CN105720270A - Preparation method of flexible anode material beta-ZnMoO4 for lithium-ion battery - Google Patents

Preparation method of flexible anode material beta-ZnMoO4 for lithium-ion battery Download PDF

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Publication number
CN105720270A
CN105720270A CN201610073082.1A CN201610073082A CN105720270A CN 105720270 A CN105720270 A CN 105720270A CN 201610073082 A CN201610073082 A CN 201610073082A CN 105720270 A CN105720270 A CN 105720270A
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ion battery
carbon cloth
preparation
lithium ion
znmoo4
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Inventor
费杰
孙谦谦
黄剑锋
刘一军
曹丽云
李嘉胤
孔新刚
欧阳海波
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a preparation method of a flexible anode material beta-ZnMoO4 for a lithium-ion battery. With zinc nitrate, zinc acetate or zinc chlorate as a zinc source, and sodium molybdate or ammonium molybdate as a molybdenum source, the beta-ZnMoO4 grows on in situ conductive carbon cloth. The prepared beta-ZnMoO4 has the advantages of high purity, uniform particle size distribution and the like; a metal current collector of a traditional lithium-ion battery is replaced with the conductive carbon cloth as the current collector; and the preparation method has the advantages that (1) the beta-ZnMoO4 is tightly attached to the surface of the carbon cloth to form a rapid electron conduction channel; (2) the contact area of an electrolyte and an active material is increased by a beta-ZnMoO4 array structure; the structure is beneficial to diffusion of the electrolyte; and the volume change in the lithium intercalation or deintercalation process can be relieved; and (3) the beta-ZnMoO4 array structure can shorten the diffusion path of the lithium-ion battery and improves the rate capability.

Description

A kind of flexible lithium ion battery negative material β-ZnMoO4Preparation method
Technical field
The invention belongs to electrochemical power source preparation field, be specifically related to a kind of flexible lithium ion battery negative material β-ZnMoO4Preparation method.
Background technology
Along with people are to growing, the reduction of fossil fuel reserves of energy demand and the aggravation of environmental pollution, open The novel energy sending out clean and effective becomes focus of concern.Lithium ion battery as a kind of energy storing device, with The features such as its environmental protection, light, high power capacity, long-life are widely used in small portable device, are expected at numerous necks Territory replaces traditional fossil energy, is applied in large-sized power battery, energy-storage battery, thus alleviates and perplex full generation at present The energy and environment problem on boundary.The electrode material of lithium ion battery is the key affecting its performance, and commercialization at present Lithium ion battery can not meet people's demand to battery performance.Therefore research and development Novel ion battery cathode material Material has the biggest development space.
Flexible electrode has a lot of prominent feature compared with traditional electrode, and these prominent features can meet newly The demand of type flexibility chemistry energy storage device.(1) energy density is high.A lot of flexible electrodes use carbon nanotube paper, stone Ink alkene film etc. flexible, the material with carbon element of high conductivity be collector, this collector gives full play to the same of collector function Time, lighter than traditional metal collector.(2) flexible.Flexible electrode can bend, and has flexibility Feature so that it is some special device demand to flexible energy storing devices can be met.(3) electrode that corrosion stability is flexible is normal Employing material with carbon element is collector, can avoid the electrolyte corrosion to tradition collector during battery charging and discharging.
β-ZnMoO4There is higher theoretical capacity, show that it has potential application energy in field of lithium ion battery Power, but owing to physical dimension is single, self-conductive is poor, and ion transmission channel is few, and cycle life is low, the most forthright The problems such as energy difference, design a kind of β-ZnMoO with superperformance4Flexible lithium ion battery negative material is following sending out Exhibition in the urgent need to.
Summary of the invention
Present invention aim at providing one to can effectively solve the problem that β-ZnMoO4Self-conductive is poor, ion transmission channel Less, in charge and discharge process volume change, cyclical stability poor, the flexible lithium-ion electric of the problems such as high rate performance difference Pond negative material β-ZnMoO4Preparation method.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
Step one: carbon cloth by the volume ratio mix homogeneously of 5:1～1:1 and is placed in one by concentrated sulphuric acid and concentrated nitric acid Carry out nitration mixture process；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put Dry in baking oven；
Step 3: zinc salt and molybdate are distributed to respectively in water, the mol ratio making zinc solution and molybdate solution is 1:7～1:9, under stirring condition, is added dropwise over molybdate solution in zinc solution, adds completely to molybdate solution After entering, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Carry out hydro-thermal reaction；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, is dried in baking oven, To β-ZnMoO4 flexible lithium ion battery material.
The carbon cloth that described step one uses uses deionized water to clean successively, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C.
Described nitration mixture processes carbon cloth 4～24h.
It is 60 DEG C that described step 2 dries temperature.
Described zinc salt is zinc nitrate, zinc acetate or zinc chloride.
Described molybdate is sodium molybdate or ammonium molybdate.
Described hydrothermal temperature is 150～180 DEG C, and the time is 2h～24h.
The invention has the beneficial effects as follows:
1) using carbon cloth as flexible lithium ion battery collector, more traditional metal collector is lighter, has higher Energy density.
2) use carbon cloth as the collector of flexible lithium ion battery, electrolyte can be avoided at battery charge and discharge process In corrosion to collector.
3) direct growth β-ZnMoO on carbon cloth4, it is to avoid the use of conductive agent and binding agent.
4)β-ZnMoO4It is attached to carbon cloth surfaces closely, defines quick electronics conduction pathway.
5)β-ZnMoO4Array structure increases the diffusion of the contact area of electrolyte and active substance, beneficially electrolyte, And the change in volume during embedding lithium/deintercalation can be alleviated.
6)β-ZnMoO4Array structure can shorten the evolving path of lithium ion battery and improve high rate performance.
Accompanying drawing explanation
Fig. 1 is β-ZnMoO prepared by the present invention4The XRD figure spectrum of flexible lithium ion battery negative material；
Fig. 2 is β-ZnMoO prepared by the present invention4The first charge-discharge figure of flexible lithium ion battery negative material.
Detailed description of the invention
Embodiment 1:
Step one: first, uses deionized water to clean successively by carbon cloth, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C；
Again carbon cloth by the volume ratio mix homogeneously of 3:1 and is placed in one and carries out nitration mixture process by concentrated sulphuric acid and concentrated nitric acid 16h；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put 60 DEG C of drying in baking oven；
Step 3: zinc nitrate and sodium molybdate are distributed in water respectively, make zinc nitrate solution and sodium molybdate solution mole Ratio is 1:7, under stirring condition, is added dropwise in zinc nitrate solution by sodium molybdate solution, complete to sodium molybdate solution After addition, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Hydro-thermal reaction 2h is carried out at 180 DEG C；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, does for 60 DEG C in baking oven Dry, obtain β-ZnMoO4 flexible lithium ion battery material.
β-the ZnMoO that will prepare4Flexible lithium ion battery materials'use sheet-punching machine carries out punching and obtains lithium-ion electric Pond negative plate, and it is placed on 80～120 DEG C of drying in vacuum drying oven, it is assembled into lithium ion battery, measures its electricity Chemical property.
Properties of product are tested:
By embodiment with 1mol/L LiPF6Three component mixed solvents (volume ratio vinyl carbonate EC: dimethyl carbonic acid Ester DMC: diethyl carbonate EMC=1:1:1) it is electrolyte, microporous polypropylene membrane is barrier film, and lithium sheet is positive pole Sheet is assembled into simulated battery.
Simulated battery is carried out performance test, uses Shenzhen new prestige cell tester that simulated battery is carried out discharge and recharge specific volume Amount cycle performance test, carries out the experiment of constant current charge-discharge specific capacity loop test with the electric current density of 100mA/g, fills Discharge voltage is limited in 0.01～3.0V.
Test result is as follows:
Fig. 1 is the β-ZnMoO of preparation4The XRD figure spectrum of flexible lithium ion battery negative material, can from figure Go out, carbon cloth has β-ZnMoO4, along with nitration mixture processes the growth of carbon cloth time, β-ZnMoO4Crystallinity weaken.
Fig. 2 is the charge-discharge property figure of simulated battery, first coulombic efficiency all up to 85%, along with nitration mixture processes The growth of time, carbon cloth surfaces structure changes, and forms more functional group at carbon cloth surfaces, makes carbon cloth have Higher activity, and then there is higher specific capacity.
Embodiment 2:
Step one: first, uses deionized water to clean successively by carbon cloth, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C；
Again carbon cloth by the volume ratio mix homogeneously of 1:1 and is placed in one and carries out nitration mixture process by concentrated sulphuric acid and concentrated nitric acid 24h；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put 60 DEG C of drying in baking oven；
Step 3: zinc acetate and ammonium molybdate are distributed in water respectively, make zinc acetate solution and ammonium molybdate solution mole Ratio is 1:9, under stirring condition, is added dropwise in zinc acetate solution by ammonium molybdate solution, complete to ammonium molybdate solution After addition, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Hydro-thermal reaction 20h is carried out at 160 DEG C；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, does for 60 DEG C in baking oven Dry, obtain β-ZnMoO4 flexible lithium ion battery material.
Embodiment 3:
Step one: first, uses deionized water to clean successively by carbon cloth, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C；
Again carbon cloth by the volume ratio mix homogeneously of 5:1 and is placed in one and carries out nitration mixture process by concentrated sulphuric acid and concentrated nitric acid 4h；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put 60 DEG C of drying in baking oven；
Step 3: zinc chloride and sodium molybdate are distributed in water respectively, make liquor zinci chloridi and sodium molybdate solution mole Ratio is 1:8, under stirring condition, is added dropwise in liquor zinci chloridi by sodium molybdate solution, complete to sodium molybdate solution After addition, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Hydro-thermal reaction 15h is carried out at 170 DEG C；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, does for 60 DEG C in baking oven Dry, obtain β-ZnMoO4 flexible lithium ion battery material.
Embodiment 4:
Step one: first, uses deionized water to clean successively by carbon cloth, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C；
Again carbon cloth by the volume ratio mix homogeneously of 4:1 and is placed in one and carries out nitration mixture process by concentrated sulphuric acid and concentrated nitric acid 10h；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put 60 DEG C of drying in baking oven；
Step 3: zinc nitrate and ammonium molybdate are distributed in water respectively, make zinc nitrate solution and ammonium molybdate solution mole Ratio is 1:7.5, under stirring condition, is added dropwise in zinc nitrate solution by ammonium molybdate solution, complete to ammonium molybdate solution After addition, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Hydro-thermal reaction 24h is carried out at 150 DEG C；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, does for 60 DEG C in baking oven Dry, obtain β-ZnMoO4 flexible lithium ion battery material.
Embodiment 5:
Step one: first, uses deionized water to clean successively by carbon cloth, the ultrasonic 1h that embathes of acetone, and dehydrated alcohol surpasses Sound embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C；
Again carbon cloth by the volume ratio mix homogeneously of 4:1 and is placed in one and carries out nitration mixture process by concentrated sulphuric acid and concentrated nitric acid 10h；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put 60 DEG C of drying in baking oven；
Step 3: zinc acetate and sodium molybdate are distributed in water respectively, make zinc acetate solution and sodium molybdate solution mole Ratio is 1:8.5, under stirring condition, is added dropwise in zinc acetate solution by sodium molybdate solution, complete to sodium molybdate solution After addition, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Hydro-thermal reaction 10h is carried out at 180 DEG C；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, does for 60 DEG C in baking oven Dry, obtain β-ZnMoO4 flexible lithium ion battery material.

Claims (7)

1. a flexible lithium ion battery negative material β-ZnMoO4Preparation method, it is characterised in that:
Step one: carbon cloth by the volume ratio mix homogeneously of 5:1～1:1 and is placed in one by concentrated sulphuric acid and concentrated nitric acid Carry out nitration mixture process；
Step 2: the carbon cloth handled well is placed in deionized water cleaning, measures its pH value and to neutrality, carbon cloth is put Dry in baking oven；
Step 3: zinc salt and molybdate are distributed to respectively in water, the mol ratio making zinc solution and molybdate solution is 1:7～1:9, under stirring condition, is added dropwise over molybdate solution in zinc solution, adds completely to molybdate solution After entering, it is further continued for stirring 10min and obtains mixed solution；
Step 4: be placed in mixed solution by carbon cloth, transfers it in autoclave liner, after good seal Carry out hydro-thermal reaction；
Step 5: after reaction terminates, by carbon cloth deionized water and dehydrated alcohol alternately punching, is dried in baking oven, To β-ZnMoO4 flexible lithium ion battery material.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its Being characterised by: the carbon cloth that described step one uses uses deionized water to clean successively, the ultrasonic 1h that embathes of acetone is anhydrous EtOH Sonicate embathes 1h, and deionized water is ultrasonic embathes 1h, is then placed in the oven for drying of 60 DEG C.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its It is characterised by: described nitration mixture processes carbon cloth 4～24h.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its It is characterised by: it is 60 DEG C that described step 2 dries temperature.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its It is characterised by: described zinc salt is zinc nitrate, zinc acetate or zinc chloride.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its It is characterised by: described molybdate is sodium molybdate or ammonium molybdate.
Flexible lithium ion battery negative material β-ZnMoO the most according to claim 14Preparation method, its Being characterised by: described hydrothermal temperature is 150～180 DEG C, the time is 2h～24h.
CN201610073082.1A 2016-02-02 2016-02-02 Preparation method of flexible anode material beta-ZnMoO4 for lithium-ion battery Pending CN105720270A (en)

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CN106532030A (en) * 2016-12-26 2017-03-22 惠州Tcl金能电池有限公司 Calcium molybdate lithium ion battery negative electrode material and preparation method thereof
CN106602086A (en) * 2016-11-23 2017-04-26 北京化工大学 Self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode catalyst and preparation method therefor
CN107199040A (en) * 2017-07-06 2017-09-26 中国科学院福建物质结构研究所 Molybdate nano-array and its preparation method and application
CN108091850A (en) * 2017-12-12 2018-05-29 江汉大学 Flexible non-sintered carbon cloth based titanium dioxide, its preparation method and the application as lithium ion battery composite cathode
CN108365197A (en) * 2018-02-08 2018-08-03 成都理工大学 A kind of nano bar-shape zinc sulphide carbon cloth electrode, preparation method and applications
CN108511726A (en) * 2018-04-19 2018-09-07 广东工业大学 Di-iron trioxide/carbon lithium ion cell negative electrode material, preparation method and applications
CN109712818A (en) * 2019-01-04 2019-05-03 内蒙古大学 A kind of manganese-base oxide composite and flexible electrode material and preparation method thereof
CN112573573A (en) * 2020-12-04 2021-03-30 青岛科技大学 ZnMoO4Electroactive material, preparation method and application
CN112909258A (en) * 2021-02-06 2021-06-04 陕西科技大学 Flexible positive and negative electrode material for high-performance magnesium-lithium double-salt ion battery and preparation method thereof
CN114203983A (en) * 2021-11-04 2022-03-18 江苏大学 Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery

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CN106602086A (en) * 2016-11-23 2017-04-26 北京化工大学 Self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode catalyst and preparation method therefor
CN106532030B (en) * 2016-12-26 2020-03-20 惠州亿纬创能电池有限公司 Calcium molybdate lithium ion battery cathode material and preparation method thereof
CN106532030A (en) * 2016-12-26 2017-03-22 惠州Tcl金能电池有限公司 Calcium molybdate lithium ion battery negative electrode material and preparation method thereof
CN107199040A (en) * 2017-07-06 2017-09-26 中国科学院福建物质结构研究所 Molybdate nano-array and its preparation method and application
CN107199040B (en) * 2017-07-06 2020-07-31 中国科学院福建物质结构研究所 Molybdate nano array and preparation method and application thereof
CN108091850A (en) * 2017-12-12 2018-05-29 江汉大学 Flexible non-sintered carbon cloth based titanium dioxide, its preparation method and the application as lithium ion battery composite cathode
CN108365197A (en) * 2018-02-08 2018-08-03 成都理工大学 A kind of nano bar-shape zinc sulphide carbon cloth electrode, preparation method and applications
CN108511726B (en) * 2018-04-19 2020-09-11 广东工业大学 Ferric oxide/carbon lithium ion battery cathode material, preparation method and application thereof
CN108511726A (en) * 2018-04-19 2018-09-07 广东工业大学 Di-iron trioxide/carbon lithium ion cell negative electrode material, preparation method and applications
CN109712818A (en) * 2019-01-04 2019-05-03 内蒙古大学 A kind of manganese-base oxide composite and flexible electrode material and preparation method thereof
CN112573573A (en) * 2020-12-04 2021-03-30 青岛科技大学 ZnMoO4Electroactive material, preparation method and application
CN112909258A (en) * 2021-02-06 2021-06-04 陕西科技大学 Flexible positive and negative electrode material for high-performance magnesium-lithium double-salt ion battery and preparation method thereof
CN114203983A (en) * 2021-11-04 2022-03-18 江苏大学 Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery
CN114203983B (en) * 2021-11-04 2022-11-18 江苏大学 Preparation method of porous zinc molybdate/zinc oxide/graphene composite material and application of porous zinc molybdate/zinc oxide/graphene composite material to negative electrode of lithium ion battery

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Application publication date: 20160629