CN108767256A - A kind of preparation method of battery anode material nickel cobalt lithium aluminate presoma - Google Patents
A kind of preparation method of battery anode material nickel cobalt lithium aluminate presoma Download PDFInfo
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- CN108767256A CN108767256A CN201810638114.7A CN201810638114A CN108767256A CN 108767256 A CN108767256 A CN 108767256A CN 201810638114 A CN201810638114 A CN 201810638114A CN 108767256 A CN108767256 A CN 108767256A
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- lithium aluminate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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Abstract
The invention discloses a kind of preparation methods of battery anode material nickel cobalt lithium aluminate presoma, are related to battery technology field.Nickel and cobalt solution is configured including step (1)；(2) sediment is prepared；(3) sediment is purified；(4) ready-mixed object is prepared；(5) final product is roasted.The present invention prepares nickel cobalt lithium aluminate presoma by using the method roasted with aluminum nitrate, it avoids because the aluminium ion settling velocity of trivalent is fast, it is difficult to form the case where bulky grain precipitates, there is larger real density by the nickel cobalt lithium aluminate presoma obtained after roasting；Meanwhile the acid group in precipitation is reduced by roasting and is remained, further increase the purity of nickel cobalt lithium aluminate presoma obtained.
Description
Technical field
The invention belongs to battery technology fields, more particularly to a kind of battery anode material nickel cobalt lithium aluminate presoma
Preparation method.
Background technology
Nickel cobalt aluminium tertiary cathode material (NCA, i.e. nickel cobalt lithium aluminate) has height ratio capacity, high voltage and good cycle
The advantages that performance, causes extensive concern in recent years.The main preparation methods of nickel cobalt aluminium tertiary cathode material are first useizations
It learns coprecipitation and prepares nickel cobalt aluminium presoma, then calcine with lithium salts to obtain NCA materials；Since the solubility product constant of aluminium hydroxide is
1.3 × 10-33, and respectively 2 × 10-15 and 1.6 × 10-15 of nickel hydroxide and cobalt hydroxide (divalent), therefore useization
When learning coprecipitation and preparing nickel cobalt aluminium presoma, the aluminium ion settling velocity of trivalent is especially fast, is not only difficult to and nickel and cobalt precipitate
Form uniform single layer structure, it is also difficult to form spherical macro precipitation, therefore presoma mixes the NCA that lithium salts is calcined
Material performance index is undesirable；Particle is loose, and structural stability difference and discharge capacity are relatively low.
Invention content
In order to solve the above technical problems, the present invention is achieved by the following technical solutions：
The present invention is a kind of preparation method of battery anode material nickel cobalt lithium aluminate presoma, is included the following steps：
(1) nickel and cobalt solution is configured；Nickel salt and cobalt salt are added in acid group solution, the solution of every liter of 1mol is made in proportioning；
(2) sediment is prepared；Ammonium hydroxide and lye are added in the nickel and cobalt solution prepared into step (1) under constant temperature,
Ph values are controlled between 10-11；Stir to get sediment；
(3) sediment is purified；It washs after the sediment that step (2) obtains is carried out centrifugal filtration, is dried after washing
Handle to obtain purifying sediment；
(4) ready-mixed object is prepared；It is ground after the purifying sediment of step (3) is mixed with aluminum nitrate；Grinding makes
Ready-mixed object is obtained after carrying out sieving processing with 300-500 mesh sieve；
(5) final product is roasted；By the ready-mixed object prepared in step (4) under constant heating rate, temperature is risen to
It is nickel cobalt lithium aluminate presoma to obtain final product at 500-600 degrees Celsius constant temperature calcining 8-10 hours, after natural cooling.
Further, the cobalt ions molar ratio in the nickel ion and cobalt salt in the step (1) in nickel salt is 16.3；Institute
It is sulfate radical solution or nitrate solutions to state step (1) acid group solution.
Further, in the step (2) ammonium hydroxide a concentration of 20-25%；The lye is that NaOH solution or KOH are molten
Liquid；Step (2) constant temperature is 50-60 degrees Celsius.
Further, drying temperature is 100-200 degrees Celsius in step (3).
Further, the molar ratio 19 of sediment and aluminum nitrate is purified in step (4):1；Milling time is 2-4 hours.
Further, step (5) heating rate is 4.5 degrees Celsius per minute.
The invention has the advantages that：
1, preparation process of the present invention is simple, easy to operate, requires reaction adjusting low.
2, the present invention is using method preparation nickel cobalt lithium aluminate presoma roast with aluminum nitrate, avoid aluminium because of trivalent from
Sub- settling velocity is fast, it is difficult to form the case where bulky grain precipitates, have by the nickel cobalt lithium aluminate presoma obtained after roasting
There is larger real density.
3, the present invention reduces the acid group in precipitation by roasting and remains, before further increasing nickel cobalt lithium aluminate obtained
Drive the purity of body.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
All other embodiment that technical staff is obtained without creative efforts belongs to the model that the present invention protects
It encloses.
The present invention is a kind of preparation method of battery anode material nickel cobalt lithium aluminate presoma, is included the following steps：
(1) nickel and cobalt solution is configured；It is 16 by nickel ion and cobalt ions molar ratio：It is molten that sulfate radical is added in 3 nickel salt and cobalt salt
In liquid or nitrate solutions solution, the solution of every liter of 1mol is made in proportioning；
Wherein, nickel salt and cobalt salt are soluble-salt such as sulfate or nitrate；It is preferable to use nitrate solutions and nitrate；
Convenient for being decomposed in follow-up roasting process, increase the purity of final product；
(2) sediment is prepared；It is added in the nickel and cobalt solution prepared into step (1) under 50-60 degrees Celsius of constant temperature
A concentration of 20-25% ammonium hydroxide and NaOH solution or KOH solution, control ph values are between 10-11；Stir to get sediment；
(3) sediment is purified；It is washed after the sediment that step (2) obtains is carried out centrifugal filtration, in 100-200 after washing
It is dried under degrees celsius and handles to obtain purifying sediment；
(4) ready-mixed object is prepared；By the purifying sediment of step (3) and aluminum nitrate in molar ratio 19:It is carried out after 1 mixing
Grinding；Grinding obtains ready-mixed object after carrying out sieving processing using 300-500 mesh sieve after 2-4 hours；
(5) final product is roasted；By the ready-mixed object prepared in step (4) with 4.5 degrees Celsius per minute of constant liter
Under warm rate, temperature is risen into constant temperature calcining 8-10 hours at 500-600 degrees Celsius, after natural cooling final product is nickel
Cobalt lithium aluminate presoma.
Embodiment 1
(1) nickel and cobalt solution is configured；It is 16 by nickel ion and cobalt ions molar ratio：It is molten that sulfate radical is added in 3 nickel salt and cobalt salt
In liquid or nitrate solutions solution, the solution of every liter of 1mol is made in proportioning；
Wherein, nickel salt and cobalt salt are soluble-salt such as sulfate or nitrate；It is preferable to use nitrate solutions and nitrate；
Convenient for being decomposed in follow-up roasting process, increase the purity of final product；
(2) sediment is prepared；Concentration is added in the nickel and cobalt solution prepared into step (1) under 55 degrees Celsius of constant temperatures
For 20% ammonium hydroxide and NaOH solution or KOH solution, control ph values are 10.7；Stir to get sediment；
(3) sediment is purified；It is washed after the sediment that step (2) obtains is carried out centrifugal filtration, in 100-200 after washing
It is dried under degrees celsius and handles to obtain purifying sediment；
(4) ready-mixed object is prepared；By the purifying sediment of step (3) and aluminum nitrate in molar ratio 19:It is carried out after 1 mixing
Grinding；Grinding obtains ready-mixed object after carrying out sieving processing using 400 mesh sieve after 3 hours；
(5) final product is roasted；By the ready-mixed object prepared in step (4) with 4.5 degrees Celsius per minute of constant liter
Under warm rate, temperature is risen into constant temperature calcining 9 hours at 550 degrees Celsius, after natural cooling final product is nickel cobalt aluminic acid
Lithium presoma.
Embodiment 2
(1) nickel and cobalt solution is configured；It is 16 by nickel ion and cobalt ions molar ratio：It is molten that sulfate radical is added in 3 nickel salt and cobalt salt
In liquid or nitrate solutions solution, the solution of every liter of 1mol is made in proportioning；
Wherein, nickel salt and cobalt salt are soluble-salt such as sulfate or nitrate；It is preferable to use nitrate solutions and nitrate；
Convenient for being decomposed in follow-up roasting process, increase the purity of final product；
(2) sediment is prepared；Concentration is added in the nickel and cobalt solution prepared into step (1) under 60 degrees Celsius of constant temperatures
For 25% ammonium hydroxide and NaOH solution or KOH solution, control ph values are 11；Stir to get sediment；
(3) sediment is purified；It is washed after the sediment that step (2) obtains is carried out centrifugal filtration, it is Celsius 200 after washing
It is dried under the conditions of degree and handles to obtain purifying sediment；
(4) ready-mixed object is prepared；By the purifying sediment of step (3) and aluminum nitrate in molar ratio 19:It is carried out after 1 mixing
Grinding；Grinding obtains ready-mixed object after carrying out sieving processing using 500 mesh sieve after 4 hours；
(5) final product is roasted；By the ready-mixed object prepared in step (4) with 4.5 degrees Celsius per minute of constant liter
Under warm rate, temperature is risen into constant temperature calcining 8 hours at 600 degrees Celsius, after natural cooling final product is nickel cobalt aluminic acid
Lithium presoma.
Embodiment 3
(1) nickel and cobalt solution is configured；It is 16 by nickel ion and cobalt ions molar ratio：It is molten that sulfate radical is added in 3 nickel salt and cobalt salt
In liquid or nitrate solutions solution, the solution of every liter of 1mol is made in proportioning；
Wherein, nickel salt and cobalt salt are soluble-salt such as sulfate or nitrate；It is preferable to use nitrate solutions and nitrate；
Convenient for being decomposed in follow-up roasting process, increase the purity of final product；
(2) sediment is prepared；Concentration is added in the nickel and cobalt solution prepared into step (1) under 50 degrees Celsius of constant temperatures
For 25% ammonium hydroxide and NaOH solution or KOH solution, control ph values are 10；Stir to get sediment；
(3) sediment is purified；It is washed after the sediment that step (2) obtains is carried out centrifugal filtration, it is Celsius 100 after washing
It is dried under the conditions of degree and handles to obtain purifying sediment；
(4) ready-mixed object is prepared；By the purifying sediment of step (3) and aluminum nitrate in molar ratio 19:It is carried out after 1 mixing
Grinding；Grinding obtains ready-mixed object after carrying out sieving processing using 300 mesh sieve after 2 hours；
(5) final product is roasted；By the ready-mixed object prepared in step (4) with 4.5 degrees Celsius per minute of constant liter
Under warm rate, temperature is risen into constant temperature calcining 10 hours at 500 degrees Celsius, after natural cooling final product is nickel cobalt aluminic acid
Lithium presoma.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the present invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to preferably explain the present invention
Principle and practical application, to enable skilled artisan to be best understood by and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (6)
1. a kind of preparation method of battery anode material nickel cobalt lithium aluminate presoma, it is characterised in that：Include the following steps：
(1) nickel and cobalt solution is configured；Nickel salt and cobalt salt are added in acid group solution, the solution of every liter of 1mol is made in proportioning；
(2) sediment is prepared；Ammonium hydroxide and lye, control are added in the nickel and cobalt solution prepared into step (1) under constant temperature
Ph values are between 10-11；Stir to get sediment；
(3) sediment is purified；It washs after the sediment that step (2) obtains is carried out centrifugal filtration, is dried after washing
Sediment must be purified；
(4) ready-mixed object is prepared；It is ground after the purifying sediment of step (3) is mixed with aluminum nitrate；Grinding uses
300-500 mesh sieve obtains ready-mixed object after carrying out sieving processing；
(5) final product is roasted；By the ready-mixed object prepared in step (4) under constant heating rate, temperature is risen to
It is nickel cobalt lithium aluminate presoma to obtain final product constant temperature calcining 8-10 hours at 500-600 degrees Celsius, after natural cooling.
2. the preparation method of battery anode material nickel cobalt lithium aluminate presoma according to claim 1, which is characterized in that institute
It is 16 to state the cobalt ions molar ratio in the nickel ion and cobalt salt in step (1) in nickel salt：3；Step (1) the acid group solution is
Sulfate radical solution or nitrate solutions.
3. the preparation method of battery anode material nickel cobalt lithium aluminate presoma according to claim 1, which is characterized in that institute
State a concentration of 20-25% of ammonium hydroxide in step (2)；The lye is NaOH solution or KOH solution；Step (2) the constant temperature item
Part is 50-60 degrees Celsius.
4. the preparation method of battery anode material nickel cobalt lithium aluminate presoma according to claim 1, which is characterized in that institute
It is 100-200 degrees Celsius to state drying temperature in step (3).
5. the preparation method of battery anode material nickel cobalt lithium aluminate presoma according to claim 1, which is characterized in that institute
State the molar ratio 19 of purifying sediment and aluminum nitrate in step (4):1；Milling time is 2-4 hours.
6. the preparation method of battery anode material nickel cobalt lithium aluminate presoma according to claim 1, which is characterized in that institute
It is 4.5 degrees Celsius per minute to state step (5) heating rate.
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Citations (6)
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|---|---|---|---|---|
| JP2000340230A (en) * | 1999-05-31 | 2000-12-08 | Dowa Mining Co Ltd | Positive electrode active material and nonaqueous secondary battery |
| CN102694166A (en) * | 2011-11-23 | 2012-09-26 | 横店集团东磁股份有限公司 | Preparation method of lithium-nickel-cobalt-aluminum composite metal oxide |
| CN103178262A (en) * | 2011-12-23 | 2013-06-26 | 西安物华新能源科技有限公司 | Method for preparing aluminum-nickel-lithium cobalt oxide-doped anode material |
| CN104779383A (en) * | 2015-04-07 | 2015-07-15 | 四川大学 | Preparation method of high-specific-energy cathode material of lithium ion battery |
| CN105489886A (en) * | 2016-01-11 | 2016-04-13 | 山东玉皇新能源科技有限公司 | Nickel-cobalt-aluminum ternary cathode material with high tap-density and preparation method of nickel-cobalt-aluminum ternary cathode material |
| CN107316990A (en) * | 2017-05-26 | 2017-11-03 | 金川集团股份有限公司 | A kind of preparation method of cladded type nickel cobalt aluminium positive electrode material precursor |
-
2018
- 2018-06-20 CN CN201810638114.7A patent/CN108767256A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000340230A (en) * | 1999-05-31 | 2000-12-08 | Dowa Mining Co Ltd | Positive electrode active material and nonaqueous secondary battery |
| CN102694166A (en) * | 2011-11-23 | 2012-09-26 | 横店集团东磁股份有限公司 | Preparation method of lithium-nickel-cobalt-aluminum composite metal oxide |
| CN103178262A (en) * | 2011-12-23 | 2013-06-26 | 西安物华新能源科技有限公司 | Method for preparing aluminum-nickel-lithium cobalt oxide-doped anode material |
| CN104779383A (en) * | 2015-04-07 | 2015-07-15 | 四川大学 | Preparation method of high-specific-energy cathode material of lithium ion battery |
| CN105489886A (en) * | 2016-01-11 | 2016-04-13 | 山东玉皇新能源科技有限公司 | Nickel-cobalt-aluminum ternary cathode material with high tap-density and preparation method of nickel-cobalt-aluminum ternary cathode material |
| CN107316990A (en) * | 2017-05-26 | 2017-11-03 | 金川集团股份有限公司 | A kind of preparation method of cladded type nickel cobalt aluminium positive electrode material precursor |
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