CN1262480C - Treating method for converting vanadium dioxide nano stick from B phase to M phase - Google Patents
Treating method for converting vanadium dioxide nano stick from B phase to M phase Download PDFInfo
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- CN1262480C CN1262480C CN 200410060859 CN200410060859A CN1262480C CN 1262480 C CN1262480 C CN 1262480C CN 200410060859 CN200410060859 CN 200410060859 CN 200410060859 A CN200410060859 A CN 200410060859A CN 1262480 C CN1262480 C CN 1262480C
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Abstract
The present invention relates to a processing method for converting a vanadium dioxide nanometer stick from a B phase to an M phase. In the method of the present invention, inorganic vanadium oxide powder is mixed with trimethylammonium bromide cationic surface active agents of C12 to C22 according to a molar ratio of 2/1, the mixture is stirred for 1 hour in an absolute alcohol medium by magnetic force, deionized water is added in the mixture, and rheological products are formed after 48 hours of stirring and ageing. The rheological products are moved to a stainless steel reaction vessel with a polytetrafluorethylene substrate to carry out hydrothermal reaction for 6 to 8 days under 180 DEG C, obtained products are washed by water and are filtered thrice, and a B phase vanadium dioxide nanometer stick is obtained after being baked for 12 hours under 80 DEG C. The B phase vanadium dioxide nanometer stick is arranged in a container according to a proportion that 8 to 20 ml of the absolute alcohol is added in every 0.5 mol of the B phase VO2 nanometer stick; under the violent agitation, 20 ml of water solutions of H2O2 with the concentration of 20 to 40 wt% are added in the container, and simultaneously, 0.25 mol of saturated solutions of cationic surface active agents are added in the container. After the complete reaction, the obtained products are washed by water, are filtered, and are dried in vacuum, and the M phase VO2 nanometer stick is obtained. The method of the present invention has the advantages of simple process, good repeatability and high controllable degree, and meets the environmental requirements.
Description
Technical field
The present invention relates to the vanadium dioxide nano rod by the B a kind of treatment process, metal nanometer material and the nanometer that change mutually of M in opposite directions
Technical field.
Background technology
In recent years, monodimension nanometer material has demonstrated good prospects for application in fields such as optics, electromagnetism, nanoelectronics, biological medicines, and becomes the forward position research field of nanosecond science and technology.Simultaneously as one of basic construction unit of nano-device, monodimension nanometer material has also caused scientific worker's extensive interest.We are by the rheology phase-vanadium dioxide B phase nanometer rod has been synthesized in the self-assembly method reaction, and patent applied for (application number 03125408.X).Yet explore suitable Technology, realize that the vanadium dioxide nano rod is by B phase (JCPDS card 31-1438, spacer C2/m) to M phase (JCPDS card 43-1051, spacer P2/a) transformation, and technology is simple, favorable reproducibility, controllable degree height, meet the research of environmental requirement, have important theory and be worth and realistic meaning.
Summary of the invention
Problem to be solved by this invention provides a kind of by the vanadium dioxide nano rod B treatment process that changes mutually of M in opposite directions.This method technology is simple, favorable reproducibility, and the controllable degree height meets environmental requirement.
Technical scheme provided by the invention is: a kind of vanadium dioxide nano rod be the steps include: by the B treatment process that changes mutually of M in opposite directions
1st, with inorganic vanadium oxide powder and C
12～22The trimethylammonium bromide cats product by 2: 1 molar ratio ingredient;
2nd, the batching that step 1 is obtained magnetic agitation 1 hour in anhydrous ethanol medium adds deionized water then, stirs ageing and forms lurid rheology attitude product after 48 hours;
3rd, the rheology attitude product that step 2 obtained moves in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, in 180 ℃ and reaction under the pressure that rises hydro-thermal reaction to fully;
4th, behind the hydro-thermal reaction product that step 3 obtained washing filter 23～4 time, more than 12 hours, obtain B phase hypovanadic oxide nanometer rod product in 80 ℃ of oven dry;
5th, press the B phase VO of 0.5mol
2Nanometer rod adds the ratio of 8-20ml dehydrated alcohol, with B phase VO
2Nanometer rod and dehydrated alcohol place container, under vigorous stirring, and the B phase VO of every 0.5mol
2Dripping 20ml concentration is 20～40wt%H
2O
2The aqueous solution, drip 0.25mol C simultaneously
12～22Trimethylammonium bromide, or drip 0.25mol monoalkyl polyoxyethylene based quaternary ammonium salt, or drip the saturated solution of the two alkyl polyoxyethylene based quaternary ammonium salt cationic surfactants of 0.25mol, question response is complete;
6th, the product washing filtering that step 5 is arrived, vacuum-drying promptly obtains M phase VO
2Nanometer rod.B phase VO of the present invention
2Rheology phase-the self-assembly preparation method thereof of nanometer rod is the method preparation of 03125408.X by number of patent application.Preparation process is: 1, with inorganic vanadium oxide powder and C
12～22The trimethylammonium bromide cats product, by 2: 1 molar ratio ingredient; 2, the batching that step 1 is obtained magnetic agitation 1 hour in anhydrous ethanol medium adds deionized water then, stirs ageing and forms rheology attitude product more than 48 hours; 3, the rheology attitude product that step 2 obtained moves in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, in 180 ℃ and reaction under the pressure that rises hydro-thermal reaction to fully; 4, behind the hydro-thermal reaction product that step 3 obtained washing filter 23～4 time, more than 12 hours, promptly obtain black vanadium dioxide nano rod product in 80 ℃ of oven dry.Above-mentioned 180 ℃ of hydro-thermal reaction times are 6～8 days.
The present invention is for realizing VO
2Transformation between the homophase and migration do not provide a new way, and technology is simple, favorable reproducibility, and the controllable degree height meets environmental requirement.
Description of drawings
B phase VO among Fig. 1 embodiment 1
2The XRD figure of nanometer rod
B phase VO among Fig. 2 embodiment 1
2The TEM figure of nanometer rod
M phase VO among Fig. 3 embodiment 1
2The XRD figure of nanometer rod
M phase VO among Fig. 4 embodiment 1
2The TEM figure of nanometer rod:
The position of each diffraction maximum of product X RD collection of illustrative plates and relative intensity all match with JCPDS card 31-1438 as seen from Figure 1, show that product is B phase VO2(space group is C2/m) do not have other diffraction peak of mixing substantially in the XRD collection of illustrative plates, illustrate to be purer B phase VO in the product2。
The TEM image of Fig. 2 shows that product is the bar-shaped structure of 1-dimention nano.
Fig. 3 illustrates that the position of each diffraction maximum of product X RD collection of illustrative plates after the processing and relative intensity and single JCPDS card 43-1051 match, and show that product has M phase VO2Crystal structure (space group P21/α)。
Product after the TEM image table of Fig. 4 is managed has in the open still kept the bar-shaped structure of 1-dimention nano.
Embodiment
Embodiment 1: with V
2O
5Powder and cetyl trimethylammonium bromide cats product are pressed 2: 1 molar ratio ingredient, and magnetic agitation is 1 hour in anhydrous ethanol medium, add appropriate amount of deionized water, stir ageing and form lurid rheology attitude product after 48 hours; It is moved in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, in 180 ℃ of hydro-thermal reactions after 6～8 days, carry out washing filtering 3 times, its filter cake promptly got black B phase hypovanadic oxide nanometer rod product (XRD figure of product is seen accompanying drawing 1, and TEM figure sees accompanying drawing 2) in 12 hours 80 ℃ of oven dry; Get the resulting B phase of 0.5mol VO
2Nanometer rod places the 10ml dehydrated alcohol, and under vigorous stirring, dripping 20ml concentration is 30wt%H
2O
2The aqueous solution, drip the saturated solution of 0.25mol cetyl trimethylammonium bromide (CTAB) simultaneously, question response fully after, with the products therefrom washing filtering, vacuum-drying promptly gets the black M phase VO with thermal induced phase transition performance
2Nanometer rod (XRD figure of product is seen accompanying drawing 3, and TEM figure sees accompanying drawing 4).
Tensio-active agent and H that embodiment 2～embodiment 5 is used
2O
2Concentration such as following table: each embodiment drips 20ml H
2O
2The aqueous solution, embodiment 2 adds the 8ml dehydrated alcohol, embodiment 7 adds the 20ml dehydrated alcohol, other experiment parameter is identical with embodiment 1 with method, can realize that the vanadium dioxide nano rod is by the B transformation of M phase in opposite directions.
| Embodiment number | Tensio-active agent | H 2O 2Mass percent concentration/% |
| Embodiment 2 | Cetyl trimethylammonium bromide | 40 |
| Embodiment 3 | Trimethyllaurylammonium bromide | 30 |
| Embodiment 4 | Monoalkyl polyoxyethylene quaternary ammonium salt | 30 |
| Embodiment 5 | Two alkyl polyoxyethylene bi-quaternary ammonium salts | 35 |
| Embodiment 6 | The docosyl trimethylammonium bromide | 20 |
| Embodiment 7 | The octadecyl trimethylammonium bromide | 25 |
Claims (1)
1, a kind of vanadium dioxide nano rod is characterised in that the steps include: by the B treatment process that changes mutually of M in opposite directions
1st, with inorganic vanadium oxide powder and C
12～22The trimethylammonium bromide cats product by 2: 1 molar ratio ingredient;
2nd, the batching that step 1 is obtained magnetic agitation 1 hour in anhydrous ethanol medium adds deionized water then, stirs ageing and forms lurid rheology attitude product after 48 hours;
3rd, the rheology attitude product that step 2 obtained moves in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, in 180 ℃ and reaction under the pressure that rises hydro-thermal reaction to fully;
4th, behind the hydro-thermal reaction product that step 3 obtained washing filter 23～4 time, more than 12 hours, obtain B phase hypovanadic oxide nanometer rod product in 80 ℃ of oven dry;
5th, press the B phase VO of 0.5mol
2Nanometer rod adds the ratio of 8-20ml dehydrated alcohol, with B phase VO
2Nanometer rod and dehydrated alcohol place container, under vigorous stirring, and the B phase VO of every 0.5mol
2Dripping 20ml concentration is 20～40wt%H
2O
2The aqueous solution, drip 0.25mol C simultaneously
12～22Trimethylammonium bromide, or drip 0.25mol monoalkyl polyoxyethylene based quaternary ammonium salt, or drip the saturated solution of the two alkyl polyoxyethylene based quaternary ammonium salt cationic surfactants of 0.25mol, question response is complete;
6th, the product washing filtering that step 5 is arrived, vacuum-drying promptly obtains M phase VO
2Nanometer rod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410060859 CN1262480C (en) | 2004-09-16 | 2004-09-16 | Treating method for converting vanadium dioxide nano stick from B phase to M phase |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410060859 CN1262480C (en) | 2004-09-16 | 2004-09-16 | Treating method for converting vanadium dioxide nano stick from B phase to M phase |
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| Publication Number | Publication Date |
|---|---|
| CN1587065A CN1587065A (en) | 2005-03-02 |
| CN1262480C true CN1262480C (en) | 2006-07-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9542423B2 (en) | 2012-12-31 | 2017-01-10 | Apple Inc. | Backup user interface |
| US10479900B2 (en) | 2014-08-26 | 2019-11-19 | The Research Foundation For The State University Of New York | VO2 and V2O5 nano- and micro-materials and processes of making and uses of same |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219256A (en) * | 2011-03-03 | 2011-10-19 | 刘爱林 | Thermochromic vanadium dioxide powder and preparation method thereof |
| CN103979607B (en) * | 2014-04-30 | 2015-08-12 | 中国科学院广州能源研究所 | A kind of vanadium oxide nano column array with thermocolour performance and preparation method thereof |
| CN114647123B (en) * | 2020-12-17 | 2023-12-26 | 中国科学院上海硅酸盐研究所 | Flexible electrochromic device and preparation method and application thereof |
-
2004
- 2004-09-16 CN CN 200410060859 patent/CN1262480C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9542423B2 (en) | 2012-12-31 | 2017-01-10 | Apple Inc. | Backup user interface |
| US10479900B2 (en) | 2014-08-26 | 2019-11-19 | The Research Foundation For The State University Of New York | VO2 and V2O5 nano- and micro-materials and processes of making and uses of same |
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| Publication number | Publication date |
|---|---|
| CN1587065A (en) | 2005-03-02 |
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