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 PDF

Info

Publication number
CN109678217A
CN109678217A CN201811538465.7A CN201811538465A CN109678217A CN 109678217 A CN109678217 A CN 109678217A CN 201811538465 A CN201811538465 A CN 201811538465A CN 109678217 A CN109678217 A CN 109678217A
Authority
CN
China
Prior art keywords
solution
lithium
concentration
temperature
tap density
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811538465.7A
Other languages
Chinese (zh)
Other versions
CN109678217B (en
Inventor
张中彩
毛秦钟
钱志挺
吉同棕
王鑫
王寅峰
吴海军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Mei Du Hai Chuang Lithium Electric Technology Co Ltd
Original Assignee
Zhejiang Mei Du Hai Chuang Lithium Electric Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Mei Du Hai Chuang Lithium Electric Technology Co Ltd filed Critical Zhejiang Mei Du Hai Chuang Lithium Electric Technology Co Ltd
Priority to CN201811538465.7A priority Critical patent/CN109678217B/en
Publication of CN109678217A publication Critical patent/CN109678217A/en
Application granted granted Critical
Publication of CN109678217B publication Critical patent/CN109678217B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/006Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/11Powder tap density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)

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

The Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method and application of material
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.
CN201811538465.7A 2018-12-16 2018-12-16 High tap density Ni0.8Co0.1Mn0.1(OH)2Preparation method and application of material Active CN109678217B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811538465.7A CN109678217B (en) 2018-12-16 2018-12-16 High tap density Ni0.8Co0.1Mn0.1(OH)2Preparation method and application of material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811538465.7A CN109678217B (en) 2018-12-16 2018-12-16 High tap density Ni0.8Co0.1Mn0.1(OH)2Preparation method and application of material

Publications (2)

Publication Number Publication Date
CN109678217A true CN109678217A (en) 2019-04-26
CN109678217B CN109678217B (en) 2021-12-31

Family

ID=66187774

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811538465.7A Active CN109678217B (en) 2018-12-16 2018-12-16 High tap density Ni0.8Co0.1Mn0.1(OH)2Preparation method and application of material

Country Status (1)

Country Link
CN (1) CN109678217B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1622371A (en) * 2004-12-30 2005-06-01 清华大学 Process for preparing high density spherical nickel-cobalt lithium manganate as anode material of lithium ion cell
CN101269849A (en) * 2008-03-05 2008-09-24 广州融捷材料科技有限公司 High-density spherical lithium nickel cobalt manganese oxygen and method for preparing the same
CN101662025A (en) * 2009-09-21 2010-03-03 昆明理工大学 Lithium ion battery anode active material and preparing method thereof
CN103482711A (en) * 2013-09-06 2014-01-01 大连瑞源动力有限公司 Ultrasonic assisted method for preparing precursor of ternary positive material of lithium ion battery
CN104852038A (en) * 2015-04-08 2015-08-19 中国科学院长春应用化学研究所 Preparation method of high-capacity quickly-chargeable/dischargeable lithium ion battery ternary anode material
CN105375020A (en) * 2015-11-28 2016-03-02 中信大锰矿业有限责任公司大新锰矿分公司 Preparation method of spherical lithium nickel cobalt manganese oxide precursor mixture
CN106058237A (en) * 2016-07-07 2016-10-26 成都翔羽科技有限公司 Method for continuously preparing nanoflower lithium ion battery layered anode material and reaction kettle thereof
CN106602004A (en) * 2015-10-19 2017-04-26 河南科隆新能源股份有限公司 High-safety power lithium ion secondary battery composite positive material and preparation method thereof
CN106745336A (en) * 2016-12-28 2017-05-31 杉杉能源(宁夏)有限公司 A kind of precursor of nickel-cobalt-lithium-manganese-oxide of nanometer sheet reunion second particle and preparation method thereof
CN107324405A (en) * 2017-07-07 2017-11-07 金驰能源材料有限公司 A kind of lithium nickel cobalt manganese oxide precursor and preparation method thereof and the lithium ion battery prepared by the presoma
CN107342417A (en) * 2016-12-28 2017-11-10 杉杉能源(宁夏)有限公司 A kind of high ni-type precursor of nickel-cobalt-lithium-manganese-oxide with specific morphology and preparation method thereof
CN107611383A (en) * 2017-08-25 2018-01-19 浙江华友钴业股份有限公司 A kind of preparation method of the nickel-cobalt-manganese ternary presoma of low-sulfur high-tap density
CN107742720A (en) * 2017-10-17 2018-02-27 哈尔滨工业大学(威海) A kind of preparation method of ternary cathode material of lithium ion battery presoma
CN108264096A (en) * 2016-12-30 2018-07-10 北京当升材料科技股份有限公司 A kind of preparation method of high density little particle nickel cobalt manganese hydroxide
CN108365216A (en) * 2018-04-18 2018-08-03 西南石油大学 The novel nickelic tertiary cathode material of one kind and preparation
CN108807968A (en) * 2018-08-09 2018-11-13 中国恩菲工程技术有限公司 Nickel-cobalt-manganese ternary persursor material and its synthetic method
CN108987682A (en) * 2017-06-02 2018-12-11 杉杉能源(宁夏)有限公司 It can prevent the preparation method of the Ni-based persursor material of richness of breakage of particles

Patent Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1622371A (en) * 2004-12-30 2005-06-01 清华大学 Process for preparing high density spherical nickel-cobalt lithium manganate as anode material of lithium ion cell
CN101269849A (en) * 2008-03-05 2008-09-24 广州融捷材料科技有限公司 High-density spherical lithium nickel cobalt manganese oxygen and method for preparing the same
CN101662025A (en) * 2009-09-21 2010-03-03 昆明理工大学 Lithium ion battery anode active material and preparing method thereof
CN103482711A (en) * 2013-09-06 2014-01-01 大连瑞源动力有限公司 Ultrasonic assisted method for preparing precursor of ternary positive material of lithium ion battery
CN104852038A (en) * 2015-04-08 2015-08-19 中国科学院长春应用化学研究所 Preparation method of high-capacity quickly-chargeable/dischargeable lithium ion battery ternary anode material
CN106602004A (en) * 2015-10-19 2017-04-26 河南科隆新能源股份有限公司 High-safety power lithium ion secondary battery composite positive material and preparation method thereof
CN105375020A (en) * 2015-11-28 2016-03-02 中信大锰矿业有限责任公司大新锰矿分公司 Preparation method of spherical lithium nickel cobalt manganese oxide precursor mixture
CN106058237A (en) * 2016-07-07 2016-10-26 成都翔羽科技有限公司 Method for continuously preparing nanoflower lithium ion battery layered anode material and reaction kettle thereof
CN106745336A (en) * 2016-12-28 2017-05-31 杉杉能源(宁夏)有限公司 A kind of precursor of nickel-cobalt-lithium-manganese-oxide of nanometer sheet reunion second particle and preparation method thereof
CN107342417A (en) * 2016-12-28 2017-11-10 杉杉能源(宁夏)有限公司 A kind of high ni-type precursor of nickel-cobalt-lithium-manganese-oxide with specific morphology and preparation method thereof
CN108264096A (en) * 2016-12-30 2018-07-10 北京当升材料科技股份有限公司 A kind of preparation method of high density little particle nickel cobalt manganese hydroxide
CN108987682A (en) * 2017-06-02 2018-12-11 杉杉能源(宁夏)有限公司 It can prevent the preparation method of the Ni-based persursor material of richness of breakage of particles
CN107324405A (en) * 2017-07-07 2017-11-07 金驰能源材料有限公司 A kind of lithium nickel cobalt manganese oxide precursor and preparation method thereof and the lithium ion battery prepared by the presoma
CN107611383A (en) * 2017-08-25 2018-01-19 浙江华友钴业股份有限公司 A kind of preparation method of the nickel-cobalt-manganese ternary presoma of low-sulfur high-tap density
CN107742720A (en) * 2017-10-17 2018-02-27 哈尔滨工业大学(威海) A kind of preparation method of ternary cathode material of lithium ion battery presoma
CN108365216A (en) * 2018-04-18 2018-08-03 西南石油大学 The novel nickelic tertiary cathode material of one kind and preparation
CN108807968A (en) * 2018-08-09 2018-11-13 中国恩菲工程技术有限公司 Nickel-cobalt-manganese ternary persursor material and its synthetic method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
彭弯弯: "高容量镍基正极材料LiNi0.8Co0.1Mn0.1O2的制备与改性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112191212B (en) * 2020-12-02 2021-02-26 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

Also Published As

Publication number Publication date
CN109678217B (en) 2021-12-31

Similar Documents

Publication Publication Date Title
US11708280B2 (en) Method of preparing MOF-coated monocrystal ternary positive electrode material
CN111509214B (en) High-nickel layered composite material and lithium ion battery anode material prepared from same
CN102315429B (en) The preparation method of aluminum-doped material of cathode of lithium ion battery with solid phase process
CN109778301A (en) The preparation of one type monocrystalline lithium-rich oxide material and application
WO2015039490A1 (en) Lithium-rich anode material and preparation method thereof
CN103904323A (en) Preparation method for spherical cobalt oxyhydroxide
CN103715424A (en) Core-shell structured cathode material and preparation method thereof
CN103715418A (en) Preparation method for spherical cobaltosic oxide
CN112310391B (en) Positive electrode material precursor, positive electrode material and preparation method thereof, lithium ion battery positive electrode, lithium ion battery and electric equipment
CN107123792A (en) Two-layer composite tertiary cathode material and preparation method thereof
CN110518221B (en) Method for preparing lithium silicate coated lithium nickel cobalt manganese oxide positive electrode material by anti-solvent method
CN113644272B (en) Cerium-bismuth composite oxide doped lithium ion battery positive electrode material and preparation method thereof
CN115000383B (en) Hollow ternary positive electrode material and preparation method thereof
CN112758995A (en) Ternary positive electrode precursor and preparation method and application thereof
CN113690430A (en) Lithium-rich manganese-based positive electrode material for realizing accurate lithium preparation and preparation method and application thereof
CN109473672A (en) A kind of lithium-rich manganese-based anode material and preparation method thereof
CN112608488A (en) MOFs-based precursor for cobalt-free lithium battery, positive electrode material and preparation method of MOFs-based precursor
CN115650318A (en) Doped P2 type layered sodium nickel manganese oxide cathode material and preparation method thereof
CN106684350B (en) Preparation method of high-voltage positive electrode material lithium nickel manganese oxide
CN111153447A (en) Grid-shaped porous precursor material, preparation method thereof and anode material
CN109678217A (en) The Ni of high-tap density0.8Co0.1Mn0.1(OH)2The preparation method and application of material
CN110350171A (en) A kind of preparation method of the high ni-type tertiary cathode material of rubidium element doping
CN105789636A (en) Method for one-step hydrothermal synthesis preparation of composite anode material of solid oxide fuel cell
CN103187564A (en) Preparation method for battery anode material LiNi0.5Mn1.5O4
CN114420911B (en) Low-residual-lithium high-nickel positive electrode material with double-shell structure, preparation method thereof and lithium ion battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information
CB02 Change of applicant information

Address after: 312300 No. 5 Weiqi East Road, Hangzhou Bay Economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province

Applicant after: Zhejiang Haichuang lithium battery technology Co.,Ltd.

Address before: 312300 No. 5 Weiqi East Road, Hangzhou Bay Economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province

Applicant before: ZHEJIANG MEIDU HAICHUANG LITHIUM ELECTRICITY TECHNOLOGY Co.,Ltd.

GR01 Patent grant
GR01 Patent grant