CN1522964A - Vanadium oxide nanometer tube adulterated with metal cation and preparation method thereof - Google Patents
Vanadium oxide nanometer tube adulterated with metal cation and preparation method thereof Download PDFInfo
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- CN1522964A CN1522964A CNA031253857A CN03125385A CN1522964A CN 1522964 A CN1522964 A CN 1522964A CN A031253857 A CNA031253857 A CN A031253857A CN 03125385 A CN03125385 A CN 03125385A CN 1522964 A CN1522964 A CN 1522964A
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Abstract
The present invention relates to a metal cation doped vanadium oxide nano tube. Said tube is prepared by adopting rheological phase reaction and self-assembly process combined method. Said method includes the following steps: mixing the vanadium oxide powder with oxide powder of any metal selected from Cu, Ag, Cr, Mo, W, La, Ce, Pr and Nd for doping (doping quantity is 0.1-4 mol% of vanadium oxide) and aliphatic amine whose carbon atomicity is 4-22 or aromatic amine surfactant whose carbon atomicity is 14-20 according to mole ratio of 2:1, stirring for 1 hr in deionized water medium, stirring and ageing for 48 hr to form rheological product, moving said rheological product into stainless reactor with teflon lining bottom, making hydrothermal reaction for 6-8 days in water 180 deg.C, water-washing and filtering for 3 times, drying at 80 deg.C so as to obtain the invented product.
Description
Technical field
The present invention relates to a kind of combining with self-assembling technique and synthesize method, metal nanometer material and the field of nanometer technology of metallic cation doped vanadium oxide nanotube by rheological phase reaction.
Background technology
The 1-dimention nano tube material produces the physical and chemical performance of many excellences thus because having significant anisotropism structure and inherent quantum confinement, peculiar 4 the different contact areas of while nanotube, be between inwall, outer wall, nanometer pipe end and wall layers, for its structural modification and performance optimization provide may, thereby attracted numerous scholars' research interest.The barium oxide nanotube is the novel material that broad prospect of application is arranged in fields such as electrochemistry, photoelectron and catalyzer that just grows up after carbon nanotube.Yet the synthetic of barium oxide nanotube mainly uses the organometallics of vanadium to be raw material, causes the Costco Wholesale height, and less to its modification research.Thereby study a kind of cost is low, controllability is good metallic cation doped vanadium oxide nanotube and preparation method thereof and be of great importance.
Summary of the invention
Problem to be solved by this invention provide a kind of with low cost, controllability good, metallic cation doped vanadium oxide nanotube and preparation method thereof.
Technical scheme provided by the invention is: a kind of barium oxide nanotube, be characterized in being doped with in this nanotube the oxide powder that is selected from any metal in copper, silver, chromium, molybdenum, tungsten, lanthanum, cerium, praseodymium, the neodymium, its doping is 0.1～4mol% of barium oxide.
Preparation method's step of metallic cation doped vanadium oxide nanotube of the present invention is:
(1) with barium oxide and be used for the adulterated oxide powder that is selected from copper, silver, chromium, molybdenum, tungsten, lanthanum, cerium, praseodymium, any metal of neodymium and carbonatoms is 14～20 an aromatic amine tensio-active agent in 4～22 aliphatic amide or the carbonatoms, by 2: 1 molar ratio ingredient;
(2) with the batching of step (1) magnetic agitation 0.5～1.5 hour in deionized water medium, stir ageing and form rheology attitude product more than 48 hours;
(3) the rheology attitude product that step (2) is obtained moves in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, and is extremely complete in 180 ℃ of reactions hydro-thermal reaction under the pressure that rises;
(4) behind the hydro-thermal reaction product that step (3) obtained washing filter 23～4 time, more than 12 hours, can obtain metallic cation doped vanadium oxide nanotube product in 80 ℃ of oven dry.
Described neutral surface active agent is any in cetylamine, n-Laurylamine, the 3-phenylpropylamine.
The described hydro-thermal reaction time is 6～8 days.
The present invention combines with self-assembling technique by rheological phase reaction, with the inorganic vanadium compound is the vanadium source, blended metal oxide is a reaction medium with the deionized water, by the barium oxide nanotube of solid solution doping principle synthetic modification modification, preparation technology is very simple, low for equipment requirements, favorable reproducibility, controllable degree height, meet environmental requirement, and greatly reduce synthetic cost.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 product
Fig. 2 (a) and (b) are respectively the SEM figure and the HRTEM figure of embodiment 1 product
Fig. 3 (a) and (b) are respectively the FTIR figure and the Raman figure of embodiment 1 product
The XRD of synthetic product shown in Figure 1 schemes the position of each diffraction maximum and relative intensity and all matches with the Performance of Vanadium Oxide Nanotubes collection of illustrative plates of bibliographical information, shows that product is the Performance of Vanadium Oxide Nanotubes of mixing copper. D value corresponding to the strongest diffraction maximum is 3.42nm, and the interlamellar spacing that the nanotube walls oxide is described is 3.42nm.
Fig. 2 illustrates that product mainly is comprised of the Performance of Vanadium Oxide Nanotubes that mixes, and the nanometer pipe range is 1～5 μ m, and diameter is 30～100nm. Nanotube walls is made of 3～10 VOx layers, and interlamellar spacing is 2.90nm, and less than the test result of XRD, this deviation may cause the part of interlayer template molecule structure to be reset owing to electron beam irradiation.
Fig. 3 explanation: Raman and FTIR spectrum have reflected the flexible or flexural vibrations of V (Cu)-O, the lattice vibration of stratiform micro-structural and the organic group vibration of template.
Embodiment
Embodiment 1:(1) with V
2O
5(copper of doping 1mol%) and the mol ratio proportioning of cetylamine by 2: 1; (2) the batching magnetic agitation in deionized water medium with step (1) stirred ageing and forms lurid rheology attitude product more than 48 hours after 1 hour; (3) above-mentioned rheology attitude product is moved in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, hydro-thermal reaction is 6～8 days under the pressure that 180 ℃ of reactions rise certainly; (4) behind the hydro-thermal reaction product that step (3) is obtained, washing filtering 3～4 times,, can obtain mixing the black barium oxide nanotube product of copper in 80 ℃ of oven dry 12 hours.
Analytical test shows (seeing accompanying drawing), and product mainly is made up of the vanadium oxidation nanometer pipe of mixing copper, and the nanometer pipe range is 1～5 μ m, and diameter is 30～100nm.Nanotube walls is made of 3～10 V (Cu) Ox layer, and interlamellar spacing is 3.42nm (according to an XRD analysis).Raman and FTIR spectrum have reflected the flexible or flexural vibration of V (Cu)-O, the lattice vibration of stratiform microstructure and the organic group vibration of template.
Embodiment 2～embodiment 7
| Raw material | Doped element/doping (mol%) | Hydro-thermal time/sky | |
| Embodiment 2 | ????V 2O 5+ n-Laurylamine | ????Mo/0.1 | ????6 |
| Embodiment 3 | ????V 2O 5+ n-Laurylamine | ????Cu/1 | ????7 |
| Embodiment 4 | ????V 2O 5+ n-Laurylamine | ????Ce/2 | ????7 |
| Embodiment 5 | ????V 2O 5+ 3-phenylpropylamine | ????Mo/4 | ????7 |
| Embodiment 6 | ????V 2O 5+ n-Laurylamine | ????Nd/0.1 | ????8 |
| Embodiment 7 | ????V 2O 5+ n-Laurylamine | ????Ag/0.1 | ????7 |
Can obtain the metallic cation doped vanadium oxide nanotube product of correspondence with reference to the method for embodiment 1 by above experiment parameter.
Claims (6)
1, a kind of barium oxide nanotube is characterized in that being doped with in this nanotube the oxide powder that is selected from any metal in copper, silver, chromium, molybdenum, tungsten, lanthanum, cerium, praseodymium, the neodymium, and its doping is 0.1～4mol% of barium oxide.
2, the preparation method of the described barium oxide nanotube of claim 1 is characterized in that this method is to combine by rheological phase reaction and self assembling process to realize, the steps include:
(1) with barium oxide and to be used for adulterated copper, silver, chromium, molybdenum, tungsten, lanthanum, cerium, praseodymium, any metal oxide powder of neodymium and the carbonatoms of being selected from be that 4～22 aliphatic amide or carbonatoms are 14～20 aromatic amine tensio-active agent, by 2: 1 molar ratio ingredient;
(2) with the batching of step (1) magnetic agitation 0.5～1.5 hour in deionized water medium, stir ageing and form rheology attitude product more than 48 hours;
(3) the rheology attitude product that step (2) is obtained moves in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, and is extremely complete in 180 ℃ of reactions hydro-thermal reaction under the pressure that rises;
(4) behind the hydro-thermal reaction product that step (3) obtained washing filter 23～4 time, more than 12 hours, can obtain metallic cation doped vanadium oxide nanotube product in 80 ℃ of oven dry.
3, preparation method as claimed in claim 2 is characterized in that described tensio-active agent is a cetylamine.
4, preparation method as claimed in claim 2 is characterized in that described tensio-active agent is a n-Laurylamine.
5, preparation method as claimed in claim 2 is characterized in that described tensio-active agent is 3-phenyl third fat.
6, preparation method as claimed in claim 2 is characterized in that the described hydro-thermal reaction time is 6～8 days.
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| CN 03125385 CN1202017C (en) | 2003-09-04 | 2003-09-04 | Vanadium oxide nanometer tube adulterated with metal cation and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100347087C (en) * | 2006-06-22 | 2007-11-07 | 同济大学 | Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature |
| CN100404426C (en) * | 2006-06-14 | 2008-07-23 | 武汉理工大学 | Precursor body of Nano tube of composite oxides of multielement vanadium, and preparation method |
| CN101205084B (en) * | 2006-12-22 | 2010-09-15 | 中国科学院大连化学物理研究所 | Nano vanadium oxide and method for making same |
| 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 |
| CN101767771B (en) * | 2010-01-08 | 2013-03-20 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
| CN103208619A (en) * | 2013-03-13 | 2013-07-17 | 武汉理工大学 | Potassium ion embedded type vanadium pentoxide nanowire and preparation method thereof and application thereof |
| CN101926360B (en) * | 2009-06-18 | 2014-01-29 | 东华大学 | Novel method for preparing micro-nano multivalent silver by soft chemistry technology |
| CN109650442A (en) * | 2019-01-14 | 2019-04-19 | 北京科技大学 | A kind of preparation method of Copper-cladding Aluminum Bar barium oxide mesomorphic dusty material |
| CN110364726A (en) * | 2019-07-10 | 2019-10-22 | 瑞海泊有限公司 | The preparation method and application of double ion doping vanadic anhydride positive electrode |
| US11292962B2 (en) | 2011-09-29 | 2022-04-05 | The Research Foundation For The State University Of New York | Doped nanoparticles and methods of making and using same |
| CN115072779A (en) * | 2022-06-08 | 2022-09-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Positive electrode material V of lithium ion battery 2 O 5 Nanotube and preparation method of lithium ion button battery thereof |
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2003
- 2003-09-04 CN CN 03125385 patent/CN1202017C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404426C (en) * | 2006-06-14 | 2008-07-23 | 武汉理工大学 | Precursor body of Nano tube of composite oxides of multielement vanadium, and preparation method |
| CN100347087C (en) * | 2006-06-22 | 2007-11-07 | 同济大学 | Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature |
| CN101205084B (en) * | 2006-12-22 | 2010-09-15 | 中国科学院大连化学物理研究所 | Nano vanadium oxide and method for making same |
| CN101926360B (en) * | 2009-06-18 | 2014-01-29 | 东华大学 | Novel method for preparing micro-nano multivalent silver by soft chemistry technology |
| CN101767771B (en) * | 2010-01-08 | 2013-03-20 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
| 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 |
| 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 |
| US11292962B2 (en) | 2011-09-29 | 2022-04-05 | The Research Foundation For The State University Of New York | Doped nanoparticles and methods of making and using same |
| CN103208619A (en) * | 2013-03-13 | 2013-07-17 | 武汉理工大学 | Potassium ion embedded type vanadium pentoxide nanowire and preparation method thereof and application thereof |
| CN103208619B (en) * | 2013-03-13 | 2015-02-04 | 武汉理工大学 | Potassium ion embedded type vanadium pentoxide nanowire and preparation method thereof and application thereof |
| CN109650442A (en) * | 2019-01-14 | 2019-04-19 | 北京科技大学 | A kind of preparation method of Copper-cladding Aluminum Bar barium oxide mesomorphic dusty material |
| CN110364726A (en) * | 2019-07-10 | 2019-10-22 | 瑞海泊有限公司 | The preparation method and application of double ion doping vanadic anhydride positive electrode |
| CN110364726B (en) * | 2019-07-10 | 2023-02-17 | 瑞海泊有限公司 | Preparation method and application of dual-ion doped vanadium pentoxide cathode material |
| CN115072779A (en) * | 2022-06-08 | 2022-09-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Positive electrode material V of lithium ion battery 2 O 5 Nanotube and preparation method of lithium ion button battery thereof |
| CN115072779B (en) * | 2022-06-08 | 2023-11-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Lithium ion battery anode material V 2 O 5 Preparation method of nanotube and lithium ion button cell thereof |
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| CN1202017C (en) | 2005-05-18 |
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