CN109065860B - Preparation method of lithium battery positive electrode material - Google Patents

Preparation method of lithium battery positive electrode material Download PDF

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CN109065860B
CN109065860B CN201810858177.3A CN201810858177A CN109065860B CN 109065860 B CN109065860 B CN 109065860B CN 201810858177 A CN201810858177 A CN 201810858177A CN 109065860 B CN109065860 B CN 109065860B
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nitrate
graphene
mixed solution
ethanol
lithium battery
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CN109065860A (en
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刘和光
游才印
赵娜娜
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Xian University of Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/582—Halogenides
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

The invention discloses a preparation method of a lithium battery anode material, which is implemented according to the following steps: step 1, preparing an ammonium fluoride solution; step 2, preparing a nitrate graphene/ethanol mixed solution; step 3, adding the ammonium fluoride solution into the nitrate graphene/ethanol mixed solution, and centrifuging and drying to obtain Ni0.5Co0.5F2The graphene composite material is a lithium battery positive electrode material. The method has simple operation and high efficiency0.5Co0.5F2The size of nickel-cobalt fluoride nanoparticles in the graphene composite material is smaller and can reach below 40 nm; meanwhile, the nickel cobalt fluoride nanoparticles have good dispersibility on the surface of graphene, and the electron mobility of the nickel cobalt fluoride can be effectively improved.

Description

Preparation method of lithium battery positive electrode material
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a preparation method of a lithium battery anode material.
Background
In the past decades, the technology of lithium ion batteries has been rapidly developed and is gradually widely applied in the field of mobile electronic devices or handheld electronic products such as mobile phones, computers, digital cameras and the like, and lithium ion batteries work by reversibly releasing and inserting lithium ions between a positive electrode and a negative electrode, and compared with other batteries, the lithium ion batteries have the advantages of high energy density, low battery cost, safety, no pollution and long service life. However, with the vigorous development in the fields of electric hybrid vehicles, large-scale power grids, and the like, higher requirements are put on the energy density of batteries. LiCoO is mostly adopted in the existing commercial lithium ion battery2The material is a positive electrode (specific capacity)<140mAh/g), the energy density is only about 300Wh/kg, and the application requirement cannot be met.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium battery anode material, which improves the specific capacity of the conventional lithium battery anode material.
The technical scheme adopted by the invention is that the preparation method of the lithium battery anode material is implemented according to the following steps:
step 1, preparing an ammonium fluoride solution;
step 2, preparing a nitrate graphene/ethanol mixed solution;
step 3, adding the ammonium fluoride solution into the nitrate graphene/ethanol mixed solution, and centrifuging and drying to obtain Ni0.5Co0.5F2The graphene composite material is a lithium battery positive electrode material.
The present invention is also characterized in that,
step 1 specifically, adding ammonium fluoride into deionized water, and stirring until the ammonium fluoride is completely dissolved to obtain 2mol/L ammonium fluoride solution.
The step 2 is implemented according to the following steps:
2.1, ultrasonically dissolving expanded graphite in ethanol by using an ultrasonic dissolver to obtain a graphene/ethanol solution, wherein the mass ratio of the expanded graphite to the ethanol is 789: 1;
step 2.2, respectively adding cobalt nitrate and nickel nitrate into the graphene/ethanol solution, and stirring until the cobalt nitrate and the nickel nitrate are completely dissolved to obtain a primary nitrate graphene/ethanol mixed solution;
and 2.3, adding oleic acid into the primary nitrate graphene mixed solution, and stirring until the oleic acid and the primary nitrate graphene mixed solution are uniformly mixed to obtain a nitrate graphene/ethanol mixed solution.
The ratio of the sum of the amounts of the cobalt nitrate and nickel nitrate substances to the amount of the ammonium fluoride substance in the ammonium fluoride solution is 1:2, and the amounts of the cobalt nitrate and nickel nitrate substances are both more than 0 mol.
The cobalt nitrate is cobalt nitrate hexahydrate Co (NO)3)2·6H2O, nickel nitrate is nickel nitrate hexahydrate Ni (NO)3)2·6H2O。
The volume ratio of the oleic acid to the ethanol in the primary nitrate graphene mixed solution is 1: 3-1: 4.
The ultrasonic dissolution time is 2.8-4 h.
Step 3 is specifically implemented according to the following steps:
step 3.1, adding an ammonium fluoride solution into a nitrate graphene/ethanol mixed solution, and uniformly stirring to obtain a mixed solution A;
step 3.2, centrifuging the mixed solution A by using a centrifuge to obtain a precipitate A, and washing the precipitate A by using deionized water for 3-5 times to obtain a sample A;
step 3.3, drying the sample A in a drying oven for 12-24 hours at the drying temperature of 78-85 ℃ to obtain a dried sample;
step 3.4, carrying out heat treatment on the sample B by using a tube furnace, and simultaneously introducing N into the tube furnace2As protective gas, the heat treatment temperature is 400 ℃, and the heat preservation time is 2 hours, so as to obtain a sample C;
step 3.5, cooling the sample C to room temperature to obtain Ni0.5Co0.5F2The graphene composite material is a lithium battery positive electrode material.
The rotating speed of the centrifugal machine is 5000 r/min-6000 r/min.
The heating rate of the heat treatment is 8-10 ℃/min.
The preparation method of the lithium battery cathode material has the advantages of simple and efficient operation, no need of high temperature and high pressure, low raw material cost and little pollution; ni produced by the invention0.5Co0.5F2The size of nickel-cobalt fluoride nanoparticles in the graphene composite material is smaller and can reach below 40 nm; meanwhile, the nickel-cobalt fluoride nanoparticles have good dispersibility on the surface of graphene and stable phase interface, can effectively improve the electron mobility of the nickel-cobalt fluoride, simultaneously ensure the contact between the nickel-cobalt fluoride and electrolyte, and promote the transmission and diffusion of lithium ions, thereby improving the electrochemical properties such as specific capacity, multiplying power and the like of the nickel-cobalt fluoride.
Drawings
FIG. 1 shows Ni obtained in example 1 of a method for preparing a positive electrode material for a lithium battery according to the present invention0.5Co0.5F2SEM photograph of/graphene composite material;
FIG. 2 shows Ni prepared in example 1 of a method for preparing a positive electrode material for a lithium battery according to the present invention0.5Co0.5F2XRD pattern of the/graphene composite material;
FIG. 3 shows Ni prepared in example 1 of a method for preparing a positive electrode material for a lithium battery according to the present invention0.5Co0.5F2Graphene and Ni prepared in comparative example 10.5Co0.5F2A cycle performance profile of the material;
FIG. 4 shows Ni prepared in example 1 of a method for preparing a positive electrode material for a lithium battery according to the present invention0.5Co0.5F2Graphene and Ni prepared in comparative example 10.5Co0.5F2Magnification graph of material.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a lithium battery anode material, which is implemented according to the following steps:
step 1, preparing ammonium fluoride solution
Step 1 specifically, adding ammonium fluoride into deionized water, and stirring until the ammonium fluoride is completely dissolved to obtain 2mol/L ammonium fluoride solution.
Step 2, preparing nitrate graphene/ethanol mixed solution
2.1, ultrasonically dissolving expanded graphite in ethanol by using an ultrasonic dissolving instrument for 2.8-4 hours to obtain a graphene/ethanol solution, wherein the mass ratio of the expanded graphite to the ethanol is 789: 1;
step 2.2, respectively adding cobalt nitrate and nickel nitrate into the graphene/ethanol solution, and stirring until the cobalt nitrate and the nickel nitrate are completely dissolved to obtain a primary nitrate graphene/ethanol mixed solution, wherein the ratio of the sum of the amounts of the cobalt nitrate and the nickel nitrate to the amount of ammonium fluoride in the ammonium fluoride solution is 1:2, the amounts of the cobalt nitrate and the nickel nitrate are both more than 0mol, and the cobalt nitrate is cobalt nitrate Co hexahydrate (NO)3)2·6H2O, nickel nitrate is nickel nitrate hexahydrate Ni (NO)3)2·6H2O；
And 2.3, adding oleic acid into the primary nitrate graphene mixed solution, stirring until the oleic acid and the primary nitrate graphene mixed solution are uniformly mixed to obtain a nitrate graphene/ethanol mixed solution, wherein the volume ratio of the oleic acid to the ethanol in the primary nitrate graphene mixed solution is 1: 3-1: 4.
Step 3, adding the ammonium fluoride solution into the nitrate graphene/ethanol mixed solution, and centrifuging and drying to obtain Ni0.5Co0.5F2Graphene composite material, namely lithium battery cathode material
Step 3.1, adding an ammonium fluoride solution into a nitrate graphene/ethanol mixed solution, and uniformly stirring to obtain a mixed solution A;
step 3.2, centrifuging the mixed solution A by using a centrifuge at the rotating speed of 5000-6000 r/min to obtain a precipitate A, and washing the precipitate A with deionized water for 3-5 times to obtain a sample A;
step 3.3, drying the sample A in a drying oven for 12-24 hours at the drying temperature of 78-85 ℃ to obtain a dried sample;
step 3.4, carrying out heat treatment on the sample B by using a tube furnace, and simultaneously introducing N into the tube furnace2As protective gas, the heating rate is 8 ℃/min-10 ℃/min, the heat treatment temperature is 400 ℃, and the heat preservation time is 2h, so as to obtain a sample C;
step 3.5, cooling the sample C to room temperature to obtain Ni0.5Co0.5F2The graphene composite material is a lithium battery positive electrode material.
Through the mode, the preparation method of the lithium battery cathode material is simple and efficient to operate, does not need high temperature and high pressure, and is low in raw material cost and small in pollution; ni produced by the invention0.5Co0.5F2The size of nickel-cobalt fluoride nanoparticles in the graphene composite material is smaller and can reach below 40 nm; meanwhile, the nickel-cobalt fluoride nanoparticles have good dispersibility on the surface of graphene and stable phase interface, can effectively improve the electron mobility of the nickel-cobalt fluoride, simultaneously ensure the contact between the nickel-cobalt fluoride and electrolyte, and promote the transmission and diffusion of lithium ions, thereby improving the electrochemical properties such as specific capacity, multiplying power and the like of the nickel-cobalt fluoride.
Example 1
The embodiment provides a preparation method of a lithium battery positive electrode material, which is implemented according to the following steps:
step 1, preparing ammonium fluoride solution
Step 1 specifically, 0.04mol of ammonium fluoride is added into 20ml of deionized water, and the mixture is stirred by a magnetic stirrer until the ammonium fluoride is completely dissolved, so that 2mol/L of ammonium fluoride solution is obtained.
Step 2, preparing nitrate graphene/ethanol mixed solution
2.1, ultrasonically dissolving 20mg of expanded graphite in 20ml of ethanol by using an ultrasonic dissolving instrument for 3 hours to obtain a graphene/ethanol solution, wherein the mass ratio of the expanded graphite to the ethanol is 789: 1;
step 2.2, respectively adding 0.01mol of cobalt nitrate hexahydrate and 0.01mol of nickel nitrate hexahydrate into the graphene/ethanol solution, and stirring by using a magnetic stirrer until the cobalt nitrate hexahydrate and the nickel nitrate hexahydrate are completely dissolved to obtain a primary nitrate graphene/ethanol mixed solution;
and 2.3, adding 5ml of oleic acid into the primary nitrate graphene mixed solution, and stirring until the mixture is uniformly mixed to obtain a nitrate graphene/ethanol mixed solution.
Step 3, adding the ammonium fluoride solution into the nitrate graphene/ethanol mixed solution, and centrifuging and drying to obtain Ni0.5Co0.5F2Graphene composite material, namely lithium battery cathode material
Step 3.1, adding an ammonium fluoride solution into a nitrate graphene/ethanol mixed solution, and uniformly stirring to obtain a mixed solution A;
step 3.2, centrifuging the mixed solution A by using a centrifuge at the rotating speed of 5000r/min to obtain a precipitate A, and washing the precipitate A with deionized water for 4 times to obtain a sample A;
step 3.3, drying the sample A in a drying oven for 12 hours at the drying temperature of 80 ℃ to obtain a sample B;
step 3.4, carrying out heat treatment on the sample B by using a tube furnace, and simultaneously introducing N into the tube furnace2As a shielding gas, the rate of temperature rise was 10The temperature of the heat treatment is 400 ℃ per minute, and the heat preservation time is 2 hours, so as to obtain a sample C;
step 3.5, cooling the sample C to room temperature to obtain Ni0.5Co0.5F2The graphene composite material is a lithium battery positive electrode material.
FIG. 1 shows Ni obtained in example 10.5Co0.5F2SEM pictures of the/graphene composite material show that the fluoride particles are relatively uniform in size distribution and are below 40nm in size. And the fluoride particles are stably combined with the graphene, and the dispersibility of the fluoride particles on the surface of the graphene is relatively uniform.
FIG. 2 shows Ni prepared in example 10.5Co0.5F2The XRD pattern of the/graphene composite material can find that the compound prepared by the method is Ni0.5Co0.5F2Diffraction peak following NiF2、CoF2Corresponding to PDF card, further explain Ni0.5Co0.5F2The/graphene composite material has no hetero-phase.
Electrical property tests were performed on the ni0.5co0.5f2/graphene composite material finally obtained in example 1: ni obtained in example 10.5Co0.5F2Mixing a graphene composite material, acetylene black and polyvinylidene fluoride (PVDF) according to a mass fraction ratio of 70:20:10 to obtain a mixed material, dissolving the mixed material in N-methylpyrrolidone (NMP), stirring for 3 hours by using a magnetic stirrer to obtain a battery positive electrode mixture, coating the pasty battery positive electrode mixture on an aluminum foil, drying for 12 hours in a vacuum drying box at 80 ℃ to obtain an electrode plate, assembling the electrode plate into a battery in a glove box, and performing electrochemical test on cycle performance and rate performance. The circulating test current density is 20mA/g, and the multiplying power test current densities are 20mA/g, 40mA/g, 80mA/g, 100mA/g and 20mA/g respectively.
Comparative example 1
This comparative example synthesized Ni by coprecipitation0.5Zn0.5F2And (3) nanoparticles.
Respectively adding 0.01mol of cobalt nitrate and 0.01mol of nickel nitrate into 20ml of ethanol solution, stirring for 1 hour by using a magnetic stirrer,completely dissolving the mixture, adding 5ml of oleic acid, and stirring for 1 hour to obtain a nitrate mixed solution; adding 20ml of deionized water into another beaker, adding 0.02mol of ammonium fluoride, and stirring for 1 hour by using a magnetic stirrer to completely dissolve the ammonium fluoride to obtain an ammonium fluoride solution; stirring the nitrate mixed solution, slowly pouring the ammonium fluoride solution into the nitrate mixed solution, and continuously stirring for 2 hours to obtain a mixed solution; centrifuging the mixed solution, extracting the precipitate, and washing the precipitate for 3 times by using deionized water to obtain a sample; drying the sample in a drying oven for 12 hours at the drying temperature of 80 ℃ to obtain a dried sample; carrying out heat treatment on the dried sample by using a tubular furnace, wherein the heating rate of the heat treatment is 10 ℃/min, the heat treatment temperature is 400 ℃, the heat preservation time is 2h, and N is introduced into the tubular furnace2(ii) a The dried sample is cooled to room temperature after heat treatment to obtain Ni0.5Co0.5F2A material.
Ni Final obtained for comparative example 10.5Co0.5F2And (3) carrying out an electrical property test on the material: ni obtained in comparative example 10.5Co0.5F2Mixing a material, acetylene black and polyvinylidene fluoride (PVDF) according to a mass fraction ratio of 70:20:10 to obtain a mixed material, dissolving the mixed material in N-methylpyrrolidone (NMP), stirring for 3 hours by using a magnetic stirrer to obtain a battery positive electrode mixture, coating the pasty battery positive electrode mixture on an aluminum foil, drying for 12 hours in a vacuum drying box at 80 ℃ to obtain an electrode plate, assembling the electrode plate into a battery in a glove box, and performing electrochemical test on the cycle performance and the rate performance. The circulating test current density is 20mA/g, and the multiplying power test current densities are 20mA/g, 40mA/g, 80mA/g, 100mA/g and 20mA/g respectively.
FIG. 3 shows Ni prepared in example 10.5Co0.5F2Graphene and Ni prepared in comparative example 10.5Co0.5F2The cycle performance curve of the material shows that Ni is formed by the test results0.5Co0.5F2The cycling performance and specific capacity of graphene are obviously superior to those of Ni0.5Co0.5F2Wherein the graphene effectively improves the metal fluoride Ni0.5Co0.5F2The cycle performance and specific capacity of (c).
FIG. 4 shows Ni prepared in example 10.5Co0.5F2Graphene and Ni prepared in comparative example 10.5Co0.5F2The multiplying power curves of the material are respectively 20mA/g, 40mA/g, 80mA/g, 100mA/g and 20 mA/g. Observing the curve, Ni0.5Co0.5F2The rate capability of graphene under the test of current density is better, and the graphene is proved to effectively improve the metal fluoride Ni0.5Co0.5F2The rate capability of (2).

Claims (7)

1. The preparation method of the lithium battery positive electrode material is characterized by comprising the following steps:
step 1, preparing an ammonium fluoride solution;
step 1 specifically comprises adding ammonium fluoride into deionized water, and stirring until the ammonium fluoride is completely dissolved to obtain 2mol/L ammonium fluoride solution;
step 2, preparing a nitrate graphene/ethanol mixed solution;
the step 2 is specifically implemented according to the following steps:
2.1, ultrasonically dissolving expanded graphite in ethanol by using an ultrasonic dissolver to obtain a graphene/ethanol solution, wherein the mass ratio of the expanded graphite to the ethanol is 789: 1;
step 2.2, respectively adding cobalt nitrate and nickel nitrate into the graphene/ethanol solution, and stirring until the cobalt nitrate and the nickel nitrate are completely dissolved to obtain a primary nitrate graphene/ethanol mixed solution;
step 2.3, adding oleic acid into the primary nitrate graphene mixed solution, and stirring until the oleic acid and the primary nitrate graphene mixed solution are uniformly mixed to obtain a nitrate graphene/ethanol mixed solution;
step 3, adding the ammonium fluoride solution into a nitrate graphene/ethanol mixed solution, and centrifuging and drying to obtain Ni0.5Co0.5F2Graphene composite materials, namely lithium battery positive electrode materials;
the step 3 is specifically implemented according to the following steps:
step 3.1, adding the ammonium fluoride solution into the nitrate graphene/ethanol mixed solution, and uniformly stirring to obtain a mixed solution A;
step 3.2, centrifuging the mixed solution A by using a centrifuge to obtain a precipitate A, and washing the precipitate A by using deionized water for 3-5 times to obtain a sample A;
step 3.3, drying the sample A in a drying oven for 12-24 hours at the drying temperature of 78-85 ℃ to obtain a sample B;
step 3.4, carrying out heat treatment on the sample B by using a tube furnace, and simultaneously introducing N into the tube furnace2As protective gas, the heat treatment temperature is 400 ℃, and the heat preservation time is 2 hours, so as to obtain a sample C;
step 3.5, cooling the sample C to room temperature to obtain Ni0.5Co0.5F2Graphene composite materials, namely lithium battery positive electrode materials;
Ni0.5Co0.5F2the size of the nickel-cobalt fluoride nano particles in the/graphene composite material is less than 40 nm.
2. The method of claim 1, wherein the ratio of the sum of the amounts of the cobalt nitrate and nickel nitrate to the amount of the ammonium fluoride in the ammonium fluoride solution is 1:2, and the amounts of the cobalt nitrate and nickel nitrate are both greater than 0 mol.
3. The method of claim 1, wherein the cobalt nitrate is cobalt nitrate hexahydrate of Co (NO)3)2·6H2O, the nickel nitrate is nickel nitrate hexahydrate Ni (NO)3)2·6H2O。
4. The method for preparing the lithium battery positive electrode material as claimed in claim 1, wherein the volume ratio of the oleic acid to the ethanol in the primary nitrate graphene mixed solution is 1: 3-1: 4.
5. The method for preparing the positive electrode material of the lithium battery as claimed in claim 1, wherein the ultrasonic dissolution time is 2.8 h-4 h.
6. The method for preparing the positive electrode material of the lithium battery as claimed in claim 1, wherein the rotation speed of the centrifuge is 5000r/min to 6000 r/min.
7. The method for preparing a positive electrode material for a lithium battery as claimed in claim 1, wherein the temperature rise rate of the heat treatment is 8 ℃/min to 10 ℃/min.
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