CN111029540A - Preparation method of battery negative electrode material - Google Patents
Preparation method of battery negative electrode material Download PDFInfo
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- CN111029540A CN111029540A CN201911122116.1A CN201911122116A CN111029540A CN 111029540 A CN111029540 A CN 111029540A CN 201911122116 A CN201911122116 A CN 201911122116A CN 111029540 A CN111029540 A CN 111029540A
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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
- 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
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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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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 invention discloses a preparation method of a battery cathode material, which specifically comprises the following steps: step 1, weighing nickel salt, putting the nickel salt into an ethanol solution, and adding an activating agent to obtain mixed slurry; step 2, adding a potassium cobalt cyanide solution, and stirring and aging to obtain a suspension; step 3, adding ammonia water and a sodium hydroxide solution, heating, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain nickel-cobalt oxide; step 4, preparing a protective layer; and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating to obtain the cathode material. The preparation method has the advantages of simple preparation process, high yield, no pollution, amorphous product structure, high safety performance, good conductivity, reversible specific capacity and good cycling stability.
Description
Technical Field
The invention belongs to the technical field of battery preparation, and relates to a preparation method of a battery cathode material.
Background
In order to meet the increasing energy demand and avoid global resource exhaustion and long-term damage to the environment, the problem to be solved urgently is to find an energy storage battery with high working voltage, high energy density, long cycle life, small self-discharge and environmental friendliness. Lithium ion batteries are highly desirable as a highly efficient energy storage battery for a wide range of applications. In recent years, lithium ion batteries have shown important application prospects in the fields of portable electronic devices, electric automobiles, aerospace and the like. However, with the increasing demand of people on the performance of energy storage batteries, lithium ion batteries with higher energy density, high specific capacity and good cycling stability are developed, which is a necessary trend for the development of future energy storage batteries, and the key point for developing high-performance lithium ion batteries lies in searching for suitable electrode materials.
Disclosure of Invention
The invention aims to provide a preparation method of a battery cathode material, which solves the problem of poor electrode cycle stability in the prior art.
The invention adopts the technical scheme that a preparation method of a battery cathode material is specifically carried out according to the following steps:
step 1, weighing nickel salt, putting the nickel salt into an ethanol solution, adding an active agent, and uniformly stirring to obtain mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, stirring, aging, and centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, heating, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain nickel-cobalt oxide;
step 4, weighing silicon powder, putting the silicon powder into an ethanol solution, ultrasonically stirring, adding titanium nitride, heating for reaction, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating to obtain the cathode material.
In the step 1, the nickel salt is any one of nickel nitrate, nickel acetate and nickel sulfate, and the activator is polyethylene glycol.
In the step 1, the mass ratio of the nickel salt to the activator is 1: 5-10, and the stirring time is 1-2 h.
In the step 2, the mass ratio of the nickel salt to the potassium cobalt cyanide is 1: 3-5, the stirring time is 1-3 hours, the aging time is 12-24 hours, and the aging temperature is 40-60 ℃.
In the step 3, the mass ratio of the turbid liquid to the sodium hydroxide to the ammonia water is 1: 1-2: 0.5-1, the heating temperature is 80-100 ℃, and the heating time is 10-15 hours.
In the step 3, the first calcination temperature is 200-300 ℃, the first calcination time is 2-4 h, the second calcination temperature is 300-500 ℃, and the second calcination time is 2-4 h.
In the step 4, the mass ratio of the silicon powder to the ethanol is 1: 10-20, wherein the mass ratio of the silicon powder to the titanium nitride is 1: 0.3-0.5, the stirring time is 1-2 hours, the heating time is 2-4 hours, and the heating temperature is 60-70 ℃.
In the step 5, the heating temperature is 800-1000 ℃, and the heating time is 15-30 min.
The preparation method has the beneficial effects that the prepared negative electrode material has strong cycle performance, the protective layer is arranged, the cycle stability of the battery negative electrode is effectively improved by the protective layer, the preparation process is simple, the yield is high, no pollution is caused, the product structure is amorphous, the safety performance is high, and the prepared negative electrode material has good conductivity, reversible specific capacity and better cycle stability.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
A preparation method of a battery negative electrode material specifically comprises the following steps:
step 1, weighing nickel salt, putting the nickel salt into an ethanol solution, adding an active agent, and uniformly stirring to obtain mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, stirring, aging, and centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, heating, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain nickel-cobalt oxide;
step 4, weighing silicon powder, putting the silicon powder into an ethanol solution, ultrasonically stirring, adding titanium nitride, heating for reaction, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating to obtain the cathode material.
In the step 1, the nickel salt is any one of nickel nitrate, nickel acetate and nickel sulfate, and the activator is polyethylene glycol.
In the step 1, the mass ratio of the nickel salt to the activator is 1: 5-10, and the stirring time is 1-2 h.
In the step 2, the mass ratio of the nickel salt to the potassium cobalt cyanide is 1: 3-5, the stirring time is 1-3 hours, the aging time is 12-24 hours, and the aging temperature is 40-60 ℃.
In the step 3, the mass ratio of the turbid liquid to the sodium hydroxide to the ammonia water is 1: 1-2: 0.5-1, the heating temperature is 80-100 ℃, and the heating time is 10-15 hours.
In the step 3, the first calcination temperature is 200-300 ℃, the first calcination time is 2-4 h, the second calcination temperature is 300-500 ℃, and the second calcination time is 2-4 h.
In the step 4, the mass ratio of the silicon powder to the ethanol is 1: 10-20, wherein the mass ratio of the silicon powder to the titanium nitride is 1: 0.3-0.5, the stirring time is 1-2 hours, the heating time is 2-4 hours, and the heating temperature is 60-70 ℃.
In the step 5, the heating temperature is 800-1000 ℃, and the heating time is 15-30 min.
The lithium battery is a rechargeable battery and mainly works by moving lithium ions between a positive electrode and a negative electrode, when the lithium battery is charged, 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 the lithium battery is discharged, 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, and the negative electrode is poor in lithium. Thus, the difference of the potentials of the anode and cathode materials relative to the metallic lithium during the insertion and extraction of lithium ions is the working voltage of the battery.
The positive electrode is the end with higher potential in the power supply, the positive electrode generally contains lithium ions, has variable-valence transition metal and is suitable for a space structure of a lithium ion extraction ground, the positive electrode material has higher oxidation-reduction potential, so that the battery has higher output voltage, the lithium ions can be greatly and reversibly inserted into and extracted from the positive electrode material, so that the battery has high capacity, the structure of the positive electrode material does not change in the lithium ion insertion/extraction process, the good cycle performance of the battery is ensured, the oxidation-reduction potential of the positive electrode changes slightly in the lithium ion insertion/extraction process, the voltage of the battery does not change significantly, so that the battery is ensured to be charged and discharged smoothly, the conductivity of the positive electrode material is higher, and the battery is charged and discharged in a large-current mode;
the negative electrode is the end with lower potential in the power supply, in the primary battery, it is the electrode with oxidation action, written on the left side in the battery reaction, from the physical point of view, it is the electrode from which the electrons flow out in the circuit, and the negative electrode material is the raw material of the negative electrode in the battery, the negative electrode of the lithium ion battery is made up by mixing the negative electrode active material carbon material or non-carbon material, adhesive and additive to make paste adhesive, evenly smearing on the two sides of the copper foil, drying and rolling.
Example 1
A preparation method of a battery negative electrode material specifically comprises the following steps:
step 1, weighing nickel nitrate, putting the nickel nitrate into an ethanol solution, adding polyethylene glycol, stirring uniformly for 2 hours to obtain mixed slurry, wherein the mass ratio of the nickel nitrate to the polyethylene glycol is 1: 5;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, wherein the mass ratio of nickel nitrate to potassium cobalt cyanide is 1:3, stirring for 3 hours, then aging for 12 hours at an aging temperature of 60 ℃, and then centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, heating the suspension, the sodium hydroxide and the ammonia water at the heating temperature of 100 ℃ for 10 hours in a mass ratio of 1:1:0.5, cooling, centrifuging, drying in vacuum, calcining, adding sodium hypophosphite, and continuously calcining to obtain the nickel-cobalt oxide, wherein the first calcining temperature is 300 ℃, the first calcining time is 2 hours, the second calcining temperature is 500 ℃, and the second calcining time is 2 hours;
step 4, weighing silicon powder, and putting the silicon powder into an ethanol solution, wherein the mass ratio of the silicon powder to the ethanol is 1: 20, ultrasonically stirring for 1h, then adding titanium nitride, wherein the mass ratio of silicon powder to titanium nitride is 1:0.5, heating for 2h at the temperature of 70 ℃, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating at 800 ℃ for 30min to obtain the cathode material.
Example 2
A preparation method of a battery negative electrode material specifically comprises the following steps:
step 1, weighing nickel acetate, putting the nickel acetate into an ethanol solution, adding polyethylene glycol, stirring uniformly for 1h, wherein the mass ratio of the nickel acetate to the polyethylene glycol is 1:10, and obtaining mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, stirring for 1h and then aging for 24h at the aging temperature of 40 ℃, and then centrifuging to obtain a suspension, wherein the mass ratio of nickel acetate to potassium cobalt cyanide is 1: 5;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, wherein the mass ratio of the suspension to the sodium hydroxide to the ammonia water is 1:2:1, heating at the temperature of 80 ℃ for 15 hours, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain nickel-cobalt oxide, wherein the first calcining temperature is 200 ℃, the first calcining time is 4 hours, the second calcining temperature is 300 ℃, and the second calcining time is 4 hours;
step 4, weighing silicon powder, and putting the silicon powder into an ethanol solution, wherein the mass ratio of the silicon powder to the ethanol is 1:10, ultrasonically stirring for 2 hours, then adding titanium nitride, wherein the mass ratio of silicon powder to titanium nitride is 1:0.3, heating for 4 hours at the temperature of 60 ℃, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating at the temperature of 1000 ℃ for 15min to obtain the cathode material.
Example 3
A preparation method of a battery negative electrode material specifically comprises the following steps:
step 1, weighing nickel sulfate, putting the nickel sulfate into an ethanol solution, adding polyethylene glycol, wherein the mass ratio of the nickel sulfate to the polyethylene glycol is 1:7, and stirring uniformly for 1.5 hours to obtain mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, wherein the mass ratio of nickel sulfate to potassium cobalt cyanide is 1:4, stirring for 2 hours, then aging for 16 hours at the aging temperature of 45 ℃, and then centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, heating the suspension, the sodium hydroxide and the ammonia water at a heating temperature of 90 ℃ for 12 hours at a mass ratio of 1:1.5:0.7, cooling, centrifuging, drying in vacuum, calcining, adding sodium hypophosphite, and continuously calcining to obtain the nickel-cobalt oxide, wherein the first calcining temperature is 210 ℃, the first calcining time is 3 hours, the second calcining temperature is 400 ℃, and the second calcining time is 3 hours;
step 4, weighing silicon powder, and putting the silicon powder into an ethanol solution, wherein the mass ratio of the silicon powder to the ethanol is 1: 15, ultrasonically stirring for 1.5h, then adding titanium nitride, wherein the mass ratio of silicon powder to titanium nitride is 1:0.4, heating for 3h at 65 ℃, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating at 900 ℃ for 20min to obtain the cathode material.
Example 4
A preparation method of a battery negative electrode material specifically comprises the following steps:
step 1, weighing nickel nitrate, putting the nickel nitrate into an ethanol solution, adding polyethylene glycol, wherein the mass ratio of nickel salt to polyethylene glycol is 1:10, and stirring for 2 hours to obtain mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, wherein the mass ratio of nickel salt to potassium cobalt cyanide is 1:3, stirring for 2 hours, then aging for 24 hours at the aging temperature of 40 ℃, and then centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, wherein the mass ratio of the suspension to the sodium hydroxide to the ammonia water is 1:2:1, heating at the temperature of 80 ℃ for 14h, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain the nickel-cobalt oxide, wherein the first calcining temperature is 300 ℃, the first calcining time is 2h, the second calcining temperature is 450 ℃, and the second calcining time is 2 h;
step 4, weighing silicon powder, and putting the silicon powder into an ethanol solution, wherein the mass ratio of the silicon powder to the ethanol is 1: 20, ultrasonically stirring for 1h, then adding titanium nitride, wherein the mass ratio of silicon powder to titanium nitride is 1:0.5, heating for 2h at the temperature of 66 ℃, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating at the temperature of 1000 ℃ for 15min to obtain the cathode material.
The prepared negative electrode material has strong cycle performance, is provided with the protective layer, the protective layer effectively improves the cycle stability of the battery negative electrode, the preparation process is simple, the yield is high, no pollution is caused, the product structure is amorphous, the safety performance is high, and meanwhile, the prepared negative electrode material has good conductivity, reversible specific capacity and better cycle stability.
Claims (8)
1. The preparation method of the battery negative electrode material is characterized by comprising the following steps:
step 1, weighing nickel salt, putting the nickel salt into an ethanol solution, adding an active agent, and uniformly stirring to obtain mixed slurry;
step 2, adding a potassium cobalt cyanide solution into the mixed slurry, stirring, aging, and centrifuging to obtain a suspension;
step 3, adding ammonia water and a sodium hydroxide solution into the suspension, heating, cooling, centrifuging, vacuum drying, calcining, adding sodium hypophosphite, and continuously calcining to obtain nickel-cobalt oxide;
step 4, weighing silicon powder, putting the silicon powder into an ethanol solution, ultrasonically stirring, adding titanium nitride, heating for reaction, and coating a layer of titanium oxide on the surface of the material to obtain a protective layer;
and 5, putting the nickel-cobalt oxide and the protective layer into a fixed bed reactor, introducing nitrogen, and heating to obtain the cathode material.
2. The method for preparing the battery negative electrode material according to claim 1, wherein in the step 1, the nickel salt is any one of nickel nitrate, nickel acetate and nickel sulfate, and the activator is polyethylene glycol.
3. The preparation method of the battery negative electrode material as claimed in claim 1, wherein in the step 1, the mass ratio of the nickel salt to the active agent is 1: 5-10, and the stirring time is 1-2 h.
4. The method for preparing the battery negative electrode material as claimed in claim 1, wherein in the step 2, the mass ratio of the nickel salt to the potassium cobalt cyanide is 1: 3-5, the stirring time is 1-3 h, the aging time is 12-24 h, and the aging temperature is 40-60 ℃.
5. The preparation method of the battery negative electrode material according to claim 1, wherein in the step 3, the mass ratio of the suspension, the sodium hydroxide and the ammonia water is 1: 1-2: 0.5-1, the heating temperature is 80-100 ℃, and the heating time is 10-15 h.
6. The method for preparing the battery negative electrode material according to claim 1, wherein in the step 3, the first calcination temperature is 200-300 ℃, the first calcination time is 2-4 h, the second calcination temperature is 300-500 ℃, and the second calcination time is 2-4 h.
7. The preparation method of the battery anode material according to claim 1, wherein in the step 4, the mass ratio of the silicon powder to the ethanol is 1: 10-20, wherein the mass ratio of the silicon powder to the titanium nitride is 1: 0.3-0.5, the stirring time is 1-2 hours, the heating time is 2-4 hours, and the heating temperature is 60-70 ℃.
8. The preparation method of the battery negative electrode material according to claim 1, wherein in the step 5, the heating temperature is 800-1000 ℃ and the heating time is 15-30 min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104051718A (en) * | 2014-06-26 | 2014-09-17 | 南京师范大学 | Preparation method for negative electrode material three-dimensional nanometer porous tin dioxide-based composite oxide of lithium ion battery |
| CN109935819A (en) * | 2019-04-02 | 2019-06-25 | 江西理工大学 | A kind of preparation method of the negative electrode material for lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104051718A (en) * | 2014-06-26 | 2014-09-17 | 南京师范大学 | Preparation method for negative electrode material three-dimensional nanometer porous tin dioxide-based composite oxide of lithium ion battery |
| CN109935819A (en) * | 2019-04-02 | 2019-06-25 | 江西理工大学 | A kind of preparation method of the negative electrode material for lithium ion battery |
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Application publication date: 20200417 |