CN105742591A - Carbon coated Na3VO4 composite anode material and preparation method and application thereof - Google Patents

Carbon coated Na3VO4 composite anode material and preparation method and application thereof Download PDF

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Publication number
CN105742591A
CN105742591A CN201610118659.6A CN201610118659A CN105742591A CN 105742591 A CN105742591 A CN 105742591A CN 201610118659 A CN201610118659 A CN 201610118659A CN 105742591 A CN105742591 A CN 105742591A
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sodium
distilled water
preparation
negative pole
ion battery
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倪世兵
唐俊
张继成
杨学林
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China Three Gorges University CTGU
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China Three Gorges University CTGU
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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
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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)
  • Composite Materials (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a carbon coated Na3VO4 composite anode material and a preparation method thereof. The preparation method comprises the following steps of separately placing a sodium source, a vanadium source and hexamethylenetetramine in 10ml of distilled water, and stirring the distilled water for 40 minutes so that the sodium source, the vanadium source and the hexamethylenetetramine are fully dissolved; transferring the obtained mixed solution into a lining of a hydrothermal kettle, adding the distilled water into the linear in an amount of 80% of the volume, carrying out reaction in an air blower at 120 DEGC for 24 hours, carrying out reaction in the air blower at 180 DEG C for 24-72 hours, and naturally cooling the air blower to a room temperature to obtain a reaction liquid; and adding citric acid, sucrose or glucose into the above reaction liquid, stirring the reaction liquid to obtain an intermediate product, drying the intermediate product in a drying oven at 80 DEG C for 12 hours, and carrying out calcination in a nitrogen or argon protection atmosphere at 400-600 DEG C for 5-10 hours to obtain the carbon coated Na3VO4 composite material. The material is endowed with relatively high electrochemical performance when applied as an anode material of a sodium ion battery.

Description

A kind of carbon cladding Na3VO4Composite negative pole material, preparation method and application
Technical field
The present invention relates to a kind of novel anode material of lithium-ion battery, particularly to Na3VO4/ C composite negative pole material, belongs to field of electrochemical power source.
Technical background
Lithium ion battery is the third generation small battery after nickel-cadmium cell, Ni-MH battery, because of it, to have energy density big, output voltage is high, and self discharge is little, memory-less effect, operating temperature range width (-20 DEG C～60 DEG C), cycle performance is superior, can fast charging and discharging, output is big, the advantages such as long service life have been widely used as the power supply of the mobile equipment such as notebook computer and mobile phone, occupy an leading position in current energy storage market.But due to the deficiency of the high cost of elemental lithium and lithium resource, make the future development of lithium ion battery be severely limited.
In order to meet the development need in future, the substitute finding lithium ion battery is imperative.Sodium and lithium are in same family, there are similar physicochemical properties, and sodium element is present in land and ocean in a salt form widely, extract simple, cheap, and sodium-ion battery has the operation principle identical with lithium ion, so sodium-ion battery is expected to, as desirable energy-storage battery of future generation, be used for substituting lithium ion battery.That develops high-performance sodium-ion battery it is critical only that research and development high-performance sodium ion battery electrode material.At present, reported multiple sodium-ion battery positive material, and anode material of lithium-ion battery was relatively deficient, needed expansion badly.Therefore, research and develop anode material of lithium-ion battery novel, high performance tool to be of great significance.
We are by finding in studying, Na3VO4There is storage sodium activity, it is possible to as a kind of potential anode material of lithium-ion battery.But Na3VO4Electric conductivity is poor, causes that its chemical property is undesirable.Currently, with respect to Na3VO4As anode material of lithium-ion battery research with application there is not been reported.
Summary of the invention
Based on above research background, invention one carbon cladding Na3VO4The preparation technology of composite negative pole material.By phase liquid between in the reaction introduces carbon source, make carbon source and mesophase spherule product be fully contacted, can either effectively suppress Na3VO4Reunion, be conducive to again carbon at Na3VO4Being uniformly distributed in granule.Prepared Na3VO4/ C composite shows the chemical property of excellence as sodium-ion battery negative pole.
A kind of compound anode material of lithium-ion battery involved in the present invention, this negative material is Na3VO4/ C composite, this material is graininess, average-size about 3 μm.Concrete preparation method step is as follows: be dissolved in the beaker equipped with 30ml distilled water by sodium carbonate, inclined vitriol acid ammonium and hexamethylenetetramine, makes it fully dissolve after stirring 40min；The mixed solution obtained transferred to water heating kettle liner and adds distilled water to the 80% of its volume, in 120 DEG C of bellowss, reacting 24h, in the convection oven of 180 DEG C, reacting 24h～72h afterwards again, naturally cool to room temperature and obtain reactant liquor；Adding citric acid, sucrose or glucose to the aforementioned reactant liquor obtained, stirring obtains intermediate product, after this intermediate product is dried 12h in 80 DEG C of baking ovens, calcines 5～10h and namely obtain Na in nitrogen or argon atmosphere at 400～600 DEG C3VO4/ C composite.
Described sodium carbonate or sodium acetate, inclined vitriol acid ammonium or vanadic anhydride are that 3:2 feeds intake by sodium vanadium mol ratio, and described citric acid, sucrose or glucose account for Na3VO4The 0-15% of quality.
Its principle utilizes hydro-thermal reaction to prepare liquid phase presoma exactly, is strengthened the Homogeneous phase mixing of organic carbon source and precursor molecule by liquid phase, then passes through high temperature sintering, makes mesophase spherule product generate Na3VO4While realize in-situ carburization.In the process, in-situ carburization can effectively suppress Na3VO4Reunion, be obviously improved material conductivity simultaneously.
Na involved in the present invention3VO4/ C anode material of lithium-ion battery and preparation method thereof has following outstanding feature:
(1) synthesis technique is simple, and mesophase spherule is liquid phase, and uniformity is good；
(2) materials synthesis is easily operated, reproducible, and cost is low；
(3) Na prepared by3VO4Na in/C3VO4Uniform with C compound, Na3VO4/ C is graininess, and mean diameter is about 3 μm；
(4) Na obtained by the present invention3VO4/ C composite is used as anode material of lithium-ion battery and has higher capacity, relatively low charge and discharge platform and good cycle performance.
Accompanying drawing illustrates:
The XRD figure spectrum of sample prepared by Fig. 1 embodiment 1.
The SEM figure of sample prepared by Fig. 2 embodiment 1.
Charge and discharge curve chart (a) of sample first three time prepared by Fig. 3 embodiment 1 and cycle performance figure (b).
Charge and discharge curve chart (a) of sample first three time prepared by Fig. 4 embodiment 2 and cycle performance figure (b).
Charge and discharge curve chart (a) of sample first three time prepared by Fig. 5 embodiment 3 and cycle performance figure (b).
Detailed description of the invention:
Embodiment 1
Materials synthesis step is as follows:
1) sodium carbonate and inclined vitriol acid ammonium are weighed 3mmol and 2mmol respectively according to mol ratio 3:2 and be dissolved in equipped with in A, B beaker of 10ml distilled water, and on magnetic stirring apparatus, stir 40min make it fully dissolve；
2) weigh 5mmol hexamethylenetetramine and be dissolved in equipped with in the C beaker of 10ml distilled water, by step 1) in B, C beaker solution be transferred in A beaker, on magnetic stirring apparatus, stir 40min obtain the solution of color even；
3) by step 1), 2) in the color even solution that obtains transfer in 50ml water heating kettle liner, and add distilled water to the 80% of its volume, in 120 DEG C of convection oven, react 24h, then in 180 DEG C of convection oven, react 24～72h, naturally cool to room temperature；
4) to step 3) in add theoretical carbon content in the product that obtains be the citric acid of 10%；
5) by step 4) intermediate product that is obtained by reacting 12h in 80 DEG C of baking ovens dries, and in nitrogen protection atmosphere, at 550 DEG C, calcining knot 5h obtains carbon cladding Na3VO4Composite.
By prepared Na3VO4Sample carries out XRD test, as shown in Figure 1.Figure is positioned at 20.2 °, 23.4 °, 33.2 °, 39.1 °, 41.1 °, 47.7 °, 51.5 °, 53.8 °, 59.1 ° and 53.3 ° respectively with Na3VO4(111) (200) (220) (311) (222) (400) (331) (420) (422) (511) crystal face corresponding, test result shows, prepared sample is Na3VO4, corresponding to XRD card JCPDS, no.27-0827.The pattern of prepared sample is via sem analysis, as in figure 2 it is shown, prepared sample is in granular form, and average-size about 3 μm.The material of embodiment 1 gained is made battery as follows: by prepared Na3VO4Sample mixes by weight the ratio for 8:1:1 with acetylene black and Kynoar, makes slurry with N-first class ketopyrrolidine for solvent, is coated on the Copper Foil of 10 μ m thick, dried at 60 DEG C, is cut into the disk of 14mm, vacuum drying 12h at 120 DEG C.With metallic sodium sheet for electrode, GradeGF/D is barrier film, is dissolved with NaPF6(1mol/L) solution of EC+DEC (volume ratio is 1:1) is electrolyte, is assembled into CR2025 type battery in the glove box of argon shield.Set of cells stands 8h after installing, then carries out constant current charge-discharge test with CT2001A battery test system, and test voltage is 3～0.02V.Fig. 3 is prepared Na3VO4The charge and discharge specific capacity first that granule shows as anode material of lithium-ion battery respectively 233.2,420mAh/g, after 100 circulations charge and discharge specific capacity respectively 158,159.6mAh/g, it is shown that well stable circulation performance.
Embodiment 2
Materials synthesis step is as follows:
1) sodium acetate and ammonium metavanadate are weighed 6mmol and 2mmol respectively according to mol ratio 3:1 and be dissolved in equipped with in A, B beaker of 10ml distilled water, and on magnetic stirring apparatus, stir 20min make it fully dissolve；
2) weigh 5mmol hexamethylenetetramine and be dissolved in equipped with in the C beaker of 10ml distilled water, by step 1) in A, B beaker solution be transferred in C beaker, on magnetic stirring apparatus, stir 40min obtain the solution of color even；
3) by step 1), 2) in the color even solution that obtains transfer in 50ml water heating kettle liner, and add distilled water to the 80% of its volume, in 120 DEG C of convection oven, react 24h, then in the convection oven of 180 DEG C, react 24～72h, naturally cool to room temperature；
4) to step 3) in add theoretical carbon content in the product that obtains be the glucose of 10%；
5) by step 4) intermediate product that is obtained by reacting 12h in 80 DEG C of baking ovens dries, sinters 5h and obtain carbon cladding Na in nitrogen protection atmosphere at 550 DEG C3VO4Composite.
The material of embodiment 2 gained is made battery by the method described in embodiment 1.Fig. 4 is prepared carbon cladding Na3VO4Composite is as the chemical property figure of anode material of lithium-ion battery.Charge and discharge specific capacity first respectively 195.3,315.6mAh/g, after 100 circulations charge and discharge specific capacity respectively 145.2,145.8mAh/g.Show good chemical property.
Embodiment 3
Materials synthesis step is as follows:
1) sodium acetate and vanadic anhydride ammonium are weighed 6mmol and 1mmol respectively according to mol ratio 6:1 and be dissolved in equipped with in A, B beaker of 10ml distilled water, and on magnetic stirring apparatus, stir 20min make it fully dissolve；
2) weigh 5mmol hexamethylenetetramine and be dissolved in equipped with in the C beaker of 10ml distilled water, by step 1) in A, B beaker solution be transferred in C beaker, on magnetic stirring apparatus, stir 40min obtain the solution of color even；
3) by step 1), 2) in the color even solution that obtains transfer in 50ml water heating kettle liner, and add distilled water to the 80% of its volume, in 120 DEG C of convection oven, react 24h, then in the convection oven of 180 DEG C, react 24～72h, naturally cool to room temperature；
4) to step 3) in add theoretical carbon content in the product that obtains be the sucrose of 10%；
5) by step 4) intermediate product that is obtained by reacting 12h in 80 DEG C of baking ovens dries, sinters 5h and obtain carbon cladding Na3VO in nitrogen protection atmosphere at 550 DEG C4Composite.
The material of embodiment 3 gained is made battery by the method described in embodiment 1.Fig. 5 is prepared carbon cladding Na3VO4Composite is as the chemical property figure of anode material of lithium-ion battery.Charge and discharge specific capacity first respectively 176.8,366.6mAh/g, after 100 circulations charge and discharge specific capacity respectively 132.9,133.2mAh/g.Show good chemical property.

Claims (4)

1. a carbon cladding Na3VO4Composite negative pole material, it is characterised in that Na3VO4Compound uniform with C, and, C is coated on Na3VO4Surface, this negative material is graininess, and average-size is less than 3 μm.
2. a carbon cladding Na3VO4The preparation method of composite negative pole material, it specifically comprises the following steps that
(1) sodium carbonate or sodium acetate, inclined vitriol acid ammonium or vanadic anhydride, hexamethylenetetramine are respectively placed in the beaker equipped with 10ml distilled water, after stirring 40min, make it fully dissolve；
(2) solution obtained in step (1) is transferred in water heating kettle liner, add distilled water to the 80% of its volume, in 120 DEG C of convection oven, react 24h, afterwards again at the temperature of 180 DEG C, convection oven is reacted 24h～72h, naturally cools to room temperature and obtain reactant liquor；
(3) reactant liquor obtained in step (2) adds citric acid, sucrose or glucose; stirring obtains intermediate product; after this intermediate product is dried 12h in 80 DEG C of baking ovens, in nitrogen or argon atmosphere, at 400～600 DEG C, calcine 5～10h namely obtain Na3VO4/ C sodium-ion battery composite negative pole material.
3. carbon according to claim 2 cladding Na3VO4The preparation method of composite negative pole material, it is characterised in that sodium source, vitriol source mol ratio be 3:2, described citric acid, sucrose or glucose phosphorus content account for Na3VO4The 0-15% of quality.
4. the carbon cladding Na described in any one of claim 1-33VO4Composite negative pole material application on sodium-ion battery.
CN201610118659.6A 2016-03-02 2016-03-02 Carbon coated Na3VO4 composite anode material and preparation method and application thereof Pending CN105742591A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106328918A (en) * 2016-11-04 2017-01-11 中南大学 NiTiO3/C compound material for sodium-ion battery, preparation method and application
CN107293722A (en) * 2017-07-10 2017-10-24 三峡大学 A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof
CN107394147A (en) * 2017-07-10 2017-11-24 三峡大学 A kind of NaVPO4F/C sodium ion anode composites and preparation method thereof
CN107482179A (en) * 2017-07-10 2017-12-15 三峡大学 A kind of anode material for lithium-ion batteries Na without lithium3V2(PO4)3/ C and preparation method thereof
CN107492635A (en) * 2017-07-10 2017-12-19 三峡大学 A kind of compound sodium-ion battery positive material Na3V2(PO4)3/ C and preparation method thereof
CN107492656A (en) * 2017-07-10 2017-12-19 三峡大学 A kind of self-supporting NaVPO4F/C sodium ion anode composites and preparation method thereof
CN112186168A (en) * 2020-10-10 2021-01-05 宁波大学 Zinc ion battery electrode material and preparation method and application thereof

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WO2014153534A1 (en) * 2013-03-21 2014-09-25 University Of Maryland, College Park Ion-conducting batteries with solid state electrolyte materials
CN104201363A (en) * 2014-07-01 2014-12-10 三峡大学 Carbon-coated Li3VO4 lithium ion battery anode material and preparation method thereof
CN104409698A (en) * 2014-11-14 2015-03-11 三峡大学 Composite lithium ion battery anode material and preparation method thereof
CN104466178A (en) * 2014-12-05 2015-03-25 武汉理工大学 Hierarchical mesoporous sodium vanadate bent nanowire as well as preparation method and application thereof

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CN102916185A (en) * 2012-10-23 2013-02-06 台塑生医科技股份有限公司 Preparation method and applications of LVP/C (lithium vanadium phosphate/carbon) composite material
WO2014153534A1 (en) * 2013-03-21 2014-09-25 University Of Maryland, College Park Ion-conducting batteries with solid state electrolyte materials
CN104201363A (en) * 2014-07-01 2014-12-10 三峡大学 Carbon-coated Li3VO4 lithium ion battery anode material and preparation method thereof
CN104409698A (en) * 2014-11-14 2015-03-11 三峡大学 Composite lithium ion battery anode material and preparation method thereof
CN104466178A (en) * 2014-12-05 2015-03-25 武汉理工大学 Hierarchical mesoporous sodium vanadate bent nanowire as well as preparation method and application thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106328918A (en) * 2016-11-04 2017-01-11 中南大学 NiTiO3/C compound material for sodium-ion battery, preparation method and application
CN107293722A (en) * 2017-07-10 2017-10-24 三峡大学 A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof
CN107394147A (en) * 2017-07-10 2017-11-24 三峡大学 A kind of NaVPO4F/C sodium ion anode composites and preparation method thereof
CN107482179A (en) * 2017-07-10 2017-12-15 三峡大学 A kind of anode material for lithium-ion batteries Na without lithium3V2(PO4)3/ C and preparation method thereof
CN107492635A (en) * 2017-07-10 2017-12-19 三峡大学 A kind of compound sodium-ion battery positive material Na3V2(PO4)3/ C and preparation method thereof
CN107492656A (en) * 2017-07-10 2017-12-19 三峡大学 A kind of self-supporting NaVPO4F/C sodium ion anode composites and preparation method thereof
CN107492656B (en) * 2017-07-10 2019-12-06 三峡大学 Self-supporting NaVPO4F/C sodium ion composite anode and preparation method thereof
CN107293722B (en) * 2017-07-10 2019-12-06 三峡大学 self-supporting NaVPO4F/C composite lithium ion battery anode and preparation method thereof
CN107492635B (en) * 2017-07-10 2020-06-02 三峡大学 Composite positive electrode material Na of sodium-ion battery3V2(PO4)3/C and preparation method thereof
CN107482179B (en) * 2017-07-10 2020-06-02 三峡大学 Lithium-free lithium ion battery cathode material Na3V2(PO4)3/C and preparation method thereof
CN112186168A (en) * 2020-10-10 2021-01-05 宁波大学 Zinc ion battery electrode material and preparation method and application thereof
CN112186168B (en) * 2020-10-10 2021-10-19 宁波大学 Zinc ion battery electrode material and preparation method and application thereof

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Application publication date: 20160706