CN102826603A - Preparation method of vanadium pentoxide nanofibers - Google Patents
Preparation method of vanadium pentoxide nanofibers Download PDFInfo
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- CN102826603A CN102826603A CN2012103522983A CN201210352298A CN102826603A CN 102826603 A CN102826603 A CN 102826603A CN 2012103522983 A CN2012103522983 A CN 2012103522983A CN 201210352298 A CN201210352298 A CN 201210352298A CN 102826603 A CN102826603 A CN 102826603A
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- Prior art keywords
- vanadium pentoxide
- nanofibers
- preparation
- nanofiber
- acid solution
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002121 nanofiber Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012265 solid product Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 3
- 230000005669 field effect Effects 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 3
- 239000011147 inorganic material Substances 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 8
- 239000013543 active substance Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 208000001308 Fasciculation Diseases 0.000 description 3
- 206010028293 Muscle contractions involuntary Diseases 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910000474 mercury oxide Inorganic materials 0.000 description 3
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- LOUBVQKDBZRZNQ-UHFFFAOYSA-M [O-2].[O-2].[OH-].O.[V+5] Chemical compound [O-2].[O-2].[OH-].O.[V+5] LOUBVQKDBZRZNQ-UHFFFAOYSA-M 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011829 room temperature ionic liquid solvent Substances 0.000 description 1
- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
一种五氧化二钒纳米纤维的制备方法，属于无机材料的制备技术领域。本发明以氧化钒粉（VO2）为原料，在硝酸溶液中通过水热反应，VO2重新结晶形成五氧化二钒纳米纤维。所制备的五氧化二钒纳米纤维长直径为10～50nm，长度为10～60μm，具有单相正交结构，结晶度好、纯度高，同一制备条件下得到的产品直径一致。本发明原料无毒无害、不需要还原剂、不需要煅烧处理，成本低，生产工艺简单，易于工业化大规模生产。所制备的五氧化二钒纳米纤维长可以用于催化剂、锂离子电池的阴极材料、电致显色、传感器，场效应晶体管、纳米刻蚀模板、电动装置等领域。
The invention discloses a method for preparing vanadium pentoxide nanofibers, belonging to the technical field of preparation of inorganic materials. The invention uses vanadium oxide powder (VO 2 ) as raw material, undergoes hydrothermal reaction in nitric acid solution, and VO 2 recrystallizes to form vanadium pentoxide nanofibers. The prepared vanadium pentoxide nanofiber has a long diameter of 10-50 nm and a length of 10-60 μm, has a single-phase orthorhombic structure, good crystallinity and high purity, and products obtained under the same preparation conditions have the same diameter. The raw material of the invention is non-toxic and harmless, does not require reducing agent, does not require calcination treatment, has low cost, simple production process, and is easy for large-scale industrial production. The prepared vanadium pentoxide nanofibers can be used in the fields of catalysts, cathode materials of lithium ion batteries, electrochromism, sensors, field effect transistors, nanometer etching templates, electric devices and the like.
Description
Technical field
The invention belongs to the preparing technical field of inorganic materials, be specifically related to the preparation method of Vanadium Pentoxide in FLAKES nanofiber.
Background technology
V
2O
5Be a kind of important inorganic materials, cause fields such as colour developing, chemical sensor at cathode material, the electricity of lithium ion battery and have broad application prospects.V
2O
5Under heating, being decomposed into oxygen and vanadium tetraoxide easily, is a kind of strong oxidizer, is prone to be reduced into various suboxides; V
2O
5Also be a kind of important catalyst, be used for inorganic and organic catalytic reaction.One-dimentional structure V
2O
5Nano wire (fiber) has unique physicochemical property; Has strong redox ability; Have big specific surface area, stronger adsorptive power, these all help the raising of its performance; Except cathode material, the electricity that can be used for lithium ion battery causes colour developing, chemical sensor and the catalyzer, also be expected to be used for fields such as transmitter, field-effect transistor, nanometer etching template, electric device.
Prepare V at present
2O
5The method of nanofiber mainly is a liquid phase method, like solvent-thermal method, electrodip process, sol-gel method etc.Hydrothermal method is wherein important a kind of method, and V generally all samples
2O
5Perhaps NH
4VO
3Be the vanadium source.As with NH
4VO
3Be raw material, add tensio-active agent P123, in aqueous hydrochloric acid, stirred 7 hours, 120 ℃ of following hydro-thermal reactions 24 hours, resulting V
2O
530 microns of nano fiber longs; Diameter 10～20nm [reference, Chunrong Xiong etc., Fabrication of Silver Vanadium Oxide and V2O5 Nanowires for Electrochromics; ACSNANO, 2 (2) 293-301 (2008)].
Another kind of V
2O
5The preparation method of nanofiber is with NH
4VO
3Be raw material, 140 ℃ of following hydrolysis under acidic conditions, the V that obtains
2O
5Nano fiber long 10 μ m; Diameter is 100n [reference; Ning Ding etc., Hydrothermal Growth and Characterization of Nanostructured Vanadium-Based Oxides, Crystal Growth & Design; CRYSTAL GROWTH & DESIGN, 9 (4) 1723-1728 (2009)].
In addition with business-like V
2O
5Powder is a raw material, adds tensio-active agent TritonX-100, supersound process 20 minutes, 170 ℃ of following hydro-thermal reactions then, drying, 400 ℃ of following roastings, gained V
2O
520 microns of nano fiber longs, diameter 50-300nm.This preparation process is not having can not to generate V under the tensio-active agent
2O
5Nanofiber.[reference, Shu-Lei Chou etc., High Capacity, Safety, and Enhanced Cyclability of Lithium Metal, Battery Using a V
2O
5NanomaterialCathode and Room Temperature Ionic Liquid Electrolyte, CHEM.MATER., 20,7044-7051 (2008)]
But above-mentioned liquid phase method prepares V
2O
5The process of nanofiber is complicated, need to add the tensio-active agent of mass expensive, and the nanowire diameter that generates is much in 100nm more.
Summary of the invention
The present invention provides a kind of preparation method of more simple Vanadium Pentoxide in FLAKES nanofiber.The present invention directly prepares the Vanadium Pentoxide in FLAKES nanofiber with commercial hypovanadic oxide powder in hydro-thermal reaction under person's acidity.Prepared Vanadium Pentoxide in FLAKES nanofiber diameter is about 10～50nm, and long 10～60 μ m are single-phase orthohormbic structure, better crystallinity degree, purity height, and the shape of product that obtains under the same preparation condition is consistent.
Technical scheme of the present invention is following:
A kind of preparation method of Vanadium Pentoxide in FLAKES nanofiber may further comprise the steps:
Step 1: preparation salpeter solution.In deionized water, add salpeter solution, be mixed with the salpeter solution that concentration is 0.01mol/L～2.0mol/L.
Step 2: the salpeter solution that step 1 is prepared is transferred to have in the teflon-lined water heating kettle, adds VO then
2Powder, VO
2The powder add-on is 2g/L～50g/L.
Step 3: hydro-thermal reaction.The reaction system that step 2 is prepared was 140～250 ℃ of following hydro-thermal reactions 10～72 hours.
Step 4: aftertreatment.Step 3 hydro-thermal reaction gained solid product is filtered, deionized water wash, 50～80 ℃ of oven dry down obtain the Vanadium Pentoxide in FLAKES nanofiber.
Cardinal principle of the present invention is with VO
2Powder is a raw material, in salpeter solution, passes through hydro-thermal reaction, VO
2Again crystallization forms the Vanadium Pentoxide in FLAKES nanofiber.
The present invention compared with prior art has following advantage:
The present invention does not need tensio-active agent, does not need calcination processing, and production technique is simple, is easy to large-scale industrialization production.The Vanadium Pentoxide in FLAKES nanowire diameter of preparation is thin, and diameter is about 10～50nm, and length is 10～60 μ m.Better crystallinity degree, purity is high, and the product diameter that obtains under the same preparation condition is consistent.Cathode material, the electricity that can be used for catalyzer, lithium ion battery cause fields such as colour developing, chemical sensor, also are hopeful to be applied to transmitter, field-effect transistor, nanometer etching template, electric device etc.
Description of drawings
Fig. 1 is the stereoscan photograph of the Vanadium Pentoxide in FLAKES nanofiber of the present invention's preparation.
Fig. 2 is the X-ray diffraction spectrum of the Vanadium Pentoxide in FLAKES nanofiber of the present invention's preparation.
Embodiment
Embodiment 1
In the teflon-lined water heating kettle, be added in the 1000ml deionized water, add salpeter solution then and be mixed with the salpeter solution that concentration is 0.01mol/L～2.0mol/L.Add 1 gram VO then
2Powder.The sealing water heating kettle, 48 hours h of 190 ℃ of following hydro-thermal reactions obtain yellow mercury oxide.With sedimentation and filtration, deionized water wash, 60 ℃ dry the back down is jonquilleous fluffy Vanadium Pentoxide in FLAKES nanofiber.It is single-phase orthohormbic structure for the X-ray diffraction spectrum proof, better crystallinity degree, and purity is high.Electron microscopic observation proves nanofiber, and diameter is 18nm, and length is 20-60 μ m, the fasciculation structure.
Embodiment 2
In the teflon-lined water heating kettle, be added in the 1000ml deionized water, add salpeter solution then and be mixed with the salpeter solution that concentration is 0.01mol/L～2.0mol/L.Add 20 gram VO then
2Powder.The sealing water heating kettle, 200 ℃ of following hydro-thermal reaction 36h obtain yellow mercury oxide.With sedimentation and filtration, deionized water wash, 60 ℃ dry the back down is jonquilleous fluffy Vanadium Pentoxide in FLAKES nanofiber.It is single-phase orthohormbic structure for the X-ray diffraction spectrum proof, better crystallinity degree, and purity is high.Electron microscopic observation proves nanofiber, and diameter is 25nm, and length is 20～60 μ m, the fasciculation structure.
Embodiment 3
In the teflon-lined water heating kettle, be added in the 1000ml deionized water, add salpeter solution then and be mixed with the salpeter solution that concentration is 0.01mol/L～2.0mol/L.Add 15 gram VO then
2Powder.The sealing water heating kettle, 180 ℃ of following hydro-thermal reactions 15 hours obtain yellow mercury oxide.With sedimentation and filtration, deionized water wash, 50 ℃ dry the back down is jonquilleous fluffy Vanadium Pentoxide in FLAKES nanofiber.It is single-phase orthohormbic structure for the X-ray diffraction spectrum proof, better crystallinity degree, and purity is high.Electron microscopic observation proves nanofiber, and diameter is 20nm, and length is 20～60 μ m, the fasciculation structure.
Claims (1)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| CN104261472A (en) * | 2014-09-22 | 2015-01-07 | 安徽工业大学 | Vanadium pentoxide nanobelt, and room-temperature synthesis method and application of vanadium pentoxide nanobelt |
| CN105382268A (en) * | 2015-09-15 | 2016-03-09 | 海南大学 | Silver-doped vanadium pentoxide nanowire, preparing method of silver-doped vanadium pentoxide nanowire and preparing method of electrochromic device |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macro inorganic semiconductor nanofiber and its preparation method and application |
| CN110804856A (en) * | 2019-10-21 | 2020-02-18 | 南通大学 | Acrylic fabric for photocatalytic degradation of reactive dyes and preparation method thereof |
| WO2020138137A1 (en) * | 2018-12-27 | 2020-07-02 | 昭和電工株式会社 | Method for purifying vanadium oxide |
| CN113481656A (en) * | 2021-06-30 | 2021-10-08 | 攀钢集团研究院有限公司 | Preparation method of high-purity vanadium pentoxide nanofiber non-woven fabric |
Citations (2)
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|---|---|---|---|---|
| CN101274777A (en) * | 2007-03-26 | 2008-10-01 | 吉首大学 | A method for extracting vanadium pentoxide from vanadium-containing liquid |
| CN102502825A (en) * | 2011-11-15 | 2012-06-20 | 华东师范大学 | A kind of bayberry shape V2O5 nanometer material and preparation method thereof |
-
2012
- 2012-09-20 CN CN2012103522983A patent/CN102826603A/en active Pending
Patent Citations (2)
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| CN101274777A (en) * | 2007-03-26 | 2008-10-01 | 吉首大学 | A method for extracting vanadium pentoxide from vanadium-containing liquid |
| CN102502825A (en) * | 2011-11-15 | 2012-06-20 | 华东师范大学 | A kind of bayberry shape V2O5 nanometer material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| KHEMCHAND DEWANGAN, ET AL.: "Synthesis and characterizaition of self-assembled nanofiber-bundles of V2O5: their electrochemical and field emission properties", 《NANOSCALE》, vol. 4, 7 December 2011 (2011-12-07) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| CN103979608B (en) * | 2014-05-22 | 2015-08-12 | 吉林大学 | A kind of preparation method of hollow core-shell Vanadium Pentoxide in FLAKES microballoon |
| CN104261472A (en) * | 2014-09-22 | 2015-01-07 | 安徽工业大学 | Vanadium pentoxide nanobelt, and room-temperature synthesis method and application of vanadium pentoxide nanobelt |
| CN105382268A (en) * | 2015-09-15 | 2016-03-09 | 海南大学 | Silver-doped vanadium pentoxide nanowire, preparing method of silver-doped vanadium pentoxide nanowire and preparing method of electrochromic device |
| WO2020138137A1 (en) * | 2018-12-27 | 2020-07-02 | 昭和電工株式会社 | Method for purifying vanadium oxide |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macro inorganic semiconductor nanofiber and its preparation method and application |
| CN110804856A (en) * | 2019-10-21 | 2020-02-18 | 南通大学 | Acrylic fabric for photocatalytic degradation of reactive dyes and preparation method thereof |
| CN113481656A (en) * | 2021-06-30 | 2021-10-08 | 攀钢集团研究院有限公司 | Preparation method of high-purity vanadium pentoxide nanofiber non-woven fabric |
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Owner name: LASER FUSION RESEARCH CENTER, CHINESE ACADEMY OF E Effective date: 20130308 |
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Effective date of registration: 20130308 Address after: 611731 Chengdu province high tech Zone (West) West source Avenue, No. 2006 Applicant after: University of Electronic Science and Technology of China Applicant after: Laser Fusion Research Center, Chinese Academy of Engineering Physics Address before: 611731 Chengdu province high tech Zone (West) West source Avenue, No. 2006 Applicant before: University of Electronic Science and Technology of China |
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Application publication date: 20121219 |