CN107500355A - A kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide - Google Patents
A kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide Download PDFInfo
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- CN107500355A CN107500355A CN201710764989.7A CN201710764989A CN107500355A CN 107500355 A CN107500355 A CN 107500355A CN 201710764989 A CN201710764989 A CN 201710764989A CN 107500355 A CN107500355 A CN 107500355A
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- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
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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
- H01M4/48—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
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Abstract
The present invention relates to a kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide, belongs to inorganic material and prepares and sodium-ion battery technical field.The method of the invention is from vanadyl acetylacetonate or ammonium metavanadate as vanadium source, hydro-thermal reaction is carried out with the hydrochloric acid of certain concentration, and strictly control temperature and the time of hydro-thermal reaction, it is prepared with layering lepidocrocite type nanometer strip vanadium dioxide, low raw-material cost selected by this method, preparation process are simple to operation；In addition, during negative active core-shell material of the layering lepidocrocite type nanometer strip vanadium dioxide prepared by using as sodium-ion battery, there is high specific capacity, high coulombic efficiency and high capability retention, show good cyclical stability.
Description
Technical field
The present invention relates to a kind of preparation of vanadium dioxide, more particularly to a kind of layering lepidocrocite type nanometer strip vanadium dioxide
Preparation method, belong to inorganic material prepare and sodium-ion battery technical field.
Background technology
Lithium ion battery has high power capacity, high voltage, long lifespan and advantages of environment protection, but due to lithium on the earth
Reserves are limited, therefore, develop new secondary cell and realize that extensive energy storage is very important.Sodium element is in elemental lithium to be changed
The same main group in the periodic table of elements is learned, has similar property, similar to lithium ion battery, sodium-ion battery can also equally be made
For energy storage carrier.From the aspects of resource reserve, sodium-ion battery has an obvious advantage, and quality of the sodium element in the earth's crust is rich
Spend for 2.64%, and elemental lithium is only 0.006%.In addition, there is also substantial amounts of sodium in ocean, this make it that sodium ion is electric
The production cost in pond will be well below lithium ion battery.Therefore, sodium-ion battery be considered as replace in terms of scale energy storage lithium from
The optimal selection of sub- battery.
Begin to work out vanadium dioxide material early in the last century 80's D.W.Muphy et al., and applied
In anode material for lithium-ion batteries, show good conductance and fast lithium ion diffusion (Murphy D W,
Christian P A,DiSalvo F J,et al.Lithium incorporation by V6O13 and related
vanadium(+4,+5)oxide cathode materials[J].Journal of The Electrochemical
Society,1981,128(10):2053-2060).Because vanadium dioxide has higher theoretical specific capacity, and with two dimension
Tunnel structure, can ensure that larger-diameter sodium ion is embedded and deintercalation, it is contemplated that by vanadium dioxide materials application in sodium from
In sub- battery.Arumugam Manthiram et al have synthesized vanadium dioxide and reduction-oxidation using the hot method of microwave radiation technology solvent
Graphene nano-rod, and it is applied to sodium-ion battery negative pole, but the high rate performance of cell negative electrode material and capability retention are not
People's will to the greatest extent, and under the conditions of low potential, it is related to deintercalation process extremely complex (He G, the Li L, Manthiram of sodium ion
A.VO2/rGO nanorods as a potential anode for sodium-and lithium-ion batteries
[J].Journal of Materials Chemistry A,2015,3(28):14750-14758)；And utilize microwave radiation technology
Solvent-thermal method, which prepares vanadium dioxide, needs to be strict controlled in atmosphere and pressure in microwave, and growth conditions is more harsh.At present,
Have and directly use V2O5VO is prepared for raw material2, due to V2O5There is severe toxicity so that building-up process is more dangerous.Using other vanadic salts materials
Carry out reduction and prepare VO2When, it is also necessary to when to use hydrazine hydrate or oxalic acid, especially vanadium source be ammonium metavanadate, it is also necessary to use salt
Acid adjusts pH to 2, and the presoma being prepared also needs to just obtain VO by the high temperature anneal2, preparation process
It is complicated.
The content of the invention
In view of the problem of prior art is present, the invention provides a kind of vanadium dioxide preparation method of simple possible, choosing
Hydrochloric acid with special vanadium source and certain concentration is raw material, and layering lepidocrocite type is directly prepared using the method for hydro-thermal reaction
Nanometer strip vanadium dioxide；When the vanadium dioxide of preparation of the present invention is as anode material of lithium-ion battery, show high
Discharge capacity and cyclical stability, and remain to keep very high capability retention and coulombic efficiency after long-time circulates.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide, methods described step is as follows,
Make vanadium source dispersed in water, form suspension；It is 0.5mol/L~1.5mol/ that concentration is added into suspension
L aqueous hydrochloric acid solution, stirring until vanadium source be completely dissolved, obtain mixed solution；Mixed solution is transferred in hydrothermal reaction kettle,
At 150 DEG C~200 DEG C after hydro-thermal reaction 15h~30h, then it is placed in ageing 24h~72h at room temperature；By the mixture after ageing
Separation of solid and liquid is carried out, the solid product separated and collected is cleaned, dried, obtains the layering lepidocrocite type nanometer strip two
Vanadium oxide.
The vanadium source is vanadyl acetylacetonate or ammonium metavanadate, preferably vanadyl acetylacetonate；Vanadium source and mole of hydrochloric acid
Than for 1~2:1.
After aqueous hydrochloric acid solution being added into suspension, time preferred 0.5h~2h of stirring.
Solid product after cleaning is placed at 60 DEG C~100 DEG C and is dried in vacuo.
The layering lepidocrocite type nanometer strip vanadium dioxide prepared using the method for the invention is applied to sodium-ion battery
During negative pole, there is high specific discharge capacity and excellent cycle performance.
Beneficial effect：
(1) the invention provides a kind of new synthetic method of vanadium dioxide, the salt of special vanadium source and certain concentration is selected
Acid carries out hydro-thermal reaction, and the temperature of strict adjusting hydrothermal reaction and time, is prepared with layering lepidocrocite type nanometer
Strip vanadium dioxide, low raw-material cost, preparation process are simple to operation；
(2) the layering lepidocrocite type nanometer strip vanadium dioxide prepared by the present invention has high specific capacity, high coulomb
Efficiency and high capability retention, when being applied to sodium-ion battery as negative active core-shell material, show good high rate performance
And cycle performance, realize that extensive energy storage provides bigger possibility instead of lithium ion battery for sodium-ion battery.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of vanadium dioxide prepared by embodiment 1.
Fig. 2 is SEM (SEM) figure of vanadium dioxide prepared by embodiment 1, and multiplication factor is 10000 times.
Fig. 3 is the SEM figures of vanadium dioxide prepared by embodiment 1, and multiplication factor is 40000 times.
Fig. 4 is the CR2032 button cells that the vanadium dioxide prepared using embodiment 1 is assembled as negative active core-shell material
Cycle life figure.
Fig. 5 is that the vanadium dioxide prepared using embodiment 1 is followed as the CR2032 button cells that negative active core-shell material assembles
The ring charging and discharging curve figure of the 1st week, the 5th week, the 10th week and the 50th week.
Embodiment
The present invention is described in further detail with reference to embodiment, wherein, methods described is especially said such as nothing
Bright is conventional method, and the raw material can obtain from open commercial sources unless otherwise instructed.
In following examples：
XRD is tested：Using the Rigaku-D/max-2550pc types x-ray powder diffraction instrument of HIT to implementing
Prepared vanadium dioxide carries out material phase analysis in example, and using Cu-k as radiation source, wavelength isFiltered using Ni
Piece, Guan Liuwei 40mA, pipe pressure are 40KV, and scanning range is 10 °~90 °, and sweep speed is 8 °/min, and step-length is 0.02 °；Thing phase
Identification and crystal structure information by JADE6.0 software analysis；
SEM is tested：Using the scanning electron microscopy tester of the S-4800 models of HITACHI companies production, accelerating potential
For 20KV, the microscopic appearance of vanadium dioxide prepared in embodiment is observed；
The assembling of CR2032 type button cells：, will be negative using vanadium dioxide prepared in embodiment as negative active core-shell material
Pole active material, acetylene black and binding agent sodium carboxymethylcellulose are according to 7:2:1 mass ratio is mixed, and will be well mixed
Slurry afterwards cuts into disk, as negative pole coated on copper foil after drying；Metallic sodium piece is as positive pole, Whatman glass fibers
It is barrier film to tie up (GF/D)；Electrolyte is by NaClO4, EC (ethylene carbonate), DEC (diethyl carbonate) and FEC (fluoro ethylenes
Alkene ester) it is formulated, NaClO4Concentration is that 1.0mol/L, EC and DEC volume ratio are 1:1, FEC quality in the electrolytic solution point
Number is 5%；CR2032 type button cells are assembled into argon gas glove box；
Electrochemical property test：Using the Land cell testers of Jin Nuo Electronics Co., Ltd.s of Wuhan City production to being assembled
CR2032 type button cells tested, test voltage is 0~3V.
Embodiment 1
0.95g (3.6mmol) vanadyl acetylacetonate is dispersed in 80mL deionized water, forms suspension；Again to outstanding
2mL 1mol/L aqueous hydrochloric acid solution is added in supernatant liquid, stirs 90min, vanadyl acetylacetonate is completely dissolved, and obtains mixing molten
Liquid；Then, mixed solution is transferred in 100mL hydrothermal reaction kettles, at 180 DEG C after hydro-thermal reaction 24h, then be placed at room temperature
It is aged 30h；Eccentric cleaning is carried out to the mixture after ageing with deionized water, ethanol successively, then the solid production collected after cleaning
Thing is placed in 60 DEG C of vacuum drying chamber and is dried in vacuo 24h, obtains being layered lepidocrocite type nanometer strip vanadium dioxide.
Vanadium dioxide prepared by the present embodiment is characterized, it is as a result as follows：
XRD spectrum in Fig. 1 meets with standard card JCPDS81-2392, and it is the lepidocrocite of pure phase to illustrate prepared product
Type vanadium dioxide；Sharp peak type illustrates that prepared vanadium dioxide crystallinity is high.Knowable to SEM figures in Fig. 2 and Fig. 3,
Prepared vanadium dioxide is nanometer strip, and the interior microscopic tissue topography with layer structure.
CR2032 type button cells are assembled into using prepared vanadium dioxide as negative active core-shell material, and in 100mAh
g-1Current density under carry out constant current charge-discharge performance test, the results detailed in Fig. 4 and Fig. 5.It can be seen from the data in Fig. 4, even
Continuous circulation 200 weeks, cycle efficieny weekly all maintain more than 99%, and after circulation 200 weeks battery capability retention still
More than 80%；It can be seen from Fig. 5 test result, in addition to first week, the electric discharge ratio of the 5th week, the 10th week and the 50th week
Capacity is not decayed substantially.It follows that illustrating that battery capacity decay is slow, there is good cyclical stability.
Embodiment 2
0.47g (2mmol) ammonium metavanadate is dispersed in 80mL deionized water, forms suspension；Again into suspension
2mL 0.5mol/L aqueous hydrochloric acid solution is added, stirs 40min, ammonium metavanadate is completely dissolved, and obtains mixed solution；Then, will
Mixed solution is transferred in 100mL hydrothermal reaction kettles, at 180 DEG C after hydro-thermal reaction 24h, then is placed in and is aged 24h at room temperature；According to
It is secondary that eccentric cleaning is carried out to the mixture after ageing with deionized water, ethanol, then the solid product collected after cleaning is placed in 60 DEG C
Vacuum drying chamber in be dried in vacuo 24h, obtain be layered lepidocrocite type nanometer strip vanadium dioxide.
The XRD spectrum of vanadium dioxide prepared by the present embodiment meets with standard card JCPDS81-2392, prepared by explanation
Be pure phase lepidocrocite type vanadium dioxide；Sharp peak type illustrates that prepared vanadium dioxide crystallinity is high.According to pattern table
The SEM figures of sign understand that prepared vanadium dioxide is nanometer strip, and the interior microscopic tissue topography with layer structure.
CR2032 type button cells are assembled into using prepared vanadium dioxide as negative active core-shell material, and in 100mAh
g-1Current density under carry out constant current charge-discharge performance test, continuous circulation 200 weeks, cycle efficieny weekly all maintains 99%
More than, and after circulating 200 weeks battery capability retention still more than 80%, illustrate that battery capacity decay is slow, have
Good cyclical stability.
Embodiment 3
0.80g (3mmol) vanadyl acetylacetonate is dispersed in 80mL deionized water, forms suspension；Again to suspension
2mL 1.5mol/L aqueous hydrochloric acid solution is added in liquid, stirs 1h, vanadyl acetylacetonate is completely dissolved, and obtains mixed solution；So
Afterwards, mixed solution is transferred in 100mL hydrothermal reaction kettles, at 200 DEG C after hydro-thermal reaction 30h, then is placed in and is aged at room temperature
24h；Eccentric cleaning is carried out to the mixture after ageing with deionized water, ethanol successively, then the solid product collected after cleaning is put
24h is dried in vacuo in 80 DEG C of vacuum drying chamber, obtains being layered lepidocrocite type nanometer strip vanadium dioxide.
The XRD spectrum of vanadium dioxide prepared by the present embodiment meets with standard card JCPDS81-2392, prepared by explanation
Be pure phase lepidocrocite type vanadium dioxide；Sharp peak type illustrates that prepared vanadium dioxide crystallinity is high.According to pattern table
The SEM figures of sign understand that prepared vanadium dioxide is nanometer strip, and the interior microscopic tissue topography with layer structure.
CR2032 type button cells are assembled into using prepared vanadium dioxide as negative active core-shell material, and in 100mAh
g-1Current density under carry out constant current charge-discharge performance test, continuous circulation 200 weeks, cycle efficieny weekly all maintains 99%
More than, and after circulating 200 weeks battery capability retention still more than 80%, illustrate that battery capacity decay is slow, have
Good cyclical stability.
Embodiment 4
0.53g (2mmol) vanadyl acetylacetonate is dispersed in 80mL deionized water, forms suspension；Again to suspension
2mL 0.5mol/L aqueous hydrochloric acid solution is added in liquid, stirs 50min, vanadyl acetylacetonate is completely dissolved, and obtains mixing molten
Liquid；Then, mixed solution is transferred in 100mL hydrothermal reaction kettles, at 180 DEG C after hydro-thermal reaction 15h, then be placed at room temperature
It is aged 36h；Eccentric cleaning is carried out to the mixture after ageing with deionized water, ethanol successively, then the solid production collected after cleaning
Thing is placed in 80 DEG C of vacuum drying chamber and is dried in vacuo 24h, obtains being layered lepidocrocite type nanometer strip vanadium dioxide.
The XRD spectrum of vanadium dioxide prepared by the present embodiment meets with standard card JCPDS81-2392, prepared by explanation
Be pure phase lepidocrocite type vanadium dioxide；Sharp peak type illustrates that prepared vanadium dioxide crystallinity is high.According to pattern table
The SEM figures of sign understand that prepared vanadium dioxide is nanometer strip, and the interior microscopic tissue topography with layer structure.
CR2032 type button cells are assembled into using prepared vanadium dioxide as negative active core-shell material, and in 100mAh
g-1Current density under carry out constant current charge-discharge performance test, continuous circulation 200 weeks, cycle efficieny weekly all maintains 99%
More than, and after circulating 200 weeks battery capability retention still more than 80%, illustrate that battery capacity decay is slow, have
Good cyclical stability.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is only limited to these explanations.The present invention includes but is not limited to above example, every essence in the present invention
God and any equivalent substitution or local improvement carried out under principle, all will be regarded as within protection scope of the present invention.
Claims (6)
- A kind of 1. preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide, it is characterised in that：Methods described step is as follows,Make vanadium source dispersed in water, form suspension；It is 0.5mol/L~1.5mol/L's that concentration is added into suspension Aqueous hydrochloric acid solution, stirring until vanadium source be completely dissolved, obtain mixed solution；Mixed solution is transferred in hydrothermal reaction kettle, At 150 DEG C~200 DEG C after hydro-thermal reaction 15h~30h, then it is placed in ageing 24h~72h at room temperature；Mixture after ageing is entered Row separation of solid and liquid, the solid product separated and collected is cleaned, dried, obtain the layering lepidocrocite type nanometer strip dioxy Change vanadium；The vanadium source is vanadyl acetylacetonate or ammonium metavanadate.
- 2. a kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide according to claim 1, its feature exist In：The molal quantity in vanadium source and the mole ratio of hydrochloric acid are 1~2:1.
- 3. a kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide according to claim 1, its feature exist In：After adding aqueous hydrochloric acid solution into suspension, the time of stirring is 0.5h~2h.
- 4. a kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide according to claim 1, its feature exist In：Solid product after cleaning is placed at 60 DEG C~100 DEG C and is dried in vacuo.
- 5. a kind of preparation method for being layered lepidocrocite type nanometer strip vanadium dioxide according to claim 1, its feature exist In：The vanadium source is vanadyl acetylacetonate.
- A kind of 6. anode material of lithium-ion battery, it is characterised in that：The negative material is by any one of Claims 1-4 institute The layering lepidocrocite type nanometer strip vanadium dioxide that the method stated is prepared.
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| WO2019054395A1 (en) * | 2017-09-15 | 2019-03-21 | 三桜工業株式会社 | Positive electrode active material, method for producing positive electrode active material, positive electrode, and secondary battery |
| CN109524661A (en) * | 2018-11-06 | 2019-03-26 | 武汉理工大学 | The preembedded stratiform Mn of manganese ion0.04V2O5·1.17H2O nanobelt material and preparation method and application |
| CN109775759A (en) * | 2019-01-10 | 2019-05-21 | 广东工业大学 | A kind of vanadium dioxide anode material of lithium-ion battery and preparation method thereof |
| CN110804856A (en) * | 2019-10-21 | 2020-02-18 | 南通大学 | Acrylic fabric for photocatalytic degradation of reactive dye and preparation method thereof |
| CN114249322A (en) * | 2021-12-27 | 2022-03-29 | 北京理工大学 | Nano flower-shaped VO2（B）/V2CTxPreparation method of composite material and sodium ion battery |
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| CN110804856A (en) * | 2019-10-21 | 2020-02-18 | 南通大学 | Acrylic fabric for photocatalytic degradation of reactive dye and preparation method thereof |
| CN114249322A (en) * | 2021-12-27 | 2022-03-29 | 北京理工大学 | Nano flower-shaped VO2（B）/V2CTxPreparation method of composite material and sodium ion battery |
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