepared into the aqueous solution of 2M in 0.8: 0.13: 0.07 in molar ratio, NaOH are formulated as the solution 2L of 6M and add the oxalic acid solution 0.2L of 1M.Then the salting liquid that the prepares flow velocity with 0.5L/h is added in the 10L reactor of the aqueous sodium carbonate that fills 2500ml 0.3M, stirring also is heated to 25 ℃, regulate and control the pH value of reaction system between 10.6～10.8 with the aqueous slkali that makes, through 28h, the presoma granularity reaches 11.528 in the solidliquid mixture, the reinforced end isolated spherical aluminum-doped nickel cobalt acid lithium presoma.Again the presoma of preparing after filtering, deionized water wash is dried 24h under 120 ℃ of temperature.Lithium hydroxide and presoma are even with 1.05: 1 mixed, mixture are placed the stove roasting again, and 700 ℃ of following roastings 24 hours, the cooling broken classification in back obtained spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density is 2.01g/cm
3, particle mean size is 10.721 μ m, and initial capacity is 174mAh/g, and 100 times the circulation volume conservation rate is 87%, and first charge-discharge efficiency is 89%.
Example 7:
Prepare by the method for example 6 and to mix aluminium nickel hydroxide cobalt precursor and mix the back temperature with lithium salts and be controlled at 800 ℃, the time is 24h, and the broken classification in cooling back obtains spherical aluminum-doped nickel cobalt acid lithium material.
Through check, this aluminum-doped nickel cobalt acid lithium tap density 2.15g/cm
3, granularity 10.215 μ m, initial capacity 170mAh/g, 100 times the circulation volume conservation rate is 85%, first charge-discharge efficiency is 84%.
As seen Shang Mian specific embodiment has better cycle performance and overcharging resisting performance with the lithium ion battery of method of the present invention preparation with the sour lithium of spherical aluminum-doped nickel cobalt thus.
Claims (7)
1. a lithium ion battery may further comprise the steps with the preparation method of spherical aluminum-doped nickel cobalt acid lithium:
(1) preparation of ball-shape nickel hydroxide cobalt aluminium presoma: a) with mol ratio be the salting liquid that 80: 15: 5 nickel, cobalt, aluminium salt is hybridly prepared into 1.5～2.5M, NaOH is mixed with the aqueous slkali of 5.5～6.5M and adds the complexing agent of 0.5～1M, the volume ratio of salting liquid and aqueous slkali is 25: 1～4: 1; Two kinds of solution that b) will prepare add simultaneously by peristaltic pump and contain in the 10L reactor that 1.5-2.5L concentration is the 0.25-0.75M carbonate aqueous solution, the mixing salt solution charging rate is 20ml/min, the charging rate of the aqueous slkali that makes in regulating a) with the pH value of control reaction system between 9～13, stirring also is heated to 20～80 ℃, reaction is carried out between 20～30h, the presoma granularity reaches 8～15 o'clock reinforced end, isolates ball-shape nickel hydroxide cobalt aluminium presoma then; C) with the oven dry after deionized water wash filters of ball-shape nickel hydroxide cobalt aluminium presoma, make ball-shape nickel hydroxide cobalt aluminium presoma;
(2) preparation of spherical aluminum-doped nickel cobalt acid lithium: a) lithium source and the ball-shape nickel hydroxide cobalt aluminium presoma that makes are mixed; B) with mixture 700～900 ℃ roasting temperature 20～30 hours, cool off after the roasting and broken classification, obtain spherical aluminum-doped nickel cobalt acid lithium.
2. preparation method according to claim 1 is characterized in that: described nickel, cobalt, aluminium salt are its sulfate, nitrate or chlorate.
3. preparation method according to claim 1 is characterized in that: described complexing agent is a kind of or wherein several mixture in ammoniacal liquor, carbonic hydroammonium, citric acid and the oxalic acid.
4. preparation method according to claim 1 is characterized in that: described carbonate is a kind of or wherein several mixture in sodium carbonate, sodium acid carbonate and the carbonic hydroammonium.
5. preparation method according to claim 1 is characterized in that: described lithium source is a kind of or wherein several mixture in LITHIUM BATTERY lithium hydroxide, lithium nitrate and the lithium carbonate.
6. preparation method according to claim 1 is characterized in that: described sintering temperature is 700～800 ℃.
7. preparation method according to claim 1 is characterized in that: described roasting time is 20～24 hours.
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| US10903516B2 (en) | 2016-12-19 | 2021-01-26 | Grst International Limited | Method of preparing cathode material for secondary battery |
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Effective date of registration: 20160128 Address after: Jintang County, Sichuan city of Chengdu province Chengdu 610017 ABA Industrial Development Zone into a business center, Chengdu street on the third floor room 6908 Patentee after: Chengdu BAMO technology limited liability company Address before: 300384 Tianjin Huayuan Industrial Park No. 5 Yuan Lu GUI Patentee before: Tianjin B & M Science and Technology Joint-Stock Co., Ltd. |