CN111725499B - Method for preparing lithium battery cathode material NCM811 by using co-precipitation method with electrolytic method - Google Patents

Method for preparing lithium battery cathode material NCM811 by using co-precipitation method with electrolytic method Download PDF

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CN111725499B
CN111725499B CN202010604109.1A CN202010604109A CN111725499B CN 111725499 B CN111725499 B CN 111725499B CN 202010604109 A CN202010604109 A CN 202010604109A CN 111725499 B CN111725499 B CN 111725499B
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electrolyte
cathode
lithium battery
electrolytic
nickel
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CN111725499A (en
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刘强
肖志飞
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Liu Qiang
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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

Abstract

A method for preparing a lithium battery cathode material NCM811 by a co-electrolytic coprecipitation method comprises the following steps: step 1: adding an electrolyte into a sealed electrolytic cell filled with inert gas; step 2: in a sealed electrolytic cell, anodes and cathodes are arranged, wherein the anodes are three and are respectively made of the following materials: nickel, manganese and cobalt, wherein the cathode material is nickel; and step 3: adding a complexing agent into the electrolyte, and adjusting the pH value of the electrolyte to be alkaline; and 4, step 4: connecting a constant current power supply with the cathode and the anode respectively, and switching on the constant current power supply to combine transition metal ions formed at the anode with hydroxyl ions formed at the cathode to form Ni in the electrolyte 0.8 Co 0.1 Mn 0.1 (OH) 2 (ii) a And 5: ni obtained in step 4 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH H 2 O, sintering at high temperature to obtain LiNi 0.8 Co 0.1 Mn 0.1 O 2 A material.

Description

Method for preparing lithium battery cathode material NCM811 by using co-precipitation method with electrolytic method
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a method for preparing a lithium battery cathode material NCM811 by using a co-precipitation method with an electrolytic method.
Background
The nickel-cobalt-manganese ternary material is one of the main materials of the current power battery, and the ternary element has different meanings for the anode material, wherein the nickel element is used for improving the battery capacity, and the higher the nickel content is, the larger the specific capacity of the material is. The specific capacity of NCM811 (nickel cobalt manganese) can reach 200mAh/g, the discharge platform is about 3.8V, and the lithium battery anode material with high energy density can be prepared. Under the background of high utilization rate and high demand of the existing anode material capacity, related lithium battery enterprises continuously promote the upgrading and capacity expansion of the NCM811 battery anode material, and simultaneously increase the development of solid lithium battery materials and lithium-rich manganese-based materials, thereby further enhancing the advantages in the field of anode materials. In the field of international power batteries, the development trend of high nickel content of positive electrode materials is more and more remarkable, and in order to strengthen the cooperation with international clients such as Tesla, the public, BMW, modern and daily products, high-volume production of NCM811 materials is prepared by various large lithium battery enterprises.
The traditional preparation method of the NCM811 material is a coprecipitation method, nickel sulfate, cobalt sulfate and manganese sulfate mixed salt solution, ammonia water as a complexing agent and sodium hydroxide as a precipitating agent are added into a reaction kettle at a certain flow rate, and the reaction time is more than 24 hours, so that a precursor of the lithium ion battery anode material is obtained. The method has complex production equipment and long reaction time, and a large amount of sodium hydroxide solution is added, thereby causing great pressure on environment protection work.
Disclosure of Invention
Aiming at the problems of complex production equipment, long reaction time and the like in the prior art, in the sealed electrolytic cell, the anode electrolyzes metal simple substances to change the metal simple substances into metal ions, the cathode separates out hydrogen to produce hydroxyl ions, and the hydroxyl ions just form precipitates with the metal ions which are separated out by electrolysis, so that sodium hydroxide required by a coprecipitation method is saved.
In order to achieve the purpose, the invention provides a method for preparing a lithium battery cathode material NCM811 by using a coprecipitation method with an electrolytic method. The adopted specific technical scheme is as follows:
a method for preparing a lithium battery cathode material NCM811 by a co-electrolytic coprecipitation method comprises the following steps:
step 1: adding an electrolyte into a sealed electrolytic cell filled with inert gas;
step 2: in a sealed electrolytic cell, anodes and cathodes are arranged, wherein the anodes are three and are respectively made of the following materials: nickel, manganese and cobalt, wherein the cathode material is nickel;
and 3, step 3: adding a complexing agent into the electrolyte, and adjusting the pH value of the electrolyte to be alkaline;
and 4, step 4: respectively connecting a constant current power supply with a cathode and an anode, and connecting the constant current power supply to combine transition metal ions formed at the anode with hydroxyl ions formed at the cathode to form Ni in the electrolyte 0.8 Co 0.1 Mn 0.1 (OH) 2 ；
And 5: ni produced in step 4 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH & H 2 O, sintering at high temperature to obtain LiNi 0.8 Co 0.1 Mn 0.1 O 2 A material.
Further, the inert gas in the step 1 is one or a combination of more of nitrogen, helium and argon. Because the system is a closed system, inert gas is introduced into the closed electrolytic cell, so that oxygen in the electrolytic cell can be discharged, the material prepared by reaction is prevented from being oxidized in the reaction process, and the material is protected.
Further, the electrolyte in the step 1 is one or a combination of more of a KCl solution, a NaCl solution, a sulfate solution and a nitrate solution, and the mass fraction of the electrolyte is 1-10%, preferably 2%. The proper electrolyte is added into the closed reaction system, so that the resistance of the electrolyte in the electrolytic process can be effectively reduced, and the voltage can be more easily and accurately controlled in a reasonable range. Meanwhile, the addition amount of electrolyte of the electrolyte is moderate, too little electrolyte can not enable the voltage to be in a reasonable range, too much electrolyte solution brings troubles to the process of washing materials in the later period, so that the materials are not washed cleanly, and impurities are introduced more easily.
Furthermore, in the step 2, the number of the cathodes is 1-3, and the cathode material is foamed nickel. The foamed nickel acts as a counter electrode and can form a closed loop with the anode.
Further, the complexing agent in step 3 is one of ammonia water, sodium acetate alkali solution and sodium carbonate alkali solution, the pH value needs to be adjusted to be within the range of 11-12, and the preferable pH value is 11.5. The complexing agent can complex nickel, cobalt and manganese transition metal ions together, after the complex is formed, hydroxide ions are replaced by the complexing agent, so that a hydroxide precursor is formed, meanwhile, the pH value of the reaction has a great influence on the material, the pH value is too low, the tap density of the material is low, the appearance is loose, the pH value is too high, the material can agglomerate, and the performance of the material is influenced.
Further, in the step 4, the constant current power supply is switched on for 12 to 20 hours, preferably 12 hours. The particle size of the material directly influences the performance of the material, the reaction time is too short, the particle size of the material is too small, the reaction time is too long, and the particle size of the material is too large, so the reaction time is controlled, and the performance of the material is better.
Further, the high-temperature sintering in the step 5 is carried out for 4 to 6 hours at 400 to 500 ℃ and then for 8 to 12 hours at 700 to 900 ℃. The high-temperature sintering can enable the material to present a better layered structure, but the material structure is easy to collapse when the temperature is too high and the sintering time is too long, and conversely, the oxidation is incomplete and the crystal structure is not good.
Furthermore, the sealed electrolytic cell is provided with a one-way conduction air outlet. Because hydrogen is generated during the reaction, the hydrogen is dangerous if not discharged in time due to safety considerations.
The beneficial effects of the invention are: the preparation method has the advantages of short time for preparing the material, rapidness and high efficiency, simpler preparation device, safety and controllability, more environmental friendliness due to the fact that alkali and ammonia water used in a coprecipitation method are omitted, large specific surface area of the prepared material, good rate capability of the material, capability of large-current charge and discharge, good stability and high first-time discharge capacity. The material is expected to be widely applied in the fields of electric automobiles, aircrafts and the like due to better electrochemical performance.
Drawings
FIG. 1 is an XRD pattern of the synthetic material of example 1 of the present invention
FIG. 2 is an SEM photograph of a synthesized material of example 1 of the present invention
FIG. 3 is an XRD pattern of the synthesized material of example 2 of the present invention
FIG. 4 is an SEM photograph of a synthesized sample of example 2 of the present invention
FIG. 5 is an XRD pattern of a synthetic material of example 3 of the present invention
FIG. 6 is an SEM photograph of a synthesized sample of example 3 of the present invention
FIG. 7 is an XRD pattern of a synthetic material of example 4 of the present invention
FIG. 8 is an SEM photograph of a synthesized sample of example 4 of the present invention
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the following detailed description of the invention is further explained, but not limited to the scope of the invention, it is noted that the embodiments and features of the embodiments of the invention can be combined with each other without conflict.
Example 1:
in the sealed electrolytic cell that is full of inert gas nitrogen, the electrolyte is 1% KCl solution, adjusts pH to 11 with the aqueous ammonia, and the positive pole is nickel, manganese, cobalt respectively, and the negative pole is 1 foam nickel, connects the negative and positive poles with constant current power supply, lets in stable electric current, and reaction time control is 12 hours, and the size control of electric current produces the speed of ion, sets up and obtains current ratio Ni through the positive pole: co: mn =8 0.8 Co 0.1 Mn 0.1 (OH) 2 Produced Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH & H 2 And O, sintering at the high temperature of 400 ℃ for 4 hours in a tube furnace, and then sintering at the high temperature of 700 ℃ for 8 hours to obtain the NCM811 material. The results of X-ray diffractometry (XRD) analysis are shown in FIG. 1, and the photographs obtained by Scanning Electron Microscopy (SEM) are shown in FIG. 2.
Example 2:
in a sealed electrolytic cell filled with inert gas helium, an electrolyte is a 2% NaCl solution, the pH value is adjusted to 11.5 by using a sodium acetate alkali solution, anodes are respectively nickel, manganese and cobalt, cathodes are 2 foamed nickel, a constant current power supply is connected with a cathode and an anode, stable current is introduced, the reaction time is controlled to be 16 hours, the speed of generating ions is controlled by the magnitude of the current, and the current ratio Ni obtained by the anode is set as follows: co: mn =8, so that the transition metal simple substance at the anode is oxidized into transition metal ions, the cathode is used for precipitating hydrogen under the action of current, the hydrogen is discharged from a one-way conduction air outlet arranged on the sealed electrolytic cell, and meanwhile, hydroxide ions generated at the cathode just form precipitates with metal ions such as nickel, cobalt and manganese, and therefore Ni =8 0.8 Co 0.1 Mn 0.1 (OH) 2 Produced Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH H 2 O, sintering at high temperature of 500 ℃ in a tube furnace 6After that, the mixture was sintered at 900 ℃ for 12 hours to obtain an NCM811 material. The results of X-ray diffractometry (XRD) analysis are shown in FIG. 3, and the photographs obtained by Scanning Electron Microscopy (SEM) are shown in FIG. 4.
Example 3:
in a sealed cell filled with argon as inert gas, the electrolyte has a K of 10% 2 SO 4 The pH of the solution is adjusted to 12 by using sodium carbonate alkali solution, the anode is nickel, manganese and cobalt respectively, the cathode is 3 pieces of foamed nickel, the solution is connected with the cathode and the anode by using a constant current power supply, stable current is introduced, the reaction time is controlled to be 20 hours, the speed of generating ions is controlled by the size of the current, and the current ratio Ni obtained by the anode is set as follows: co: mn =8, so that the transition metal simple substance at the anode is oxidized into transition metal ions, the cathode is used for precipitating hydrogen under the action of current, the hydrogen is discharged from a one-way conduction air outlet arranged on the sealed electrolytic cell, and meanwhile, hydroxide ions generated at the cathode just form precipitates with metal ions such as nickel, cobalt and manganese, and therefore Ni =8 0.8 Co 0.1 Mn 0.1 (OH) 2 Produced Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH H 2 And O, sintering at the high temperature of 450 ℃ for 5 hours in a tube furnace, and then sintering at the high temperature of 800 ℃ for 10 hours to obtain the NCM811 material. The results of X-ray diffractometry (XRD) analysis are shown in FIG. 5, and the photographs obtained by Scanning Electron Microscopy (SEM) are shown in FIG. 6.
Example 4:
in a sealed electrolytic cell filled with inert gases nitrogen and helium, the electrolyte is 2% KNO 3 The solution, adjust pH to 11.5 with the aqueous ammonia, the positive pole is nickel, manganese, cobalt respectively, and the negative pole is 3 foam nickel, connects the negative and positive poles with constant current power supply, lets in stable electric current, and reaction time control is in 12 hours, and the size control of electric current produces the speed of ion, sets up and obtains current ratio Ni through the positive pole: co: mn =8 0.8 Co 0.1 Mn 0.1 (OH) 2 Prepared Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOHH 2 And O, sintering at the high temperature of 400 ℃ for 4 hours in a tube furnace, and then sintering at the high temperature of 700 ℃ for 8 hours to obtain the NCM811 material. The results of X-ray diffractometry (XRD) analysis are shown in FIG. 7, and the photographs obtained by Scanning Electron Microscopy (SEM) are shown in FIG. 8.
The NCM811 of the invention is LiNi 0.8 Co 0.1 Mn 0.1 O 2 。
In the analysis of the NCM811 material synthesized in examples 1-4, it was found that:
(1) XRD analysis: all XRD patterns correspond to PDF (006-0063) standard cards, the material is in a laminated alpha-NaFeO 2 laminated structure, the space group is R-3m, the intensity of each diffraction peak is high, the material is high in crystallinity, no impurity peak is generated, the material is high in purity, and the splitting peak at the 008/110 position indicates that the prepared material is high in crystallinity and good in laminated structure.
(2) SEM analysis: all samples showed spherical structures, the particle size of the material was relatively average, and the surface of the material was relatively dense, indicating that the material had better cycle stability.
On the basis, the samples of the examples 1 to 4 are subjected to constant current charge and discharge test and rate performance test:
first, the constant current charge and discharge test is performed by assembling a button cell using a material as a positive electrode of a lithium ion battery and performing the constant current charge and discharge test in the LAND battery test system 2001A. The cycle test is a 0.1C (1C = 200mAh/g) charge and discharge test in a voltage range of 2.8-4.3V, and all samples have good cycle stability and high capacity retention rate.
Secondly, rate performance test: the battery is subjected to charge-discharge test at a current density of 0.1C,0.2C,0.5C,1C,2C,5C (1C=200mAh/g) in a range of 2.8-4.3V, and all samples show better rate multiplying performance.
Note that: all discharge capacity units are mAh/g
The specific experimental comparative data are as follows:
(1) Constant current charge and discharge test
First discharge capacity at 0.1C 0.1C 100 cycle discharge capacity Capacity retention after 0.1C 100 cycles
Example 1 167 94.6 56.6％
Example 2 170.1 110.2 64.8％
Example 3 169.1 109.2 64.6％
Example 4 192.3 141 73.3％
(2) Rate capability test
0.2C discharge capacity 0.2C discharge capacity 0.5C discharge capacity 1C discharge capacity 2C discharge capacity 5C discharge capacity
Example 1 167 158.6 152.4 144.3 142.4 131.9
Example 2 170.1 159.6 152.2 142.5 135.2 126.1
Example 3 169.1 162.5 155 145.8 135.7 117.5
Example 4 192.3 180.1 170.3 163.7 158.8 150
The electrochemical reaction is comprehensively analyzed by combining XRD, SEM and constant current charge and discharge tests, the electrolytic current is set to be 0.2A, the reaction PH =11.5, the reaction time is 12h, and the electrochemical reaction is the optimal material preparation condition.
The method for preparing the cathode material NCM811 of the lithium battery by combining the electrolytic coprecipitation method is described by specific examples. The technical personnel can use the content of the invention to change the process flow or the process parameters and other links appropriately to realize other corresponding purposes, and the related changes do not depart from the content of the invention, and any modification, equivalent replacement, improvement and the like made within the spirit and the principle of the invention are all included in the protection scope of the invention.

Claims (4)

1. A method for preparing a lithium battery positive electrode material NCM811 by a co-electrolytic coprecipitation method is characterized by comprising the following steps:
step 1: adding an electrolyte into a sealed electrolytic cell filled with inert gas;
and 2, step: in a sealed electrolytic cell, anodes and cathodes are arranged, wherein the number of the anodes is three, and the anodes are respectively made of the following materials: nickel, manganese and cobalt, wherein the cathode material is nickel;
and step 3: adding a complexing agent into the electrolyte, and adjusting the pH value of the electrolyte to be alkaline;
and 4, step 4: connecting a constant current power supply with the cathode and the anode respectively, and switching on the constant current power supply to combine transition metal ions formed at the anode with hydroxyl ions formed at the cathode to form Ni in the electrolyte 0.8 Co 0.1 Mn 0.1 (OH) 2 ；
And 5: ni produced in step 4 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding LiOH & H 2 O, sintering at high temperature to obtain LiNi 0.8 Co 0.1 Mn 0.1 O 2 A material;
step 2, the number of the cathodes is 1-3, and the cathode material is foamed nickel;
the complexing agent in the step 3 is one of ammonia water, sodium acetate alkali solution and sodium carbonate alkali solution; the pH is 11-12;
step 4, the time for switching on the constant current power supply is 12-20 hours; setting the current ratio Ni to Co to Mn =8 to 1 of the anode;
sintering at high temperature in the step 5, namely sintering for 4-6 hours at 400-500 ℃ and sintering for 8-12 hours at 700-900 ℃;
and the sealed electrolytic cell is provided with a unidirectional conduction air outlet.
2. The method for preparing the positive electrode material NCM811 for the lithium battery by the co-electrolytic co-precipitation method according to claim 1, wherein the inert gas in step 1 is one or more of nitrogen, helium and argon.
3. The method for preparing the positive electrode material NCM811 for the lithium battery by the co-electrolytic co-precipitation method according to claim 1, wherein the electrolyte in the step 1 is a combination of more than one of a KCl solution, a NaCl solution, a sulfate solution and a nitrate solution.
4. The method for preparing the lithium battery cathode material NCM811 by the co-electrolytic co-precipitation method according to claim 1, wherein the electrolyte in the step 1 has a mass fraction of 1-10%.
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