CN101880058A - Method for preparing nano strip V2O5 - Google Patents

Method for preparing nano strip V2O5 Download PDF

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Publication number
CN101880058A
CN101880058A CN 201010181326 CN201010181326A CN101880058A CN 101880058 A CN101880058 A CN 101880058A CN 201010181326 CN201010181326 CN 201010181326 CN 201010181326 A CN201010181326 A CN 201010181326A CN 101880058 A CN101880058 A CN 101880058A
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solution
preparation
nano strip
nano
temperature
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CN101880058B (en
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袁定胜
夏南南
莫珊珊
刘应亮
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Jinan University
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Jinan University
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Abstract

The invention discloses a method for synthesizing nano strip V2O5 by a low-temperature hydrothermal process. The method comprises the following steps of: (1) dissolving surfactant into secondary deionized water to obtain 0.001 to 0.01M solution 1; (2) dissolving NH4VO3 into the solution 1, and stirring the solution till dissolution to obtain 14.2 to 428mM solution 2; (3) adding a reducing agent into the solution 2 in a volume ratio of 1: 5-1: 10, stirring the solution, transferring the solution into a lining reaction kettle of polytetrafluoroethylene, performing hydrothermal reaction for 12 to 24 hours at the temperature of between 160 and 180 DEG C, and drying a reaction product to obtain NH4V4O10 sediment; and (4) thermally treating the dried sediment for 1 to 3 hours at the temperature of between 300 and 500 DEG C to obtain the nano strip V2O5. The nano strip V2O5 can be used for preparing a sensor, a spinning electronic device, a nano photo-etching template or a high-capacity electrode material.

Description

A kind of nano strip V 2O 5The preparation method
Technical field
The invention belongs to field of nano material preparation, particularly a kind of simple, low temperature hydro-thermal reaction prepares the method for nano strip Vanadium Pentoxide in FLAKES.
Background technology
Vanadium oxide is a kind of important functional material, the multivalence attitude of vanadium, its oxide compound VO xHave multi-functional oxidation reduction dependency, have widespread use aspect catalysis, electrochromism and the electrochemistry.The vanadic anhydride nanobelt is by V 2O 5The one-dimentional structure that the width that forms is even, long.Vanadium pentoxide nanometer material can be used as sensor, spin electric device and nano-photoetching template and high-capacity electrode material etc. owing to have feature on the nano material size concurrently and the characteristic of vanadic anhydride.
The barium oxide nanostructured, mainly synthetic by sol-gel, template, hydro-thermal and four kinds of methods of solvent heat.In 1885, Ditte reported first: in platinum alloy crucible, heat NH 4VO 3, subsequently with the HNO of heat 3Solution reaction, afterwards and H 2O mixes, and makes red V 2O 5Colloidal sol.Then, find again VOCl 3The aqueous solution produces V under heating condition 2O 5Colloidal sol.In addition, 800 ℃ of heating barium oxides obtain directly to produce V in the impouring water under the fused mass high temperature 2O 5Gel.The template more complicated is a masterplate to contain pore membrane mainly, synthesizes to have the nano material of ad hoc structure.Hydro-thermal and solvent heat are synthetic to be another kind of effectively synthetic method, the variation of reaction temperature and system pH, and solvent strength, the introducing of template and additive and removing, selection of reactor coefficient etc. forms the pattern with nano-scale.
The present invention uses ammonium metavanadate as the vanadium source, has realized the banded vanadic anhydride of growing nano under the lower temperature hydrothermal condition.
Summary of the invention
For the shortcoming and deficiency that remedy prior art, primary and foremost purpose of the present invention is to provide a kind of nano strip V 2O 5The preparation method; This method cost is low, and preparation technology is simple.
Another object of the present invention is to provide the nano strip V of said method preparation 2O 5
Another purpose of the present invention is to provide above-mentioned nano strip V 2O 5Application.
Purpose of the present invention is achieved through the following technical solutions: a kind of nano strip V 2O 5The preparation method, comprise following each step:
(1) tensio-active agent is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.001～0.01M;
(2) with NH 4VO 3Powder joins in step (1) the gained solution 1, is stirred to dissolving, and obtaining concentration is the solution 2 of 14.2mM～428mM;
(3) reducing agent was added in step (2) the gained solution 2 in 1: 5 by volume～1: 10, stir, change in the reactor, carry out hydro-thermal reaction 12～24h under 160 ℃～180 ℃ conditions, drying obtains NH 4V 4O 10Precipitation;
(4) dried being deposited in the air atmosphere heated 1～3h with 300 ℃～500 ℃ of temperature, get nano strip V 2O 5
The described tensio-active agent of step (1) is Pluronic P123, Pluronic F127 or cetyl trimethylammonium bromide (CTAB).
The described reductive agent of step (3) is a Virahol.
The described reactor of step (3) is the polytetrafluoroethyllining lining reactor.
The time of the described stirring of step (3) is 2～10min.
The described exsiccant temperature of step (3) is 50～100 ℃.
A kind of nano strip V according to the said method preparation 2O 5
Above-mentioned nano strip V 2O 5Be applied to prepare sensor, spin electric device, nano-photoetching template or high-capacity electrode material.
The present invention compared with prior art has following advantage: use the present invention to prepare the nano strip vanadic anhydride, carry out under the low temperature, cost is low, and preparation technology is simple, and experimental period is short, good reproducibility, and product is high temperature resistant; Because vanadium has the multivalence attitude, its oxide VO xHave multi-functional oxidation reduction dependence, have the made nano strip V of extensive use the present invention aspect catalysis, electrochromism and the electrochemistry 2O 5Can be applicable to sensor, spin electric device and the fields such as nano-photoetching template and high-capacity electrode material, and aspect preparation electricity and the optical switch huge application potential is being arranged.
Description of drawings
Fig. 1 is nano strip V 2O 5Electron scanning micrograph SEM figure; Wherein (a) is embodiment 1 gained nano strip V 2O 5SEM figure, figure (b) is embodiment 3 gained nano strip V 2O 5SEM figure, figure (c) is embodiment 4 gained nano strip V 2O 5SEM figure.
Fig. 2 is nano strip V 2O 5Cyclic voltammetry curve figure, wherein a is embodiment 1 gained nano strip V 2O 5Cyclic voltammetry curve figure, b is embodiment 3 gained nano strip V 2O 5Cyclic voltammetry curve figure, figure c be embodiment 4 gained nano strip V 2O 5Cyclic voltammetry curve figure.
Fig. 3 nano strip V 2O 5XRD figure, wherein a is embodiment 1 gained nano strip V 2O 5XRD figure, b is embodiment 3 gained nano strip V 2O 5XRD figure, c is embodiment 4 gained nano strip V 2O 5XRD figure.
Embodiment
Below in conjunction withspecific examples and drawings the present invention is described in further detail, but implementation method of the present invention is flexible, is not limited only to this routine described concrete operations mode.
Embodiment 1
(1) tensio-active agent Pluronic P123 is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.01M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is faint yellow, and obtaining concentration is the solution 2 of 14.2mM;
(3) in 36ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 10min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 24h at 160 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 60 ℃ of dryings obtain blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 2h with 400 ℃ of temperature, obtain crocus V 2O 5Material (S-1).
Product S-1 is carried out electron microscope scanning, obtain electron scanning micrograph SEM figure, shown in Fig. 1 (a), V 2O 5Nanobelt is radiation and arranges good dispersion, similar petal.
With product S-1 is working electrode, and platinized platinum is a supporting electrode, and SCE is a reference electrode, and 1MLiClO4/EC/DMC is an electrolytic solution, forms three-electrode system and carries out electrochemical property test.Cyclic voltammetry curve figure is shown in Fig. 2 a, and cyclic voltammetry scan speed is 1mV/s, and sweep interval is-1.5V～1V that single electrode is 336F/g than electric capacity.
Product S-1 is carried out X-ray diffraction measures, XRD figure shown in Fig. 3 a, in 2 θ=15.5,20.4,21.7,26.3,31.1,34.4,41.47 ° correspond respectively to V 2O 5(020), (001), (011), (110), (040), (130), (002) (JCPDS No.85-0601) diffraction crystal face.
Embodiment 2
(1) tensio-active agent Pluronic P123 is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.001M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is faint yellow, and obtaining concentration is the solution 2 of 428mM;
(3) in 32ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 2min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 12h at 180 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 50 ℃ of dryings obtain blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 2h with 400 ℃ of temperature, obtain crocus V 2O 5Material (S-2), its structure, character and pattern such as S-1 are radiation and arrange good dispersion, similar petal.Hydrothermal temperature is between 160 ℃～180 ℃ the time, the product unanimity.
Embodiment 3
(1) tensio-active agent Pluronic P123 is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.005M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is faint yellow, and obtaining concentration is the solution 2 of 30mM;
(3) in 40ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 8min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 15h at 160 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 100 ℃ of dryings get blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 3h with 300 ℃ of temperature, obtain yellow green V 3O 7H 2O material (S-3).
Product S-3 is carried out electron microscope scanning, obtain electron scanning micrograph SEM figure, shown in Fig. 1 (b), V 3O 7H 2The O nanobelt is radiation and arranges good dispersion, similar petal.
With product S-3 is working electrode, and platinized platinum is a supporting electrode, and SCE is a reference electrode, and 1MLiClO4/EC/DMC is an electrolytic solution, forms three-electrode system and carries out electrochemical property test.Cyclic voltammetry curve figure is shown in Fig. 2 b, and cyclic voltammetry scan speed is 1mV/s, and sweep interval is-1.5V～1V that single electrode is 313F/g than electric capacity.
Product S-3 is carried out X-ray diffraction measures, XRD figure shown in Fig. 3 b, in 2 θ=15.5,20.4,21.7,26.3,31.1,34.4,41.47 ° correspond respectively to V 2O 5(020), (001), (011), (110), (040), (130), (002) (JCPDS No.85-0601) diffraction crystal face.
Embodiment 4
(1) tensio-active agent Pluronic P123 is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.008M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is faint yellow, and obtaining concentration is the solution 2 of 100mM;
(3) in 20ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 5min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 18h at 160 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 80 ℃ of dryings get blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 1h with 500 ℃ of temperature, obtain Chinese red V 2O 5Material (S-4).
Product S-4 is carried out electron microscope scanning, obtain electron scanning micrograph SEM figure, shown in Fig. 1 (c), V after 500 ℃ of heat treatment 2O 5Although material also is banded, the fracture of part nanobelt is reunited.
With product S-4 is working electrode, and platinized platinum is a supporting electrode, and SCE is a reference electrode, and 1MLiClO4/EC/DMC is an electrolytic solution, forms three-electrode system and carries out electrochemical property test.Cyclic voltammetry curve figure is shown in Fig. 2 c, and cyclic voltammetry scan speed is 1mV/s, and sweep interval is-1.5V～1V that single electrode is 262F/g than electric capacity.
Since high-temperature process, V 2O 5Reuniting appears in particle, and nanobelt pattern part is destroyed, and performance changes, and reduces than electric capacity.
Product S-4 is carried out X-ray diffraction measure, XRD figure is shown in Fig. 3 c, and in 2 θ=10.5,21.4,32.3 ° correspond respectively to V 3O 7H 2O (200), (220), (401) (JCPDS No.85-2401) diffraction crystal face.
Embodiment 5
(1) tensio-active agent Pluronic F127 is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.003M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is faint yellow, and obtaining concentration is the solution 2 of 428mM;
(3) in 24ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 2min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 15h at 180 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 50 ℃ of dryings obtain blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 2h with 400 ℃ of temperature, obtain crocus V 2O 5Material (S-5) at electron microscope scanning, is radiation and arranges good dispersion, similar petal.
Embodiment 6
(1) the tensio-active agent cetyl trimethylammonium bromide is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.006M;
(2) in step (1) gained solution 1, add NH 4VO 3Powder is stirred to the solution dissolving and is orange-yellow, and obtaining concentration is the solution 2 of 200mM;
(3) in 28ml step (2) gained solution 2, add 4ml reducing agent isopropyl alcohol, behind the stirring 2min, change in the liner reactor of polytetrafluoroethylene (PTFE), keep 20h at 180 ℃, be cooled to room temperature, suction filtration, water and ethanol washing 6 times, 70 ℃ of dryings obtain blackish green NH 4V 4O 10Precipitation;
(4) with blackish green NH 4V 4O 10Be deposited in the air atmosphere and heat 1h with 300 ℃ of temperature, obtain crocus V 2O 5Material (S-6) at electron microscope scanning, is radiation and arranges good dispersion, similar petal.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (8)

1. nano strip V 2O 5The preparation method, it is characterized in that comprising following each step:
(1) tensio-active agent is dissolved in the secondary deionized water, obtaining concentration is the solution 1 of 0.001～0.01M;
(2) with NH 4VO 3Powder joins in step (1) the gained solution 1, is stirred to dissolving, and obtaining concentration is the solution 2 of 14.2mM～428mM;
(3) reducing agent was added in step (2) the gained solution 2 in 1: 5 by volume～1: 10, stir, change in the reactor, carry out hydro-thermal reaction 12～24h under 160 ℃～180 ℃ conditions, drying obtains NH 4V 4O 10Precipitation;
(4) dried being deposited in the air atmosphere heated 1～3h with 300 ℃～500 ℃ of temperature, get nano strip V 2O 5
2. preparation method according to claim 1 is characterized in that: the described tensio-active agent of step (1) is Pluronic P123, Pluronic F127 or cetyl trimethylammonium bromide.
3. preparation method according to claim 1 is characterized in that: the described reductive agent of step (3) is a Virahol.
4. preparation method according to claim 1 is characterized in that: the described reactor of step (3) is the polytetrafluoroethyllining lining reactor.
5. preparation method according to claim 1 is characterized in that: the time of the described stirring of step (3) is 2～10min.
6. preparation method according to claim 1 is characterized in that: the described exsiccant temperature of step (3) is 50～100 ℃.
7. nano strip V according to each described method preparation of claim 1～6 2O 5
8. according to the described nano strip V of claim 7 2O 5Be applied to prepare sensor, spin electric device, nano-photoetching template or high-capacity electrode material.
CN2010101813260A 2010-05-18 2010-05-18 Method for preparing nano strip V2O5 Expired - Fee Related CN101880058B (en)

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CN102351431A (en) * 2011-06-22 2012-02-15 哈尔滨工业大学 Self-assembly method for air-water interface vanadium oxide nano film
CN102515563A (en) * 2011-11-03 2012-06-27 中国科学院上海硅酸盐研究所 Organic vanadium source for preparation of vanadium dioxide intelligent temperature control film and preparation method of film
CN103241773A (en) * 2012-02-11 2013-08-14 中国科学院合肥物质科学研究院 Nano vanadium oxide and preparation method thereof
CN103531764A (en) * 2013-10-29 2014-01-22 福州大学 Sodium-ion battery positive material spherical ammonium vanadium oxide and preparation method therefor
WO2014120096A1 (en) * 2013-02-04 2014-08-07 Nanyang Technological University Method of preparing a vanadium oxide compound and use thereof in electrochemical cells
CN103985850A (en) * 2014-05-20 2014-08-13 武汉纺织大学 Method for preparing vanadium pentoxide/conductive substrate composite electrode material
CN104407483A (en) * 2014-12-25 2015-03-11 中国科学院宁波材料技术与工程研究所 Electrochromic device and preparation method and application thereof
CN104779382A (en) * 2015-02-06 2015-07-15 武汉理工大学 Three-dimensional hierarchical heterostructure nano-material, and gradient hydro-thermal preparation method and application thereof
CN106315674A (en) * 2016-08-17 2017-01-11 武汉科技大学 Feather-like niobium pentoxide nanobelt as well as preparation method and application thereof
CN107658447A (en) * 2017-09-15 2018-02-02 陕西科技大学 A kind of N doping carbon-coating cladding flower ball-shaped V2O5Preparation method
CN107779905A (en) * 2017-09-19 2018-03-09 同济大学 A kind of preparation method of vanadium oxide nanobelt
CN109678208A (en) * 2017-10-19 2019-04-26 深圳市寒暑科技新能源有限公司 A kind of hollow vanadic anhydride material and preparation method thereof for Zinc ion battery
CN110817958A (en) * 2019-10-11 2020-02-21 攀钢集团攀枝花钢铁研究院有限公司 Carbon-coated nano vanadium pentoxide lithium battery positive electrode material and liquid-phase in-situ preparation method thereof
CN110817959A (en) * 2019-11-25 2020-02-21 清华大学 V-shaped groove2O5Preparation method of nanobelt
CN110988046A (en) * 2019-10-30 2020-04-10 广州钰芯传感科技有限公司 V capable of detecting ethanol gas2O5Preparation method of nano material and application of nano material in gas sensor
CN114039044A (en) * 2021-11-16 2022-02-11 安阳工学院 Three-dimensional electrode material composed of carbon-coated nanosheets and preparation method thereof
CN114920294A (en) * 2022-05-16 2022-08-19 中南大学 Double-layer structure V 2 O 5 Nano-belt electrode material and preparation method and application thereof

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CN102351431B (en) * 2011-06-22 2013-03-13 哈尔滨工业大学 Self-assembly method for air-water interface vanadium oxide nano film
CN102351431A (en) * 2011-06-22 2012-02-15 哈尔滨工业大学 Self-assembly method for air-water interface vanadium oxide nano film
CN102515563B (en) * 2011-11-03 2014-07-16 中国科学院上海硅酸盐研究所 Organic vanadium source for preparation of vanadium dioxide intelligent temperature control film and preparation method of film
CN102515563A (en) * 2011-11-03 2012-06-27 中国科学院上海硅酸盐研究所 Organic vanadium source for preparation of vanadium dioxide intelligent temperature control film and preparation method of film
CN103241773A (en) * 2012-02-11 2013-08-14 中国科学院合肥物质科学研究院 Nano vanadium oxide and preparation method thereof
WO2014120096A1 (en) * 2013-02-04 2014-08-07 Nanyang Technological University Method of preparing a vanadium oxide compound and use thereof in electrochemical cells
US10263253B2 (en) 2013-02-04 2019-04-16 Nanyang Technological University Method of preparing a vanadium oxide compound and use thereof in electrochemical cells
CN103531764B (en) * 2013-10-29 2015-07-22 福州大学 Sodium-ion battery positive material spherical ammonium vanadium oxide and preparation method therefor
CN103531764A (en) * 2013-10-29 2014-01-22 福州大学 Sodium-ion battery positive material spherical ammonium vanadium oxide and preparation method therefor
CN103985850A (en) * 2014-05-20 2014-08-13 武汉纺织大学 Method for preparing vanadium pentoxide/conductive substrate composite electrode material
CN103985850B (en) * 2014-05-20 2016-12-07 武汉纺织大学 A kind of preparation method of vanadium pentoxide nanowires/conductive substrates combination electrode material
CN104407483A (en) * 2014-12-25 2015-03-11 中国科学院宁波材料技术与工程研究所 Electrochromic device and preparation method and application thereof
CN104779382A (en) * 2015-02-06 2015-07-15 武汉理工大学 Three-dimensional hierarchical heterostructure nano-material, and gradient hydro-thermal preparation method and application thereof
CN104779382B (en) * 2015-02-06 2017-03-22 武汉理工大学 Three-dimensional hierarchical heterostructure nano-material, and gradient hydro-thermal preparation method and application thereof
CN106315674A (en) * 2016-08-17 2017-01-11 武汉科技大学 Feather-like niobium pentoxide nanobelt as well as preparation method and application thereof
CN106315674B (en) * 2016-08-17 2017-10-27 武汉科技大学 A kind of featheriness niobium pentoxide nano band and preparation method and application
CN107658447A (en) * 2017-09-15 2018-02-02 陕西科技大学 A kind of N doping carbon-coating cladding flower ball-shaped V2O5Preparation method
CN107779905A (en) * 2017-09-19 2018-03-09 同济大学 A kind of preparation method of vanadium oxide nanobelt
CN109678208A (en) * 2017-10-19 2019-04-26 深圳市寒暑科技新能源有限公司 A kind of hollow vanadic anhydride material and preparation method thereof for Zinc ion battery
CN110817958A (en) * 2019-10-11 2020-02-21 攀钢集团攀枝花钢铁研究院有限公司 Carbon-coated nano vanadium pentoxide lithium battery positive electrode material and liquid-phase in-situ preparation method thereof
CN110988046A (en) * 2019-10-30 2020-04-10 广州钰芯传感科技有限公司 V capable of detecting ethanol gas2O5Preparation method of nano material and application of nano material in gas sensor
CN110817959A (en) * 2019-11-25 2020-02-21 清华大学 V-shaped groove2O5Preparation method of nanobelt
CN110817959B (en) * 2019-11-25 2021-02-02 清华大学 V-shaped groove2O5Preparation method of nanobelt
CN114039044A (en) * 2021-11-16 2022-02-11 安阳工学院 Three-dimensional electrode material composed of carbon-coated nanosheets and preparation method thereof
CN114039044B (en) * 2021-11-16 2023-11-17 安阳工学院 Preparation method of three-dimensional electrode material composed of carbon-coated nano sheets
CN114920294A (en) * 2022-05-16 2022-08-19 中南大学 Double-layer structure V 2 O 5 Nano-belt electrode material and preparation method and application thereof

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