CN106935824A - A kind of preparation method of tertiary cathode material - Google Patents
A kind of preparation method of tertiary cathode material Download PDFInfo
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- CN106935824A CN106935824A CN201710168700.5A CN201710168700A CN106935824A CN 106935824 A CN106935824 A CN 106935824A CN 201710168700 A CN201710168700 A CN 201710168700A CN 106935824 A CN106935824 A CN 106935824A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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 present invention provides a kind of preparation method of tertiary cathode material, comprises the following steps：Step one：At room temperature, it is 1 according to volume ratio by water and organic solvent：(0.7~1.4) is configured to organic solution, and the organic solution that will be configured is added in autoclave, adds nickel source, cobalt source, manganese source and lithium source, continuously adds complexing of metal ion agent, stirs 0.5 3h, obtains well mixed solution；Step 2：To precipitating reagent is added in solution obtained in step one, 0.5~3h is stirred, fully after dissolving, carry out solvent thermal reaction, solvent thermal reaction temperature is 150 250 DEG C, and the reaction time is 2~36h, is cooled to room temperature, and mixed liquor is obtained；Step 3：Mixed liquor obtained in step 2 is filtered, is precipitated, alternately washing 3~5 times are carried out to precipitation with absolute ethyl alcohol and distilled water, dry 1~24h, obtain persursor material；Step 4：The persursor material that step 3 is obtained is calcined, final tertiary cathode material LiNi is obtained1‑x‑yCoxMnyO2, wherein the ﹤ y ﹤ 1 of 0 ﹤ x ﹤ 1,0.
Description
【Technical field】
The present invention relates to battery material technical field, more particularly to a kind of preparation method of tertiary cathode material.
【Background technology】
When electrode material of lithium battery is synthesized, if raw material or synthetic method are different, pattern, the grain of prepared electrode material
Footpath is distributed and crystal parameterses can be different, thus its electrical property plays different.
At present, lithium battery tertiary cathode material (LiNi is prepared1-x-yCoxMnyO2Or LiNi1-x-yCoxAlyO2) there are various sides
Method, such as high temperature solid-state method, coprecipitation, sol-gel process, combustion method, spray drying process and solvent heat (including hydro-thermal) are closed
Cheng Fa.High temperature solid-state method, although process is simple, but during raw mill mixing, time-consuming and mixture homogeneity is limited, and product exists
There is larger difference in the aspects such as composition, structure, size distribution, material electrochemical performance is difficult to control；Coprecipitation, although gold
Category ion can be well mixed in water, but easily reunite, it is necessary to be carried out sternly to overall process prepared by powder when powder is prepared
The control of lattice；Sol-gel process, the method prepare ternary material uniformity it is good, purity is high, but expend organic solvent compared with
It is many, high cost；Combustion method and spray drying process are required for by high-temperature sintering process, generally more than 800 DEG C, long-time high temperature
Can there is dislocation and the impurities phase Li of Li ions and Ni ions in sintering2MnO3Appearance, be unfavorable for generation stoichiometry and high-purity
The product of degree.
In consideration of it, real be necessary to provide a kind of preparation method of new tertiary cathode material to overcome disadvantages described above.
【The content of the invention】
It is an object of the invention to provide it is a kind of can avoid component volatilization, pattern it is good, with larger specific surface area, energy
Reach and electrolyte is fully contacted, concentration polarization is small, the preparation method of stable electrochemical property tertiary cathode material.
To achieve these goals, the present invention provides a kind of preparation method of tertiary cathode material, comprises the following steps：
Step one：At room temperature, it is 1 according to volume ratio by water and organic solvent：(0.7~1.4) is configured to organic solution, will
The organic solution for being configured is added in autoclave, adds nickel source, cobalt source, manganese source and lithium source, continuously add metal from
Sub- complexing agent, stirs 0.5-3h, obtains well mixed solution；
Step 2：To precipitating reagent is added in solution obtained in step one, 0.5~3h is stirred, fully after dissolving, carry out solvent
Thermal response, solvent thermal reaction temperature is 150-250 DEG C, and the reaction time is 2~36h, is cooled to room temperature, and mixed liquor is obtained；
Step 3：Mixed liquor obtained in step 2 is filtered, is precipitated, precipitation is carried out with absolute ethyl alcohol and distilled water
Alternately washing 3~5 times, dry 1~24h, obtain persursor material；
Step 4：The persursor material that step 3 is obtained is calcined, final tertiary cathode material LiNi is obtained1-x- yCoxMnyO2, wherein the ﹤ y ﹤ 1 of 0 ﹤ x ﹤ 1,0.
In a preferred embodiment, the amount of complexing of metal ion agent and nickel source in the step one, cobalt source, manganese source with
And the mol ratio of total amount of metal ion of lithium source is (1.1~1.5)：1.
In a preferred embodiment, the organic solvent in the step one is diethylene glycol (DEG), triethylene glycol, ethylene glycol, poly-
One or more in ethylene glycol.
In a preferred embodiment, the nickel source in the step one is nickel acetate, nickel chloride, nickel nitrate, nickel sulfate
In one or more；Cobalt source in the step one is one or more in cobalt acetate, cobalt chloride, cobalt nitrate, cobaltous sulfate；
Manganese source in the step one is one or more in manganese acetate, manganese chloride, manganese nitrate, manganese sulfate；In the step one
Lithium source is one or more in lithium acetate, lithium nitrate, lithium citrate.
In a preferred embodiment, the metal chelating agent in the step one is disodium ethylene diamine tetraacetate or ammonia
Water.
In a preferred embodiment, the precipitating reagent in the step 2 is urea or hexamethylenetetramine.
In a preferred embodiment, the calcining heat in the step 4 be 600~950 DEG C, calcination time be 4~
16h。
The preparation method of the tertiary cathode material provided compared to prior art, the present invention, using solvent-thermal process method, system
For the tertiary cathode material that a kind of lamella piles up flower-like structure is gone out, prepared tertiary cathode material has larger specific surface
Product, can be fully contacted with electrolyte, and uniformity is good and purity is high, using the electricity that tertiary cathode material obtained in the present invention is assembled
Pond chemical property is good, and specific capacity is high, and cycle performance is excellent.
【Brief description of the drawings】
The tertiary cathode material LiNi prepared by embodiment 3 that Fig. 1 is provided for the present invention0.5Co0.2Mn0.3O2X-ray spread out
Penetrate collection of illustrative plates；
The SEM figures of the tertiary cathode material prepared by embodiment 3 that Fig. 2 is provided for the present invention；
The tertiary cathode material prepared by embodiment 3 that Fig. 3 is provided for the present invention is assembled into the cycle performance figure after battery.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with accompanying drawing and
Specific embodiment, the present invention will be described in further detail.It should be appreciated that the specific implementation described in this specification
Mode is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention provides a kind of preparation method of tertiary cathode material, comprises the following steps：
Step one：At room temperature (25 DEG C), it is 1 according to volume ratio by water and organic solvent：(0.7~1.4) is configured to organic
Solution, the organic solution that will be configured is added in autoclave, adds nickel source, cobalt source, manganese source and lithium source, is continuously added
Complexing of metal ion agent, stirs 0.5-3h, obtains well mixed solution；
Step 2：To precipitating reagent is added in solution obtained in step one, 0.5~3h is stirred, fully after dissolving, carry out solvent
Thermal response, solvent thermal reaction temperature is 150-250 DEG C, and the reaction time is 2~36h, is cooled to room temperature, and mixed liquor is obtained；
Step 3：Mixed liquor obtained in step 2 is filtered, is precipitated, precipitation is carried out with absolute ethyl alcohol and distilled water
Alternately washing 3~5 times, dry 1~24h, obtain persursor material；
Step 4：The persursor material that step 3 is obtained is calcined, final tertiary cathode material LiNi is obtained1-x- yCoxMnyO2, wherein the ﹤ y ﹤ 1 of 0 ﹤ x ﹤ 1,0.
Specifically, in the step one amount of complexing of metal ion agent and nickel source, cobalt source, manganese source and lithium source total metal
The mol ratio of ionic weight is (1.1~1.5)：1.
Specifically, the organic solvent in the step one is the one kind in diethylene glycol (DEG), triethylene glycol, ethylene glycol, polyethylene glycol
Or it is several.
Specifically, the nickel source in the step one is one or more in nickel acetate, nickel chloride, nickel nitrate, nickel sulfate；
Cobalt source in the step one is one or more in cobalt acetate, cobalt chloride, cobalt nitrate, cobaltous sulfate；In the step one
Manganese source is one or more in manganese acetate, manganese chloride, manganese nitrate, manganese sulfate；Lithium source in the step one is lithium acetate, nitre
One or more in sour lithium, lithium citrate.
Specifically, the metal chelating agent in the step one is disodium ethylene diamine tetraacetate or ammoniacal liquor.
Specifically, the precipitating reagent in the step 2 is urea or hexamethylenetetramine.
Specifically, the calcining heat in the step 4 is 600~950 DEG C, calcination time is 4~16h.
Embodiment 1：
It is 1 by volume ratio：1 water is added in autoclave with the mixed liquor of polyethylene glycol, then is added in reactor
Enter mol ratio for nickel acetate：Cobalt acetate：Manganese acetate：Lithium acetate=1：1：1：3 slaine, continuously adds ethylenediamine tetra-acetic acid two
Sodium, it is 1.1 with total metal ion mol ratio of the slaine for adding to control it：1,1h is stirred, well mixed solution is obtained；To
The urea with total metal ion equimolar amounts is added in well mixed solution, 1h is stirred, fully after dissolving, solvent heat is carried out anti-
Should, reaction temperature is 180 DEG C, and the reaction time is 8h, is cooled to room temperature, and mixed liquor is obtained；The mixed liquor filtering for completing will be reacted,
It is precipitated, with alternately washing 3~5 times of absolute ethyl alcohol and distilled water, is placed in and 3h is dried in baking box, obtains persursor material；Will
Obtained persursor material calcines 8h at 750 DEG C, obtains the final tertiary cathode material that floriform appearance is piled up with lamella
LiNi1/3Co1/3Mn1/3O2。
Embodiment 2：
It is 1 by volume ratio：1.25 water is added in autoclave with diethylene glycol (DEG) mixed liquor, then is added in reactor
Mol ratio is nickel nitrate：Cobalt nitrate：Manganese nitrate：Lithium nitrate=8：1：1：10 slaine, continuously adds ethylenediamine tetra-acetic acid two
Sodium, it is 1.25 with total metal ion mol ratio of the slaine for adding to control it：1,1.5h is stirred, it is obtained well mixed molten
Liquid；To hexamethylenetetramine is added in well mixed solution, it is 3 with total amount of metal ion mol ratio to control it：1,2h is stirred,
Fully after dissolving, solvent thermal reaction is carried out, reaction temperature is 190 DEG C, and the reaction time is 6h, is cooled to room temperature, and mixed liquor is obtained；
The mixed liquor filtering for completing will be reacted, is precipitated, with alternately washing 3~5 times of absolute ethyl alcohol and distilled water, be placed in baking box and do
Dry 5h, obtains persursor material；The persursor material that will be obtained calcines 7h at 800 DEG C, obtains final being piled up with lamella
The tertiary cathode material LiNi of floriform appearance0.8Co0.1Mn0.1O2。
Embodiment 3：
It is 1 by volume ratio：0.7 water is added in autoclave with the mixed liquor of triethylene glycol, then is added in reactor
Enter mol ratio for nickel nitrate：Cobalt nitrate：Manganese nitrate：Lithium nitrate=5：2：3：10 slaine, continuously adds ethylenediamine tetra-acetic acid
Disodium, it is 1.3 with total metal ion mol ratio of the slaine for adding to control it：1,2.5h is stirred, it is obtained well mixed molten
Liquid；To hexamethylenetetramine is added in well mixed solution, it is 4 with total amount of metal ion mol ratio to control it：1, stirring
After 1.5h, fully dissolving, solvent thermal reaction is carried out, reaction temperature is 200 DEG C, and the reaction time is 6h, is cooled to room temperature, be obtained mixed
Close liquid；The mixed liquor filtering for completing will be reacted, is precipitated, with alternately washing 3~5 times of absolute ethyl alcohol and distilled water, be placed in roasting
4h is dried in case, persursor material is obtained；Obtained persursor material is calcined into 7h at 800 DEG C, obtains final with piece
Layer piles up the tertiary cathode material LiNi of floriform appearance0.5Co0.2Mn0.3O2。
To the tertiary cathode material LiNi prepared by embodiment 30.5Co0.2Mn0.3O2Carry out physico-chemical property and chemical property
Tested.The tertiary cathode material LiNi prepared by embodiment 3 that Fig. 1 is provided for the present invention0.5Co0.2Mn0.3O2X-ray
Diffracting spectrum, as shown in Figure 1, in the tertiary cathode material prepared by embodiment 3 that the present invention is provided, all of diffraction maximum is returned
Belong to LiNi0.5Co0.2Mn0.3O2, there is no any impurity peak, i.e., the present invention has successfully prepared pure phase tertiary cathode material
LiNi0.5Co0.2Mn0.3O2。
The SEM figures of the tertiary cathode material prepared by embodiment 3 that Fig. 2 is provided for the present invention, as seen from Figure 2, this
Tertiary cathode material prepared by inventive embodiments 3 shows flower-like structure, and flower-like structure is piled up by lamella and formed, soilless sticking
Phenomenon.
The tertiary cathode material prepared by embodiment 3 that Fig. 3 is provided for the present invention is assembled into the cycle performance figure after battery,
As seen from Figure 3, under the multiplying power of 1C, specific capacity is up to 173mAh/g, and after circulating 200 times, specific capacity is still maintained
164mAh/g, its capability retention is up to 94.79%, i.e., the lamella prepared by embodiment 3 that the present invention is provided piles up flower-shaped knot
Structure tertiary cathode material has excellent chemical property, and specific capacity is high, and good cycle.
The preparation method of the tertiary cathode material that the present invention is provided, using solvent-thermal process method, prepares a kind of lamella heap
The tertiary cathode material of product flower-like structure, prepared tertiary cathode material has larger specific surface area, can be with electrolyte
It is fully contacted, uniformity is good and purity is high, the battery performance assembled using tertiary cathode material obtained in the present invention is good,
Specific capacity is high, and cycle performance is excellent.
The present invention is not restricted to described in specification and implementation method, therefore for the personnel of familiar field
Additional advantage and modification are easily achieved, therefore in the essence of the universal limited without departing substantially from claim and equivalency range
In the case of god and scope, the present invention is not limited to specific details, representational equipment and shown here as the diagram with description
Example.
Claims (7)
1. a kind of preparation method of tertiary cathode material, it is characterised in that：Comprise the following steps：
Step one：At room temperature, it is 1 according to volume ratio by water and organic solvent：(0.7~1.4) is configured to organic solution, will be matched somebody with somebody
The organic solution put is added in autoclave, adds nickel source, cobalt source, manganese source and lithium source, continuously adds metal ion network
Mixture, stirs 0.5-3h, obtains well mixed solution；
Step 2：To precipitating reagent is added in solution obtained in step one, 0.5~3h is stirred, fully after dissolving, carry out solvent heat anti-
Should, solvent thermal reaction temperature is 150-250 DEG C, and the reaction time is 2~36h, is cooled to room temperature, and mixed liquor is obtained；
Step 3：Mixed liquor obtained in step 2 is filtered, is precipitated, precipitation is replaced with absolute ethyl alcohol and distilled water
Washing 3~5 times, dries 1~24h, obtains persursor material；
Step 4：The persursor material that step 3 is obtained is calcined, final tertiary cathode material LiNi is obtained1-x- yCoxMnyO2, wherein the ﹤ y ﹤ 1 of 0 ﹤ x ﹤ 1,0.
2. the preparation method of tertiary cathode material as claimed in claim 1, it is characterised in that：Metal ion in the step one
The amount of complexing agent is (1.1~1.5) with the mol ratio of total amount of metal ion of nickel source, cobalt source, manganese source and lithium source：1.
3. the preparation method of tertiary cathode material as claimed in claim 1, it is characterised in that：It is organic molten in the step one
Agent is one or more in diethylene glycol (DEG), triethylene glycol, ethylene glycol, polyethylene glycol.
4. the preparation method of tertiary cathode material as claimed in claim 2, it is characterised in that：Nickel source in the step one is
One or more in nickel acetate, nickel chloride, nickel nitrate, nickel sulfate；Cobalt source in the step one is cobalt acetate, cobalt chloride,
One or more in cobalt nitrate, cobaltous sulfate；Manganese source in the step one is in manganese acetate, manganese chloride, manganese nitrate, manganese sulfate
One or more；Lithium source in the step one is one or more in lithium acetate, lithium nitrate, lithium citrate.
5. the preparation method of tertiary cathode material as claimed in claim 3, it is characterised in that：Metal network in the step one
Mixture is disodium ethylene diamine tetraacetate or ammoniacal liquor.
6. the preparation method of tertiary cathode material as claimed in claim 4, it is characterised in that：Precipitating reagent in the step 2
It is urea or hexamethylenetetramine.
7. the preparation method of tertiary cathode material as claimed in claim 5, it is characterised in that：Calcining temperature in the step 4
It is 600~950 DEG C to spend, and calcination time is 4~16h.
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Cited By (10)
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| CN107394164A (en) * | 2017-07-26 | 2017-11-24 | 天津银隆新能源有限公司 | Tertiary cathode material and preparation method thereof |
| CN107482192A (en) * | 2017-07-31 | 2017-12-15 | 深圳市德方纳米科技股份有限公司 | Monocrystalline tertiary cathode material and preparation method thereof and lithium ion battery |
| CN108264098A (en) * | 2018-02-26 | 2018-07-10 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
| CN108281604A (en) * | 2017-12-12 | 2018-07-13 | 昆明理工大学 | A kind of method of anode material for lithium-ion batteries solvent-thermal process |
| CN109574068A (en) * | 2018-12-03 | 2019-04-05 | 江苏清源新材料科技有限公司 | A method of solid state lithium battery critical material is produced using Hydrolyze method |
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| CN112054182A (en) * | 2019-06-06 | 2020-12-08 | 惠州比亚迪实业有限公司 | Nickel cobalt lithium manganate ternary precursor and preparation method thereof, and nickel cobalt lithium manganate positive electrode material |
| WO2021008423A1 (en) * | 2019-07-15 | 2021-01-21 | 比亚迪股份有限公司 | Lithium ion battery positive electrode material and preparation method therefor, and lithium ion battery |
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| CN107394164A (en) * | 2017-07-26 | 2017-11-24 | 天津银隆新能源有限公司 | Tertiary cathode material and preparation method thereof |
| CN107482192A (en) * | 2017-07-31 | 2017-12-15 | 深圳市德方纳米科技股份有限公司 | Monocrystalline tertiary cathode material and preparation method thereof and lithium ion battery |
| CN107482192B (en) * | 2017-07-31 | 2021-01-01 | 深圳市德方纳米科技股份有限公司 | Single crystal ternary positive electrode material, preparation method thereof and lithium ion battery |
| CN108281604A (en) * | 2017-12-12 | 2018-07-13 | 昆明理工大学 | A kind of method of anode material for lithium-ion batteries solvent-thermal process |
| CN108281604B (en) * | 2017-12-12 | 2020-08-25 | 昆明理工大学 | Solvothermal synthesis method of lithium ion battery anode material |
| CN110120518A (en) * | 2018-02-05 | 2019-08-13 | 电子科技大学 | Prepare LixMyOzThe method of graphene composite material and anode material of lithium battery and preparation method thereof |
| CN108264098B (en) * | 2018-02-26 | 2019-10-25 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
| CN108264098A (en) * | 2018-02-26 | 2018-07-10 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
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| CN110136984A (en) * | 2019-05-24 | 2019-08-16 | 西北工业大学 | Raspberry shape Ni/NiO/CoO/Mn for supercapacitor3O4Layered heterostructure and preparation method thereof |
| CN112054182A (en) * | 2019-06-06 | 2020-12-08 | 惠州比亚迪实业有限公司 | Nickel cobalt lithium manganate ternary precursor and preparation method thereof, and nickel cobalt lithium manganate positive electrode material |
| WO2021008423A1 (en) * | 2019-07-15 | 2021-01-21 | 比亚迪股份有限公司 | Lithium ion battery positive electrode material and preparation method therefor, and lithium ion battery |
| CN113471424A (en) * | 2021-07-12 | 2021-10-01 | 青海师范大学 | Ternary cathode material of lithium ion battery and preparation method thereof |
| CN113471424B (en) * | 2021-07-12 | 2022-05-24 | 青海师范大学 | Ternary cathode material of lithium ion battery and preparation method thereof |
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