CN103332744B - A kind of microwave-ultraviolet that adopts prepares h-MoO 3the method of nanometer rod - Google Patents

A kind of microwave-ultraviolet that adopts prepares h-MoO 3the method of nanometer rod Download PDF

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CN103332744B
CN103332744B CN201310244777.8A CN201310244777A CN103332744B CN 103332744 B CN103332744 B CN 103332744B CN 201310244777 A CN201310244777 A CN 201310244777A CN 103332744 B CN103332744 B CN 103332744B
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moo
microwave
solution
ultraviolet
nanometer rod
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CN103332744A (en
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曹丽云
马凤兰
黄剑锋
吴建鹏
费杰
卢靖
李翠艳
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Shaanxi University of Science and Technology
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Abstract

A kind of microwave-ultraviolet that adopts prepares h-MoO 3the method of nanometer rod, joins ammonium molybdate in deionized water and obtains solution A; The pH value of regulator solution A be 0.5 ~ 2.0 solution B; Solution B to be poured in four neck round-bottomed flasks and be placed in after the reaction of microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument terminates and naturally cool to room temperature; The washing of taking-up product is placed on electric vacunm drying case inner drying and namely obtains h-MoO 3nanometer rod.The present invention expands h-MoO 3nanocrystalline synthetic technology scope; Preparation h-MoO 3nanometer rod technique is simple, and raw material is easy to get, and productive rate is higher, and reaction time is short, and cost is low; By the h-MoO of the inventive method gained 3nanometer rod is grown complete, and purity is higher, has higher oriented growth characteristic; The h-MoO that can synthesize on a large scale 3nanometer rod.

Description

A kind of microwave-ultraviolet that adopts prepares h-MoO 3the method of nanometer rod
Technical field
The present invention relates to one and prepare MoO 3the method of nanometer rod, particularly one adopts microwave-ultraviolet to prepare h-MoO 3the method of nanometer rod.
Technical background
MoO 3as a kind of important functional inorganic materials, be the core material of the device such as electrochromism, photochromic, gas-discoloration, gas sensing, intelligence camouflage, in fields such as energy-conservation, the information displaying of building and automobile and storage, environmental monitoring, foodstuffs industry, military affairs, there is great application prospect.MoO 3there is the crystalline structure that three kinds common: thermodynamically stable orthorhombic phase α-MoO 3, the monoclinic phase β-MoO of thermodynamics metastable structure 3with six side phase h-MoO 3.The h-MoO of six side's phases 3nanocrystalline due to the extensive concern that there is renewal, more superior physical and chemical activity is more and more subject to investigator.Find h-MoO 3nanocrystalline simply, synthetic method effectively and rapidly, explore h-MoO 3nanocrystalline Theory and applications in optics, electricity and catalysis all will be of practical significance more.At present about h-MoO 3nanocrystalline method is all some traditional preparation methods, as sonochemistry method, hydrothermal method etc.[S.R.Dhage, M.S.Hassan, O.Bong Yang, the Low temperature fabrication of hexagon shaped h-MoO such as S.R.Dhage 3nanorods and its phase transformation ［ J ］ .Materials Chemistry and Physics, 2009,114:511-514] ammonium molybdate, urea, sodium lauryl sulphate have been synthesized six side phase h-MoO by the method for ultrasound probe at 70 DEG C 3nanometer rod; [the Zhuangzhi Wu such as the Wu Zhuanzhi of Central South University, Dezhi Wang, Xun Liang, Aokui Sun, Ultrasonic-assisted preparation of metastable hexagonal MoO3nanorods and their transformation to microbelts [J], Ultrasonics Sonochemistry, 2011,18:288-292] by sonochemistry method with ammonium dimolybdate and hydrochloric acid for h-MoO successfully prepared by raw material 3nanometer rod.[Lei Zheng, Yang Xu, Dong Jin, and Yi Xie, the Novel Metastable Hexagonal MoO such as the Lei Zheng in Anhui nano material and nanochemistry laboratory 3nanobelts:Synthesis, Photochromic, and Electrochromic Properties [J], Chem.Mater, 2009,21:5681-5690] with Mo powder, H 2o 2and NaNO 3h-MoO has been synthesized for raw material adopts hydrothermal method to be incubated 12h at 150 DEG C 3nano belt; [A.Chithambararaj, A.Chandra Bose, the Hydrothermal synthesis of hexagonal and orthorhombic MoO such as A.Chithambararaj 3nanoparticles [J] .Journal of Alloys and Compounds, 2011,509:8105-8110] ammonium molybdate and nitric acid are also adopted water heat transfer six side phase h-MoO at 90 DEG C 3nano particle.Due to water heat transfer h-MoO 3nanocrystalline exist the shortcomings such as temperature of reaction is relatively high, long reaction time, and sonochemistry method synthesis h-MoO 3nanocrystalline existence reaction is not easy to control, have the shortcomings such as side reaction generation, so find a kind of low temperature, easily control, Fast back-projection algorithm h-MoO 3nanocrystalline method has great importance.
Summary of the invention
A kind of microwave-ultraviolet that adopts is the object of the present invention is to provide to prepare h-MoO 3the method of nanometer rod, the method equipment is simple, easily controls, and is applicable to scale operation; Simply raw materials used, can the synthesis h-MoO of low cost 3nanometer rod; By the h-MoO that preparation method of the present invention makes 3nanometer rod purity is high, and crystallization homogeneity is higher, and crystal has obvious oriented growth trend.
For achieving the above object, the preparation method that the present invention adopts is as follows:
1) by analytically pure (NH 4) 6mo 7o 244H 2it is the solution A of 0.005 ~ 0.05mol/L that O joins the concentration that deionized water for stirring obtains ammonium molybdate;
2) by solution A stirring and dissolving evenly after the pH value of regulator solution A be 0.5 ~ 2.0 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round bottom flask be equipped with are entered in microwave ultraviolet excess sound wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 40 ~ 80 DEG C, time 60 ~ 120min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, taking-up product washs the electric vacunm drying case inner drying being placed on 50 ~ 70 DEG C and namely obtains h-MoO 3nanometer rod.
Described step 2) adopt the HNO of 3 ~ 6mol/L 3the pH value of solution regulator solution A is 0.5 ~ 2.0.
The microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument of described step 3) adopts the microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument of UWave-1000 type.
The washing of described step 5) adopts deionized water and dehydrated alcohol repeated washing 3 ~ 7 times.
Useful effect: the present invention expands h-MoO 3nanocrystalline synthetic technology scope; Preparation h-MoO 3nanometer rod technique is simple, and raw material is easy to get, and productive rate is higher, and reaction time is short, and cost is low; By the h-MoO of the inventive method gained 3nanometer rod is grown complete, and purity is higher, has higher oriented growth characteristic; The h-MoO that can synthesize on a large scale 3nanometer rod.
Accompanying drawing explanation
Fig. 1 is h-MoO prepared by the inventive method 3nanocrystalline XRD figure spectrum.
Fig. 2 is h-MoO prepared by the inventive method 3the SEM photo of nanometer rod.
Embodiment
Embodiment 1:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.005mol/L;
2), after solution A stirring and dissolving is even, the HNO of 3mol/L is adopted 3the pH value of solution regulator solution A be 1.0 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 60 DEG C, time 100min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 60 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
Embodiment 2:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.01mol/L;
2), after solution A stirring and dissolving is even, the HNO of 4mol/L is adopted 3the pH value of solution regulator solution A be 1.5 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 70 DEG C, time 90min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 70 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
Embodiment 3:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.008mol/L;
2), after solution A stirring and dissolving is even, the HNO of 5mol/L is adopted 3the pH value of solution regulator solution A be 0.8 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 50 DEG C, time 120min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 50 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
Embodiment 4:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.02mol/L;
2), after solution A stirring and dissolving is even, the HNO of 6mol/L is adopted 3the pH value of solution regulator solution A be 1.5 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 60 DEG C, time 100min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 70 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
Embodiment 5:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.03mol/L;
2), after solution A stirring and dissolving is even, the HNO of 4mol/L is adopted 3the pH value of solution regulator solution A be 0.5 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 40 DEG C, time 110min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 55 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
Embodiment 6:
1) by analytical pure ammonium molybdate ((NH 4) 6mo 7o 244H 2o) joining the concentration that deionized water for stirring obtains ammonium molybdate is the solution A of 0.05mol/L;
2), after solution A stirring and dissolving is even, the HNO of 6mol/L is adopted 3the pH value of solution regulator solution A be 2.0 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round-bottomed flasks be equipped with are put into UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring);
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 80 DEG C, time 60min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open UWave-1000 type microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, take out product, namely the electric vacunm drying case inner drying adopting deionized water and dehydrated alcohol repeated washing to be placed on 65 DEG C for 3 ~ 7 times successively obtains h-MoO 3nanometer rod.
As can be seen from Figure 1, prepared h-MoO 3nanometer rod good crystallinity, purity is higher, has obvious oriented growth characteristic.The nanometer rod that as can be seen from Figure 2 prepared by present method physically well develops.

Claims (1)

1. one kind adopts microwave-ultraviolet to prepare h-MoO 3the method of nanometer rod, is characterized in that comprising the following steps:
1) by analytically pure (NH 4) 6mo 7o 244H 2it is the solution A of 0.005 ~ 0.05mol/L that O joins the concentration that deionized water for stirring obtains ammonium molybdate;
2) by solution A stirring and dissolving evenly after the pH value of regulator solution A be 0.5 ~ 2.0 solution B;
3) solution B is poured in four neck round-bottomed flasks, the four neck round bottom flask be equipped with are entered in microwave ultraviolet excess sound wave trinity synthesis extractive reaction instrument, and fix, adopt direct temperature measurement mode thermometric;
4) microwave-ultraviolet synthesis model is adopted, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, selective temperature-time service pattern, setting temperature of reaction 40 ~ 80 DEG C, time 60 ~ 120min, microwave heating time is set to 10min, the output rating of insulating process microwave is 24W, naturally cools to room temperature after reaction terminates;
5) open microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument, taking-up product washs the electric vacunm drying case inner drying being placed on 50 ~ 70 DEG C and namely obtains h-MoO 3nanometer rod;
Described step 2) adopt the HNO of 3 ~ 6mol/L 3the pH value of solution regulator solution A is 0.5 ~ 2.0;
Described step 5) washing adopts deionized water and dehydrated alcohol repeated washing 3 ~ 7 times;
Described step 3) microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument adopt the microwave ultraviolet ultrasonic wave trinity synthesis extractive reaction instrument of UWave-1000 type.
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CN103771516A (en) * 2014-01-24 2014-05-07 天津理工大学 Preparation method of hexagonal-phase molybdenum trioxide microrod
CN109052475B (en) * 2018-09-27 2020-07-21 济南大学 Rod-shaped MoO with particles loaded on surface3/ZnMoO4Method for synthesizing structure
CN110085860B (en) * 2019-04-26 2020-09-22 陕西科技大学 Preparation method of copper phosphide nanotube

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086435A (en) * 2011-11-03 2013-05-08 中国科学院兰州化学物理研究所 Preparation method of molybdenum trioxide nanorod

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086435A (en) * 2011-11-03 2013-05-08 中国科学院兰州化学物理研究所 Preparation method of molybdenum trioxide nanorod

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Morphology-controlled synthesis of Mo compounds from a nitric acid solution by the microwave heating and/or Zr-addition;Masahiko Osaka et al.;《Journal of Nuclear Materials》;20120522;第427卷;384-388 *
室温离子液体对花球状α-氧化钼微波加热合成产物结构的影响;刘志等;《材料导报》;20110331;第25卷(第3期);38-41 *
赵文彦等.辐射化学法制备纳米材料.《辐射加工技术及其应用》.兵器工业出版社,2003,191,193-194. *

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