CN101723462A - Method for preparing fibrous MoO3 nanobelt - Google Patents
Method for preparing fibrous MoO3 nanobelt Download PDFInfo
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- CN101723462A CN101723462A CN200910218829A CN200910218829A CN101723462A CN 101723462 A CN101723462 A CN 101723462A CN 200910218829 A CN200910218829 A CN 200910218829A CN 200910218829 A CN200910218829 A CN 200910218829A CN 101723462 A CN101723462 A CN 101723462A
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Abstract
The invention discloses a method for preparing a fibrous MoO3 nanobelt, which comprises the following steps: adding Mo powder into aqueous solution of H2O2 and performing centrifugation to remove little residue to obtain solution of peroxomolybdic acid sol; pouring the solution of peroxomolybdic acid sol into a microwave hydrothermal reaction kettle and placing the microwave hydrothermal reaction kettle into an MDS-8 type temperature-control and pressure-control microwave hydrothermal reactor; selecting a temperature control mode for reaction and naturally cooling the microwave hydrothermal reaction kettle to room temperature after the reaction ends; and centrifugating a product, washing the product with deionized water and absolute ethyl alcohol or the deionized water and isopropanol respectively, finally soaking the product into the absolute ethyl alcohol and then drying the soaked product to obtain a final product, namely, the fibrous MoO3 nanobelt. In the method, an infinitely extended plane layer is quickly prepared and the layers are coupled into fibrous MoO3 nanocrystals through weak interaction; the method has the advantages of one-step reaction, no need of subsequent treatment, short preparation period, simple processing equipment and low cost; and the prepared fibrous MoO3 nanobelt has a regular shape, good dispersity and high crystallinity.
Description
Technical field
The present invention relates to a kind of MoO
3The preparation method of nano belt is specifically related to a kind of fibrous MoO
3The preparation method of nano belt.
Background technology
Transition metal oxide (WO
3, MoO
3Deng) being used as the controllable color change thin-film material widely, this material is by electronics and small cation (H
+, Li
+, Na
+, K
+Deng) dual injection, ultraviolet photon irradiation, gas molecule absorption etc., the noticeable change of characteristics such as optics, electricity can take place, therefore can be used as the core material of devices such as electrochromism, photochromic, gas-discoloration, gas sensing, intelligence camouflage, building and aspects such as energy-conservation, the information demonstration of automobile and storage, environmental monitoring, foodstuffs industry, military affairs have great application prospect.In this class transition metal oxide, MoO
3Nano thin-film is again with its advantages of higher stability, variable color rate and be subjected to paying close attention to widely.In addition, MoO
3At visible region more smooth absorption spectrum curve is arranged, thereby show than WO
3More soft neutral color has better vision aesthetic effect.
The at present existing amorphous MoO of multiple preparation
3The method of film is as vacuum vapour deposition [YAO J N, HASHIMOTO K, FUJISHIMA A.Photochromism induced in anelectrolytically pretreated MoO
3Thin film by visble light.355 (1992) 624～626], chemical Vapor deposition process [CROSS J S, SCHRADER G L.Lowpressure chemical vapor deposition of molybdenum oxide frommolybdenum hexacarbonyl and oxygen.259 (1995) 5～13], radio frequency sputtering method [SCARMINIO J, LOURENCO A, GORENSTEIN A.Electrochromism andphotochromism in amorphous molybdenum oxide films 302 (1997) 66～70], strike [Yao Jiannian, Chen Ping, the rattan island is clear. and electrolytic deposition film forming legal system is equipped with the research .14 (1996) 224～228 of molybdenum oxide film] sol-gel method [HINOKUMA K, KISHIMOTO A, KUDO T.Coloration dynamics of spin-coated MoO
3NH
2O electrochromicfilms fabricat-ed from peroxo-polymolybdate solution.141 (1994) 876～879] etc.The relative additive method of sol-gel method wherein, it is simple to have equipment, and mild condition is easy to control, and the gained film is smooth evenly, the quality advantages of higher, thereby have application prospect most.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of not only preparation cost low, and fibrous MoO simple to operate, that reaction time is short
3The preparation method of nano belt.
For achieving the above object, the technical solution used in the present invention is:
1) the metal M o powder of getting 4.5～5.5g places beaker, is 30% H with 40～50mL volume parts
2O
2The aqueous solution slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 10～20min, leave standstill back centrifugal residue of removing trace under the rotating speed of 2500～3500r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%～80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃～220 ℃, and the reaction times is controlled at 1min-120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 1h-8h under 30 ℃～120 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
A unlimited plane layer that extends is prepared by present method fast, is coupled into fibrous MoO by weak interaction between layer and the layer
3Nanocrystal.One step of reaction finishes, and does not have follow-up processing, and preparation cycle is short, and processing unit is simple, and cost is low, the fibrous MoO of gained
3Nano belt regular shape, good dispersity, crystallinity height.
Description of drawings
Fig. 1 is 140 ℃ of molybdenum trioxide nano band stereoscan photographs of preparation down.
Fig. 2 is 160 ℃ of molybdenum trioxide nano band stereoscan photographs of preparation down.
The molybdenum trioxide nano band X-Ray diffractogram of Fig. 3 for preparing under the differing temps.Among the figure a:140 ℃; B:160 ℃.
Embodiment
Embodiment 1:1) the metal M o powder (analytical pure, Tianjin chemical reagents corporation) of getting 4.5g places beaker, is 30% H with the 40mL volume parts
2O
2The aqueous solution (analytical pure, Tao Pu chemical plant, Shanghai) slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 15min, leave standstill back centrifugal residue of removing trace under the rotating speed of 2500r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃, and the reaction times is controlled at 120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 5h under 60 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
Embodiment 2:1) the metal M o powder (analytical pure, Tianjin chemical reagents corporation) of getting 4.8g places beaker, is 30% H with the 45mL volume parts
2O
2The aqueous solution (analytical pure, Tao Pu chemical plant, Shanghai) slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 17min, leave standstill back centrifugal residue of removing trace under the rotating speed of 3000r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 60%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 160 ℃, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 8h under 40 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
Embodiment 3:1) the metal M o powder (analytical pure, Tianjin chemical reagents corporation) of getting 5.2g places beaker, is 30% H with the 48mL volume parts
2O
2The aqueous solution (analytical pure, Tao Pu chemical plant, Shanghai) slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 10min, leave standstill back centrifugal residue of removing trace under the rotating speed of 3500r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 50%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 200 ℃, and the reaction times is controlled at 40min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 3h under 80 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
Embodiment 4:1) the metal M o powder (analytical pure, Tianjin chemical reagents corporation) of getting 5.5g places beaker, is 30% H with the 50mL volume parts
2O
2The aqueous solution (analytical pure, Tao Pu chemical plant, Shanghai) slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 13min, leave standstill back centrifugal residue of removing trace under the rotating speed of 2800r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 70%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 180 ℃, and the reaction times is controlled at 100min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 8h under 30 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
Embodiment 5:1) the metal M o powder (analytical pure, Tianjin chemical reagents corporation) of getting 5g places beaker, is 30% H with the 47mL volume parts
2O
2The aqueous solution (analytical pure, Tao Pu chemical plant, Shanghai) slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 20min, leave standstill back centrifugal residue of removing trace under the rotating speed of 3200r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 220 ℃, and the reaction times is controlled at 1min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 1h under 120 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
Referring to Fig. 1,2,3, comprehensive above-mentioned scanning electron microscope, X-Ray diffraction analysis show: under the condition that does not have catalyzer and organic formwork agent, with stable peroxide molybdic acid colloidal sol is that the reaction precursor body has successfully prepared molybdenum trioxide nano band degree of crystallinity height, epigranular under hydrothermal condition, single nano belt smooth surface zero defect, the direction of growth of nano belt is the c axle.140 ℃ of molybdenum trioxide nano bands that prepare down mostly are irregular band shape; 160 ℃ of molybdenum trioxide nano belt shape rules that prepare down, neat, the degree of crystallinity height.
Claims (1)
1. fibrous MoO
3The preparation method of nano belt is characterized in that:
1) the metal M o powder of getting 4.5～5.5g places beaker, is 30% H with 40～50mL volume parts
2O
2The aqueous solution slowly is added drop-wise in the beaker under the cold water water bath condition, and constantly stirs to avoid overheated;
2) wait to drip complete after, continue to stir 10～20min, leave standstill back centrifugal residue of removing trace under the rotating speed of 2500～3500r/min then, the peroxide molybdic acid sol solutions of transparent salmon;
3) above-mentioned peroxide molybdic acid sol solutions is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%～80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃～220 ℃, and the reaction times is controlled at 1min-120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is removed supernatant liquor and collecting precipitation through after centrifugal, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol then respectively, be soaked at last in the dehydrated alcohol, dry 1h-8h under 30 ℃～120 ℃ promptly gets the fibrous MoO of final product
3Nano belt.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
| CN103818959A (en) * | 2014-01-17 | 2014-05-28 | 天津大学 | Low-temperature hydrothermal preparation method of molybdenum trioxide nanorod material |
| CN104326509A (en) * | 2014-10-10 | 2015-02-04 | 昆明理工大学 | Method for microwave roasting of molybdenite concentrate to produce high-purity molybdenum oxide |
| CN104466148A (en) * | 2014-12-17 | 2015-03-25 | 桂林理工大学 | Preparation method and application of H0.6MoO3 three-dimensional nano ultrathin sheet |
| CN104659351A (en) * | 2015-02-10 | 2015-05-27 | 武汉理工大学 | Sodium ion pre-embedded MoO3 nanobelt as well as preparation method and application of sodium ion pre-embedded MoO3 nanobelt |
| MD4347C1 (en) * | 2014-07-15 | 2015-11-30 | Виорел ТРОФИМ | Gas sensor based on MoO3 |
| CN105819510A (en) * | 2016-03-23 | 2016-08-03 | 哈尔滨工业大学 | Preparation method of reduced molybdenum oxide quantum dot material |
| CN106746724A (en) * | 2017-02-21 | 2017-05-31 | 上海第二工业大学 | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof |
| CN108728674A (en) * | 2018-04-20 | 2018-11-02 | 中南大学 | A method of it extracting molybdenum from thick molybdic acid and prepares molybdenum product |
| CN109778351A (en) * | 2019-03-08 | 2019-05-21 | 东华大学 | A kind of molybdenum oxide nanofiber of macroscopic view and its preparation and application |
| CN110143614A (en) * | 2019-05-31 | 2019-08-20 | 南京倍格电子科技有限公司 | A kind of preparation method and applications of one-dimensional nano structure molybdenum oxide |
| CN110787829A (en) * | 2019-11-11 | 2020-02-14 | 深圳大学 | Mo nanosphere cocatalyst and preparation method and application thereof |
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2009
- 2009-10-30 CN CN200910218829A patent/CN101723462A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
| CN103818959A (en) * | 2014-01-17 | 2014-05-28 | 天津大学 | Low-temperature hydrothermal preparation method of molybdenum trioxide nanorod material |
| MD4347C1 (en) * | 2014-07-15 | 2015-11-30 | Виорел ТРОФИМ | Gas sensor based on MoO3 |
| CN104326509A (en) * | 2014-10-10 | 2015-02-04 | 昆明理工大学 | Method for microwave roasting of molybdenite concentrate to produce high-purity molybdenum oxide |
| CN104326509B (en) * | 2014-10-10 | 2016-06-22 | 昆明理工大学 | A kind of microwave calcining molybdenite concentrate produces the method for high-pure molybdenum oxide |
| CN104466148A (en) * | 2014-12-17 | 2015-03-25 | 桂林理工大学 | Preparation method and application of H0.6MoO3 three-dimensional nano ultrathin sheet |
| CN104659351A (en) * | 2015-02-10 | 2015-05-27 | 武汉理工大学 | Sodium ion pre-embedded MoO3 nanobelt as well as preparation method and application of sodium ion pre-embedded MoO3 nanobelt |
| CN105819510B (en) * | 2016-03-23 | 2017-04-05 | 哈尔滨工业大学 | A kind of preparation method of reduction-state molybdenum oxide quanta point material |
| CN105819510A (en) * | 2016-03-23 | 2016-08-03 | 哈尔滨工业大学 | Preparation method of reduced molybdenum oxide quantum dot material |
| CN106746724A (en) * | 2017-02-21 | 2017-05-31 | 上海第二工业大学 | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof |
| CN106746724B (en) * | 2017-02-21 | 2019-11-12 | 上海第二工业大学 | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof |
| CN108728674A (en) * | 2018-04-20 | 2018-11-02 | 中南大学 | A method of it extracting molybdenum from thick molybdic acid and prepares molybdenum product |
| CN108728674B (en) * | 2018-04-20 | 2020-08-28 | 中南大学 | Method for extracting molybdenum from crude molybdic acid and preparing molybdenum product |
| CN109778351A (en) * | 2019-03-08 | 2019-05-21 | 东华大学 | A kind of molybdenum oxide nanofiber of macroscopic view and its preparation and application |
| CN110143614A (en) * | 2019-05-31 | 2019-08-20 | 南京倍格电子科技有限公司 | A kind of preparation method and applications of one-dimensional nano structure molybdenum oxide |
| CN110787829A (en) * | 2019-11-11 | 2020-02-14 | 深圳大学 | Mo nanosphere cocatalyst and preparation method and application thereof |
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