CN110165172A - Fe for anode material of lithium-ion battery2+Support the preparation method of MXene - Google Patents

Fe for anode material of lithium-ion battery2+Support the preparation method of MXene Download PDF

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Publication number
CN110165172A
CN110165172A CN201910412638.9A CN201910412638A CN110165172A CN 110165172 A CN110165172 A CN 110165172A CN 201910412638 A CN201910412638 A CN 201910412638A CN 110165172 A CN110165172 A CN 110165172A
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China
Prior art keywords
mxene
ion battery
fecl
lithium
anode material
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Pending
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CN201910412638.9A
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Chinese (zh)
Inventor
牛棱渊
张雨杉
刘卯成
张小美
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Hangzhou Realistic New Materials Technology Co Ltd
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Hangzhou Realistic New Materials Technology Co Ltd
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Priority to CN201910412638.9A priority Critical patent/CN110165172A/en
Publication of CN110165172A publication Critical patent/CN110165172A/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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • 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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to a kind of Fe for anode material of lithium-ion battery2+The simple technology of preparing for supporting MXene, belongs to field of material preparation, main preparation step are as follows: prepares FeCl2Aqueous solution, and single layer MXene ultrasonic disperse is obtained into MXene dispersion liquid in deionized water；FeCl will be slowly added under MXene dispersion stirring2Aqueous solution stirs 12 h at room temperature, the Fe for anode material of lithium-ion battery can be obtained after gained washing of precipitate is dry2+Support MXene.

Description

Fe for anode material of lithium-ion battery2+Support the preparation method of MXene
Technical field
The present invention relates to the Fe for anode material of lithium-ion battery2+Support the technology of preparing of MXene.
Background technique
For lithium ion battery, metallic sodium used in sodium-ion battery has abundance, low in cost etc. Advantage, and telescopiny and lithium ion of the sodium ion in negative electrode material are very much like, therefore sodium-ion battery is expected to become not Carry out extensive, the chemical accumulation power supply of low cost and by favor.MXene has good due to its unique two-dimensional layered structure Sodium ion intercalation/deintercalation characteristic, be one of ideal anode material of lithium-ion battery at present.But MXene is in use The phenomenon that will appear from stacking, prevents its active surface from being fully utilized, and hinder the intercalation/deintercalation of sodium ion, cause Its high rate performance is relatively low.Therefore by by Fe2+It is supported on MXene interlayer, the existing from stacking of MXene can be effectively prevented As, and the interlamellar spacing of further expansion MXene, to be obviously improved diffusion rate of the sodium ion in MXene body phase, Jiang Nengxian Write the high magnification storage sodium performance for promoting MXene.However, the pillared MXene of the ion reported at present is required to using otheralkali metal Ion or organic molecule it is pre- it is pillared could realize, preparation process is complex.Therefore, proposed by the present invention to use Fe2+Support MXene is to pass through Fe as anode material of lithium-ion battery2+Electrostatic interaction between single layer MXene attracts each other, to reach To directly supporting.This method does not need pre- pillared, enormously simplifies the preparation process of the pillared MXene of ion, is to current research Important innovation and effectively supplement.
Summary of the invention
The object of the present invention is to provide a kind of Fe for anode material of lithium-ion battery2+Support the simple of MXene material Preparation method.
The present invention is the Fe for anode material of lithium-ion battery2+The simple preparation method for supporting MXene, the steps include: By FeCl2Deionized water, which is dissolved in, by a certain concentration obtains FeCl2Aqueous solution；Deionized water is dispersed by single layer MXene powder ultrasonic Obtain MXene dispersion liquid；FeCl will be slowly added under the stirring of MXene dispersion liquid2Aqueous solution washes gained precipitating after stirring 12h It washs dry to get the Fe arrived for sodium-ion battery cathode2+The MXene of support, concrete operation step:
(1) certain density FeCl is prepared210 mL of solution；
(2) 10 mL deionized waters are added in 50mg single layer MXene powder, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) MXene dispersion liquid obtained by step (2) is added slowly with stirring FeCl obtained by step (1)2In solution；
(4) 12 h are stirred at room temperature, and 3000rad/min centrifuge washing three times, is dried to obtain and can be used for sodium-ion battery cathode material The Fe of material2+The MXene of support.
Specific embodiment
The present invention is the Fe for anode material of lithium-ion battery2+The simple preparation method for supporting MXene, the steps include: By FeCl2Deionized water, which is dissolved in, by a certain concentration obtains FeCl2Aqueous solution；Deionized water is dispersed by single layer MXene powder ultrasonic Obtain MXene dispersion liquid；FeCl will be slowly added under the stirring of MXene dispersion liquid2Aqueous solution washes gained precipitating after stirring 12h It washs dry to get the Fe arrived for sodium-ion battery cathode2+The MXene of support.
The above-described Fe for anode material of lithium-ion battery2+Support the preparation method of MXene, specific steps Are as follows:
(1) certain density FeCl is prepared210 mL of solution；
(2) 10 mL deionized waters are added in 50mg single layer MXene powder, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) MXene dispersion liquid obtained by step (2) is added slowly with stirring FeCl obtained by step (1)2In solution；
(4) 12 h are stirred at room temperature, and 3000rad/min centrifuge washing three times, is dried to obtain and can be used for sodium-ion battery cathode material The Fe of material2+The MXene of support.
The above is used for the Fe of anode material of lithium-ion battery2+The preparation method of the MXene of support, described MXene For Ti3C2TxOr Ti2CTxOr V2CTxOr Mo3C2Tx。
The above is used for the Fe of anode material of lithium-ion battery2+The preparation method of the MXene of support, described FeCl2 Concentration be 0.005 mol/L perhaps 0.015 mol/L perhaps 0.025 mol/L or 0.035 mol/L.
The above is used for the Fe of anode material of lithium-ion battery2+The preparation method of the MXene of support, described stirring are Magnetic agitation.
The above is used for the Fe of anode material of lithium-ion battery2+The preparation method of the MXene of support, described drying are Freeze-drying.
Embodiment 1
(1) compound concentration is the FeCl of 0.005mol/L210 mL of solution；
(2) 50mg single layer MXene powder is added in 10 mL deionized waters, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) by MXene dispersion liquid that step (2) obtains, agitation and dropping enters the FeCl that step (1) obtains dropwise2In solution；
(4) at room temperature, 12 h are stirred to react, then 3000rad/min centrifuge washing three times, is finally dried to obtain Fe2+Support MXene。
Embodiment 2
(1) compound concentration is the FeCl of 0.015mol/L210 mL of solution；
(2) 50mg single layer MXene powder is added in 10 mL deionized waters, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) by MXene dispersion liquid that step (2) obtains, agitation and dropping enters the FeCl that step (1) obtains dropwise2In solution；
(4) at room temperature, 12 h are stirred to react, then 3000rad/min centrifuge washing three times, is finally dried to obtain Fe2+Support MXene。
Embodiment 3
(1) compound concentration is the FeCl of 0.025mol/L210 mL of solution；
(2) 50mg single layer MXene powder is added in 10 mL deionized waters, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) by MXene dispersion liquid that step (2) obtains, agitation and dropping enters the FeCl that step (1) obtains dropwise2In solution；
(4) at room temperature, 12 h are stirred to react, then 3000rad/min centrifuge washing three times, is finally dried to obtain Fe2+Support MXene。
Embodiment 4
(1) compound concentration is the FeCl of 0.035mol/L210 mL of solution；
(2) 50mg single layer MXene powder is added in 10 mL deionized waters, ice-bath ultrasonic 1h obtains MXene dispersion liquid；
(3) by MXene dispersion liquid that step (2) obtains, agitation and dropping enters the FeCl that step (1) obtains dropwise2In solution；
(4) at room temperature, 12 h are stirred to react, then 3000rad/min centrifuge washing three times, is finally dried to obtain Fe2+Support MXene。
The above is the embodiment of the present invention, is not intended to limit the scope of the invention, all to be said using the present invention Equivalent structure or equivalent flow shift made by bright book content is applied directly or indirectly in other relevant field technologies, It similarly include in the invention patent protection scope.

Claims (5)

1. being used for the Fe of anode material of lithium-ion battery2+The simple preparation method for supporting MXene, the steps include: FeCl2By one Determine concentration and be dissolved in deionized water to obtain FeCl2Aqueous solution；Deionized water, which is dispersed, by single layer MXene powder ultrasonic obtains MXene Dispersion liquid；FeCl will be slowly added under the stirring of MXene dispersion liquid2Aqueous solution is dried gained washing of precipitate after stirring 12 h, i.e., Obtain the Fe for sodium-ion battery cathode2+The MXene of support, concrete operation step:
(1) certain density FeCl is prepared210 mL of solution；
(2) 10 mL deionized waters are added in 50 mg single layer MXene powder, 1 h of ice-bath ultrasonic obtains MXene dispersion liquid；
(3) MXene dispersion liquid obtained by step (2) is added slowly with stirring FeCl obtained by step (1)2In solution；
(4) 12 h are stirred at room temperature, and 3000 rad/min centrifuge washings three times, are dried to obtain and can be used for sodium-ion battery cathode The Fe of material2+The MXene of support.
2. the Fe according to claim 1 for anode material of lithium-ion battery2+The simple preparation side of the MXene of support Method, it is characterised in that: described MXene is Ti3C2, Ti2C and Mo3C2。
3. the Fe according to claim 1 for anode material of lithium-ion battery2+The simple preparation side of the MXene of support Method, it is characterised in that: described FeCl2Concentration be 0.005 mol/L, 0.015 mol/L, 0.025 mol/L and 0.035 mol/L。
4. the Fe according to claim 1 for anode material of lithium-ion battery2+The simple preparation side of the MXene of support Method, it is characterised in that: described stirring is magnetic agitation.
5. the Fe according to claim 1 for anode material of lithium-ion battery2+The simple preparation side of the MXene of support Method, it is characterised in that: described drying is freeze-drying.
CN201910412638.9A 2019-05-17 2019-05-17 Fe for anode material of lithium-ion battery2+Support the preparation method of MXene Pending CN110165172A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106099064A (en) * 2016-08-03 2016-11-09 常州大学 A kind of SnS2the preparation method of/CNTs composite nano materials and the application as anode material of lithium-ion battery thereof
CN106229488A (en) * 2016-08-26 2016-12-14 浙江工业大学 A kind of oxide pillared MXene composite and application thereof
US20180342730A1 (en) * 2017-05-23 2018-11-29 The Hong Kong Polytechnic University MnO2 ANODE FOR LI-ION AND NA-ION BATTERIES
CN109402662A (en) * 2018-12-14 2019-03-01 哈尔滨工业大学 A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106099064A (en) * 2016-08-03 2016-11-09 常州大学 A kind of SnS2the preparation method of/CNTs composite nano materials and the application as anode material of lithium-ion battery thereof
CN106229488A (en) * 2016-08-26 2016-12-14 浙江工业大学 A kind of oxide pillared MXene composite and application thereof
US20180342730A1 (en) * 2017-05-23 2018-11-29 The Hong Kong Polytechnic University MnO2 ANODE FOR LI-ION AND NA-ION BATTERIES
CN109402662A (en) * 2018-12-14 2019-03-01 哈尔滨工业大学 A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material

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Application publication date: 20190823

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