CN109942031A - A kind of nickel-base anode material precursor and preparation method thereof - Google Patents
A kind of nickel-base anode material precursor and preparation method thereof Download PDFInfo
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- CN109942031A CN109942031A CN201910212627.6A CN201910212627A CN109942031A CN 109942031 A CN109942031 A CN 109942031A CN 201910212627 A CN201910212627 A CN 201910212627A CN 109942031 A CN109942031 A CN 109942031A
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- nickel
- anode material
- material precursor
- base anode
- conductive agent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of nickel-base anode material precursors and preparation method thereof, belong to field of lithium ion battery material, conductive agent is mixed in the nickel-base anode material precursor, the conductive agent is wrapped in the inside of nickel-base anode material precursor as the nucleus of nickel-base anode material precursor；It introduces conductive agent material in reaction solution, prepares the nickel-base anode material precursor for being enclosed with conductive agent particle while preparing presoma according to coprecipitation.The present invention introduces conductive agent in nickel-base anode material precursor, by the excellent electrical conductivity of conductive agent, unobstructed conductive network structure is formed inside nickel-base anode material precursor, improves lithium ion diffusion rate and electron transfer rate, has significant increase to the high rate performance of battery；And its preparation process is simple, actual production operating cost is low, is easy to industrialization mass production.
Description
Technical field
The present invention relates to field of lithium ion battery material, it is specifically related to a kind of nickel-base anode material precursor and its preparation
Method.
Background technique
Battery capacity is improved, accelerates charging rate, reduce the development trend that the charging time is current lithium ion battery.It utilizes
Structure, pattern, constituent and the tap density of the lithium ion battery material presoma of coprecipitation preparation will have a direct impact on
The performance of positive electrode, so can directly improve the performance of battery material to the improvement of battery material presoma, i.e., improvement lithium from
Sub- battery material presoma, to the promotion battery material structural stability of charge and discharge and safety and enhancing under high current
The application power of lithium battery has great progradation.The study on the modification of battery material is to the improvement current weakness of battery material and mentions
Rising material property has very big meaning.LiCoO2It is earliest commercialized anode material for lithium-ion batteries, cycle performance is more steady
It is fixed, it is applied to 3C Product technically reliable, but Co is at high cost, LiCoO2Specific capacity there was only 140mAh/g, be applied to power electric
Tankage is relatively low, it is difficult to reach the requirement of power battery continuation of the journey for a long time.The nickel-base anode material that scientific research personnel is researching and developing at present
Material, such as LiNi0.8Co0.1Mn0.1O2Capacity be up to 200mAh/g, have certain promotion to battery durable, but a nickel-base anode material
Due to lithium, the mixing of nickel ion and poorly conductive etc., the consequence that charge-discharge performance is poor under big multiplying power electric current is caused,
Initial capacity is high but decaying is fast.
Summary of the invention
1. technical problems to be solved
The technical problem to be solved in the present invention is that provide charge-discharge performance under a kind of big multiplying power electric current it is preferable it is Ni-based just
Pole material precursor and preparation method thereof, preparation process is simple, and actual production operating cost is low, is easy to industrialization and largely gives birth to
It produces.
2. technical solution
To solve the above problems, the present invention adopts the following technical scheme that:
A kind of nickel-base anode material precursor is mixed with conductive agent, the conduction in the nickel-base anode material precursor
Agent is wrapped in the inside of nickel-base anode material precursor, the nickel-base anode material as the nucleus of nickel-base anode material precursor
The general formula of material precursor is NixCoyMz(OH)2/ C, wherein M is Al or Mn, and 0 < x <, 1,0 < y <, 1,0 < z < 1, x+y+z
=1.
Specifically, the conductive agent is graphene, carbon nanotube CNT, carbon fiber VGCF, Ketjen black, acetylene black, SUPER-
P, any one in KS-6, KS-15, S-O.
The present invention also provides the preparation methods of above-mentioned nickel-base anode material precursor, include the following steps:
(1) nickel-base anode material precursor Ni is pressedxCoyMz(OH)2The stoichiometric ratio of element weighs soluble nickel in/C
The soluble-salt of salt, soluble element compound containing Co and M element, then adds them into deionized water, obtains salt-mixture
Solution；
(2) conductive agent and dispersing agent are taken, ultrasonic disperse obtains conductive agent solution in deionized water；
(3) precipitating reagent and complexing agent are taken, is dissolved in deionized water, mixed ammonium/alkali solutions are obtained；
(4) by institute in conduction agent solution obtained in mixing salt solution obtained in step (1), step (2) and step (3)
The mixed ammonium/alkali solutions obtained are added in reaction kettle with peristaltic pump, and carry out heating stirring, while N is passed through into reaction kettle2It protects
Gas, the pH value for controlling reaction system in reaction kettle is 8~12, and reaction temperature is 25~90 DEG C, and it is anti-that co-precipitation occurs in reaction kettle
It answers；After having reacted, precipitated product is washed with deionized and is filtered, then carries out drying and processing, finally obtain and be mixed with
The nickel-base anode material precursor Ni of conductive agentxCoyMz(OH)2/C。
Specifically, the soluble-salt of nickel element described in step (1) is any one in nickel chloride, nickel sulfate and nickel nitrate
Kind.
Specifically, the soluble-salt of M element described in step (1) is any in chlorination M, sulfuric acid M, nitric acid M and acetic acid M
It is a kind of.
Further, the additive amount of conductive agent described in step (2) is the 0.001%~30% of forerunner's weight.
Specifically, precipitating reagent described in step (3) be sodium hydroxide, sodium carbonate and potassium hydroxide in any one or it is several
The mixture of kind.
Further, first the conductive agent solution is uniformly mixed in step (4) with mixing salt solution, is then mixed with described
Aqueous slkali is closed to be added in reaction kettle simultaneously.Convenient for being sufficiently mixed for main function substance conductance agent solution and mixing salt solution.
3. beneficial effect
(1) present invention introduces conductive agent material in nickel-base anode material precursor, and obtaining has penetrating conductive network
The nickel-base anode material conductive agent presoma of structure, the introducing of conductive agent without change presoma crystal structure, in presoma
It is wrapped in conductive agent particle, enhances the conductivity of presoma, lithium ion diffusion rate and electron transfer rate are improved, to electricity
The high rate performance in pond has significant increase.
(2) present invention prepares nickel-base anode material precursor using coprecipitation, and conductive agent material is introduced in reaction solution
Material, and conductive agent used is lithium ion common used material, particle is tiny, as long as a small amount of addition is obtained with good effect,
Simple process, actual production operating cost is low, is easy to industrialization mass production.
To sum up, nickel-base anode material precursor provided by the present invention charge-discharge performance under big multiplying power electric current is preferable, and
Its preparation process is simple, and actual production operating cost is low, is easy to industrialization mass production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of nickel-base anode material precursor, chemical formula Ni0.8Co0.15Al0.05(OH)2/ C, the nickel-base anode material
Conductive agent carbon nanotube CNT is mixed in presoma, the conductive agent is wrapped up as the nucleus of nickel-base anode material precursor
In the inside of nickel-base anode material precursor.
The preparation method of above-mentioned nickel-base anode material precursor includes the following steps:
(1) the molar ratio 0.8:0.15:0.05 for pressing nickel, cobalt, aluminum metal ion, nickel sulfate, cobaltous sulfate, aluminum sulfate are dissolved in
In deionized water, match to obtain 1L mixing salt solution, wherein nickel, cobalt and aluminum ions total concentration are 2mol/L；
(2) take 3g carbon nanotube CNT as conductive agent, and appropriate dispersing agent together ultrasonic disperse in 1L deionized water,
Obtain conductive agent solution；
(3) it takes sodium hydroxide as precipitating reagent, takes ammonium hydroxide as complexing agent, be configured to the mixed base that 1L concentration is 4mol/L
Solution；
(4) conduction agent solution obtained in step (2), and heat temperature raising are first added in a kettle；Then by step (1)
In mixed ammonium/alkali solutions made in made mixing salt solution and step (3) pass through peristaltic pump simultaneously and be added dropwise in reaction kettle, and
Heating stirring is carried out, while being passed through N into reaction kettle2Make protection gas, the temperature for controlling reaction system in reaction kettle is 60 DEG C, pH
Constant is 10.65, and coprecipitation reaction occurs in reaction kettle；After having reacted, precipitated product is washed with deionized and is filtered,
Then the drying and processing that 36h is carried out in 120 DEG C of temperature environment, finally obtains before being mixed with the nickel-base anode material of conductive agent
Drive body Ni0.8Co0.15Al0.05(OH)2/C。
Embodiment 2
A kind of nickel-base anode material precursor, chemical formula Ni0.8Co0.1Al0.1(OH)2/ C, before the nickel-base anode material
Drive in body and be mixed with conductive agent graphene, the conductive agent as the nucleus of nickel-base anode material precursor be wrapped in it is Ni-based just
The inside of pole material precursor.
The preparation method of above-mentioned nickel-base anode material precursor includes the following steps:
(1) the molar ratio 0.8:0.1:0.1 for pressing nickel, cobalt, aluminum metal ion, nickel sulfate, cobaltous sulfate, aluminum sulfate are dissolved in
In ionized water, match to obtain 1L mixing salt solution, wherein nickel, cobalt and aluminum ions total concentration are 2mol/L；
(2) take 8g graphene as conductive agent, and appropriate dispersing agent together led in 1L deionized water by ultrasonic disperse
Electric agent solution；
(3) it takes sodium hydroxide as precipitating reagent, takes ammonium hydroxide as complexing agent, be configured to the mixed base that 1L concentration is 4mol/L
Solution；
(4) first conduction agent solution obtained in step (2) is uniformly mixed with mixing salt solution made in step (1)
Afterwards, then pass through peristaltic pump simultaneously with mixed ammonium/alkali solutions made in step (3) to be added dropwise in reaction kettle, and carry out heating stirring,
N is passed through into reaction kettle simultaneously2Make protection gas, the temperature for controlling reaction system in reaction kettle is 40 DEG C, and pH constant is 11.1, instead
It answers and coprecipitation reaction occurs in kettle；After having reacted, precipitated product is washed with deionized and is filtered, then at 140 DEG C
The drying and processing that 36h is carried out in temperature environment, finally obtains the nickel-base anode material precursor for being mixed with conductive agent
Ni0.8Co0.1Al0.1(OH)2/C。
Embodiment 3
A kind of nickel-base anode material precursor, chemical formula Ni0.85Co0.05Mn0.1(OH)2/ C, the nickel-base anode material
Conductive agent acetylene black is mixed in presoma, the conductive agent is wrapped in Ni-based as the nucleus of nickel-base anode material precursor
The inside of positive electrode material precursor.
The preparation method of above-mentioned nickel-base anode material precursor includes the following steps:
(1) the molar ratio 0.85:0.05:0.1 for pressing nickel, cobalt, manganese Metal ion, nickel sulfate, cobaltous sulfate, manganese sulfate are dissolved in
In deionized water, match to obtain 1L mixing salt solution, wherein the total concentration of nickel, cobalt and manganese ion is 2mol/L；
(2) take 12g acetylene black as conductive agent, and ultrasonic disperse obtains appropriate dispersing agent in 1L deionized water together
Conductive agent solution；
(3) it takes sodium hydroxide as precipitating reagent, takes ammonium hydroxide as complexing agent, be configured to the mixed base that 1L concentration is 4mol/L
Solution；
(4) conduction agent solution obtained in step (3), and heat temperature raising are first added in a kettle；Then by step (1)
In mixed ammonium/alkali solutions made in made mixing salt solution and step (2) pass through peristaltic pump simultaneously and be added dropwise in reaction kettle, and
Heating stirring is carried out, while being passed through N into reaction kettle2Make protection gas, the temperature for controlling reaction system in reaction kettle is 25 DEG C, pH
Constant is 11.25, and coprecipitation reaction occurs in reaction kettle；After having reacted, precipitated product is washed with deionized and is filtered,
Then the drying and processing that 40h is carried out in 100 DEG C of temperature environment, finally obtains before being mixed with the nickel-base anode material of conductive agent
Drive body Ni0.85Co0.05Mn0.1(OH)2/C。
Embodiment 4
A kind of nickel-base anode material precursor, chemical formula Ni0.8Co0.1Mn0.1(OH)2/ C, before the nickel-base anode material
Drive in body and be mixed with conductive agent graphene, the conductive agent as the nucleus of nickel-base anode material precursor be wrapped in it is Ni-based just
The inside of pole material precursor.
The preparation method of above-mentioned nickel-base anode material precursor includes the following steps:
(1) the molar ratio 0.8:0.1:0.1 for pressing nickel, cobalt, manganese Metal ion, nickel sulfate, cobaltous sulfate, manganese sulfate are dissolved in
In ionized water, match to obtain 1L mixing salt solution, wherein nickel, cobalt and aluminum ions total concentration are 2mol/L；
(2) take 8g graphene as conductive agent, and appropriate dispersing agent together led in 1L deionized water by ultrasonic disperse
Electric agent solution；
(3) it takes sodium hydroxide as precipitating reagent, takes ammonium hydroxide as complexing agent, be configured to the mixed base that 1L concentration is 4mol/L
Solution；
(4) first conduction agent solution obtained in step (2) is uniformly mixed with mixing salt solution made in step (1)
Afterwards, then pass through peristaltic pump simultaneously with mixed ammonium/alkali solutions made in step (3) to be added dropwise in reaction kettle, and carry out heating stirring,
N is passed through into reaction kettle simultaneously2Make protection gas, the temperature for controlling reaction system in reaction kettle is 40 DEG C, pH constant is 11.1, instead
It answers and coprecipitation reaction occurs in kettle；After having reacted, precipitated product is washed with deionized and is filtered, then at 140 DEG C
The drying and processing that 36h is carried out in temperature environment, finally obtains the nickel-base anode material precursor for being mixed with conductive agent
Ni0.8Co0.1Mn0.1(OH)2/C。
Those of ordinary skill in the art it should be appreciated that more than embodiment be intended merely to illustrate the present invention,
And be not used as limitation of the invention, as long as the change in spirit of the invention, to embodiment described above
Change, modification will all be fallen in scope of the presently claimed invention.
Claims (8)
1. a kind of nickel-base anode material precursor, which is characterized in that it is mixed with conductive agent in the nickel-base anode material precursor,
The conductive agent is wrapped in the inside of nickel-base anode material precursor, the nickel as the nucleus of nickel-base anode material precursor
The general formula of base anode material presoma is NixCoyMz(OH)2/ C, wherein M is Al or Mn, and 0 < x <, 1,0 < y <, 1,0 < z
< 1, x+y+z=1.
2. a kind of nickel-base anode material precursor according to claim 1, which is characterized in that the conductive agent is graphite
Alkene, carbon nanotube CNT, carbon fiber VGCF, Ketjen black, acetylene black, any one in SUPER-P, KS-6, KS-15, S-O.
3. the preparation method of nickel-base anode material precursor according to claim 2, which is characterized in that including walking as follows
It is rapid:
(1) nickel-base anode material precursor Ni is pressedxCoyMz(OH)2The stoichiometric ratio of element weighs soluble nickel salt, solvable in/C
The soluble-salt of property element compound containing Co and M element, then adds them into deionized water, obtains mixing salt solution；
(2) conductive agent and dispersing agent are taken, ultrasonic disperse obtains conductive agent solution in deionized water；
(3) precipitating reagent and complexing agent are taken, is dissolved in deionized water, mixed ammonium/alkali solutions are obtained；
It (4) will be obtained in conduction agent solution obtained in mixing salt solution obtained in step (1), step (2) and step (3)
Mixed ammonium/alkali solutions are added in reaction kettle with peristaltic pump, and carry out heating stirring, while N is passed through into reaction kettle2Make protection gas, controls
The pH value of reaction system is 8~12 in reaction kettle processed, and reaction temperature is 25~90 DEG C, and coprecipitation reaction occurs in reaction kettle；Instead
After having answered, precipitated product is washed with deionized and is filtered, then carries out drying and processing, finally obtain and be mixed with conductive agent
Nickel-base anode material precursor NixCoyMz(OH)2/C。
4. a kind of preparation method of nickel-base anode material precursor according to claim 3, which is characterized in that step (1)
Described in nickel element soluble-salt be nickel chloride, nickel sulfate and nickel nitrate in any one.
5. a kind of preparation method of nickel-base anode material precursor according to claim 3, which is characterized in that step (1)
Described in M element soluble-salt be chlorination M, sulfuric acid M, nitric acid M and acetic acid M in any one.
6. a kind of preparation method of nickel-base anode material precursor according to claim 3, which is characterized in that step (2)
Described in conductive agent additive amount be forerunner's weight 0.001%~30%.
7. a kind of preparation method of nickel-base anode material precursor according to claim 3, which is characterized in that step (3)
Described in precipitating reagent be sodium hydroxide, sodium carbonate and potassium hydroxide in any one or a few mixture.
8. a kind of preparation method of nickel-base anode material precursor according to claim 3, which is characterized in that step (4)
It is middle to be first uniformly mixed the conductive agent solution with mixing salt solution, reaction kettle is then added simultaneously with the mixed ammonium/alkali solutions
It is interior.
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Application publication date: 20190628 |