CN103094546A - Method for preparing nickel-cobalt lithium aluminate as anode material of lithium ion battery - Google Patents
Method for preparing nickel-cobalt lithium aluminate as anode material of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a method for preparing nickel-cobalt lithium aluminate as an anode material of a lithium ion battery. The method comprises the following steps: (1) mixing a nickel-cobalt metal salt water solution, a sodium metaaluminate solution, a complexing agent and a precipitant, regulating the pH value of a reaction system to be 9 to 12, and then maintaining a stirring state to carrying out a reaction at the temperature of 30 to 80 DEG C for 20 to 200 hours, thereby obtaining nickel-cobalt aluminum hydroxide precipitates; (2) washing the nickel-cobalt aluminum hydroxide precipitates by using pure water of 50 to 100 DEG C, drying, screening the part of precipitates capable of passing through a sieve being 300 meshes, adding a lithium source to the precipitates, mixing evenly, and sintering at the temperature of 600 to 1000 DEG C, wherein oxygen is filled during the sintering process; and finally sintering for 5 to 50 hours, thereby obtaining the nickel-cobalt lithium aluminate. According to the method, the sodium metaaluminate is adopted as the lithium source, so that the nickel-cobalt aluminum elements can evenly form a coprecipitation, so that the aluminum is evenly distributed in the nickel-cobalt lithium aluminate material. As a result, the electrical performance of the material is improved, and especially the cycling performance of the material is improved.
Description
Technical field
The present invention relates to a kind of method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate.
Background technology
The advantages such as lithium ion battery has that energy density is large, discharge platform is high, has extended cycle life, memory-less effect have been widely used in the fields such as mobile phone, camera, notebook computer, also will be applied to the electrokinetic cell such as electric bicycle, electric automobile field simultaneously.
Cobalt acid lithium, lithium nickelate, lithium nickel cobalt dioxide, nickle cobalt lithium manganate etc. with layer structure are the positive electrodes of present most study.Lithium cobaltate cathode material is to realize the earliest business-like positive electrode, but cobalt resource is limited and expensive, pollutes greatly, has limited its further development.Although lithium nickelate has very high discharge capacity, due to synthetic more difficult and stability of material is relatively poor, affect its application.Lithium nickel cobalt dioxide has higher capacity, cobalt mix the synthetic difficulty that has reduced material, but its cycle performance is not ideal enough, how changing its cycle performance is the difficult point that lithium nickel cobalt dioxide is used.The advantages such as it is high that nickel-cobalt lithium manganate cathode material has cost performance, and electrical property is better will have the trend that progressively replaces cobalt acid lithium, but the energy density that how further to improve material is still waiting research.
Nickel cobalt lithium aluminate has the energy density greater than 180mhA/g, due to the stability of greatly having improved material structure of mixing of aluminium, has improved the cycle performance of material, in the power field, boundless application market will be arranged.
Synthetic main aluminium ion and the nickel cobalt ions of adopting of nickel cobalt lithium aluminate precipitates by NaOH together at present.Such as Chinese patent CN101262061A discloses a kind of lithium ion battery with spherical aluminum-doped nickel cobalt lithium aluminate and preparation method thereof, adopt the metal salt solution of nickel cobalt aluminium and NaOH precipitation to synthesize nickel cobalt aluminium presoma.Chinese patent CN102173465A discloses a kind of preparation method of lithium ion anode material nickel cobalt lithium aluminate, adopt metal salt solution and the synthetic nickel cobalt aluminium presoma of precipitation reagent precipitation of nickel cobalt aluminium, due to the hydrolysis ph value of aluminium salt in 3.2 left and right, and the pH value of selective precipitation is 10 ~ 12, aluminium ion is more difficult like this forms homogeneous coprecipitation with the nickel cobalt ions, be difficult to reach the equally distributed purpose of nickel cobalt aluminium element, will cause aluminium skewness in nickel cobalt lithium aluminate material, affect the electrical property of material, especially cycle performance.
Summary of the invention
In order to overcome in the existing method for preparing nickel cobalt lithium aluminate, aluminium ion is more difficult forms the problem of co-precipitation with the nickel cobalt ions, the object of the present invention is to provide a kind of method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate, the method can make nickel cobalt aluminium be formed uniformly co-precipitation better, the nickel cobalt lithium aluminate anode material spherical degree for preparing is good, capacity is high, cycle performance is good, has wide market prospects.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate comprises the following steps:
(1) with nickel cobalt aqueous metal salt, sodium aluminate solution, complexing agent and precipitant mix, the pH value of conditioned reaction system is 9-12, then keep to stir, reaction 20-200 hour under 30-80 ℃, obtains nickel cobalt aluminium hydroxide precipitation;
(2) with nickel cobalt aluminium hydroxide precipitation with 50-100 ℃ of pure water washing, drying, screening can be crossed the part of 300 mesh sieves, adds the lithium source, mix rear at 600-1000 ℃ of lower sintering, during pass into oxygen, obtain nickel cobalt lithium aluminate after sintering 5-50 hour;
Described sodium aluminate solution can adopt more than one hydro-oxidation sodium solutions of aluminum sulfate, aluminum nitrate, aluminium chloride or sodium metaaluminate formulated;
The preferred ammoniacal liquor of described complexing agent;
The preferred NaOH of described precipitation reagent;
The described stirring of step (1) is the rotating speed stirring with 100-500 rev/min;
The described oxygen that passes into of step (2), its flow is 0.1-10L/h.
The present invention has following advantage and effect with respect to prior art:
In method of the present invention, aluminium source employing sodium metaaluminate can make nickel cobalt aluminium element evenly form co-precipitation, and aluminium is evenly distributed in nickel cobalt lithium aluminate material, can improve the material electrical property, especially cycle performance.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the nickel cobalt lithium aluminate that obtains of embodiment 1.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate comprises the following steps:
(1) be that 8:1.5, nickel cobalt total mol concentration are 200 liters of the solution of 2.0mol/L with nickelous sulfate, cobaltous sulfate preparation nickel cobalt mol ratio;
(2) be 100 liters of 0.2mol/L sodium aluminate solutions with 4.0mol/L sodium hydroxide solution compound concentration;
(3) the above-mentioned aqueous metal salt for preparing, sodium aluminate solution are added in reactor by certain flow and stream, add simultaneously that NaOH is done precipitation reagent, ammoniacal liquor is made complexing agent, controlling the reaction kettle for reaction temperature is 55 ℃, ammonia concn is 10.0g/L, pH value in reaction is 11.50, react after 40 hours sedimentation and filtration, with after 80 ℃ of pure hot water washing sediments, washing, sediment being put into 110 ℃ of drying boxes dry 10 hours, after drying, sediment is carried out obtaining nickel cobalt aluminium hydroxide after 300 mesh sieves divide.
(4) with above-mentioned hydroxide and 1.05 times of theoretical amount (in theory, the consumption of lithium carbonate be the hydroxide quality 37.93%) lithium carbonate mix, put into atmosphere Muffle furnace sintering after mixing, 820 ℃ of sintering temperatures, sintering time 15 hours, oxygen flow 2.0L/h, sintering obtains nickel cobalt lithium aluminate complete dividing through broken and 200 mesh sieves.
Fig. 1 is the scanning electron microscope (SEM) photograph of the nickel cobalt lithium aluminate that obtains of the present embodiment, and as seen from Figure 1: the nickel cobalt lithium aluminate particle that the present embodiment obtains is spherical in shape.
The chemical composition composition of preparation-obtained nickel cobalt lithium aluminate particle sees Table one, and its physical property sees Table two.
Table one: chemical composition (analyzing with the plasmatron spectrographic analysis method)
| Element | Ni | Co | Al | Li |
| The quality percentage composition | 48.02 | 9.05 | 1.52 | 7.22 |
Table two: physical property
The particle size distribution of the preparation-obtained nickel cobalt of the present embodiment lithium aluminate particle is moderate as can be seen from Table II, and tap density is higher, and initial capacity is high, good cycle.
Embodiment 2
A kind of method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate comprises the following steps:
(1) be that 7:2.5, nickel cobalt manganese total mol concentration are 200 liters of the solution of 2.0mol/L with nickelous sulfate, cobaltous sulfate preparation nickel cobalt mol ratio;
(2) be 100 liters of 0.2mol/L sodium aluminate solutions with 4.0mol/L sodium hydroxide solution compound concentration;
(3) the above-mentioned aqueous metal salt for preparing, sodium aluminate solution are added in reactor by certain flow and stream, add simultaneously that NaOH is done precipitation reagent, ammoniacal liquor is made complexing agent, controlling the reaction kettle for reaction temperature is 30 ℃, ammonia concn is 10.0g/L, pH value in reaction is 9.0, react after 200 hours sedimentation and filtration, with after 50 ℃ of pure hot water washing sediments, washing, sediment being put into 110 ℃ of drying boxes dry 10 hours, after drying, sediment is carried out obtaining nickel cobalt aluminium hydroxide after 300 mesh sieves divide.
(4) with above-mentioned hydroxide and 1.05 times of theoretical amount (in theory, the consumption of lithium carbonate be the hydroxide quality 38.01%) lithium carbonate mix, put into atmosphere Muffle furnace sintering after mixing, 600 ℃ of sintering temperatures, sintering time 50 hours, oxygen flow 2.0L/h, sintering obtains nickel cobalt lithium aluminate complete dividing through broken and 200 mesh sieves.
The testing result of product is as follows:
Table three: chemical composition (analyzing with the plasmatron spectrographic analysis method)
| Element | Ni | Co | Al | Li |
| The quality percentage composition | 42.12 | 15.15 | 1.50 | 7.12 |
Table four: physical property
The particle size distribution of the preparation-obtained nickel cobalt of the present embodiment lithium aluminate particle is moderate as can be seen from Table IV, and tap density is higher, and initial capacity is high, good cycle.
Above-described embodiment is the better execution mode of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (4)
1. method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate is characterized in that comprising the following steps:
(1) with nickel cobalt aqueous metal salt, sodium aluminate solution, complexing agent and precipitant mix, the pH value of conditioned reaction system is 9-12, then keep to stir, reaction 20-200 hour under 30-80 ℃, obtains nickel cobalt aluminium hydroxide precipitation;
(2) with nickel cobalt aluminium hydroxide precipitation with 50-100 ℃ of pure water washing, drying, screening can be crossed the part of 300 mesh sieves, adds the lithium source, mix rear at 600-1000 ℃ of lower sintering, during pass into oxygen, obtain nickel cobalt lithium aluminate after sintering 5-50 hour.
2. the method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate according to claim 1, it is characterized in that: described complexing agent is ammoniacal liquor.
3. the method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate according to claim 1, it is characterized in that: described precipitation reagent is NaOH.
4. the method for preparing the lithium ion battery anode material nickel cobalt lithium aluminate according to claim 1, it is characterized in that: the described oxygen that passes into of step (2), its flow is 0.1-10L/h.
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| CN103700844A (en) * | 2013-12-18 | 2014-04-02 | 江苏科捷锂电池有限公司 | Preparation method of lithium ion battery nickel, cobalt and aluminum composite ternary cathode material |
| CN103904319A (en) * | 2014-03-04 | 2014-07-02 | 广东邦普循环科技有限公司 | Preparation method of power type nickel-cobalt lithium manganate positive electrode material |
| CN104649336A (en) * | 2015-02-09 | 2015-05-27 | 深圳市贝特瑞新能源材料股份有限公司 | Preparation method of spherical nickel-cobalt-aluminum hydroxide precursor |
| CN105355910A (en) * | 2015-11-13 | 2016-02-24 | 中南大学 | A preparing method of a spherical nickel cobalt lithium aluminate cathode material for lithium ion batteries |
| CN105390667A (en) * | 2015-12-14 | 2016-03-09 | 山东精工电子科技有限公司 | Method for preparing spherical lithium battery cathode material LiNixCoyAl1xyO2 based on normal distribution of aluminum concentration |
| CN106328936A (en) * | 2016-09-06 | 2017-01-11 | 多氟多（焦作）新能源科技有限公司 | Preparation method of coated spherical nickel-cobalt-aluminum precursor, and preparation method of nickel-cobalt-lithium aluminate pole materials |
| CN106992285A (en) * | 2017-03-17 | 2017-07-28 | 广东芳源环保股份有限公司 | A kind of preparation method of nickel cobalt aluminium ternary precursor |
| CN108172824A (en) * | 2017-11-28 | 2018-06-15 | 清远佳致新材料研究院有限公司 | A kind of method for preparing battery material presoma nickel cobalt aluminium |
| CN108321365A (en) * | 2017-12-22 | 2018-07-24 | 合肥国轩高科动力能源有限公司 | TiO 22Method for coating modified NCA positive electrode material |
| EP3297072A4 (en) * | 2015-05-08 | 2018-10-31 | Guangzhou Libode New Material Co., Ltd | Methods for preparing nickel-cobalt-aluminum precursor material and or positive electrode material with gradient distribution of aluminum element |
| CN109264794A (en) * | 2018-08-31 | 2019-01-25 | 天能电池(芜湖)有限公司 | Lithium ion battery nickel cobalt aluminium ternary anode material precursor preparation process |
| CN109560283A (en) * | 2018-11-30 | 2019-04-02 | 中钢集团安徽天源科技股份有限公司 | A kind of preparation method of the nickel cobalt aluminium ternary precursor of continuous concentration gradient |
| CN110061208A (en) * | 2019-04-03 | 2019-07-26 | 深圳鸿鹏新能源科技有限公司 | Lithium battery anode active material presoma and preparation method thereof, lithium battery anode active material and preparation method thereof and lithium battery |
| CN110752366A (en) * | 2019-10-29 | 2020-02-04 | 广东省稀有金属研究所 | Nickel-cobalt-aluminum hydroxide precursor, preparation method thereof, positive electrode material and battery |
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| CN103904319B (en) * | 2014-03-04 | 2015-10-07 | 广东邦普循环科技有限公司 | A kind of preparation method of power type nickel-cobalt lithium manganate cathode material |
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| CN105355910A (en) * | 2015-11-13 | 2016-02-24 | 中南大学 | A preparing method of a spherical nickel cobalt lithium aluminate cathode material for lithium ion batteries |
| CN105390667A (en) * | 2015-12-14 | 2016-03-09 | 山东精工电子科技有限公司 | Method for preparing spherical lithium battery cathode material LiNixCoyAl1xyO2 based on normal distribution of aluminum concentration |
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| CN113809321A (en) * | 2021-09-15 | 2021-12-17 | 深圳石墨烯创新中心有限公司 | Preparation method and application of precursor of aluminum and zirconium doped lithium nickelate cathode material |
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| CN115057489B (en) * | 2022-07-28 | 2023-08-08 | 中南大学 | Cobalt-free positive electrode material, precursor thereof and preparation method |
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