CN109678217A - The Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method and application of material - Google Patents
The Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method and application of material Download PDFInfo
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Abstract
A kind of Ni of high-tap density of the present invention0.8Co0.1Mn0.1(OH)2The preparation method of material, specific implementation step is as follows: with molar ratio being solution a that 8:1:1 is configured to concentration as 2mol/L by nickel sulfate, cobaltous sulfate, manganese sulfate, concentrated ammonia liquor is diluted to the solution b that concentration is 3~5mol/L, concentrated ammonia liquor is diluted to the solution c that concentration is 5~8mol/L, sodium hydroxide is configured to the solution d of 3mol/L;Dissolution of ascorbic acid is formed into solution e in water.Then solution b and solution e are successively poured into the reaction kettle of 20L as bottom liquid.Nitrogen is passed into reaction kettle as protective gas.Temperature sets 55 DEG C, is 800r/min by stirring rate, controls pH value between 10-11.Crude product Ni is obtained after reacting 50h0.8Co0.1Mn0.1(OH)2Material.Crude product is heat-treated in atmosphere furnace and obtains the Ni of high-tap density0.8Co0.1Mn0.1(OH)2Material.Present invention process is simple, safe, low in cost, gained hydroxide nickel cobalt manganese persursor material even particle distribution, with excellent microstructure, and has preferable chemical property.
Description
Technical field
The present invention relates to lithium ion battery material technical field, in particular to a kind of Ni of high-tap density0.8Co0.1Mn0.1
(OH)2The preparation method of material, the Ni as made from this method0.8Co0.1Mn0.1(OH)2Material and its application.
Background technique
The problem of environmental pollution got worse forces people to abandon using three great tradition fossil fuels.And annual automobile is disappeared
The fossil fuel of consumption is just difficult to estimate, and more frighteningly, annual automobile quantity is also increasing.And lithium ion battery is incited somebody to action
This status can be reversed.It is being pursued by people using the new-energy automobile of lithium ion battery.The energy storage of new-energy automobile
The quality of equipment will directly influence its cruising ability.
Currently, the energy storage device of new-energy automobile uses lithium ion battery.Lithium ion battery is by positive electrode, bears
What the critical materials such as pole material, diaphragm, electrolyte, shell were constituted.Therefore, the superiority and inferiority of positive electrode performance will directly influence electricity
The quality of pond performance.
First generation positive electrode is mainly cobalt acid lithium, good cycling stability, gram volume height.But cobalt is as important war
Slightly resource price is expensive, and large-scale commercial use cost is too high.In recent years, nickel-cobalt-manganternary ternary anode material causes people's
Greatly concern.The gram volume of ternary material is high, good cycling stability, and voltage platform is high, and the price of nickel salt and manganese salt is insufficient
Cobalt salt is 1/10th.Wherein the content of nickel is higher in ternary material, and gram volume is higher;Meanwhile the content of manganese is lower, knot
Structure is more unstable, so 811 type nickel-cobalt-manganternary ternary anode materials most application value.
And the key technology for preparing 811 type nickel-cobalt-manganternary ternary anode materials is to prepare presoma-Ni0.8Co0.1Mn0.1
(OH)2Material.The main method for preparing presoma at present has solid phase method, ball-milling method, Sol-gel method, coprecipitation etc..Wherein most
Good preparation method is when first-elected coprecipitation, because the presoma homogeneity of coprecipitation preparation is good, sphericity is high, and pattern can
Control.But there are many control factor of coprecipitation, such as: pH value, reaction temperature, the concentration of salting liquid, the concentration of ammonia, alkali it is dense
Degree, flow velocity of the flow velocity of salting liquid, the flow velocity of ammonia, alkali etc. can all influence the pattern and its tap density of presoma.At present
Presoma reported in the literature all shows not fully up to expectations on pattern and tap density the two important indicators.Therefore, we
It is proposed a kind of Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method of material.
Summary of the invention
Poor in order to improve 811 type ternary anode material precursor material spherical degree, the problems such as tap density is low, the present invention mentions
A kind of Ni of high-tap density is gone out0.8Co0.1Mn0.1(OH)2The preparation method of material, as made from this method
Ni0.8Co0.1Mn0.1(OH)2Material and its application.
The present invention provides a kind of Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method of material, preparation process
It is configured to concentration for the ratio by nickel sulfate, cobaltous sulfate, manganese sulfate with molar ratio for 8:1:1 as the solution a of 2mol/L, it will be industrial
Concentrated ammonia liquor is diluted to the solution b that concentration is 3~5mol/L, and industrial concentrated ammonia liquor is diluted to the solution c that concentration is 5~8mol/L,
Sodium hydroxide is configured to the solution d of 3mol/L;Suitable dissolution of ascorbic acid is formed into solution e in water.Then by solution b
It is successively poured into solution e in the reaction kettle of 25L as bottom liquid, stirring rate is set as 200r/min, temperature of reaction kettle setting
It is 40-60 DEG C.Nitrogen is passed into reaction kettle as protective gas, to guarantee Mn2+Not oxidized, wherein the flow velocity of nitrogen is set
Being set to 100mL/min is advisable.When temperature is increased to set temperature, stirring rate is increased to 800r/min, and start to be pumped into
Solution a, adding rate are set as 3mL/min;It is immediately pumped into solution c, adding rate is set as 2mL/min;Finally by
The additive amount of solution d is controlled to control pH value between 10-13.Solution is taken out after reacting 50h, is filtered, 80-120 DEG C true
The dry 24-48h of sky, then sieve with 100 mesh sieve to obtain crude product Ni0.8Co0.1Mn0.1(OH)2Material.By crude product in air dry oven
2-15h is kept the temperature at 120-250 DEG C obtains the Ni of high-tap density0.8Co0.1Mn0.1(OH)2Material.
The present invention also provides a kind of Ni0.8Co0.1Mn0.1(OH)2Material passes through above-mentioned high-tap density
Ni0.8Co0.1Mn0.1(OH)2The preparation method of material is made.
The present invention also provides a kind of above-mentioned Ni0.8Co0.1Mn0.1(OH)2The application of material, specially high-tap density
Spherical Ni0.8Co0.1Mn0.1(OH)2The presoma that material can be used as tertiary cathode material uses, by Ni0.8Co0.1Mn0.1(OH)2Material
The superior 811 type tertiary cathode material of chemical property can be obtained in high temperature sintering again after material mixing lithium source.Wherein sintering step
Are as follows: above-mentioned persursor material is mixed with lithium source according to the ratio uniform that lithium metal molar ratio is 1:1.02~1:1.2, will be mixed
Powder afterwards can get high-performance after the processing such as wet-treating, two burning of cladding after being heat-treated 10-20h at 700 DEG C -900 DEG C
811 type tertiary cathode materials.
Further, the lithium source is one or both of lithium carbonate, monohydrate lithium hydroxide, lithium acetate, lithium nitrate.
Further, the lithium metal molar ratio of presoma and lithium source is set as 1:1.04~1 in the high-temperature burning process:
1.10。
Further, heat treatment temperature is 700 DEG C -850 DEG C in the high-temperature burning process.
Further, the high-temperature burning process soaking time is set as 10-15h.
Compared with prior art, the beneficial effects of the present invention are:
The present invention is prepared for the hydroxide nickel cobalt manganese persursor material of high-tap density using coprecipitation.It is anti-by adjusting
The flow velocity of temperature, pH value, salinity, ammonia concn, alkali concentration, the flow velocity of salt, ammonia flow rate and alkali during answering is controlled
Make its pattern and tap density.The persursor material of high-tap density will directly influence sintered tertiary cathode material
Energy density.
A kind of Ni prepared by the present invention0.8Co0.1Mn0.1(OH)2Material is pure phase, and even particle size distribution has high vibration density
Degree and spherical morphology.Vibration 200 times per minute, the tap density of persursor material reaches as high as after 3000 concussion tests
2.4g/cm3.It mixes the processing such as the primary calcining of the later warp of lithium source, wet-treating, two burning of cladding and obtains nickelic tertiary cathode material
Chemical property is superior (selecting optimal electrochemical data): the specific discharge capacity at 0.1C is up to 205.6.mAh g-1, for the first time
Coulombic efficiency is up to 90.33%, and the capacity retention ratio after 3.0-4.2V, lower 800 circulations of 1C/1C charge and discharge system is
94%, cycle performance is superior.
Detailed description of the invention
Fig. 1 and Fig. 2 is respectively the X-ray diffractogram of 2 sample of embodiment 1 and embodiment.Wherein, abscissa be 2 θ/°, θ is
The angle of diffraction;
Fig. 3 and Fig. 4 is respectively the scanning electron microscope diagram under 3,000 times of embodiment 1 and 2 sample of embodiment;
Fig. 5 and Fig. 6 is respectively 2 sample finished product tertiary cathode material full battery cycle performance curve of embodiment 1 and embodiment;
Fig. 7 is the Ni of the application0.8Co0.1Mn0.1(OH)2The schematic diagram of the preparation method of material.
Specific embodiment
A kind of Ni of high-tap density of the present invention0.8Co0.1Mn0.1(OH)2The preparation method of material, specifically as follows
Implement:
As shown in fig. 7, the ratio by nickel sulfate, cobaltous sulfate, manganese sulfate with molar ratio for 8:1:1 is configured to concentration is
Industrial concentrated ammonia liquor is diluted to the solution b that concentration is 3~5mol/L, industrial concentrated ammonia liquor is diluted to concentration by the solution a of 2mol/L
For the solution c of 5~8mol/L, sodium hydroxide is configured to the solution d of 3mol/L;By suitable dissolution of ascorbic acid Yu Shuizhong shape
At solution e.Then solution b and solution e are successively poured into the reaction kettle of 25L as bottom liquid, stirring rate is set as 200r/
Min, temperature of reaction kettle are set as 40-60 DEG C.Nitrogen is passed into reaction kettle as protective gas, to guarantee Mn2+Not by oxygen
Change, wherein the flow rate set of nitrogen is advisable for 100mL/min.When temperature is increased to set temperature, stirring rate is increased to
800r/min, and start to be pumped into solution a, adding rate is set as 3mL/min;Immediately it is pumped into solution c, adding rate setting
For 2mL/min;PH value is controlled between 10-13 finally by the additive amount of control solution d.Solution is taken after reacting 50h
Out, it filters, 80-120 DEG C of vacuum drying 24-48h, then sieves with 100 mesh sieve to obtain crude product Ni0.8Co0.1Mn0.1(OH)2Material.It will be thick
Product keep the temperature 2-15h in air dry oven and obtain the Ni of high-tap density at 120-250 DEG C0.8Co0.1Mn0.1(OH)2Material.
The Ni of 1 high-tap density of embodiment0.8Co0.1Mn0.1(OH)2The preparation of material
Ratio by nickel sulfate, cobaltous sulfate, manganese sulfate with molar ratio for 8:1:1 is configured to concentration as the solution a of 2mol/L,
Industrial concentrated ammonia liquor is diluted to the solution b that concentration is 4mol/L, industrial concentrated ammonia liquor is diluted to the solution c that concentration is 5mol/L,
Sodium hydroxide is configured to the solution d of 3mol/L;Suitable dissolution of ascorbic acid is formed into solution e in water.Then by solution b
It is successively poured into solution e in the reaction kettle of 25L as bottom liquid, stirring rate is set as 200r/min, temperature of reaction kettle setting
It is 60 DEG C.Nitrogen is passed into reaction kettle as protective gas, the flow rate set of nitrogen is advisable for 100mL/min.Work as temperature
When being increased to set temperature, stirring rate is increased to 800r/min, and starts to be pumped into solution a, adding rate is set as 3mL/
min;It is immediately pumped into solution c, adding rate is set as 2mL/min;PH is controlled finally by the additive amount of control solution d
Value is 11.Solution is taken out after reacting 50h, is filtered, 80 DEG C of vacuum drying for 24 hours, then sieve with 100 mesh sieve to obtain crude product
Ni0.8Co0.1Mn0.1(OH)2Material.Crude product is kept the temperature at 120 DEG C to 10h in air dry oven and obtains high-tap density
Ni0.8Co0.1Mn0.1(OH)2Material.
Performance test and characterization
Fig. 1 is 1 sample XRD diagram of embodiment, and discovery diffraction maximum is consistent with standard card JCPDS (14-117) diffraction maximum,
With the typical layer structure feature of tertiary cathode material.Diffraction maximum in figure is all very sharp, illustrates that the crystal form of sample is more complete
It is whole.There is no impurity peaks to illustrate that the purity of material is very high.
Table first is that 1 sample of embodiment Atomic Emission Spectrometer AES testing result, analysis data can be found that embodiment sample
Element ratio and design at the beginning of be consistent substantially.More illustrate the reliability of this technique.
One embodiment 1ICP of table test
Fig. 3 is the SEM figure of 1 sample of embodiment.It is apparent that the sphericity of embodiment sample is very high, homogeneity is good, particle ruler
It is very little substantially in 10 microns.Tap density is up to 2.29g/cm3, by a burning, wet-treating, cladding two after mixing lithium source
Nickelic tertiary cathode material chemical property is as shown in Figure 5 after the processing such as burning: the specific discharge capacity at 0.1C is up to
203.6.mAh g-1, coulombic efficiency is up to 89.70% for the first time, after 3.0-4.2V, lower 500 circulations of 1C/1C charge and discharge system
Capacity retention ratio be 95%, cycle performance is superior.
The Ni of 2 high-tap density of embodiment0.8Co0.1Mn0.1(OH)2The preparation of material
Ratio by nickel sulfate, cobaltous sulfate, manganese sulfate with molar ratio for 8:1:1 is configured to concentration as the solution a of 2mol/L,
Industrial concentrated ammonia liquor is diluted to the solution b that concentration is 5mol/L, industrial concentrated ammonia liquor is diluted to the solution c that concentration is 7mol/L,
Sodium hydroxide is configured to the solution d of 3mol/L;Suitable dissolution of ascorbic acid is formed into solution e in water.Then by solution b
It is successively poured into solution e in the reaction kettle of 25L as bottom liquid, stirring rate is set as 200r/min, temperature of reaction kettle setting
It is 50 DEG C.Nitrogen is passed into reaction kettle as protective gas, the flow rate set of nitrogen is advisable for 100mL/min.Work as temperature
When being increased to set temperature, stirring rate is increased to 800r/min, and starts to be pumped into solution a, adding rate is set as 3mL/
min;It is immediately pumped into solution c, adding rate is set as 2mL/min;PH is controlled finally by the additive amount of control solution d
Value is 11.Solution is taken out after reacting 50h, is filtered, 120 DEG C of vacuum drying for 24 hours, then sieve with 100 mesh sieve to obtain crude product
Ni0.8Co0.1Mn0.1(OH)2Material.Crude product is kept the temperature at 200 DEG C to 10h in air dry oven and obtains high-tap density
Ni0.8Co0.1Mn0.1(OH)2Material.
Performance test and characterization
Fig. 2 is 1 sample XRD diagram of embodiment, and discovery diffraction maximum is consistent with standard card JCPDS (14-117) diffraction maximum,
With the typical layer structure feature of tertiary cathode material.Diffraction maximum in figure is all very sharp, illustrates that the crystal form of sample is more complete
It is whole.There is no impurity peaks to illustrate that the purity of material is very high.
Table second is that embodiment sample Atomic Emission Spectrometer AES testing result, analysis data can be found that embodiment sample
It is consistent substantially at the beginning of element ratio and design.More illustrate the reliability of this technique.
Two embodiment 2ICP of table test
Fig. 4 is the SEM figure of 2 sample of embodiment.It is apparent that the sphericity of embodiment sample is very high, homogeneity is good, particle ruler
It is very little substantially in 10 microns.Tap density is up to 2.33g/cm3, by a burning, wet-treating, cladding two after mixing lithium source
Nickelic tertiary cathode material chemical property is as shown in Figure 6 after the processing such as burning: the specific discharge capacity at 0.1C is up to 204.6mA
h g-1, coulombic efficiency is up to 90.12% for the first time, and the capacity after 3.0-4.2V, lower 500 circulations of 1C/1C charge and discharge system is protected
Holdup is 95%, and cycle performance is superior.
Claims (8)
1. the Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method of material, which comprises the steps of:
Step 1: the ratio by nickel sulfate, cobaltous sulfate, manganese sulfate with molar ratio for 8:1:1 is configured to concentration as the solution of 2mol/L
Industrial concentrated ammonia liquor is diluted to the solution b that concentration is 3~5mol/L by a, and it is 5~8mol/L that industrial concentrated ammonia liquor, which is diluted to concentration,
Solution c, sodium hydroxide is configured to the solution d of 3mol/L;Suitable dissolution of ascorbic acid is formed into solution e in water;
Step 2: solution b and solution e being successively poured into the reaction kettle of 25L as bottom liquid, stirring rate is set as 200r/
Min, temperature of reaction kettle are set as 55 DEG C;Nitrogen is passed into reaction kettle as protective gas, to guarantee Mn2+It is not oxidized,
Wherein the flow rate set of nitrogen is 100mL/min;
Step 3: when temperature is increased to 40-60 DEG C, stirring rate being increased to 800r/min, and starts to be pumped into solution a, is added
Rate is set as 3mL/min;It is immediately pumped into solution c, adding rate is set as 2mL/min;Finally by control solution d's
Additive amount controls pH value between 10-13;
Step 4: solution being taken out after reaction 50h, is filtered, 80-120 DEG C of vacuum drying 24-48h, then sieve with 100 mesh sieve to obtain crude product
Ni0.8Co0.1Mn0.1(OH)2Material;
Step 5: crude product being kept the temperature at 120-250 DEG C to 2-15h in air dry oven and obtains high-tap density
Ni0.8Co0.1Mn0.1(OH)2Material.
2. a kind of Ni0.8Co0.1Mn0.1(OH)2Material, which is characterized in that be made by preparation method described in claim 1.
3. a kind of Ni as claimed in claim 20.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the high-tap density
Ni0.8Co0.1Mn0.1(OH)2The presoma that material can be used as tertiary cathode material uses, by Ni0.8Co0.1Mn0.1(OH)2Material
Superior 811 type three of chemical property can be obtained after handling after mixing lithium source using high-temperature calcination, wet-treating, two burnings of cladding
First positive electrode.
4. Ni according to claim 30.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the high-temperature calcination step
Suddenly are as follows:
Above-mentioned persursor material is mixed with lithium source according to the ratio uniform that lithium metal molar ratio is 1:1.02~1:1.2, will be mixed
Powder after conjunction can get 811 type tertiary cathode materials after being heat-treated 10-20h at 700 DEG C -900 DEG C.
5. Ni according to claim 40.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the lithium source is carbonic acid
One or both of lithium, monohydrate lithium hydroxide, lithium acetate, lithium nitrate.
6. Ni according to claim 40.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the high-temperature calcination
The lithium metal molar ratio of presoma and lithium source is set as 1:1.04~1:1.10 in journey.
7. Ni according to claim 40.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the high-temperature calcination
Heat treatment temperature is 700 DEG C -850 DEG C in journey.
8. Ni according to claim 40.8Co0.1Mn0.1(OH)2The application of material, which is characterized in that the high-temperature calcination
Journey soaking time is set as 10-15h.
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CN112191212A (en) * | 2020-12-02 | 2021-01-08 | 河南科隆新能源股份有限公司 | Reaction kettle and method for preparing precursor of lithium ion battery anode material |
CN114655998A (en) * | 2022-03-01 | 2022-06-24 | 西安理工大学 | Preparation method of high-nickel ternary positive electrode precursor |
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