CN112421006A - Preparation method of lithium ion battery anode material - Google Patents

Preparation method of lithium ion battery anode material Download PDF

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Publication number
CN112421006A
CN112421006A CN202011301901.6A CN202011301901A CN112421006A CN 112421006 A CN112421006 A CN 112421006A CN 202011301901 A CN202011301901 A CN 202011301901A CN 112421006 A CN112421006 A CN 112421006A
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lithium ion
ion battery
hydrothermal reaction
anode material
preparation
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宋昌才
许家欣
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Jiangus University Jingjiang College
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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
    • 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
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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 relates to a preparation method of a lithium ion battery anode material, belonging to the technical field of lithium ion battery electrode materials. The method comprises the steps of adding 50-200 mg of ferric chloride hexahydrate, 5-40 mg of nickel chloride hexahydrate and 3-20 mg of carbon nano tubes into a mixed solvent consisting of water and DMF, adding 1-5ml of 0.1M sodium sulfide solution into the mixed solution, heating and refluxing, transferring into a hydrothermal kettle for hydrothermal reaction to obtain a hydrothermal reaction product, and carrying out microwave plasma treatment to obtain the product. FeNiS prepared by the invention2The CNTs material has good chemical properties and larger graphitization defectsMore active sites are exposed, and the preparation method is environment-friendly, simple and convenient for large-scale production.

Description

Preparation method of lithium ion battery anode material
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a transition metal sulfide loaded carbon nanotube material serving as a lithium ion battery anode material.
Background
In recent years, lithium ion battery cathode materials have made a great breakthrough, the specific capacity of novel silicon-based and tin-based materials is obviously improved compared with that of graphite carbon, and the development of cathode materials is relatively slow. Due to the limitation of the theoretical specific capacity of the traditional cathode material, the cathode material with higher specific capacity needs to be searched urgently. The sulfur has abundant reserves on the earth and wide sources, and can be used as the anode material of the lithium ion battery. The lithium-sulfur secondary battery is a secondary battery taking metal lithium as a negative electrode and elemental sulfur or a sulfur-based composite material as a positive electrode, the theoretical energy density of the secondary battery is 2600Wh/kg, the actual energy density can reach 300Wh/kg at present, and the theoretical energy density is probably increased to about 600Wh/kg in the coming years, so that the lithium-sulfur secondary battery is considered to be one of the secondary battery systems which are most attractive to research at present.
Compared with metal oxides, the sulfur-based composite material has the advantages of rich sulfur resources, low price, environmental friendliness, easiness in large-scale application and the like, and is rapidly the most potential anode material of a novel energy storage system. Wherein the lithium-based anode is electrochemically paired with a lithium anode based on 16Li + S8＝8Li2The lithium-sulfur battery with the electrochemical reaction has ultrahigh theoretical energy density (2600 Wh.kg < -1 >), which is about 10 times of the energy density actually achieved by the current commercial lithium-ion battery, and the successful application of the lithium-sulfur battery is predicted to show great value in the fields of electric automobile power batteries, smart grids, clean energy large-scale energy storage batteries and the like, so that the lithium-sulfur battery with the electrochemical reaction attracts people' S extensive attention and becomes the research focus of a new generation of high-energy density battery in recent years.
Elemental sulfur is an electronic insulator at room temperature, and modification of the sulfur positive electrode material generally involves the mixing of sulfur with conductive additives. The carbon material loaded transition metal compound is widely applied to the anode material of the lithium ion battery, because the carbon material is easily obtained in nature, has large surface area, porosity and low resistivity, and has excellent surface chemical environment and physical and chemical properties, low cost and the like. And the high conductivity and strong adsorption capacity are often used as additives of the sulfur-containing composite material. The storage of energy in lithium ion batteries is primarily a charge at the electrode and electrolyte surfaces. Due to the unique properties of the porous carbon material, the synthetic raw materials are rich and easy to obtain, so that the porous carbon material has common application in modern science. In addition, the porous carbon material has a series of characteristics of high chemical stability, acid and alkali resistance, high temperature resistance, good electrical conductivity, excellent thermal conductivity and the like, and the material generally has developed pores, high specific surface area, high chemical stability, excellent heat resistance, acid and alkali resistance and unique electronic conduction property, and is one of essential important materials in modern industry.
Transition gold sulfide can be used as a positive electrode material of a lithium ion battery, but has certain defects, such as certain expansion in the charging and discharging process and poor cycle stability. The material has poor inverse kinetics and tighter charge-discharge electric hysteresis. The poor cycling stability of transition metal sulfides is mainly three points: the first is that the conductivity is poor, the diffusion coefficient of ions or electrons is not large, the reversibility of electrode reaction is reduced, and the capacity attenuation is fast during circulation; secondly, the transition metal sulfide material repeatedly reacts with Li to generate pulverization, electric contact among active particles, collective flow and the active particles is lost, the particles losing contacts do not participate in electrode reaction any more, and further capacity is attenuated; thirdly, the transition metal sulfide material reacts with Li to generate metal nano-particles, and the particles are agglomerated after multiple cycles, so that the active substances are reduced and the capacity is reduced.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a preparation method of a lithium ion battery anode material2The material increases the conductivity of the material by compounding with a carbon material and processing the surface of the material by a plasma device, and Fe and Ni outer layers have similar electronic structures to form a synergistic effect, so that the electrochemical activity of the material is increased. The preparation method is simple to operate, environment-friendly and convenient for large-scale production of the lithium ion battery anode material, and the prepared lithium ion battery anode material has high specific surface area, more active sites and good electrochemical performance.
Technical scheme
A preparation method of a lithium ion battery anode material comprises the following steps:
(1) adding 50-200 mg of ferric chloride hexahydrate, 5-40 mg of nickel chloride hexahydrate and 3-20 mg of carbon nano tube into a mixed solvent consisting of water and DMF (N, N-dimethylformamide) to obtain a mixed solution; adding 1-5ml of 0.1M sodium sulfide solution into the mixed solution, heating and refluxing, transferring the obtained mixture into a hydrothermal kettle for hydrothermal reaction to obtain a hydrothermal reaction product;
(2) and (3) performing microwave plasma treatment on the hydrothermal reaction product to obtain the catalyst.
Further, in the step (1), the volume ratio of water to DMF in the mixed solvent is 1: 4.
Further, in the step (1), the temperature of heating reflux is 100-120 ℃, and the time is 8-24 h.
Further, in the step (1), the temperature of the hydrothermal reaction is 180-220 ℃, and the time is 8-12 h.
Further, in the step (2), the microwave frequency of the microwave plasma treatment is 2.45GHz, the power is 150w, the vacuum degree is 5Pa, and the microwave plasma treatment time is 3-45 min.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the eighth group element iron and nickel are selected as the anode materials of the ion battery, and as the electronic structures of the same group elements are similar, the electronic layer structures are similar, and peripheral electrons can adjust the electronic structures of the metal elements through charge transfer, so that the electrochemical performance of the parent metal center is improved.
2. The porous carbon material is prepared by taking the carbon nano tube as the carbon source, and the carbon nano tube has an excellent structure, has higher content of the loaded transition metal sulfide and is easy to expose more active sites, so that the electrochemical performance of the material is enhanced.
3. The degree of graphitization defect of the lithium ion battery anode material prepared by the invention, namely the D band peak value of Raman spectrum: the ratio of the G band peak value is 1.2-1.8 (graphene oxide I)D：IG1:1), which shows that the material prepared by the invention has more active sites exposed on the periphery and has good electrochemical performance.
4. The method adopts a plasma microwave heating method to treat the nano material, so that the nano material is uniformly distributed on the carbon material, and the composite material prepared by the method has high specific surface area and more active sites, and has wide application prospect in lithium ion batteries, supercapacitors and even electrocatalysis.
Drawings
FIG. 1 is a Raman shift spectrum of the lithium ion battery positive electrode material prepared in example 2;
fig. 2 is a graph showing the charge-discharge specific capacity and the charge-discharge efficiency of the positive electrode material for a lithium ion battery obtained in example 2.
Detailed Description
The invention is further described with reference to the following figures and specific examples. In the following examples, the microwave plasma treatment was performed using a pitot XTY5115219 quartz tube type microwave plasma generator, but is not limited thereto.
Example 1
A preparation method of a lithium ion battery anode material comprises the following steps:
(1) adding 70mg of ferric chloride hexahydrate, 5mg of nickel chloride hexahydrate and 5mg of carbon nano tubes into a mixed solvent consisting of 10ml of water and DMF (N, N-dimethylformamide) in a volume ratio of 1:4, then adding 1.5ml of 0.1M sodium sulfide aqueous solution, heating and refluxing at 100 ℃ for 20h, transferring the obtained mixture into a hydrothermal kettle, and carrying out hydrothermal reaction at 200 ℃ for 8h to obtain a hydrothermal reaction product;
(2) and (3) carrying out microwave plasma treatment on the hydrothermal reaction product for 10min (the microwave frequency is 2.45GHz, the power is 150w, and the vacuum degree is 5Pa) to obtain the catalyst.
The BET test gave a material with a specific surface area of 72.5m2/g。
Example 2
A preparation method of a lithium ion battery anode material comprises the following steps:
(1) adding 70mg of ferric chloride hexahydrate, 10mg of nickel chloride hexahydrate and 7mg of carbon nano tubes into 12.5ml of mixed solvent consisting of water and DMF (N, N-dimethylformamide) in a volume ratio of 1:4, then adding 2ml of 0.1M sodium sulfide aqueous solution, heating and refluxing for 16h at 100 ℃, transferring the obtained mixture into a hydrothermal kettle, and carrying out hydrothermal reaction for 10h at 200 ℃ to obtain a hydrothermal reaction product;
(2) and (3) performing microwave plasma treatment on the hydrothermal reaction product for 20min (the microwave frequency is 2.45GHz, the power is 150w, and the vacuum degree is 5Pa) to obtain the catalyst.
The BET test gave a specific surface area of 211.3m2/g。
The raman shift spectrogram of the lithium ion battery anode material prepared in the embodiment is shown in fig. 1, and it can be seen that ID：IG1.45 ratio of graphene oxide ID：IGWhen the ratio is 1:1, the degree of graphitization defects is increased, the number of active sites is increased, and the electrochemical performance is improved.
Example 3
A preparation method of a lithium ion battery anode material comprises the following steps:
(1) adding 73mg of ferric chloride hexahydrate, 14mg of nickel chloride hexahydrate and 8mg of carbon nano tubes into 12.5ml of mixed solvent consisting of water and DMF (N, N-dimethylformamide) in a volume ratio of 1:4, then adding 2ml of 0.1M sodium sulfide aqueous solution, heating and refluxing at 100 ℃ for 12h, transferring the obtained mixture into a hydrothermal kettle, and carrying out hydrothermal reaction at 220 ℃ for 12h to obtain a hydrothermal reaction product;
(2) and (3) performing microwave plasma treatment on the hydrothermal reaction product for 20min (the microwave frequency is 2.45GHz, the power is 150w, and the vacuum degree is 5Pa) to obtain the catalyst.
The BET test gave a material with a specific surface area of 132.6m2/g。
Application test:
respectively grinding the lithium ion battery positive electrode materials prepared in the embodiments 1-3, then respectively weighing 20mg, then weighing 2.5mg of carbon black and 0.25ml of 10mg/ml polytetrafluoroethylene, then adding a little N-methyl pyrrolidone, stirring into uniform slurry on a magnetic stirrer, coating the uniform slurry on an aluminum foil with the thickness of 1mm, and then drying; pressing the aluminum foil into small wafers, assembling the pressed wafers into button cells, testing the specific discharge capacity and the charge-discharge efficiency of the cells, and completing the test on an LANA cell test system (Wuhan blue electronic Co., Ltd.) and an electrochemical workstation CHI760E (Shanghai Chenghua).
The specific charge-discharge capacity and charge-discharge efficiency of the lithium ion battery cathode material prepared in example 2 are shown in fig. 2, and the test results of the lithium ion battery cathode materials prepared in examples 1 to 3 are shown in table 1:
TABLE 1
Figure BDA0002787163110000051
As can be seen from fig. 2 and the test results in table 1, the lithium ion battery positive electrode material prepared in the embodiment of the present invention has high specific discharge capacity and high charge-discharge efficiency, wherein the lithium ion battery positive electrode material prepared in the embodiment 2 has the best specific discharge capacity and charge-discharge efficiency.

Claims (5)

1. A preparation method of a lithium ion battery anode material is characterized by comprising the following steps:
(1) adding 50-200 mg of ferric chloride hexahydrate, 5-40 mg of nickel chloride hexahydrate and 3-20 mg of carbon nano tube into a mixed solvent consisting of water and DMF to obtain a mixed solution; adding 1-5ml of 0.1M sodium sulfide solution into the mixed solution, heating and refluxing, transferring the obtained mixture into a hydrothermal kettle for hydrothermal reaction to obtain a hydrothermal reaction product;
(2) and (3) performing microwave plasma treatment on the hydrothermal reaction product to obtain the catalyst.
2. The method for preparing the positive electrode material of the lithium ion battery according to claim 1, wherein in the step (1), the volume ratio of water to DMF in the mixed solvent is 1: 4.
3. The method for preparing the anode material of the lithium ion battery as claimed in claim 1, wherein the temperature of the heating reflux in the step (1) is 100-120 ℃, and the time is 8-24 h.
4. The method for preparing the anode material of the lithium ion battery as claimed in claim 1, wherein in the step (1), the temperature of the hydrothermal reaction is 180-220 ℃ and the time is 8-12 h.
5. The method for preparing the lithium ion battery cathode material according to any one of claims 1 to 4, wherein in the step (2), the microwave plasma treatment has a microwave frequency of 2.45GHz, a power of 150w, a vacuum degree of 5Pa and a microwave plasma treatment time of 3-45 min.
CN202011301901.6A 2020-11-19 2020-11-19 Preparation method of lithium ion battery anode material Pending CN112421006A (en)

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Cited By (7)

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US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US11633785B2 (en) 2019-04-30 2023-04-25 6K Inc. Mechanically alloyed powder feedstock
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
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US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
US11963287B2 (en) 2021-09-20 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11839919B2 (en) 2015-12-16 2023-12-12 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
US11633785B2 (en) 2019-04-30 2023-04-25 6K Inc. Mechanically alloyed powder feedstock
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US11855278B2 (en) 2020-06-25 2023-12-26 6K, Inc. Microcomposite alloy structure
US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
US11963287B2 (en) 2021-09-20 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma

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Application publication date: 20210226