CN103288136A - Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals - Google Patents
Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals Download PDFInfo
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- CN103288136A CN103288136A CN2012100457272A CN201210045727A CN103288136A CN 103288136 A CN103288136 A CN 103288136A CN 2012100457272 A CN2012100457272 A CN 2012100457272A CN 201210045727 A CN201210045727 A CN 201210045727A CN 103288136 A CN103288136 A CN 103288136A
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Abstract
The invention discloses a hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals, belonging to the field of inorganic non-metal materials. The method comprises the following steps: dissolving ammonium molybdate in water, adding a right amount of auxiliary reagent as a template, regulating the pH value to 0.5-1 with an HCl solution, heating the precipitate and the solution in a high-pressure kettle, and regulating the polyethyleneglycol/water proportion to prepare molybdenum dioxide nano structures in different shapes. The method has the advantages of simple technique and simple operation steps; the product has the advantages of controllable shape, high purity and low cost, and can implement mass synthesis; and thus, the invention has obvious economic benefit and social benefit.
Description
Technical field
The present invention relates to the hydrothermal synthesis method of the controlled molybdenum dioxide sub-micron crystal of a kind of pattern, belong to field of inorganic nonmetallic material.
Background technology
The molybdenum dioxide nano material has important application at aspects such as catalyzer, sensor, photochromic, electrochromism, record disc and field emmision materials.These special performances that the molybdenum dioxide nano material has and the size of its structure, pattern and particle diameter etc. have close relationship.Therefore, the preparation of special construction and pattern molybdenum dioxide and property research become the extremely content of people's concern.
The synthetic method of molybdenum dioxide nano particle relates generally to the physical method of thermal evaporation, condensation or the decomposition of reactant under the hot conditions, and also less relatively about the report of liquid phase chemical synthetic route.Hydro-thermal is synthetic to have lower synthesis temperature, and product does not need high-temperature calcination, and therefore the agglomeration traits that can avoid high temperature to bring becomes a kind of important method of synthesis of nano powder, is particularly suitable for extensive synthetic.But, also few about the research of the synthetic molybdenum dioxide nano-powder of hydro-thermal at present.The method of hydrothermal method synthesis of nano molybdenum dioxide particle needs auxiliary reagent as pattern and the size of template control target product usually, and template commonly used has hexadecyl trimethyl ammonium bromide (CTAB), carboxymethyl cellulose (CMC) etc.But these template can not satisfy the needs of control molybdenum dioxide pattern and size fully.
The invention provides the novel method for synthesizing of the controlled molybdenum dioxide sub-micron crystal of a kind of pattern, (PEG) 400 is different with water volume ratio for the regulation and control polyoxyethylene glycol, and the product pattern is by band shape → band shape+spherical → spherical differentiation.
Summary of the invention
The invention provides the hydrothermal synthesis method of the controlled molybdenum dioxide sub-micron crystal of a kind of pattern, the present invention adopts following technical scheme:
(1) ammonium molybdate is soluble in water, in addition an amount of polyoxyethylene glycol (PEG) 400 template are added to the water, the two certain proportion is mixed and stirring;
(2) the pH value with HCl solution regulator solution is between the 0.5-1, supersound process 10-30 minute;
(3) will precipitate and solution join in the autoclave of inner liner polytetrafluoroethylene, in 180 ℃ of following constant temperature 48h;
(4) cooled and filtered or centrifuge washing obtain powder with absolute ethanol washing at last; Powder is obtained the molybdenum dioxide nano-powder in drying at room temperature.Compare with existing additive method and technology, the present invention has following advantage:
(1) the present invention adopts polyoxyethylene glycol (PEG) 400 to synthesize the controlled molybdenum dioxide submicron particle of pattern first for auxiliary;
What (2) the molybdenum dioxide submicron particle that obtains of the present invention adopted is hydrothermal method, the product size evenly, the mean diameter of molybdenum dioxide submicron particle is 100-150nm, does not have and reunites.
Description of drawings
Fig. 1: X-ray diffraction (XRD) collection of illustrative plates that preparation method's of the present invention molybdenum dioxide is nanocrystalline;
Fig. 2: scanning electronic microscope (SEM) collection of illustrative plates of preparation method's of the present invention molybdenum dioxide nano belt;
Fig. 3: scanning electronic microscope (SEM) collection of illustrative plates of preparation method's of the present invention molybdenum dioxide nano belt and nanometer ball;
Fig. 4: scanning electronic microscope (SEM) collection of illustrative plates of preparation method's of the present invention molybdenum dioxide nanometer ball;
Fig. 5: projection electron microscope (TEM) collection of illustrative plates of preparation method's of the present invention molybdenum dioxide nanometer ball;
Fig. 1 shows the XRD figure of 180 ℃ of hydro-thermal 48h products therefroms, main diffraction peak and the MoO of collection of illustrative plates
2The diffraction peak position unanimity of (JCPDS card No.76-1807) can know that from the X diffracting spectrum of Fig. 1 oxide powder is molybdenum dioxide.
From the image of the scanning electronic microscope of Fig. 2 as can be seen, the pattern of sample is diameter 200-300nm, the nano belt of several microns pattern homogeneous of length.
From the image of the scanning electronic microscope of Fig. 3 as can be seen, when PEG400 in the hydrothermal system and water volume ratio are 5: 10, except strand of product, also have spherical product, namely morphology change is that nano belt begins to melt the formation ball.(upper right corner illustration of Fig. 3) can more be clear that from the photo of magnification, and the diameter of ball is about 1-3 μ m, is to be formed by a large amount of littler nanoparticle aggregates.
Fig. 4 is PEG400 and water volume ratio 10: 10 o'clock, and solution is at the SEM of 180 ℃ of made samples of hydro-thermal reaction 48h figure, and from the image of the scanning electronic microscope of Fig. 4 as can be seen, the product pattern is spherical.
Fig. 5 is PEG400 and water volume ratio 10: 10 o'clock, and solution is at the TEM of 180 ℃ of made samples of hydro-thermal reaction 48h figure.Can be clear that more that from figure product is with the consistent size of the sub-micro ball of Fig. 4 demonstration, sub-micron ball is made up of the nanoparticle of many 20-40nm.
Hence one can see that, by adding an amount of polyoxyethylene glycol (PEG) as template, can obtain the molybdenum dioxide submicron particle that size distribution is even, pattern is controlled under relatively mild condition.
Embodiment provided by the invention is as follows:
Following Example is to further specify of the present invention, rather than limits the scope of the invention.
Implementation example: take by weighing 1g (NH
4)
6Mo
7O
244H
2O is dissolved in the deionized water of 20ml, stirs to make it to dissolve fully, adds 10ml (5ml or 0ml) PEG400, under constantly stirring, at the uniform velocity drips 3molL
-1The pH value of HCl conditioned reaction solution continued ultrasonic 30 minutes, moved in the stainless steel cauldron of teflon lined, put baking oven in 180 ℃ of heating 48 hours.After reaction finished, product was blue solid.After naturally cooling to room temperature, suction filtration is used dehydrated alcohol, deionized water wash 6 times respectively, and flush away remains in the ion in the product as far as possible, and drying at room temperature namely obtains MoO
2Submicron particle.
Claims (1)
1. the hydrothermal synthesis method of the controlled molybdenum dioxide sub-micron crystal of a pattern, it is characterized in that utilizing soluble molybdenum salt and hydrochloric acid to be raw material, add auxiliary, in hydro-thermal reaction liquid, along with the increase of the add-on of polyoxyethylene glycol (PEG) 400, product pattern evolution process is: banded → banded+spherical → spherical, and the ball size progressively reduces, finally can make mean diameter is the molybdenum dioxide submicron particle of 100-150nm, and it may further comprise the steps:
(1) ammonium molybdate is dissolved in the 20ml-25ml water, adds 10ml (5ml or 0ml) polyoxyethylene glycol (PEG);
(2) use 1.5-3molL
-1The pH value of HCl solution regulator solution is between the 0.5-1, supersound process 10-20 minute;
(3) will precipitate and solution move in the stainless steel cauldron of teflon lined, put into baking oven in 180 ℃ the heating 48 hours;
(4) cooled and filtered obtains powder with absolute ethanol washing at last; Powder is obtained the molybdenum dioxide submicron particle in drying at room temperature.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109690A (en) * | 2014-06-19 | 2014-10-22 | 中山大学附属第一医院 | Functional nano gene transfer material and preparation method and application thereof |
| CN105152212A (en) * | 2015-07-31 | 2015-12-16 | 桂林理工大学 | Preparation method and application of H4.5Mo5.25O18*( H2O)1.36 hexagonal columnar micrometer rod and application |
| CN107285384A (en) * | 2017-07-20 | 2017-10-24 | 西安理工大学 | A kind of preparation method of flower-shaped molybdenum dioxide nanometer powder |
| CN109103444A (en) * | 2018-08-30 | 2018-12-28 | 上海力信能源科技有限责任公司 | A kind of LiMPO4The preparation method of In-situ reaction graphene |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN110358526A (en) * | 2018-04-08 | 2019-10-22 | 中国科学技术大学 | Photochromic material and application thereof |
| CN112978798A (en) * | 2021-02-02 | 2021-06-18 | 昆明理工大学 | Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size |
| US11161095B1 (en) * | 2018-01-17 | 2021-11-02 | University Of South Florida | Synthesis and characterization of MoO2 nanoparticles and their ability to decontaminate water |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780981A (en) * | 2009-01-14 | 2010-07-21 | 新疆教育学院 | Hydro-thermal synthesis method of molybdenum dioxide nano particle |
-
2012
- 2012-02-27 CN CN2012100457272A patent/CN103288136A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780981A (en) * | 2009-01-14 | 2010-07-21 | 新疆教育学院 | Hydro-thermal synthesis method of molybdenum dioxide nano particle |
Non-Patent Citations (2)
| Title |
|---|
| 蔡万玲 等: ""MoO2亚微米球的可控水热合成和表征"", 《中国钨业》 * |
| 蔡万玲 等: ""微晶MoO3纳米带转变为MoO2纳米棒的可控水热合成"", 《新疆师范大学学报（自然科学版）》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109690A (en) * | 2014-06-19 | 2014-10-22 | 中山大学附属第一医院 | Functional nano gene transfer material and preparation method and application thereof |
| CN104109690B (en) * | 2014-06-19 | 2017-04-26 | 中山大学附属第一医院 | Functional nano gene transfer material and preparation method and application thereof |
| CN105152212A (en) * | 2015-07-31 | 2015-12-16 | 桂林理工大学 | Preparation method and application of H4.5Mo5.25O18*( H2O)1.36 hexagonal columnar micrometer rod and application |
| CN105152212B (en) * | 2015-07-31 | 2016-09-28 | 桂林理工大学 | A kind of H4.5mo5.25o18(H2o)1.36the preparation method and application of hexagonal columnar micron bar |
| CN107285384A (en) * | 2017-07-20 | 2017-10-24 | 西安理工大学 | A kind of preparation method of flower-shaped molybdenum dioxide nanometer powder |
| US11161095B1 (en) * | 2018-01-17 | 2021-11-02 | University Of South Florida | Synthesis and characterization of MoO2 nanoparticles and their ability to decontaminate water |
| CN110358526A (en) * | 2018-04-08 | 2019-10-22 | 中国科学技术大学 | Photochromic material and application thereof |
| CN110358526B (en) * | 2018-04-08 | 2022-05-13 | 中国科学技术大学 | Photochromic material and application thereof |
| CN109103444A (en) * | 2018-08-30 | 2018-12-28 | 上海力信能源科技有限责任公司 | A kind of LiMPO4The preparation method of In-situ reaction graphene |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN109399722B (en) * | 2018-12-27 | 2020-10-30 | 陕西科技大学 | Preparation method of porous rod-like molybdenum dioxide/carbon composite material |
| CN112978798A (en) * | 2021-02-02 | 2021-06-18 | 昆明理工大学 | Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size |
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Application publication date: 20130911 |