CN101229928A - Method for preparing spherical nickel-cobalt lithium manganate material - Google Patents
Method for preparing spherical nickel-cobalt lithium manganate material Download PDFInfo
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- CN101229928A CN101229928A CNA2007100343181A CN200710034318A CN101229928A CN 101229928 A CN101229928 A CN 101229928A CN A2007100343181 A CNA2007100343181 A CN A2007100343181A CN 200710034318 A CN200710034318 A CN 200710034318A CN 101229928 A CN101229928 A CN 101229928A
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Abstract
The invention discloses a preparation method of spherical nickel cobalt manganese acid lithium which takes the carbonate as a precipitant by adopting a coprecipitation method. Three solutions of metal iron of nickel cobalt manganese mixed metallic salt solution with certain concentration as well as carbonate solution and ammonium salt solution are respectively continuously added into the reactor. The flow rate is controlled until the pH value of the reaction solution is 7.9-8.5. In the solution, the concentration of the NH4<+> is 0.1mol/L-0.5mol/L and the reaction temperature is 45 DEG C-60 DEG C. The spherical precursor body material is prepared. A preheating treatment is carried out and the spherical precursor body material is then evenly mixed with the preheating treatment for the heating treatment to obtain the finishes product. The precursor body of the invention has a fast speed of being formed into a sphere and the particle size is evenly distributed with advantages of good sphericity, higher concentration and higher capacity.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, particularly relate to a kind of preparation method of lithium ion battery anode material spherical nickle cobalt lithium manganate.
Background technology
In lithium ion battery, generally adopt cobalt acid lithium as its anodal energy storage material, but, the positive electrode material that substitutes cobalt acid lithium is had higher requirement nickle cobalt lithium manganate LiNi wherein along with aspects such as the expansion of lithium ion battery applications scope, resources costs rising are considered
xCo
yMn
1-x-yO
2Material is with characteristics such as its cheap cost, heavy body and high safety performances and become the material of tool advantage.Through exploration for many years, at present the nickle cobalt lithium manganate preparation method mainly contains simple high temperature solid-state method, sol-gel method, coprecipitation method, and several different methods such as spray-drying process.But simple high temperature solid-state method is unfavorable for that because of the ununiformity of batch mixing material forms the homogeneous phase eutectic, and methods such as sol-gel method, dry spray method, all the complicacy because of its process control can't realize scale operation.The most general and the tool application prospect of research at present be to prepare persursor material with coprecipitation method, again with presoma with prepare nickel-cobalt lithium manganate material through special high-temperature heat treatment mode after mix in the lithium source.This method can be controlled the particle diameter and the sphericity of presoma product by regulating deposition condition, thereby realizes the particle diameter of the finished product and the control of distribution thereof, and the control of this condition is easy to realize in large-scale production.
Preparing with coprecipitation method in the method for persursor material, most investigator concentrates on oxyhydroxide and makes the middle presoma (Ni of precipitation agent preparation mixing
xCo
yMn
1-x-y) (OH)
2Method, disclose with the preparation method of oxyhydroxide in its patent application " based on the preparation method of the high activity anode material of lithium ion battery of crystallization control method " (CN 1218304A) and patent application " preparation method of anode material for lithium-ion batteries high density spherical nickel-cobalt lithium manganate " (CN 1622371A) as people such as Jiang Changyin as precipitation agent.With oxyhydroxide is that precipitation agent prepares in the process of presoma, because the oxyhydroxide of cobalt, manganese is very unstable, oxidation extremely easily, need protection of inert gas, the formation of its nucleus and process of growth are difficult to control, be difficult for generating spherical presoma, the technology controlling and process complexity is unfavorable for large batch of suitability for industrialized production; And, exist presoma balling-up speed slower, particle growth speed waits defective more slowly, and as the CN1622371A disclosed method, its coprecipitation reaction needs just can obtain the spheric presoma more than 20 hours; Some product sphericity is bad, is " potato " shape, thereby causes defectives such as density is little, volume and capacity ratio is less, has limited the commercial applications of spherical nickel-cobalt lithium manganate.
Summary of the invention
The present invention aims to provide that a kind of presoma balling-up speed is fast, and size distribution is even, the preparation method of product good sphericity, density is higher, electrical capacity is higher spherical nickel-cobalt lithium manganate.
The present invention includes following steps:
(1) mixed aqueous solution of preparation nickel salt, cobalt salt, manganese salt, wherein the mol ratio of three metal ion species is 1: 1: 1;
(2) preparation carbonate aqueous solution, CO
3 2-With the ratio of the volumetric molar concentration of total metal ion of solution (1) be 1.0～1.5: 1;
(3) preparation ammonium salt aqueous solution, NH
4 +The ionic volumetric molar concentration is 0.2～1.5mol/L;
(4) with (1), the solution of (2), the preparation of (3) step joins in the reactor of belt stirrer continuously with volume pump respectively, the flow of three kinds of solution of control, making the pH value of reaction solution is 7.9～8.5, NH in the reaction solution
4 +Concentration be controlled between 0.1mol/L～0.5mol/L, control reaction temperature is 45 ℃～60 ℃, controlling stirring velocity simultaneously is 500～1000 rev/mins, the overflow port nature overflow of the presoma material of generation from reactor discharged;
(5) persursor material that (4) step was made carries out solid-liquid separation, cleans sulfate ion with pure water, descends dry 3～5 hours at 60 ℃～80 ℃ then, obtains the mixed carbonate of spherical nickel-cobalt manganese;
(6) (5) mixed carbonate that obtains of step is carried out thermal pretreatment, the technology of thermal pretreatment is, rises to 480 ℃～550 ℃ with 2 ℃～5 ℃/minute temperature rise rates from room temperature, is incubated 4～6 hours;
(7) lithium salts with metering mixes by mass ratio 1: 1.2～1.5 with pure water, and ball milling is 3～4 hours in ball mill), make the lithium salts slurry;
(8) with lithium salts slurry and persursor material after thermal pretreatment Li in molar ratio: (Ni+Co+Mn)=1～1.1: 1 mixed 25～35 minutes;
(9) product of gained in the step (8) is heat-treated, thermal treatment process is, elder generation rises to 480 ℃～550 ℃ with 1 ℃～2 ℃/minute temperature rise rate from room temperature, be incubated 2～4 hours, rise to 850 ℃～950 ℃ with 1 ℃～2 ℃/minute temperature rise rate then, be incubated 15～25 hours, naturally cooling in stove obtains the spherical nickel-cobalt lithium manganate.
And the preferred 1mol/L～2.2mol/L of metal ion total concn of metal-salt mixed aqueous solution wherein, the CO of carbonate aqueous solution
3 2-Preferred 8.0～8.3 with the pH value of the reaction solution described in preferred 1.1～1.2: 1, the (4) step of ratio of the volumetric molar concentration of total metal ion of solution (1), NH
4 +The preferred 0.3mol/L～0.4mol/L of concentration, preferred 50 ℃～55 ℃ of temperature of reaction; The described lithium salts of step (7) is selected from a kind of in Quilonum Retard, lithium hydroxide, lithium nitrate or the lithium acetate.
Compare with the existing preparation processing method, the present invention has the following advantages:
1. presoma balling-up speed is fast.Can in 1 hour, make the presoma balling-up, promptly can reach ideal size 8-12 μ m in 10 hours.
2. the particle diameter of product is normal distribution, good sphericity.The spherical nickel-cobalt lithium manganate material median size for preparing is 8-10 μ m, is evenly distributed, and observes under scanning electron microscope, and as shown in drawings, the material major part all presents good ball shape.
3. the density of product and electrical capacity are higher.Because the good sphericity of product is normal distribution, helps build-up of particles, thereby makes product have higher density, after testing, the tap density of product is generally 2.3～2.5g/cm
3, be negative pole with the lithium sheet, record that the 0.2C first discharge specific capacity is 170～190mAh/g under the above-mentioned materials room temperature.
Description of drawings
Fig. 1 is the sem photograph of the spherical nickel-cobalt lithium manganate material of embodiment 1 preparation.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but these embodiment must not be used to explain limiting the scope of the invention.
Embodiment 1
(1) adopt single nickel salt, rose vitriol, manganous sulfate preparation mixed salt solution, total concentration of metal ions is 1.8mol/L, and the ratio of the volumetric molar concentration of three metal ion species is 1: 1: 1 in the solution;
(2) compound concentration is the aqueous sodium carbonate of 2mol/L, CO
3 2-With the molar concentration rate of total metal ion of solution (1) be 1.1: 1;
(3) preparation NH
4 +Ionic concn is the ammonium bicarbonate aqueous solution of 0.6mol/L;
(4) above-mentioned three kinds of solution being joined the effective volume that band stirs continuously with volume pump respectively is in the reactor of 3L, the flow of three kinds of solution of control, and making the pH value of reaction solution is 8～8.3, NH in the reaction solution
4 +Concentration be 0.2mol/L～0.3mol/L; Control reaction temperature is 60 ℃; Stirring velocity is 1000 rev/mins, and continuously feeding stopped charging after 10 hours, and the overflow port nature overflow of the presoma material of generation from reactor discharged.
(5) remove supernatant liquid after the presoma material that obtains is left standstill, use the deionized water wash solid again, the sulfate ion in cleaning the presoma material; Behind the suction filtration,, obtain the mixed carbonate of spherical nickel-cobalt manganese in 80 ℃ of dryings 2.5 hours.
(6) above-mentioned mixed carbonate is carried out thermal pretreatment, the technology of thermal pretreatment is, rises to 480 ℃ with 2 ℃/minute temperature rise rates from room temperature, is incubated 6 hours;
(7) Quilonum Retard is added in the ball grinder, press lithium salts and pure water mass ratio and add deionized water at 1: 1.2, ball milling 3 hours makes the Quilonum Retard slurry.
(8) according to Li: be 1: 1 (mol ratio) (Ni+Co+Mn), take by weighing the above-mentioned Quilonum Retard slurry of respective amount and the presoma material after the thermal pretreatment respectively, add the low speed ball milling that carried out in the ball grinder 25 minutes and mix.
(9) product of gained in the step (8) is heat-treated, thermal treatment process is that elder generation rises to 480 ℃ with 1 ℃/minute temperature rise rate from room temperature, be incubated 4 hours, rise to 850 ℃ with 1 ℃/minute temperature rise rate then, be incubated 25 hours, naturally cooling in stove obtains the spherical nickel-cobalt lithium manganate.
After testing, the spherical nickel-cobalt lithium manganate material median size for preparing is 10 μ m, is evenly distributed, and observes under scanning electron microscope, and the material major part all presents good ball shape; The tap density of product is 2.5g/cm
3, be negative pole with the lithium sheet, record that the 0.2C first discharge specific capacity is 190mAh/g under the above-mentioned materials room temperature.
Fig. 1 is the sem photograph of the prepared spherical nickel-cobalt lithium manganate of present embodiment.
Embodiment 2
(1) adopt nickelous chloride, cobalt chloride, Manganous chloride tetrahydrate preparation mixed salt solution, total concentration of metal ions is 1mol/L, and the ratio of the volumetric molar concentration of three metal ion species is 1: 1: 1 in the solution;
(2) compound concentration is the wet chemical of 1.5mol/L, CO
3 2-With the molar concentration rate of total metal ion of solution (1) be 1.5: 1;
(3) preparation NH
4 +Ionic concn concentration is the ammonium carbonate solution of 0.2mol/L,
(4) above-mentioned three kinds of solution are joined in the reactor of band stirring continuously with volume pump respectively, the flow of three kinds of solution of control, making the pH value of reaction solution is 7.9～8.1, NH in the reaction solution
4 +Concentration be 0.1mol/L～0.2mol/L; Control reaction temperature is 50 ℃; Stirring velocity is 800 rev/mins, and continuously feeding stopped charging after 10 hours, and the overflow port nature overflow of the presoma material of generation from reactor discharged.
(5) remove supernatant liquid after the presoma material that obtains is left standstill, clean chlorion in the presoma material with pure water again; Behind the suction filtration,, obtain the mixed carbonate of spherical nickel-cobalt manganese in 70 ℃ of dryings 3 hours.
(6) above-mentioned mixed carbonate is carried out thermal pretreatment, the technology of thermal pretreatment is incubated 5 hours for to rise to 500 ℃ with the temperature rise rate from 3 ℃/minute from room temperature;
(7) lithium nitrate is added in the ball grinder, press lithium salts and pure water mass ratio and add deionized water at 1: 1.5, ball milling 4 hours makes the lithium nitrate slurry.
(8) according to Li: be 1.05: 1 (mol ratio) (Ni+Co+Mn), take by weighing the above-mentioned lithium nitrate slurry of respective amount and the presoma material after the thermal pretreatment respectively, add the low speed ball milling that carried out in the ball grinder 30 minutes and mix.
(9) product of gained in the step (8) is heat-treated, thermal treatment process is incubated 3 hours for first temperature rise rate with 2 ℃/minute rises to 500 ℃ ℃ from room temperature, rise to 950 ℃ with 2 ℃/minute temperature rise rate then, be incubated 15 hours, naturally cooling in stove obtains the spherical nickel-cobalt lithium manganate.
After testing, the spherical nickel-cobalt lithium manganate material median size for preparing is 8 μ m, is evenly distributed, and observes under scanning electron microscope, and the material major part all presents good ball shape; The tap density of product is 2.4g/cm
3, be negative pole with the lithium sheet, record that the 0.2C first discharge specific capacity is 170mAh/g under the above-mentioned materials room temperature.
Embodiment 3
(1) adopt nickelous nitrate, Xiao Suangu, manganous nitrate preparation mixed salt solution, total concentration of metal ions is 2.2mol/L, and the ratio of the volumetric molar concentration of three metal ion species is 1: 1: 1 in the solution;
(2) compound concentration is the wet chemical of 2.6mol/L, CO
3 2-Be about 1.2: 1 with the molar concentration rate of total metal ion of solution (1);
(3) preparation NH
4 +Ionic concn concentration is the ammonium bicarbonate aqueous solution of 1.5mol/L,
(4) above-mentioned three kinds of solution are joined in the reactor of band stirring continuously with volume pump respectively, the flow of three kinds of solution of control, the pH value that makes reaction solution is NH in 8.3～8.5 reaction solutions
4 +Concentration be 0.4mol/L～0.5mol/L; Control reaction temperature is 55 ℃; Stirring velocity is 600 rev/mins, and continuously feeding stopped charging after 10 hours, and the overflow port nature overflow of the presoma material of generation from reactor discharged.
(5) remove supernatant liquid after the presoma material that obtains is left standstill, clean nitrate ion in the presoma material with pure water again; Behind the suction filtration,, obtain the mixed carbonate of spherical nickel-cobalt manganese in 80 ℃ of dryings 3 hours.
(6) above-mentioned mixed carbonate is carried out thermal pretreatment, the technology of thermal pretreatment is incubated 4 hours for to rise to 550 ℃ with the temperature rise rate from 5 ℃/minute from room temperature;
(7) lithium acetate is added in the ball grinder, press lithium salts and pure water mass ratio and add deionized water at 1: 1.3, ball milling 4 hours makes the lithium acetate slurry.
(8) according to Li: be 1.1: 1 (mol ratio) (Ni+Co+Mn), take by weighing the above-mentioned lithium acetate slurry of respective amount and the presoma material after the thermal pretreatment respectively, add the low speed ball milling that carried out in the ball grinder 35 minutes and mix.
(9) product of gained in the step (8) is heat-treated, thermal treatment process is incubated 2 hours for first temperature rise rate with 2 ℃/minute rises to 550 ℃ from room temperature, rise to 900 ℃ with 2 ℃/minute temperature rise rate then, be incubated 20 hours, naturally cooling in stove obtains the spherical nickel-cobalt lithium manganate.
After testing, the spherical nickel-cobalt lithium manganate material median size for preparing is 12 μ m, is evenly distributed, and observes under scanning electron microscope, and the material major part all presents good ball shape; The tap density of product is 2.5g/cm
3, be negative pole with the lithium sheet, record that the 0.2C first discharge specific capacity is 1 80mAh/g under the above-mentioned materials room temperature.
Claims (7)
1. the preparation method of a spherical nickel-cobalt lithium manganate material is characterized in that, may further comprise the steps:
(1) mixed aqueous solution of preparation nickel salt, cobalt salt, manganese salt, wherein the mol ratio of three metal ion species is 1: 1: 1;
(2) preparation carbonate aqueous solution, CO
3 2-With the molar concentration rate of the total metal ion in the mixing solutions in (1) step be 1.0～1.5: 1;
(3) preparation ammonium salt aqueous solution, NH
4 +The ionic volumetric molar concentration is 0.2～1.5mol/L;
(4) solution with the preparation of (1) (2) (3) step joins in the reactor of band stirring continuously with volume pump respectively, the flow of three kinds of solution of control, and making the pH value of reaction solution is 7.9～8.5, NH in the reaction solution
4 +Concentration be controlled between 0.1mol/L～0.5mol/L, control reaction temperature is 50 ℃～60 ℃, stirring velocity is 600～1000 rev/mins, the overflow port nature overflow of the presoma material of generation from reactor discharged;
(5) persursor material that (4) step was made carries out solid-liquid separation, cleans with pure water, descends dry 3～5 hours at 60 ℃～80 ℃ then, obtains the mixed carbonate of spherical nickel-cobalt manganese;
(6) (5) mixed carbonate that obtains of step is carried out thermal pretreatment, the technology of thermal pretreatment is, rises to 480 ℃～550 ℃ with 2 ℃～5 ℃/minute temperature rise rates from room temperature, is incubated 4～6 hours;
(7) lithium salts with metering mixes by mass ratio 1: 1.2～1.5 with pure water, and ball milling is 3～4 hours in ball mill, makes the lithium salts slurry;
(8) with lithium salts slurry and persursor material after thermal pretreatment Li in molar ratio: (Ni+Co+Mn)=1～1.1: 1 mixed 25～35 minutes;
(9) product of gained in the step (8) is heat-treated, thermal treatment process is, elder generation rises to 480 ℃～550 ℃ with 1 ℃～2 ℃/minute temperature rise rate from room temperature, be incubated 2～4 hours, rise to 850 ℃～950 ℃ with 1 ℃～2 ℃/minute temperature rise rate then, be incubated 15～25 hours, naturally cooling in stove obtains the spherical nickel-cobalt lithium manganate.
2. the preparation method of spherical nickel-cobalt lithium manganate material as claimed in claim 1, the lithium salts that it is characterized in that described step (7) is selected from a kind of in Quilonum Retard, lithium hydroxide, lithium nitrate or the lithium acetate.
3. the preparation method of spherical nickel-cobalt lithium manganate material as claimed in claim 1 is characterized in that the metal ion total concn of described metal-salt mixed aqueous solution is 1mol/L～2.2mol/L.
4. as the preparation method of claim 1 or 2 or 3 described spherical nickel-cobalt lithium manganate materials, it is characterized in that the CO of described carbonate aqueous solution
3 2-With the ratio of the volumetric molar concentration of the total metal ion of solution of described (1) step preparation be 1.1～1.2: 1.
5. as the preparation method of claim 1 or 2 or 3 described spherical nickel-cobalt lithium manganate materials, it is characterized in that the pH value of the reaction solution in described (4) step is 8.0～8.3.
6. as the preparation method of claim 1 or 2 or 3 described spherical nickel-cobalt lithium manganate materials, it is characterized in that NH in described (4) reaction solution that goes on foot
4 +Concentration be 0.2mol/L～0.3mol/L.
7. as the preparation method of claim 1 or 2 or 3 described spherical nickel-cobalt lithium manganate materials, it is characterized in that control reaction temperature is 50 ℃～55 ℃ in described (4) step.
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| CN109160545A (en) * | 2018-07-24 | 2019-01-08 | 格林美股份有限公司 | A kind of precursor of nickel-cobalt-lithium-manganese-oxide synthesizer |
| CN110854384A (en) * | 2019-11-26 | 2020-02-28 | 河北省科学院能源研究所 | Preparation method of surface-modified nickel-based electrode material |
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