CN111600002A - Preparation method of aluminum triethoxide coated nickel cobalt lithium manganate modified material - Google Patents

Preparation method of aluminum triethoxide coated nickel cobalt lithium manganate modified material Download PDF

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Publication number
CN111600002A
CN111600002A CN202010480224.2A CN202010480224A CN111600002A CN 111600002 A CN111600002 A CN 111600002A CN 202010480224 A CN202010480224 A CN 202010480224A CN 111600002 A CN111600002 A CN 111600002A
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stirring
nickel cobalt
lithium manganate
modified material
time
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袁亚彬
徐亚峰
邹小江
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Haihong Tanghe New Energy Technology Co ltd
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Haihong Tanghe New Energy Technology Co ltd
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    • 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
    • H01M4/362Composites
    • H01M4/364Composites as mixtures
    • 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
    • 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
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028Positive electrodes
    • 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

Abstract

The invention relates to the technical field of battery production, and discloses a preparation method of a triethanolammonium-coated nickel cobalt lithium manganate modified material. According to the invention, anhydrous ethanol is used as a solvent, compared with water used as a solvent raw material, the anhydrous ethanol is more easily dissolved in an organic solvent, and when the mixed liquid is heated to evaporate water in the solution, the evaporation time can be reduced due to less water in the solution, energy used in the evaporation process is saved, and the purposes of improving efficiency and saving energy are achieved.

Description

Preparation method of aluminum triethoxide coated nickel cobalt lithium manganate modified material
Technical Field
The invention relates to the technical field of battery production, in particular to a preparation method of a triethanolammonium coating nickel cobalt lithium manganate modified material.
Background
The lithium ion battery is a two-time battery system which respectively uses two different lithium intercalation compounds capable of reversibly inserting and extracting lithium ions as a positive electrode and a negative electrode of the battery, when in charging, the lithium ions are extracted from crystal lattices of a positive electrode material and inserted into the crystal lattices of a negative electrode material after passing through an electrolyte, so that the negative electrode is rich in lithium, the positive electrode is poor in lithium, when in discharging, the lithium ions are extracted from the crystal lattices of the negative electrode material and inserted into the crystal lattices of the positive electrode material after passing through the electrolyte, so that the positive electrode is rich in lithium, the negative electrode is poor in lithium, therefore, the difference of the potentials of the positive electrode material and the negative electrode material relative to metal lithium when in inserting and extracting the lithium ions is the working voltage of the battery, the lithium battery mainly comprises the positive electrode material, the negative electrode material, a diaphragm, electrolyte and the like, the positive electrode material occupies more than 40% of the total cost of the lithium battery, therefore, the lithium battery positive electrode material occupies a core position in the lithium battery, and the lithium battery positive electrode material which is already marketed at present comprises products such as lithium cobaltate, lithium manganate, lithium iron phosphate, ternary materials and the like, wherein the lithium nickel cobalt manganese oxide positive electrode material is increasingly widely produced and used due to considerable charge-discharge capacity and excellent cycle stability, and shows a huge market prospect.
At present, the existing method for preparing the lithium nickel cobalt manganese oxide modified material is slow in preparation efficiency, the raw material needs to be dissolved by mixed liquid of water and an organic solvent when a solution is prepared, the raw material is uniformly stirred in the solvent, the obtained solution is heated later, the heating time can be prolonged by water evaporation, a large amount of heat energy is wasted, the lithium nickel cobalt manganese oxide modified material cannot contact water when being used, the normal use of the lithium nickel cobalt manganese oxide modified material is influenced by an external humid environment, and the lithium nickel cobalt manganese oxide modified material can be better worked only by being isolated from the external humid environment.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a triethanolaluminum-coated nickel cobalt lithium manganate modified material, which has the advantages of reducing heating time, saving energy, placing products to be affected by damp and the like, and solves the problem that the material cannot be affected by damp due to slow preparation efficiency of the method.
(II) technical scheme
In order to achieve the purposes of reducing heating time, saving energy and keeping products under the influence of moisture for normal use, the invention provides a preparation method of a triethanolaluminum-coated nickel cobalt lithium manganate modified material, which comprises the following steps:
1) weighing nickel sulfate, cobalt sulfate, manganese sulfate and lithium hydroxide according to a molar ratio of 1:0.4:0.6:4 by using a weighing tool, putting the weighed standby raw materials into storage equipment for standby, weighing absolute ethyl alcohol by using an amount, and enabling the mass ratio of the absolute ethyl alcohol to the mass of all the standby raw materials to be 3:1, weighing the thickening agent by using a measuring tool to enable the mass ratio of the thickening agent to the absolute ethyl alcohol to be 0.3:1, weighing the deionized water by using a weighing tool to enable the mass ratio of the deionized water to the absolute ethyl alcohol to be 0.1:1, and weighing the concentrated sulfuric acid by using the weighing tool to enable the mass ratio of the concentrated sulfuric acid to the absolute ethyl alcohol to be 0.3: 1.
2) Pouring the absolute ethyl alcohol weighed in the step 1) into a stirring container, pouring the nickel sulfate, the cobalt sulfate and the manganese sulfate weighed in the step 1) into the stirring container, pouring the deionized water weighed in the step 1) into the stirring container, pre-stirring a mixture in the stirring container by using a stirring device, adding the lithium hydroxide weighed in the step 1) into the stirring container, and stirring for the second time to prepare a first mixed solution.
3) Heating the first mixed solution in the step 2) to maintain the temperature of the first mixed solution at a first temperature value, adding the concentrated sulfuric acid weighed in the step 1) into a stirring container, stirring for the third time, and maintaining the temperature at a second temperature value to obtain a second mixed solution.
4) Adding the thickener weighed in the step 1) into a stirring container, stirring for the fourth time, and adding a pH adjusting reagent to adjust the pH value of the mixed solution to obtain a third mixed solution.
5) Transferring the third mixed solution obtained in the step 4) to a heating plate, placing the heating plate in a calcining furnace for heating to finish primary calcining, then raising the temperature in the calcining furnace and carrying out secondary calcining in a vacuum environment to finally obtain a molding material.
6) And (3) soaking the molding material obtained in the step 5) in aluminum triethoxide for 3-5 min to obtain a pre-product, and then transferring the pre-product to a drying box at 100-120 ℃ for drying to obtain a finished product of the aluminum triethoxide-coated nickel cobalt lithium manganate modified material.
Preferably, the pre-stirring time in the step 2) is 10-12 min, and the second stirring time in the step 2) is 20-22 min.
Preferably, the first temperature value in the step 3) is 75-85 ℃, and the second temperature value in the step 3) is 45-55 ℃.
Preferably, the first calcination temperature in the step 5) is 550-650 ℃, the calcination time is 8-9 hours, the second calcination temperature in the step 5) is 900-1100 ℃, and the calcination time is 9-10 hours.
Preferably, the stirring container is an SZCL-2 digital display intelligent temperature control magnetic stirrer.
Preferably, the third stirring time in the step 3) is 1.5-2 hours.
Preferably, the fourth stirring time in the step 4) is 4-5 h.
Preferably, the PH adjusting agent used in step 4) is citric acid and ammonia water.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of a triethanol aluminum coated nickel cobalt lithium manganate modified material, which has the following beneficial effects:
1. according to the preparation method of the aluminum triethoxide coated nickel cobalt lithium manganate modified material, the anhydrous ethanol is used as the solvent, and compared with water used as the solvent raw material, the aluminum triethoxide coated nickel cobalt lithium manganate modified material is easier to dissolve in an organic solvent, and when the mixed liquid is heated to evaporate water in the solution, the evaporation time can be shortened due to less water in the solution, the energy used in the evaporation process is saved, and the purposes of improving the efficiency and saving the energy are achieved.
2. According to the preparation method of the aluminum triethoxide-coated nickel cobalt lithium manganate modified material, the aluminum triethoxide is coated on the outer surface of the forming material, the moisture on the surface of the material can be absorbed by utilizing the moisture absorption characteristic of the aluminum triethoxide, the nickel cobalt lithium manganate modified material is separated from the external environment, and the nickel cobalt lithium manganate modified material can be prevented from deteriorating due to the external environment when in use, so that the purpose of prolonging the service life of a battery is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of a triethanolate aluminum coated nickel cobalt lithium manganate modified material comprises the following steps:
step 1): weighing nickel sulfate, cobalt sulfate, manganese sulfate and lithium hydroxide according to a molar ratio of 1:0.4:0.6:4 by using a weighing tool, putting the weighed standby raw materials into storage equipment for standby, weighing absolute ethyl alcohol by using an amount, and enabling the mass ratio of the absolute ethyl alcohol to the mass of all the standby raw materials to be 3:1, weighing the thickening agent by using a measuring tool to enable the mass ratio of the thickening agent to the absolute ethyl alcohol to be 0.3:1, weighing the deionized water by using a weighing tool to enable the mass ratio of the deionized water to the absolute ethyl alcohol to be 0.1:1, and weighing the concentrated sulfuric acid by using the weighing tool to enable the mass ratio of the concentrated sulfuric acid to the absolute ethyl alcohol to be 0.3: 1.
Step 2): pouring the absolute ethyl alcohol weighed in the step 1) into a stirring container, wherein the stirring container is an SZCL-2 digital display intelligent temperature control magnetic stirrer, pouring the nickel sulfate, the cobalt sulfate and the manganese sulfate weighed in the step 1) into the stirring container, pouring the deionized water weighed in the step 1) into the stirring container, pre-stirring the mixture in the stirring container by using a stirring device for 10min, adding the lithium hydroxide weighed in the step 1) into the stirring container, and stirring for the second time to prepare a first mixed solution, wherein the stirring time for the second time is 20 min.
Step 3): heating the first mixed solution in the step 2) to maintain the temperature of the first mixed solution at a first temperature value which is 80 ℃, adding the concentrated sulfuric acid weighed in the step 1) into a stirring container, stirring for the third time, wherein the stirring time for the third time is 1.5h, maintaining the temperature at a second temperature value and the second temperature value at 50 ℃, and obtaining a second mixed solution.
Step 4): adding the thickener weighed in the step 1) into a stirring container, stirring for the fourth time, wherein the stirring time for the fourth time is 4 hours, adding a pH adjusting reagent to adjust the pH value of the mixed solution, and using citric acid and ammonia water as the pH adjusting reagent to obtain a third mixed solution.
Step 5): transferring the third mixed solution obtained in the step 4) into a heating plate, placing the heating plate in a calcining furnace, heating to finish the first calcining at the temperature of 550 ℃ for 9 hours, raising the temperature in the calcining furnace, and performing the second calcining in a vacuum environment at the temperature of 1000 ℃ for 9 hours to obtain the molding material.
Step 6): and (3) soaking the molding material obtained in the step 5) in aluminum triethoxide for 5min to obtain a pre-product, and then transferring the pre-product to a drying box at 110 ℃ for drying to obtain a finished product of the aluminum triethoxide coated nickel cobalt lithium manganate modified material.
Compared with the prior art, the solvent is changed into the sewage ethanol from water, the solvent is divided into two time periods when being calcined, namely, the water in the mixed solution can be effectively removed, the preparation time can be obviously shortened, and the aluminum triethoxide can form protection outside the nickel cobalt lithium manganate modified material, so that the service life of the battery is prolonged.
Example two:
a preparation method of a triethanolate aluminum coated nickel cobalt lithium manganate modified material comprises the following steps:
step 1): weighing nickel sulfate, cobalt sulfate, manganese sulfate and lithium hydroxide according to a molar ratio of 1:0.4:0.6:4 by using a weighing tool, putting the weighed standby raw materials into storage equipment for standby, weighing absolute ethyl alcohol by using an amount, and enabling the mass ratio of the absolute ethyl alcohol to the mass of all the standby raw materials to be 3:1, weighing the thickening agent by using a measuring tool to enable the mass ratio of the thickening agent to the absolute ethyl alcohol to be 0.3:1, weighing the deionized water by using a weighing tool to enable the mass ratio of the deionized water to the absolute ethyl alcohol to be 0.1:1, and weighing the concentrated sulfuric acid by using the weighing tool to enable the mass ratio of the concentrated sulfuric acid to the absolute ethyl alcohol to be 0.3: 1.
Step 2): pouring the absolute ethyl alcohol weighed in the step 1) into a stirring container, wherein the stirring container is an SZCL-2 digital display intelligent temperature control magnetic stirrer, pouring the nickel sulfate, the cobalt sulfate and the manganese sulfate weighed in the step 1) into the stirring container, pouring the deionized water weighed in the step 1) into the stirring container, pre-stirring the mixture in the stirring container by using a stirring device for 10min, adding the lithium hydroxide weighed in the step 1) into the stirring container, and stirring for the second time to prepare a first mixed solution, wherein the stirring time for the second time is 20 min.
Step 3): heating the first mixed solution in the step 2) to maintain the temperature of the first mixed solution at a first temperature value which is 80 ℃, adding the concentrated sulfuric acid weighed in the step 1) into a stirring container, stirring for the third time, wherein the stirring time for the third time is 1.5h, maintaining the temperature at a second temperature value and the second temperature value at 50 ℃, and obtaining a second mixed solution.
Step 4): adding the thickener weighed in the step 1) into a stirring container, stirring for the fourth time, wherein the stirring time for the fourth time is 4 hours, adding a pH adjusting reagent to adjust the pH value of the mixed solution, and using citric acid and ammonia water as the pH adjusting reagent to obtain a third mixed solution.
Step 5): transferring the third mixed solution obtained in the step 4) into a heating plate, placing the heating plate in a calcining furnace, heating to finish the first calcining at the temperature of 550 ℃ for 8 hours, raising the temperature in the calcining furnace, and performing the second calcining in a vacuum environment at the temperature of 1000 ℃ for 9 hours to obtain the molding material.
Step 6): and (3) soaking the molding material obtained in the step 5) in aluminum triethoxide for 5min to obtain a pre-product, and then transferring the pre-product to a drying box at 110 ℃ for drying to obtain a finished product of the aluminum triethoxide coated nickel cobalt lithium manganate modified material.
Compared with the first embodiment, the calcination time is changed to 8h when the first calcination is carried out, the time spent in the preparation step is shortened by one hour, the conductivity of the product is within the error allowable range compared with the product prepared in the first embodiment, and the energy consumed during heating is obviously reduced.
Example three:
a preparation method of a triethanolate aluminum coated nickel cobalt lithium manganate modified material comprises the following steps:
step 1): weighing nickel sulfate, cobalt sulfate, manganese sulfate and lithium hydroxide according to a molar ratio of 1:0.4:0.6:4 by using a weighing tool, putting the weighed standby raw materials into storage equipment for standby, weighing absolute ethyl alcohol by using an amount, and enabling the mass ratio of the absolute ethyl alcohol to the mass of all the standby raw materials to be 3:1, weighing the thickening agent by using a measuring tool to enable the mass ratio of the thickening agent to the absolute ethyl alcohol to be 0.3:1, weighing the deionized water by using a weighing tool to enable the mass ratio of the deionized water to the absolute ethyl alcohol to be 0.1:1, and weighing the concentrated sulfuric acid by using the weighing tool to enable the mass ratio of the concentrated sulfuric acid to the absolute ethyl alcohol to be 0.3: 1.
Step 2): pouring the absolute ethyl alcohol weighed in the step 1) into a stirring container, wherein the stirring container is an SZCL-2 digital display intelligent temperature control magnetic stirrer, pouring the nickel sulfate, the cobalt sulfate and the manganese sulfate weighed in the step 1) into the stirring container, pouring the deionized water weighed in the step 1) into the stirring container, pre-stirring the mixture in the stirring container by using a stirring device for 10min, adding the lithium hydroxide weighed in the step 1) into the stirring container, and stirring for the second time to prepare a first mixed solution, wherein the stirring time for the second time is 20 min.
Step 3): heating the first mixed solution in the step 2) to maintain the temperature of the first mixed solution at a first temperature value which is 80 ℃, adding the concentrated sulfuric acid weighed in the step 1) into a stirring container, stirring for the third time, wherein the stirring time for the third time is 1.5h, maintaining the temperature at a second temperature value and the second temperature value at 50 ℃, and obtaining a second mixed solution.
Step 4): adding the thickener weighed in the step 1) into a stirring container, stirring for the fourth time, wherein the stirring time for the fourth time is 4 hours, adding a pH adjusting reagent to adjust the pH value of the mixed solution, and using citric acid and ammonia water as the pH adjusting reagent to obtain a third mixed solution.
Step 5): transferring the third mixed solution obtained in the step 4) into a heating plate, placing the heating plate in a calcining furnace, heating to finish the first calcining at the temperature of 550 ℃ for 9 hours, raising the temperature in the calcining furnace, and performing the second calcining in a vacuum environment at the temperature of 1000 ℃ for 10 hours to obtain the molding material.
Step 6): and (3) soaking the molding material obtained in the step 5) in aluminum triethoxide for 5min to obtain a pre-product, and then transferring the pre-product to a drying box at 110 ℃ for drying to obtain a finished product of the aluminum triethoxide coated nickel cobalt lithium manganate modified material.
Compared with the first embodiment, the calcination time is changed to 10h when the second calcination is performed, the time taken by the preparation step is increased by one hour as a whole, and the conductivity of the product is increased compared with the product prepared by the first embodiment, but the energy consumed during heating is obviously increased.
The invention has the beneficial effects that: through utilizing absolute ethyl alcohol as the solvent, compare in regard to as the solvent raw materials with water and dissolve in organic solvent more easily, and when heating the mixed liquid and make the water evaporation in the solution, because the water in the solution is still less, can reduce the time of evaporation, practice thrift the energy that uses among the evaporation process, reach the purpose of raising the efficiency and energy saving, through wrapping up triethanol aluminium at the forming material surface, can utilize the moisture absorption's of triethanol aluminium characteristic with the material surface moisture absorption, separate nickel cobalt lithium manganate modified material and outside environment, can avoid nickel cobalt lithium manganate modified material to deteriorate because the external environment when using, thereby reach the purpose of extension battery life.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A preparation method of a triethanolate aluminum coated nickel cobalt lithium manganate modified material is characterized by comprising the following steps: the method comprises the following steps:
1) weighing nickel sulfate, cobalt sulfate, manganese sulfate and lithium hydroxide according to a molar ratio of 1:0.4:0.6:4 by using a weighing tool, putting the weighed standby raw materials into storage equipment for standby, weighing absolute ethyl alcohol by using an amount, and enabling the mass ratio of the absolute ethyl alcohol to the mass of all the standby raw materials to be 3:1, weighing the thickening agent by using a measuring tool to enable the mass ratio of the thickening agent to the absolute ethyl alcohol to be 0.3:1, weighing the deionized water by using a weighing tool to enable the mass ratio of the deionized water to the absolute ethyl alcohol to be 0.1:1, and weighing the concentrated sulfuric acid by using the weighing tool to enable the mass ratio of the concentrated sulfuric acid to the absolute ethyl alcohol to be 0.3: 1.
2) Pouring the absolute ethyl alcohol weighed in the step 1) into a stirring container, pouring the nickel sulfate, the cobalt sulfate and the manganese sulfate weighed in the step 1) into the stirring container, pouring the deionized water weighed in the step 1) into the stirring container, pre-stirring a mixture in the stirring container by using a stirring device, adding the lithium hydroxide weighed in the step 1) into the stirring container, and stirring for the second time to prepare a first mixed solution.
3) Heating the first mixed solution in the step 2) to maintain the temperature of the first mixed solution at a first temperature value, adding the concentrated sulfuric acid weighed in the step 1) into a stirring container, stirring for the third time, and maintaining the temperature at a second temperature value to obtain a second mixed solution.
4) Adding the thickener weighed in the step 1) into a stirring container, stirring for the fourth time, and adding a pH adjusting reagent to adjust the pH value of the mixed solution to obtain a third mixed solution.
5) Transferring the third mixed solution obtained in the step 4) to a heating plate, placing the heating plate in a calcining furnace for heating to finish primary calcining, then raising the temperature in the calcining furnace and carrying out secondary calcining in a vacuum environment to finally obtain a molding material.
6) And (3) soaking the molding material obtained in the step 5) in aluminum triethoxide for 3-5 min to obtain a pre-product, and then transferring the pre-product to a drying box at 100-120 ℃ for drying to obtain a finished product of the aluminum triethoxide-coated nickel cobalt lithium manganate modified material.
2. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the pre-stirring time in the step 2) is 10-12 min, and the second stirring time in the step 2) is 20-22 min.
3. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the first temperature value in the step 3) is 75-85 ℃, and the second temperature value in the step 3) is 45-55 ℃.
4. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the first calcination temperature in the step 5) is 550-650 ℃, the calcination time is 8-9 hours, the second calcination temperature in the step 5) is 900-1100 ℃, and the calcination time is 9-10 hours.
5. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the stirring container is an SZCL-2 digital display intelligent temperature control magnetic stirrer.
6. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the third stirring time in the step 3) is 1.5-2 h.
7. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the fourth stirring time in the step 4) is 4-5 hours.
8. The method for preparing the aluminum triethoxide coated nickel cobalt lithium manganate modified material according to claim 1, characterized in that: the pH adjusting reagent used in the step 4) is citric acid and ammonia water.
CN202010480224.2A 2020-05-30 2020-05-30 Preparation method of aluminum triethoxide coated nickel cobalt lithium manganate modified material Pending CN111600002A (en)

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CN106299299A (en) * 2016-09-21 2017-01-04 哈尔滨工业大学 A kind of anode material for lithium-ion batteries with surface hydrophobic and preparation method thereof
CN108376784A (en) * 2018-03-08 2018-08-07 西北工业大学 Improve the method for tertiary cathode material hygroscopicity and pulp gel phenomenon
CN109873140A (en) * 2019-02-18 2019-06-11 合肥工业大学 A kind of silicon/carbon/graphite in lithium ion batteries alkene complex ternary positive electrode and preparation method thereof
CN110838578A (en) * 2019-11-08 2020-02-25 常州博杰新能源材料有限公司 Preparation method of nickel cobalt lithium manganate positive electrode material

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Application publication date: 20200828