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CN107492641A - A kind of titanium carbide four vulcanizes three titanium composite materials and preparation method thereof - Google Patents

A kind of titanium carbide four vulcanizes three titanium composite materials and preparation method thereof Download PDF

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Publication number
CN107492641A
CN107492641A CN201710638809.0A CN201710638809A CN107492641A CN 107492641 A CN107492641 A CN 107492641A CN 201710638809 A CN201710638809 A CN 201710638809A CN 107492641 A CN107492641 A CN 107492641A
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China
Prior art keywords
titanium carbide
titanium
accordion
preparation
composite materials
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CN201710638809.0A
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Inventor
武卫明
周丽敏
张长松
侯绍刚
王书红
赵凌
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Anyang Institute of Technology
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Anyang Institute of Technology
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Priority to CN201710638809.0A priority Critical patent/CN107492641A/en
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

Vulcanize Tritanium/Trititanium (Ti the invention discloses a kind of microstructure for the titanium carbide four of accordion like3S4) composite and preparation method thereof, with hf etching Ti3SiC2、Ti3AlC2Or Ti2Accordion like titanium carbide material prepared by AlC ceramic powder materials is raw material, is reacted under the high temperature conditions by elemental sulfur and above-mentioned titanium carbide, can prepare the titanium carbide four that microstructure is accordion like and vulcanize Tritanium/Trititanium (Ti3S4) composite nano materials.With the titanium carbide four vulcanization Tritanium/Trititanium (Ti3S4) negative material of the composite nano materials as lithium ion battery, the composite shows higher specific capacity, good high rate performance and charge-discharge performance.

Description

A kind of titanium carbide-four vulcanizes three titanium composite materials and preparation method thereof
Technical field
The present invention relates to the preparation field of nano composite material, specifically a kind of microstructure is carbonized for " accordion " shape Titanium-Ti3S4The preparation method of composite nano materials.
Background technology
Graphene and class graphene two-dimension nano materials are nano materials emerging in recent years, due to its unique structure And property, it is can be widely applied to the fields such as energy storage, catalysis, electronics.Titanium carbide two-dimension nano materials are a kind of new Class graphene nano material, have the advantages that thickness of thin, electrical conductivity are high, can apply to lithium ion battery, lithium-sulfur cell, super The fields such as capacitor, fuel cell, but its relatively low specific discharge capacity limits its further development and application.
Pass through chemical etching Ti3SiC2、Ti3AlC2Or Ti2The method of AlC laminate ceramics can prepare microcosmic knot Structure is the assembly of " accordion " shape two-dimensional structure titanium carbide nanometer sheet, by further vulcanizing treatment, can keep carbon Change titanium microstructure to vulcanize its part surface or edge while do not change, generate the sulfide of titanium, so can be While keeping titanium carbide high conductivity, its surface is modified with the sulfide of titanium, its storage lithium specific volume is improved so as to reach The ability of amount and high rate performance.
The content of the invention
In order to improve the specific capacity of lithium ion battery, high rate performance and charge-discharge performance, it is an object of the invention to It is " accordion " shape titanium carbide-Ti to provide a kind of microstructure3S4Composite nano materials and preparation method thereof, with the composite It is applied to for negative pole in lithium ion battery, specific capacity, high rate performance and the charge and discharge cycles of lithium ion battery can be effectively improved Performance.
To reach above-mentioned purpose, the technical scheme is that：
First, Ti is chemically treated by HF3SiC2、Ti3AlC2Or Ti2AlC ceramic materials, can prepare microstructure is The titanium carbide two-dimension nano materials assembly of " accordion " shape, is wherein incorporated in one between titanium carbide nanometer sheet by Van der Waals force Rise；Secondly, in 600-1300oUnder C hot conditions, with N2Or Ar inert gases are carrier gas, pass through elemental sulfur and above-mentioned carbonization Titanium nano material is reacted, and can be vulcanized the part surface of titanium carbide nanometer sheet or edge, so as to prepare microcosmic knot Structure is the titanium carbide-Ti of " accordion " shape3S4Nano composite material.
The excellent results of the present invention are：
It is " hand wind that can prepare microstructure by titanium carbide nanometer sheet under the high temperature conditions and the chemical reaction of elemental sulfur Titanium carbide-the Ti of qin " shape3S4Nano composite material, this method has that technique is simple, high income, low cost and other advantages, is easy to Industrialized production.Titanium carbide-the Ti prepared with the present invention3S4Nano composite material for negative pole be applied to lithium ion battery in, energy Enough significantly improve specific capacity, high rate performance and the charge-discharge performance of lithium ion battery.
1. titanium carbide-the Ti prepared using the present invention3S4Negative material of the nano composite material piece as lithium ion battery, The specific capacity of lithium ion battery is effectively increased, improves the high rate performance and charge-discharge performance of lithium ion battery.
It is " accordion " shape titanium carbide-Ti that 2. the present invention, which prepares microstructure,3S4Nano composite material method, have The advantages that yield is high, cost is low, technique is simple, is easy to industrial amplification production.
3. titanium carbide-the Ti prepared using the present invention3S4Nano composite material, while titanium carbide high conductivity is kept, Ti3S4Nanometer sheet or nano-particle can be grown on the face of titanium carbide nanometer sheet and edge with good adhesion.
Embodiment
Embodiment 1
Ti is handled by 40% HF solution at ambient temperature3SiC2Dusty material, microstructure is prepared as accordion like Ti3C2Material, by the Ti3C2Material is positioned over tube furnace middle position, the position placed as close as thermocouple, simultaneously Simple substance sulphur powder is placed on Ti3C2The uptake position of material, using Ar as carrier gas, with 5oC/min heating rate rises to 1000oC, insulation 1h can obtain the Ti that microstructure is " accordion " shape3C2-Ti3S4Nano composite material.With prepared Ti3C2-Ti3S4Nano composite material is electrode material, by being coated on after being mixed with acetylene black and Kynoar on copper sheet （Mass ratio is 80:10:10）, electrode is used as after vacuum drying, using metal lithium sheet as to electrode, with L containing 1mol-1 LiPF6Ethylene carbonate (EC), dimethyl carbonate（DMC）Mixed solution is electrolyte（EC/DMC volume ratio is 1:1）, Under 0.01-3V test voltage, the reversible specific capacity of the electrode is 560 mAh g after 50 circulations of discharge and recharge-1, remain to The 95% of initial capacity is enough kept, in 1000mA g-1Current density under, the reversible specific capacity of electrode is up to 230 mAh g-1。
Embodiment 2
Ti is handled by 30% HF solution at ambient temperature3AlC2Dusty material, microstructure is prepared as accordion like Ti3C2Material, by the Ti3C2Material is positioned over tube furnace middle position, the position placed as close as thermocouple, simultaneously Simple substance sulphur powder is placed on Ti3C2The uptake position of material, with N2For carrier gas, with 5oC/min heating rate rises to 1100oC, Insulation 30min can obtain the Ti that microstructure is " accordion " shape3C2-Ti3S4Nano composite material.With prepared Ti3C2- Ti3S4Nano composite material is electrode material, by being coated on after being mixed with acetylene black and Kynoar on copper sheet（Quality Than for 80:10:10）, electrode is used as after vacuum drying, using metal lithium sheet as to electrode, with L containing 1mol-1 LiPF6's Ethylene carbonate (EC), dimethyl carbonate（DMC）Mixed solution is electrolyte（EC/DMC volume ratio is 1:1）, in 0.01-3V Test voltage under, the reversible specific capacity of the electrode is 530 mAh g after the circulation of discharge and recharge 50 times-1, it still is able to keep The 93% of initial capacity, in 1000mA g-1Current density under, the reversible specific capacity of electrode is up to 215 mAh g-1。
Embodiment 3
Ti is handled by 15% HF solution at ambient temperature2AlC dusty materials, microstructure is prepared as accordion like Ti2C-material, by the Ti2C-material is positioned over tube furnace middle position, the position placed as close as thermocouple, simultaneously will Simple substance sulphur powder is placed on Ti3C2The uptake position of material, with N2For carrier gas, with 5oC/min heating rate rises to 900oC, protect Warm 2h can obtain the Ti that microstructure is " accordion " shape2C-Ti3S4Nano composite material.With prepared Ti2C-Ti3S4Receive Nano composite material is electrode material, by being coated on after being mixed with acetylene black and Kynoar on copper sheet（Mass ratio is 80: 10:10）, electrode is used as after vacuum drying, using metal lithium sheet as to electrode, with L containing 1mol-1 LiPF6Ethylene Alkene ester (EC), dimethyl carbonate（DMC）Mixed solution is electrolyte（EC/DMC volume ratio is 1:1）, in 0.01-3V test Under voltage, the reversible specific capacity of the electrode is 480 mAh g after 50 circulations of discharge and recharge-1, it still is able to keep initially to hold The 91% of amount, in 1000mA g-1Current density under, the reversible specific capacity of electrode is up to 190 mAh g-1。

Claims (5)

1. a kind of titanium carbide-four vulcanizes three titanium composite materials and preparation method thereof, it is characterised in that：Titanium carbide is two-dimensional nano piece The assembly of structure, microstructure are " accordion " shape, and four vulcanization Tritanium/Trititaniums are grown on the face of titanium carbide nanometer sheet and edge, should Composite can be used as negative material to be applied in lithium ion battery.
2. vulcanizing three titanium composite materials and preparation method thereof according to a kind of titanium carbide-four described in claim 1, its feature exists In：It is prepared under the high temperature conditions with the reaction with " accordion " shape titanium carbide nanometer sheet assembly by elemental sulfur.
3. vulcanize three titanium composite materials and preparation method thereof, its feature according to a kind of titanium carbide-four described in claim 1 or 2 It is：" accordion " shape titanium carbide nanometer sheet assembly passes through HF chemical etchings Ti3SiC2、Ti3AlC2And Ti2AlC ceramic powders It is prepared by the method at end.
4. vulcanize three titanium composite materials and preparation method thereof, its feature according to a kind of titanium carbide-four described in claim 1 or 3 It is：" accordion " shape titanium carbide nanometer sheet, its chemical composition are Ti3C2Or Ti2C。
5. vulcanize three titanium composite materials and preparation method thereof, its feature according to a kind of titanium carbide-four described in claim 1 or 2 It is：The condition that elemental sulfur reacts with " accordion " shape titanium carbide nanometer sheet is elemental sulfur and the temperature of titanium carbide nanometer sheet reaction Degree is in 600-1300oBetween C, the reaction time is between 5min-12h.
CN201710638809.0A 2017-07-31 2017-07-31 A kind of titanium carbide four vulcanizes three titanium composite materials and preparation method thereof Pending CN107492641A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110165164A (en) * 2019-05-08 2019-08-23 合肥国轩高科动力能源有限公司 Silicon-layered titanium carbide negative electrode material and preparation method thereof
CN110902657A (en) * 2018-09-17 2020-03-24 北京航空航天大学 Method for preparing expansion transition metal sulfur group compound
CN113943003A (en) * 2021-11-09 2022-01-18 滁州学院 With Ti3SiC2Preparation of two-dimensional Material Ti for precursor3C2Method (2)
CN114276141A (en) * 2020-11-12 2022-04-05 郑州伯利森新材料科技有限公司 Method for preparing titanium carbide two-dimensional nanosheet through high-temperature vulcanization heat treatment method
CN114538505A (en) * 2022-03-18 2022-05-27 中国地质大学（武汉） Nano flaky TiS2/Ti3C2TX MXene/C composite material and preparation method and application thereof

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WO2016012275A1 (en) * 2014-07-22 2016-01-28 Basf Se Composites comprising mxenes for cathodes of lithium sulfur cells
CN105449186A (en) * 2015-11-18 2016-03-30 中国科学院深圳先进技术研究院 Novel secondary battery and preparation method therefor
CN105887015A (en) * 2016-04-15 2016-08-24 中国科学院上海技术物理研究所 Step-by-step gas phase method for preparing large-area single-layer tungsten disulfide and molybdenum disulfide structures
CN106025200A (en) * 2016-05-24 2016-10-12 浙江大学 Preparation method and application of nitrogen-doped MXene battery anode material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016012275A1 (en) * 2014-07-22 2016-01-28 Basf Se Composites comprising mxenes for cathodes of lithium sulfur cells
CN105449186A (en) * 2015-11-18 2016-03-30 中国科学院深圳先进技术研究院 Novel secondary battery and preparation method therefor
CN105887015A (en) * 2016-04-15 2016-08-24 中国科学院上海技术物理研究所 Step-by-step gas phase method for preparing large-area single-layer tungsten disulfide and molybdenum disulfide structures
CN106025200A (en) * 2016-05-24 2016-10-12 浙江大学 Preparation method and application of nitrogen-doped MXene battery anode material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110902657A (en) * 2018-09-17 2020-03-24 北京航空航天大学 Method for preparing expansion transition metal sulfur group compound
CN110902657B (en) * 2018-09-17 2021-06-18 北京航空航天大学 Method for preparing expansion transition metal sulfur group compound
CN110165164A (en) * 2019-05-08 2019-08-23 合肥国轩高科动力能源有限公司 Silicon-layered titanium carbide negative electrode material and preparation method thereof
CN114276141A (en) * 2020-11-12 2022-04-05 郑州伯利森新材料科技有限公司 Method for preparing titanium carbide two-dimensional nanosheet through high-temperature vulcanization heat treatment method
CN114276141B (en) * 2020-11-12 2023-05-05 鱼台齐鑫化工有限公司 Method for preparing titanium carbide two-dimensional nano-sheet by high-temperature vulcanization heat treatment method
CN113943003A (en) * 2021-11-09 2022-01-18 滁州学院 With Ti3SiC2Preparation of two-dimensional Material Ti for precursor3C2Method (2)
CN114538505A (en) * 2022-03-18 2022-05-27 中国地质大学（武汉） Nano flaky TiS2/Ti3C2TX MXene/C composite material and preparation method and application thereof

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Application publication date: 20171219