CN110474047A - A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof - Google Patents
A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof Download PDFInfo
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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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- 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 present invention provides a kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof, it is the proportional arrangement of 5:2:3 containing the mixing salt solution of nickel salt, cobalt salt and manganese salt that method, which includes according to the molar ratio of nickel, cobalt and manganese Metal ion,;Sodium chlorate is added thereto, obtains the first mixed solution after mixing evenly;The first mixed liquor of gained and sodium hydroxide solution and ammonia spirit cocurrent are added in the reaction kettle with Vltrasonic device under conditions of being passed through protective gas; keeping temperature is 50~60 DEG C; and it is stirred with the speed of 500~850r/min to reaction and is terminated; sediment is obtained after aged and separation of solid and liquid; gained sediment is washed and dry, obtains Ni0.5Co0.2Mn0.3(OH)2Precursor powder.Gained precursor powder has hexagonal pattern flaky nanometer structure, and specific surface area is 5.2~5.7m2/ g, gained positive electrode chemical property are good.
Description
Technical field
The present invention relates to battery material preparation technical field, in particular to a kind of nickel-cobalt-manganese ternary presoma and its preparation side
Method and application.
Background technique
Lithium ion battery has many advantages, such as high-energy, long-life, memory-less effect and low pollution, is widely used in hand
Each field such as machine, computer, electric car.Currently, the positive electrode that lithium ion battery uses mainly has cobalt acid lithium, ferric phosphate
Lithium, LiMn2O4 and nickle cobalt lithium manganate etc..Wherein, the maximum positive electrode of occupation rate of market is cobalt acid lithium, but cobalt is as strategy
Property resource reserve is seldom, expensive, and the security performance of cobalt acid lithium is poor, limits the further development of the material.And
Nickle cobalt lithium manganate has many advantages, such as that specific capacity is high, thermal stability is good and cheap, be in anode material for lithium-ion batteries most
Potential one kind has a good application prospect in dynamic fields such as electric vehicle, electric tools.
Currently, the common method for preparing nickle cobalt lithium manganate has high temperature solid-state method and co-precipitation-high temperature solid-state method.High temperature solid-state
Method is that nickel source, cobalt source, manganese source, lithium source ball milling then are carried out high-temperature calcination.The disadvantages of the method are as follows being difficult to nickel cobalt manganese three
The pattern for the material that kind element is uniformly mixed, therefore cannot give full play to the synergistic effect of three, and prepare is difficult to control,
The powder body material usually synthesized is made of random particle, and the bulk density of this material is low, and poor fluidity is unfavorable for anode
The production of material.Another method is co-precipitation-high temperature solid-state method, that is, first passes through coprecipitation and prepare nickel cobalt manganese hydroxide
Presoma adds lithium source sintering, obtains nickle cobalt lithium manganate.This method does not change substantially in the sintering process being added after lithium source
Become the pattern and granularity of presoma, and the pattern of nickel-cobalt lithium manganate material, granularity play in many performances of lithium ion battery
Crucial effect, therefore synthesize the nickel cobalt manganese hydroxide precursor with suitable pattern and granularity as influence nickel cobalt mangaic acid
The key factor of lithium performance.Chinese patent CN101202343 disclose lithium ion battery positive pole material cobalt nickel oxide manganses lithium and its
Preparation method, the presoma which is related to the preparation method comprises the following steps: using the soluble-salt of nickel, cobalt and manganese as raw material, with ammonium hydroxide or
Ammonium salt is complexing agent, and sodium hydroxide is precipitating reagent, adding water soluble dispersing agent, adding water soluble antioxidant or is controlled with inert gas
And protection, solution is added in reaction kettle in a manner of cocurrent and is reacted, basic treatment is aged, and is separated by solid-liquid separation, and washing is dried to obtain nickel
Cobalt manganese hydroxide precursor.The nickel cobalt manganese hydroxide precursor that the above method is prepared is spherical structure, specific surface
Product is smaller, and also small with the contact area of electrolyte in application process, the charge-discharge performance of battery is to be improved.
Therefore, it is necessary to which the pattern and granularity to nickel-cobalt-manganese ternary presoma control, the electrification of positive electrode is improved
Learn performance.
Summary of the invention
The present invention provides a kind of nickel-cobalt-manganese ternary presomas and the preparation method and application thereof, before promoting
It drives nucleus in production procedure to be formed, refines crystal grain, increase the specific surface area of nickel-cobalt-manganese ternary presoma, improve anode
The chemical property of material.
In order to achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of nickel-cobalt-manganese ternary presoma, includes the following steps:
It (1) is the proportional arrangement of 5:2:3 containing nickel salt, cobalt salt and manganese salt according to the molar ratio of nickel, cobalt and manganese Metal ion
Mixing salt solution, the total concentration of the mixing salt solution are 1~2mol/L;
(2) sodium chlorate is added into mixing salt solution obtained by step (1), obtains the first mixed solution after mixing evenly;Its
In, the quality of sodium chlorate be nickel in mixing salt solution, cobalt, three metal ion species gross mass of manganese 1~3%;
(3) by the first mixed liquor obtained by step (2) and sodium hydroxide solution and ammonia under conditions of being passed through protective gas
Aqueous solution cocurrent is added in the reaction kettle with Vltrasonic device, and keeping temperature is 50~60 DEG C, and with the speed of 500~850r/min
Degree stirring to reaction terminates, and sediment is obtained after aged and separation of solid and liquid, and gained sediment is washed and dry, obtains
Ni0.5Co0.2Mn0.3(OH)2Precursor powder;
Wherein, the additional amount of the sodium hydroxide solution is that pH value of solution is made to be maintained at 9~12;The molal quantity of the ammonium hydroxide with
Nickel, cobalt, three metal ion species total moles of manganese ratio be 1~10:1;The power of the Vltrasonic device is set as 480~540W.
Preferably, nickel salt described in step (1) is nickel sulfate, nickel chloride, nickel acetate or nickel nitrate;The cobalt salt is sulfuric acid
Cobalt, cobalt acetate or cobalt nitrate;The manganese salt is manganese sulfate, manganese chloride, manganese acetate or manganese nitrate.
Preferably, density of sodium chlorate described in step (2) is 1~2g/L.
Preferably, protective gas described in step (3) is nitrogen or argon gas.
Preferably, the concentration of sodium hydroxide solution described in step (3) is 2~8mol/L.
Preferably, the concentration of ammonia spirit described in step (3) is 5~10mol/L.
Preferably, digestion time is 24~72h in step (3).
Preferably, dry for vacuum drying described in step (3), drying temperature is 90~105 DEG C, drying time is 20~
24h。
The present invention also provides a kind of nickel-cobalt-manganese ternary presoma, chemical formula Ni0.5Co0.2Mn0.3(OH)2, the presoma
It is prepared by the above method.
The present invention also provides a kind of positive electrode, chemical formula LiNi0.5Co0.2Mn0.3O2, the positive electrode is by above-mentioned
Presoma is made after being mixed, being sintered with lithium source.
Sodium hydroxide is as precipitating reagent in the present invention, ammonium hydroxide as complexing agent, due to the solubility of compound be it is determining,
Therefore present invention defines the concentration of the precipitating reagent and the complexing agent: the additional amount of the sodium hydroxide solution is to make solution
PH is maintained at 9~12;The molal quantity of the ammonium hydroxide and the ratio of nickel, cobalt, three metal ion species total moles of manganese are 1~10:1.
Above scheme of the invention have it is following the utility model has the advantages that
The preparation method of nickel-cobalt-manganese ternary presoma provided by the invention, in step (2) into nickel cobalt manganese mixing salt solution
Sodium chlorate is added and forms the first mixed solution, sodium chlorate is here as oxidant by the part bivalent manganese oxygen in mixing salt solution
Manganic is turned to, to promote the formation of nucleus, refines a crystal grain of presoma, reaches and increases forerunner's surface area per unit volume
Long-pending purpose.Ni obtained in embodiment0.5Co0.2Mn0.3(OH)2The specific surface area of precursor powder material is 5.2~5.7m2/
g。
The present invention provides the preparation method of nickel-cobalt-manganese ternary presoma, by the first mixed liquor and sodium hydroxide in step (3)
Solution and ammonia spirit cocurrent are added in the reaction kettle with Vltrasonic device, and the effect of ultrasonic wave in the present invention is embodied in:
On the one hand with making each stock dispersion of reaction process more evenly, the reunion of nano material in reaction process can significantly be inhibited;Separately
On the one hand, localized hyperthermia, high-energy brought by ultrasonic cavitation facilitate the formation of nucleus, effectively shorten the reaction time, and
The size and shape of particle can be controlled by adjusting ultrasonic frequency.The power of Vltrasonic device is set as 480 by the present invention~
540W forms the Ni with hexagonal pattern flaky nanometer structure in conjunction with the regulation of addition oxidant0.5Co0.2Mn0.3(OH)2Before
Drive body dusty material.Compared to dense spherical material, the material of nanometer chip architecture has bigger specific surface area, higher compares table
Face energy, increases contact of the active material with electrolyte, reduces Li+Diffusion length, effectively increase the electrochemistry of material
Performance.The presoma made from embodiment is assembled into button cell after positive electrode is made, and cell testing results are
169.5mAhg-1(0.2C), 161mAhg-1(0.5C), 153.5mAhg-1(1C), 145mAhg-1(2C), 138mAhg-1(5C),
129.5mAhg-1(10C).90.5% or more capacity retention ratio after 2C is recycled 300 weeks.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
Embodiment 1
A kind of preparation method of nickel-cobalt-manganese ternary presoma provided in this embodiment, includes the following steps:
(1) proportional arrangement sulfur acid nickel, cobaltous sulfate and the sulphur for being 5:2:3 according to the molar ratio of nickel, cobalt and manganese Metal ion
The mixing salt solution of sour manganese, the total concentration of the mixing salt solution are 1mol/L;
(2) sodium chlorate that concentration is 1g/L is added into mixing salt solution obtained by step (1), obtains first after mixing evenly
Mixed solution;Wherein, the quality of sodium chlorate be mixing salt solution in nickel, cobalt, three metal ion species gross mass of manganese 1%;
(3) using pH value be 10 ammonia spirit as bottom liquid, by step under conditions of being passed through nitrogen as protective gas
(2) sodium hydroxide solution and 5mol/L ammonia spirit cocurrent that the first mixed liquor of gained and concentration are 2mol/L are added with super
In the reaction kettle of acoustic device, keeping temperature is 55 DEG C, and is stirred with the speed of 700r/min to reaction and terminate, and ageing 36h is laggard
Row is separated by solid-liquid separation, and obtains sediment, and gained sediment is washed, and is dried in vacuo for 24 hours at 90 DEG C, and Ni is obtained0.5Co0.2Mn0.3
(OH)2Precursor powder;
Wherein, the additional amount of the sodium hydroxide solution makes pH value of solution be maintained at 11;The molal quantity and nickel of the ammonium hydroxide,
Cobalt, three metal ion species total moles of manganese ratio be 1:1;The power of the Vltrasonic device is set as 540W.
The nickel-cobalt-manganese ternary presoma that the above process is prepared is made of hexagonal pattern flaky nanometer structure, and particle is opposite
Uniformly.Testing the presoma specific surface area size by dynamic method specific surface instrument is 5.3m2/g。
(4) by Li2CO3With Ni obtained by step (2)0.5Co0.2Mn0.3(OH)2Presoma be in molar ratio 1.03 ratio it is mixed
It closes uniformly, obtains with lithium presoma, gained is sintered 12h with lithium presoma at 850 DEG C, carries out powder after cooled to room temperature
Broken and sieving, obtains LiNi0.5Co0.2Mn0.3O2Positive electrode;
Positive electrode obtained by the present embodiment is assembled into button cell to test, specially the following steps are included:
A. according to positive electrode: carbon black: suitable N- methyl pyrrole network is added in the mixing of segregation vinyl fluoride=90:2:8 ratio
Alkanone stirs to form uniform sizing material, and then gained slurry is coated uniformly on aluminium foil, drying, roll-in, cutting, forms anode
Piece;
B. positive plate, cathode (lithium piece), electrolyte, diaphragm and battery case are assembled into and are buckled in the glove box of argon gas protection
Formula battery carries out electrochemical property test, test result 165.5mAhg-1(0.2C), 156mAhg-1(0.5C),
143.5mAhg-1(1C), 136mAhg-1(2C), 128mAhg-1(5C), 120.5mAhg-1(10C).Capacity is protected after 2C is recycled 300 weeks
89.5% or more holdup.
Embodiment 2
A kind of preparation method of nickel-cobalt-manganese ternary presoma provided in this embodiment, includes the following steps:
(1) proportional arrangement chloride containing nickel, cobalt acetate and the chlorine for being 5:2:3 according to the molar ratio of nickel, cobalt and manganese Metal ion
Change the mixing salt solution of manganese, the total concentration of the mixing salt solution is 1.5mol/L;
(2) sodium chlorate that concentration is 2g/L is added into mixing salt solution obtained by step (1), obtains first after mixing evenly
Mixed solution;Wherein, the quality of sodium chlorate be mixing salt solution in nickel, cobalt, three metal ion species gross mass of manganese 3%;
(3) using pH value be 11 ammonia spirit as bottom liquid, by step under conditions of being passed through argon gas as protective gas
(2) sodium hydroxide solution and 8mol/L ammonia spirit cocurrent that the first mixed liquor of gained and concentration are 6mol/L are added with super
In the reaction kettle of acoustic device, keeping temperature is 60 DEG C, and is stirred with the speed of 850r/min to reaction and terminate, and is aged laggard for 24 hours
Row is separated by solid-liquid separation, and obtains sediment, gained sediment is washed, and in 105 DEG C of vacuum drying 20h, obtains Ni0.5Co0.2Mn0.3
(OH)2Precursor powder;
Wherein, the additional amount of the sodium hydroxide solution makes pH value of solution be maintained at 9;The molal quantity of the ammonium hydroxide and nickel, cobalt,
The ratio of three metal ion species total moles of manganese is 8:1;The power of the Vltrasonic device is set as 480W.
The nickel-cobalt-manganese ternary presoma that the above process is prepared is made of hexagonal pattern flaky nanometer structure, and particle is opposite
Uniformly.Testing the presoma specific surface area size by dynamic method specific surface instrument is 5.7m2/g。
(4) by Li2CO3With Ni obtained by step (2)0.5Co0.2Mn0.3(OH)2Presoma be in molar ratio 1.03 ratio it is mixed
It closes uniformly, obtains with lithium presoma, gained is sintered 12h with lithium presoma at 850 DEG C, carries out powder after cooled to room temperature
Broken and sieving, obtains LiNi0.5Co0.2Mn0.3O2Positive electrode;
Positive electrode obtained by the present embodiment is assembled into button cell according to the method for embodiment 1 to test, test knot
Fruit is 169.5mAhg-1(0.2C), 161mAhg-1(0.5C), 153.5mAhg-1(1C), 145mAhg-1(2C), 138mAhg-1
(5C), 129.5mAhg-1(10C).90.5% or more capacity retention ratio after 2C is recycled 300 weeks.
Embodiment 3
A kind of preparation method of nickel-cobalt-manganese ternary presoma provided in this embodiment, includes the following steps:
(1) contain nickel nitrate, cobalt nitrate and nitre according to the proportional arrangement that the molar ratio of nickel, cobalt and manganese Metal ion is 5:2:3
The mixing salt solution of sour manganese, the total concentration of the mixing salt solution are 2mol/L;
(2) sodium chlorate that concentration is 2g/L is added into mixing salt solution obtained by step (1), obtains first after mixing evenly
Mixed solution;Wherein, the quality of sodium chlorate be mixing salt solution in nickel, cobalt, three metal ion species gross mass of manganese 2%;
(3) using pH value be 11 ammonia spirit as bottom liquid, by step under conditions of being passed through argon gas as protective gas
(2) the first mixed liquor of gained has with sodium hydroxide solution and the addition of 10mol/L ammonia spirit cocurrent that concentration is 8mol/L
In the reaction kettle of Vltrasonic device, keeping temperature is 50 DEG C, and is stirred with the speed of 500r/min to reaction and terminate, after being aged 72h
It is separated by solid-liquid separation, obtains sediment, gained sediment is washed, and in 100 DEG C of vacuum drying 22h, obtains
Ni0.5Co0.2Mn0.3(OH)2Precursor powder;
Wherein, the additional amount of the sodium hydroxide solution makes pH value of solution be maintained at 12;The molal quantity and nickel of the ammonium hydroxide,
Cobalt, three metal ion species total moles of manganese ratio be 10:1;The power of the Vltrasonic device is set as 500W.
The nickel-cobalt-manganese ternary presoma that the above process is prepared is made of hexagonal pattern flaky nanometer structure, and particle is opposite
Uniformly.Testing the presoma specific surface area size by dynamic method specific surface instrument is 5.2m2/g。
(4) by Li2CO3With Ni obtained by step (2)0.5Co0.2Mn0.3(OH)2Presoma be in molar ratio 1.03 ratio it is mixed
It closes uniformly, obtains with lithium presoma, gained is sintered 12h with lithium presoma at 850 DEG C, carries out powder after cooled to room temperature
Broken and sieving, obtains LiNi0.5Co0.2Mn0.3O2Positive electrode;
Positive electrode obtained by the present embodiment is assembled into button cell according to the method for embodiment 1 to test, test knot
Fruit is 160.5mAhg-1(0.2C), 151mAhg-1(0.5C), 142.5mAhg-1(1C), 133.5mAhg-1(2C), 125mAhg-1
(5C), 113.5mAhg-1(10C).87.5% or more capacity retention ratio after 2C is recycled 300 weeks.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nickel-cobalt-manganese ternary presoma, which comprises the steps of:
It (1) is the proportional arrangement of 5:2:3 containing the mixing of nickel salt, cobalt salt and manganese salt according to the molar ratio of nickel, cobalt and manganese Metal ion
Salting liquid, the total concentration of the mixing salt solution are 1~2mol/L;
(2) sodium chlorate is added into mixing salt solution obtained by step (1), obtains the first mixed solution after mixing evenly;Wherein, chlorine
The quality of sour sodium be mixing salt solution in nickel, cobalt, three metal ion species gross mass of manganese 1~3%;
(3) under conditions of being passed through protective gas that the first mixed liquor obtained by step (2) and sodium hydroxide solution and ammonium hydroxide is molten
Liquid cocurrent is added in the reaction kettle with Vltrasonic device, and keeping temperature is 50~60 DEG C, and is stirred with the speed of 500~850r/min
Mixing to reaction terminates, and sediment is obtained after aged and separation of solid and liquid, and gained sediment is washed and dry, obtains
Ni0.5Co0.2Mn0.3(OH)2Precursor powder;
Wherein, the additional amount of the sodium hydroxide solution is that pH value of solution is made to be maintained at 9~12;The molal quantity and nickel of the ammonium hydroxide,
Cobalt, three metal ion species total moles of manganese ratio be 1~10:1;The power of the Vltrasonic device is set as 480~540W.
2. preparation method according to claim 1, which is characterized in that nickel salt described in step (1) be nickel sulfate, nickel chloride,
Nickel acetate or nickel nitrate;The cobalt salt is cobaltous sulfate, cobalt acetate or cobalt nitrate;The manganese salt is manganese sulfate, manganese chloride, manganese acetate
Or manganese nitrate.
3. preparation method according to claim 1, which is characterized in that density of sodium chlorate described in step (2) is 1~2g/L.
4. preparation method according to claim 1, which is characterized in that protective gas described in step (3) is nitrogen or argon gas.
5. preparation method according to claim 1, which is characterized in that the concentration of sodium hydroxide solution described in step (3) is 2
~8mol/L.
6. preparation method according to claim 1, which is characterized in that the concentration of ammonia spirit described in step (3) be 5~
10mol/L。
7. preparation method according to claim 1, which is characterized in that digestion time is 24~72h in step (3).
8. preparation method according to claim 1, which is characterized in that dry for vacuum drying, dry temperature described in step (3)
Degree be 90~105 DEG C, drying time be 20~for 24 hours.
9. a kind of nickel-cobalt-manganese ternary presoma, chemical formula Ni0.5Co0.2Mn0.3(OH)2, which is characterized in that the presoma is by weighing
Benefit requires 1~8 any one the method to be prepared.
10. a kind of positive electrode, chemical formula LiNi0.5Co0.2Mn0.3O2, which is characterized in that the positive electrode is by claim
Nickel-cobalt-manganese ternary presoma or the nickel-cobalt-manganese ternary that any one the method is prepared according to claim 1~8 described in 9
Presoma mixed with lithium source, be sintered after be made.
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CN111370683A (en) * | 2020-03-26 | 2020-07-03 | 东莞东阳光科研发有限公司 | Preparation method of mono-like nickel cobalt lithium manganate |
CN111370683B (en) * | 2020-03-26 | 2022-04-26 | 东莞东阳光科研发有限公司 | Preparation method of mono-like nickel cobalt lithium manganate |
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Inventor after: Yang Yihua Inventor after: Wang Haitao Inventor after: Zhong Yi Inventor after: Song Jie Inventor before: Yang Yihua Inventor before: Wang Haitao Inventor before: Zhong Yi |
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Application publication date: 20191119 |