CN107381576A - A kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet - Google Patents

A kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet Download PDF

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Publication number
CN107381576A
CN107381576A CN201710638807.1A CN201710638807A CN107381576A CN 107381576 A CN107381576 A CN 107381576A CN 201710638807 A CN201710638807 A CN 201710638807A CN 107381576 A CN107381576 A CN 107381576A
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nanometer sheet
titanium carbide
synthesizing
electrochemical method
alc
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武卫明
张长松
周丽敏
侯绍刚
王书红
张楠
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Anyang Institute of Technology
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Anyang Institute of Technology
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    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Electric Double-Layer Capacitors Or The Like (AREA)
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Abstract

The invention discloses a kind of electrochemical method for preparing ultra-thin two-dimension titanium carbide nanometer sheet, by with Ti3SiC2, Ti3AlC2Or the material such as TiAlC is positive pole, to contain F‑And SO4 2‑The aqueous solution be electrolyte, anode material directly can be prepared into by ultra-thin two-dimension titanium carbide nanometer sheet by the electrochemical reaction occurred on positive pole under certain voltage.The two-dimensional nano piece individually also can be used in combination with other materials, among being used for lithium ion battery, ultracapacitor as electrode material, can be used for the fields such as electronics.

Description

A kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet
Technical field
The present invention relates to the preparation field of two-dimension nano materials, specifically a kind of ultra-thin two-dimension titanium carbide nano material Preparation method.
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.
Ti3SiC2、Ti3AlC2Or Ti2AlC is a kind of ceramic material with layer structure, can by the method for chemistry So that Si the or Al atom-lithographies in material to be fallen, so as to generate the titanium carbide material with accordion like, by further Processing can peel off into titanium carbide two-dimension nano materials, but this method generally requires high toxicity, the hydrofluoric acid chemistry of high concentration Reagent, injury easily is produced to operating personnel and environment, it is also desirable to which many more manipulations can just prepare the wiener of titanium carbide two Rice material.Electrochemical method can realize the preparation of graphene and class graphene two-dimension nano materials under mild conditions, Therefore, can attempt to prepare titanium carbide two-dimension nano materials by the method for electrochemistry.
The content of the invention
In order to realize it is efficient in a mild condition prepare ultra-thin two-dimension titanium carbide nano material,
Can be in a mild condition by Ti it is an object of the invention to provide one kind3SiC2、Ti3AlC2Or Ti2AlC ceramics materials Material is prepared into the electrochemical method of titanium carbide two-dimension nano materials.
To reach above-mentioned purpose, the technical scheme is that：
With Ti3SiC2、Ti3AlC2Or Ti2AlC ceramic materials are positive pole, and the positive pole can be by dry pressing by these ceramic powders Powder material is pressed into certain shape, and the effigurate electrode of tool is prepared into by sintering under an inert atmosphere；To contain F-, SO4 2-Acidity or neutral aqueous solution be electrolyte, wherein F-With SO4 2-Concentration in 0.1-5 molL-1Between, electrolyte Temperature in 0-60oBetween C；With graphite or inert metal such as platinum, palladium is negative pole, and voltage is controlled between 0.3-10.0V, is led to Ultra-thin two-dimension titanium carbide nanometer sheet can be prepared by crossing the method for control voltage.
The excellent results of the present invention are：
Can be in a mild condition by Ti by using the method for electrochemistry3SiC2、Ti3AlC2Or Ti2AlC ceramic materials are carved Ultra-thin two-dimension titanium carbide nanometer sheet is lost into, critical conditions and highly toxic chemical reagent without HTHP, and can be with one Footwork efficiently completes the preparation of titanium carbide two-dimensional nano piece, without subsequent steps such as ultrasound strippings.
1. the present invention experiment condition harsh without high temperature, high pressure etc., can prepare titanium carbide nanometer sheet with one-step method.
2. the titanium carbide nanometer sheet prepared using the present invention, has the advantages that thickness of thin, electrical conductivity are high.
3. using the ultra-thin two-dimension titanium carbide nanometer sheet for preparing of the present invention, can individually or with the compound conduct of other materials Electrode material is applied among lithium ion battery and ultracapacitor, improves the high rate performance and electric capacity of lithium ion battery The capacity of device.
4. using the ultra-thin two-dimension titanium carbide nanometer sheet for preparing of the present invention, can with electrode active material is compound is used as anode Applied in fuel cell, effectively increasing catalytic performance of the fuel cell to fuel such as hydrogen, methanol.
Brief description of the drawings
Accompanying drawing 1：With 1 mol L-1NaF and 1 mol L-1Na2SO4Mixed aqueous solution is Ti prepared by electrolyte electrochemical2C The SEM figures of nanometer sheet；
Accompanying drawing 2：Prepare Ti2The XRD spectra of C nano piece.
Embodiment
Embodiment 1
With Ti3SiC2Material is positive pole, wherein Ti3SiC2The preparation of electrode is with Ti3SiC2Powder body material is raw material, by It is dry-pressing formed under 50MPa, then sinter 1000 under argon gas protectionoC, form within 2 hours, with containing NaF and Na2SO4Mixing The aqueous solution is electrolyte, and its concentration is respectively 0.5 mol L-1With 2 mol L-1, using graphite as negative pole, control voltage 1.2 V, Ti is carried out at ambient temperature3SiC2The electrochemical etching of positive pole and stripping, ultra-thin two-dimension material can be separated, has been peeled off Into rear by containing Ti3C2The electrolyte of nanometer sheet is filtered by vacuum and deionized water cleaning, and freeze-drying can obtain Ti3C2Nanometer sheet powder body material.
Embodiment 2
With Ti3AlC2Material is positive pole, wherein Ti3AlC2The preparation of electrode is with Ti3AlC2Powder body material is raw material, by It is dry-pressing formed under 50MPa, then sinter 900 under argon gas protectionoC, form within 2 hours, with containing NaF and Na2SO4The aqueous solution For electrolyte, its concentration is respectively 0.2 mol L-1With 3 mol L-1, using graphite as negative pole, control voltage is 0.9 V, in room Ti is carried out under the conditions of temperature3AlC2The electrochemical etching of positive pole and stripping, ultra-thin two-dimension Ti can be separated3C2Nanometer sheet material, stripping By to containing Ti from after the completion of3C2The electrolyte vacuum of nanometer sheet filters, deionized water cleaning, and freeze-drying can obtain Ti3C2Nanometer sheet powder body material.
Embodiment 3
With Ti2AlC materials are positive pole, wherein Ti2The preparation of AlC electrodes is with Ti2AlC powder body materials are raw material, by 40MPa Under it is dry-pressing formed, then argon gas protection under sinter 800oC, form within 2 hours, with containing NaF and Na2SO4The aqueous solution for electricity Xie Zhi, its concentration are respectively 0.1 mol L-1With 1 mol L-1, using graphite as negative pole, control voltage is 0.9 V, in room temperature bar Ti is carried out under part2The electrochemical etching of AlC positive poles and stripping, ultra-thin two-dimension Ti can be prepared2C nano sheet material, peel off and complete Afterwards by containing Ti2The electrolyte vacuum of C nano piece filters, deionized water cleaning, and freeze-drying can obtain Ti2C nano Piece powder body material.
Embodiment 4
With Ti3SiC2Material is positive pole, wherein Ti3SiC2The preparation of electrode is with Ti3SiC2Powder body material is raw material, by 50 It is dry-pressing formed under MPa, then sinter 1000 under argon gas protectionoC, form within 2 hours, with containing HF and Na2SO4Mixing it is water-soluble Liquid is electrolyte, and its concentration is respectively 0.5 mol L-1With 2 mol L-1, using graphite as negative pole, control voltage 0.9V, in room Ti is carried out under the conditions of temperature3SiC2The electrochemical etching of positive pole and stripping, ultra-thin two-dimension Ti can be prepared3C2Nanometer sheet material, stripping By to containing Ti from after the completion of3C2The electrolyte vacuum of nanometer sheet filters, deionized water cleaning, and freeze-drying can obtain Ti3C2Nanometer sheet powder body material.

Claims (5)

  1. A kind of 1. electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet, it is characterised in that：The side that the nanometer sheet passes through electrochemistry It is prepared by method.
  2. 2. according to a kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet described in claim 1, it is characterised in that：With Ti3SiC2、Ti3AlC2Or Ti2AlC materials are positive pole, using graphite, metal platinum or palladium as negative pole, between positive pole and negative pole Voltage is between 0.3-10.0.
  3. 3. according to a kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet described in claim 1, it is characterised in that：With containing F-And SO4 2-The aqueous solution of ion is electrolyte, wherein F-The concentration of ion is in 0.1-5 molL-1Between, SO4 2-Ion it is dense Degree is in 0.1-5 molL-1Between.
  4. 4. according to a kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet described in claim 1, it is characterised in that：Electrolysis Matter temperature is 0-60oBetween C.
  5. 5. according to a kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet described in claim 1, it is characterised in that：It is described The chemical composition of titanium carbide is Ti3C2Or Ti2C, nanometer sheet gross thickness is between 1 nanometer -50 nanometers.
CN201710638807.1A 2017-07-31 2017-07-31 A kind of electrochemical method for synthesizing of two-dimentional titanium carbide nanometer sheet Pending CN107381576A (en)

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN108003520A (en) * 2017-12-07 2018-05-08 黑龙江科技大学 A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material
CN108328616A (en) * 2018-04-20 2018-07-27 昆明理工大学 A kind of preparation method of three-dimensional MXene
CN108383121A (en) * 2018-03-02 2018-08-10 东莞理工学院 The preparation method and application of MXene nanometer sheets with the vacancy Mo
CN109694074A (en) * 2019-03-04 2019-04-30 青岛大学 A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece
RU2686897C1 (en) * 2018-08-24 2019-05-06 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" Device for production of titanium carbide-based powder
RU2687423C1 (en) * 2018-09-26 2019-05-13 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" Method of producing titanium carbide-based powder
CN111591991A (en) * 2020-04-26 2020-08-28 深圳瀚光科技有限公司 Device for electrochemically preparing MXene
CN111668559A (en) * 2019-03-08 2020-09-15 南京理工大学 Based on Ti3Al1-xC2Aqueous zinc ion battery of positive electrode material
CN111661848A (en) * 2020-04-28 2020-09-15 深圳瀚光科技有限公司 Method for electrochemically preparing MXene
CN113461010A (en) * 2021-07-07 2021-10-01 南京林业大学 Method for preparing fluorine-free MXene by adopting electrochemical etching method
CN115094257A (en) * 2022-07-11 2022-09-23 安阳工学院 Preparation method of one-dimensional alloy nano material

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003520B (en) * 2017-12-07 2020-04-17 陕西科技大学 Preparation method of polyvinylidene fluoride titanium carbide nanosheet composite material with high dielectric property
CN108003520A (en) * 2017-12-07 2018-05-08 黑龙江科技大学 A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material
CN108383121A (en) * 2018-03-02 2018-08-10 东莞理工学院 The preparation method and application of MXene nanometer sheets with the vacancy Mo
CN108328616A (en) * 2018-04-20 2018-07-27 昆明理工大学 A kind of preparation method of three-dimensional MXene
RU2686897C1 (en) * 2018-08-24 2019-05-06 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" Device for production of titanium carbide-based powder
RU2687423C1 (en) * 2018-09-26 2019-05-13 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" Method of producing titanium carbide-based powder
CN109694074A (en) * 2019-03-04 2019-04-30 青岛大学 A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece
CN109694074B (en) * 2019-03-04 2022-08-05 青岛大学 Method for preparing MXenes and derivative nanosheets thereof through electrochemical method
CN111668559A (en) * 2019-03-08 2020-09-15 南京理工大学 Based on Ti3Al1-xC2Aqueous zinc ion battery of positive electrode material
CN111591991A (en) * 2020-04-26 2020-08-28 深圳瀚光科技有限公司 Device for electrochemically preparing MXene
CN111661848A (en) * 2020-04-28 2020-09-15 深圳瀚光科技有限公司 Method for electrochemically preparing MXene
CN113461010A (en) * 2021-07-07 2021-10-01 南京林业大学 Method for preparing fluorine-free MXene by adopting electrochemical etching method
CN113461010B (en) * 2021-07-07 2023-06-09 南京林业大学 Method for preparing fluorine-free MXene by adopting electrochemical etching method
CN115094257A (en) * 2022-07-11 2022-09-23 安阳工学院 Preparation method of one-dimensional alloy nano material

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