CN113582220A - TiO 22Preparation method of/carbon composite interlayer - Google Patents

TiO 22Preparation method of/carbon composite interlayer Download PDF

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Publication number
CN113582220A
CN113582220A CN202110634478.XA CN202110634478A CN113582220A CN 113582220 A CN113582220 A CN 113582220A CN 202110634478 A CN202110634478 A CN 202110634478A CN 113582220 A CN113582220 A CN 113582220A
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solution
carbon composite
composite interlayer
preparation
steps
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CN202110634478.XA
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曲婕
丁明珍
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Hunan Normal University
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Hunan Normal University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • 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
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • 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
    • 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
    • C01B32/20—Graphite
    • C01B32/21—After-treatment
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon
    • 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 provides a TiO2The preparation method of the/carbon composite interlayer comprises the steps of preparing a water/ethanol solution (solution 1) of oxalic acid and sodium dodecyl benzene sulfonate, and soaking a carbon material into the solution; dissolving a titanium source and an appropriate amount of acid in an ethanol solution (solution 2), then dropwise adding the solution 2 to the solution 1 containing the carbon material, and heating and stirring until the precipitation is completed(ii) a Drying, calcining in tubular furnace to obtain TiO2A/carbon composite interlayer.

Description

TiO 22Preparation method of/carbon composite interlayer
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a preparation method of an interlayer for a lithium ion battery.
Background
With the development of science and technology, lithium ion batteries are widely applied to various portable electronic devices, and the fields of electric vehicles, smart power grids and the like. The rechargeable lithium iodine battery has the advantages of low cost, good rate performance, high specific capacity up to 211 mAh/g, rich iodine element content and the like, so that the rechargeable lithium iodine battery has commercial application prospects in the aspect of energy storage such as electric vehicles and large-scale power grid storage. Despite the above advantages, practical application of rechargeable lithium iodine batteries still has some problems. Iodine and iodide are easily dissolved in an organic electrolyte solution and shuttle to a negative electrode to react with metallic lithium, so that a self-discharge phenomenon is caused, the coulomb efficiency of the battery is reduced, and simultaneously lithium dendrites are generated to pierce a diaphragm, so that the battery is short-circuited, and even explosion is caused. How to effectively inhibit the shuttle effect of iodine has important significance for the practical application of the lithium iodine electrode.
The problem of iodide dissolution can be effectively solved by limiting iodine to the positive electrode by utilizing carbon base, but the adsorption capacity of the carbon base material to iodine is limited. And the physical adsorption capacity of the carbon-based material is not sufficient to limit the shuttling effect of iodine in the cycle for a long period of time. The chemical adsorption mainly utilizes the weak bond effect of surface polar atoms of the material and iodine and iodide ions, and has strong adsorption capacity. The interlayer with strong chemical action can effectively solve the shuttle effect of the lithium iodine battery, lock the polyiodide at the anode and inhibit the lithium iodide from corroding the metallic lithium cathode.
Disclosure of Invention
The invention aims to: provides a TiO compound2A preparation process of the/carbon composite interlayer.
Another object of the present invention is to: providing TiO2Use of a/carbon composite interlayer.
In order to achieve the purpose, the technical scheme of the invention is realized in such a way.
TiO 22The preparation method of the/carbon composite interlayer comprises the steps of preparing a water/ethanol solution (solution 1) of oxalic acid and sodium dodecyl benzene sulfonate, and soaking a carbon material into the solution; dissolving a titanium source and a proper amount of acid in an ethanol solution (solution 2), then dropwise adding the solution 2 into the solution 1 containing the carbon material, and heating and stirring until the precipitation is complete; drying, calcining in tubular furnace to obtain TiO2A/carbon composite interlayer.
Further, the titanium source includes, but is not limited to, tetrabutyl titanate, titanium tetrachloride, titanium isopropoxide, titanium sulfate, titanyl difluoride, and the like; acids include, but are not limited to, acetic acid, citric acid, nitric acid, and the like; carbon materials include, but are not limited to, carbon fibers, graphite felt, graphene oxide, carbon nanotubes, and the like.
Further, the concentration of the oxalic acid is 0.05-5 mol/L; the concentration of the sodium dodecyl benzene sulfonate is 0.001-0.1 mol/L.
Further, the volume ratio of the ethanol to the water is 10: 1-1: 10.
further, the concentration of the titanium source is 0.05-3 mol/L; the concentration of the acid is 0.01-1 mol/L.
Further, the mass ratio of the titanium source to the carbon material is 20: 1-1: 1.
further, the volume ratio of the solution 1 to the solution 2 is 5: 1-1: 5.
further, the heating and stirring time is 0.5-10 hours; the heating temperature is 30-90 ℃.
Further, the sintering temperature is 300-800 ℃; the sintering time is 0.5-5 hours; atmospheres include, but are not limited to, nitrogen, argon, and the like.
Drawings
FIG. 1 shows TiO 2 based on example 12Scanning electron microscope pictures of the/carbon composite interlayer.
FIG. 2 shows TiO 2 based on example 12Ultraviolet absorption spectrum of the/carbon composite interlayer to iodide.

Claims (9)

1. TiO 22The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: preparing a water/ethanol solution (solution 1) of oxalic acid and sodium dodecyl benzene sulfonate, and soaking a carbon material into the solution; dissolving a titanium source and a proper amount of acid in an ethanol solution (solution 2), then dropwise adding the solution 2 into the solution 1 containing the carbon material, and heating and stirring until the precipitation is complete; drying, calcining in tubular furnace to obtain TiO2A/carbon composite interlayer.
2. A TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: sources of titanium include, but are not limited to, tetrabutyl titanate, titanium tetrachloride, titanium isopropoxide, titanium sulfate, titanyl difluoride, and the like; acids include, but are not limited to, acetic acid, citric acid, nitric acid, and the like; carbon materials include, but are not limited to, carbonFibers, graphite felt, graphene oxide, carbon nanotubes, and the like.
3. A TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the concentration of the oxalic acid is 0.05-5 mol/L; the concentration of the sodium dodecyl benzene sulfonate is 0.001-0.1 mol/L.
4. A TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the volume ratio of the ethanol to the water is 10: 1-1: 10.
5. a TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the concentration of the titanium source is 0.05-3 mol/L; the concentration of the acid is 0.01-1 mol/L.
6. A TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the mass ratio of the titanium source to the carbon material is 20: 1-1: 1.
7. a TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the volume ratio of the solution 1 to the solution 2 is 5: 1-1: 5.
8. a TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: heating and stirring for 0.5-10 hours; the heating temperature is 30-90 ℃.
9. A TiO according to claim 12The preparation method of the/carbon composite interlayer is characterized by comprising the following steps: the sintering temperature is 300-800 ℃; the sintering time is 0.5-5 hours; atmospheres include, but are not limited to, nitrogen, argon, and the like.
CN202110634478.XA 2021-06-08 2021-06-08 TiO 22Preparation method of/carbon composite interlayer Pending CN113582220A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110059315A1 (en) * 2009-09-10 2011-03-10 The National Titanium Dioxide Co. Ltd. (Cristal) Methods of producing titanium dioxide nanoparticles
CN102324505A (en) * 2011-07-27 2012-01-18 天津大学 Preparation method of graphene loaded with anatase type nano titanium dioxide and application thereof
CN102627320A (en) * 2012-04-25 2012-08-08 中国科学院宁波材料技术与工程研究所 Preparation method for nano titanium dioxide lithium ion battery cathode material
CN102983334A (en) * 2012-12-18 2013-03-20 中国科学院宁波材料技术与工程研究所 Positive pole material of lithium ion battery and preparation method of material
CN106129343A (en) * 2016-05-25 2016-11-16 福建翔丰华新能源材料有限公司 A kind of preparation method of Graphene titanium dioxide microballoon sphere
CN106531968A (en) * 2016-12-23 2017-03-22 中国工程物理研究院材料研究所 Preparation method of reduced graphene oxide/TiO2-B composite material for negative electrode of lithium-ion battery
CN107331839A (en) * 2017-06-28 2017-11-07 福建师范大学 A kind of preparation method of carbon nanotube loaded nano titanium oxide
CN108511696A (en) * 2017-02-27 2018-09-07 天津工业大学 A kind of preparation method of titanium dioxide/graphene composite material
CN112332025A (en) * 2020-11-10 2021-02-05 南京工业大学 Diaphragm for lithium-sulfur battery and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110059315A1 (en) * 2009-09-10 2011-03-10 The National Titanium Dioxide Co. Ltd. (Cristal) Methods of producing titanium dioxide nanoparticles
CN102324505A (en) * 2011-07-27 2012-01-18 天津大学 Preparation method of graphene loaded with anatase type nano titanium dioxide and application thereof
CN102627320A (en) * 2012-04-25 2012-08-08 中国科学院宁波材料技术与工程研究所 Preparation method for nano titanium dioxide lithium ion battery cathode material
CN102983334A (en) * 2012-12-18 2013-03-20 中国科学院宁波材料技术与工程研究所 Positive pole material of lithium ion battery and preparation method of material
CN106129343A (en) * 2016-05-25 2016-11-16 福建翔丰华新能源材料有限公司 A kind of preparation method of Graphene titanium dioxide microballoon sphere
CN106531968A (en) * 2016-12-23 2017-03-22 中国工程物理研究院材料研究所 Preparation method of reduced graphene oxide/TiO2-B composite material for negative electrode of lithium-ion battery
CN108511696A (en) * 2017-02-27 2018-09-07 天津工业大学 A kind of preparation method of titanium dioxide/graphene composite material
CN107331839A (en) * 2017-06-28 2017-11-07 福建师范大学 A kind of preparation method of carbon nanotube loaded nano titanium oxide
CN112332025A (en) * 2020-11-10 2021-02-05 南京工业大学 Diaphragm for lithium-sulfur battery and preparation method thereof

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Application publication date: 20211102