CN110010870A - A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material - Google Patents

A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material Download PDF

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Publication number
CN110010870A
CN110010870A CN201910268297.2A CN201910268297A CN110010870A CN 110010870 A CN110010870 A CN 110010870A CN 201910268297 A CN201910268297 A CN 201910268297A CN 110010870 A CN110010870 A CN 110010870A
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deionized water
graphene oxide
preparation
lithium ion
ion battery
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车春玲
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Shandong Xinghuo Science Technology Institute
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Shandong Xinghuo Science Technology Institute
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • 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
    • H01M4/362—Composites
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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 present invention provides a kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material, includes the following steps: the preparation of (1) graphene oxide；(2) preparation of graphene oxide suspension；(3) preparation of mixed solution；(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, deionized water is added, after covering tightly, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 12-18h, it then takes out to its cooled to room temperature, obtained hydrothermal product is washed 3 times, and the dry 12-18h in 80 DEG C of vacuum ovens respectively through deionized water and dehydrated alcohol, obtains novel graphene/SnS2 composite material lithium ion battery negative material.The present invention effectively improves the stability and electric conductivity of material, improves battery performance, has biggish specific capacity and preferable cycle performance.

Description

A kind of system of the lithium ion battery negative material of novel graphene/SnS2 composite material Preparation Method
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of lithium of novel graphene/SnS2 composite material The preparation method of ion battery cathode material.
Background technique
Lithium ion battery have operating voltage is high, energy density is big, self discharge is small, have extended cycle life with it is environmental-friendly etc. excellent Point, the power supply as portable electronic device are widely used, but its performance needs to be further increased, to meet new The application in the fields such as energy electric vehicle.Electrode material, especially negative electrode material are a weights for influencing performance of lithium ion battery Want factor.Current commercial Li-ion battery mainly using graphite as negative electrode material, but the lower theoretical capacity of graphite and Poor high rate performance makes it be difficult to meet lithium ion battery to want in the application in some higher energy density and power density field It asks.
Summary of the invention
The purpose of the present invention is to provide a kind of novel graphene/SnS2 composite material lithium ion battery negative materials Preparation method effectively improves the stability and electric conductivity of material, improves battery performance, with biggish specific capacity and preferably Cycle performance.
To achieve the goals above, the invention adopts the following technical scheme: a kind of novel graphene/SnS2 composite material The preparation method of lithium ion battery negative material, includes the following steps:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, Oxidant, and temperature reaction is added, then uses hydrogen peroxide, dilute hydrochloric acid and deionized water respectively, washs repeatedly, 40 DEG C of dryings obtain Graphene oxide solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；
(2) graphene oxide for obtaining step 1 is added in deionized water, and ultrasonic disperse 1-3h obtains graphene oxide Suspension；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, so The graphene oxide suspension that step 2 obtains is added afterwards, ultrasonic 30-60min obtains mixed solution；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water, lid is added It is next, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 12-18h, then takes out to its cooled to room temperature, will obtain Hydrothermal product washed respectively 3 times through deionized water and dehydrated alcohol, and the dry 12-18h in 80 DEG C of vacuum ovens is obtained Novel graphene/SnS2 composite material lithium ion battery negative material.
Preferably, step 1, natural graphite, the concentrated sulfuric acid, oxidant mass ratio be 2-6:40-80:1-3.
Preferably, step 2, graphene oxide, deionized water mass ratio be 2-6:50-120.
Preferably, step 3, stannic chloride pentahydrate, deionized water, L-cysteine, the quality of graphene oxide suspension Than for 1-4:50-180:1-5:2-6.
Preferably, step 4, mixed solution, deionized water mass ratio be 10-30:50-180.
The invention has the following advantages: a kind of novel graphene/SnS2 composite material lithium-ion electric of the invention The preparation method of pond negative electrode material effectively improves the stability and electric conductivity of material, improves battery performance, has biggish Specific capacity and preferable cycle performance；Hydrothermal technique is assisted to synthesize novel graphene/SnS2 composite wood by L-cysteine The lithium ion battery negative material of material, and the amount by changing L-cysteine controls the content of SnS2 in composite material； Effectively act synergistically between SnS2 and graphene, in ceaselessly charge and discharge process, graphene can both prevent well by Falling off for bring electrode material is collapsed and ruptured in the overlapping of SnS2, improves the cycle performance of SnS2；It simultaneously can also be effectively It solves the problems, such as SnS2 poorly conductive, is showed so as to improve the high rate performance of SnS2.
Specific embodiment
Embodiment 1
A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material, including walk as follows It is rapid:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, Oxidant, and temperature reaction is added, then uses hydrogen peroxide, dilute hydrochloric acid and deionized water respectively, washs repeatedly, 40 DEG C of dryings obtain Graphene oxide solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；Natural graphite, The concentrated sulfuric acid, oxidant mass ratio be 2:40:1；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 1h, and it is outstanding to obtain graphene oxide Supernatant liquid；Graphene oxide, deionized water mass ratio be 2:50；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, so The graphene oxide suspension that step 2 obtains is added afterwards, ultrasonic 30min obtains mixed solution；Stannic chloride pentahydrate, deionization Water, L-cysteine, graphene oxide suspension mass ratio be 1:50:1:2；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water, lid is added It is next, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 12h, then takes out the water that its cooled to room temperature, will be obtained Hot is washed 3 times respectively through deionized water and dehydrated alcohol, and the dry 12h in 80 DEG C of vacuum ovens, obtains novel stone Black alkene/SnS2 composite material lithium ion battery negative material；Mixed solution, deionized water mass ratio be 10:50.
Embodiment 2
A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material, including walk as follows It is rapid:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, Oxidant, and temperature reaction is added, then uses hydrogen peroxide, dilute hydrochloric acid and deionized water respectively, washs repeatedly, 40 DEG C of dryings obtain Graphene oxide solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；Natural graphite, The concentrated sulfuric acid, oxidant mass ratio be 6:80:3；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 3h, and it is outstanding to obtain graphene oxide Supernatant liquid；Graphene oxide, deionized water mass ratio be 6:120；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, so The graphene oxide suspension that step 2 obtains is added afterwards, ultrasonic 60min obtains mixed solution；Stannic chloride pentahydrate, deionization Water, L-cysteine, graphene oxide suspension mass ratio be 4:180:5:6；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water, lid is added It is next, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 18h, then takes out the water that its cooled to room temperature, will be obtained Hot is washed 3 times respectively through deionized water and dehydrated alcohol, and the dry 18h in 80 DEG C of vacuum ovens, obtains novel stone Black alkene/SnS2 composite material lithium ion battery negative material；Mixed solution, deionized water mass ratio be 30:180.
Embodiment 3
A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material, including walk as follows It is rapid:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, Oxidant, and temperature reaction is added, then uses hydrogen peroxide, dilute hydrochloric acid and deionized water respectively, washs repeatedly, 40 DEG C of dryings obtain Graphene oxide solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；Natural graphite, The concentrated sulfuric acid, oxidant mass ratio be 3:55:1；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 2h, and it is outstanding to obtain graphene oxide Supernatant liquid；Graphene oxide, deionized water mass ratio be 3:80；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, so The graphene oxide suspension that step 2 obtains is added afterwards, ultrasonic 34min obtains mixed solution；Stannic chloride pentahydrate, deionization Water, L-cysteine, graphene oxide suspension mass ratio be 2:80:2:3；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water, lid is added It is next, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 14h, then takes out the water that its cooled to room temperature, will be obtained Hot is washed 3 times respectively through deionized water and dehydrated alcohol, and the dry 14h in 80 DEG C of vacuum ovens, obtains novel stone Black alkene/SnS2 composite material lithium ion battery negative material；Mixed solution, deionized water mass ratio be 26:90.
Embodiment 4
A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material, including walk as follows It is rapid:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, Oxidant, and temperature reaction is added, then uses hydrogen peroxide, dilute hydrochloric acid and deionized water respectively, washs repeatedly, 40 DEG C of dryings obtain Graphene oxide solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；Natural graphite, The concentrated sulfuric acid, oxidant mass ratio be 5:70:2；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 2h, and it is outstanding to obtain graphene oxide Supernatant liquid；Graphene oxide, deionized water mass ratio be 5:100；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, so The graphene oxide suspension that step 2 obtains is added afterwards, ultrasonic 50min obtains mixed solution；Stannic chloride pentahydrate, deionization Water, L-cysteine, graphene oxide suspension mass ratio be 3:160:4:5；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water, lid is added It is next, hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 16h, then takes out the water that its cooled to room temperature, will be obtained Hot is washed 3 times respectively through deionized water and dehydrated alcohol, and the dry 16h in 80 DEG C of vacuum ovens, obtains novel stone Black alkene/SnS2 composite material lithium ion battery negative material；Mixed solution, deionized water mass ratio be 25:150.

Claims (5)

1. a kind of preparation method of novel graphene/SnS2 composite material lithium ion battery negative material, which is characterized in that packet Include following steps:
(1) preparation of graphene oxide: under condition of ice bath, natural graphite being added in the concentrated sulfuric acid, and is stirred continuously, and is added Oxidant, and temperature reaction, then hydrogen peroxide, dilute hydrochloric acid and deionized water are used respectively, it washs repeatedly, 40 DEG C of dryings are aoxidized Graphene solid, then by the fine grinding of graphene oxide solid, simultaneously microwave treatment obtains the graphene oxide；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 1-3h, obtains graphene oxide suspension Liquid；
(3) stannic chloride pentahydrate is dissolved in deionized water, adds L-cysteine, stirred until being completely dissolved, then plus Enter the graphene oxide suspension that step 2 obtains, ultrasonic 30-60min obtains mixed solution；
(4) mixed solution for obtaining step 3 is transferred in the hydrothermal reaction kettle of tetrafluoroethene, and deionized water is added, after covering tightly, Hydrothermal reaction kettle is moved in 180 DEG C of baking ovens and keeps 12-18h, then takes out the hydro-thermal that its cooled to room temperature, will be obtained Product washs 3 times respectively through deionized water and dehydrated alcohol, and the dry 12-18h in 80 DEG C of vacuum ovens, obtains novel stone Black alkene/SnS2 composite material lithium ion battery negative material.
2. a kind of system of the lithium ion battery negative material of novel graphene/SnS2 composite material according to claim 1 Preparation Method, which is characterized in that step 1, natural graphite, the concentrated sulfuric acid, oxidant mass ratio be 2-6:40-80:1-3.
3. a kind of system of the lithium ion battery negative material of novel graphene/SnS2 composite material according to claim 1 Preparation Method, which is characterized in that step 2, graphene oxide, deionized water mass ratio be 2-6:50-120.
4. a kind of system of the lithium ion battery negative material of novel graphene/SnS2 composite material according to claim 1 Preparation Method, which is characterized in that step 3, stannic chloride pentahydrate, deionized water, L-cysteine, the matter of graphene oxide suspension Amount is than being 1-4:50-180:1-5:2-6.
5. a kind of system of the lithium ion battery negative material of novel graphene/SnS2 composite material according to claim 1 Preparation Method, which is characterized in that step 4, mixed solution, deionized water mass ratio be 10-30:50-180.
CN201910268297.2A 2019-04-03 2019-04-03 A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material Withdrawn CN110010870A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102142549A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene nano sheet and SnS2 composite nano material and synthesis method thereof
CN102142540A (en) * 2011-02-25 2011-08-03 浙江大学 Lithium ion battery electrode made of graphene/SnS2 composite nanometer material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102142549A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene nano sheet and SnS2 composite nano material and synthesis method thereof
CN102142540A (en) * 2011-02-25 2011-08-03 浙江大学 Lithium ion battery electrode made of graphene/SnS2 composite nanometer material and preparation method thereof

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Application publication date: 20190712