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Method for preparing orthorhombic phase molybdenum trioxide nano wire

A molybdenum trioxide and nanowire technology, applied in the direction of molybdenum oxide/molybdenum hydroxide, can solve the problems of poor applicability, time-consuming and energy-consuming, etc., and achieve the effects of easy control of reaction conditions, good reaction repeatability and simple equipment.

Inactive Publication Date: 2009-05-06
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires a long process of dissolution and solvothermal treatment, which is time-consuming and energy-consuming
[0006] "A Method for Synthesizing Molybdenum Trioxide Single Crystal Nanobelts" proposed by Chinese Patent No. 02104181.4 adopts the method of hydrothermally treating the molybdate solution acidified by perchloric acid to prepare orthorhombic phase molybdenum trioxide nanobelts. This method not only requires Hydrothermal treatment, and the concentration of hydrogen ions in the solution and the rate of acid addition must be strictly controlled, and soluble molybdate must be used, which is not widely applicable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Preparation of molybdenum trioxide nanowires with molybdic acid as raw material

[0015] 12 mmol of molybdic acid monohydrate (H 2 MoO 4 ·H 2 O) dissolved in 34ml concentration is 4mol L -1 Add 6mol·L dropwise to the ethylenediamine aqueous solution under magnetic stirring -1 Hydrochloric acid solution until the pH value of the system was 4.5, a large amount of white precipitate appeared in the solution; after stirring for 15 minutes, the reaction mixture was separated by suction filtration, the solid powder was washed with distilled water several times, and dried at 120°C to obtain a white dry powder.

[0016] X-ray diffraction proves that the white powder is pure orthorhombic molybdenum trioxide; scanning electron microscope characterization shows that the sample is composed of nanowires with a diameter of 200-300nm and a length of 20-30μm, and the electron diffraction pattern shows that the nanowires are edge [001 ] direction of the growth of single cr...

Embodiment 2

[0018] Example 2: Preparation of molybdenum trioxide nanowires with molybdenum trioxide reagent powder as raw material

[0019] Dissolve 20mmol of reagent grade molybdenum trioxide in 40ml at a concentration of 2mol L -1 Add 4mol·L dropwise to the aqueous solution of ethylenediamine under magnetic stirring -1 sulfuric acid solution until the pH value of the system was 4, and after continuing to stir for 20 minutes, the mixture was separated by suction filtration, the solid powder was washed with distilled water several times, and dried at 120°C to obtain a white fibrous powder.

[0020] X-ray diffraction proves that the white powder is pure orthorhombic molybdenum trioxide; scanning electron microscope characterization shows that the sample is composed of nanowires with a diameter of 200-300nm and a length of 30-40μm, and the electron diffraction pattern shows that the nanowires are edge [001 ] direction of the growth of single crystals.

[0021] After the prepared molybdenu...

Embodiment 3

[0022] Embodiment 3: Preparation of molybdenum trioxide nanowires with potassium molybdate as raw material

[0023] Take 40ml of the mother liquor after separating the product in Example 1, add 9ml of water and 2ml of ethylenediamine, stir well; then add 10mmol potassium molybdate, stir until clear; add 3mol L dropwise under magnetic stirring -1 Perchloric acid solution until the pH value of the system is 5, that is, stop dropping. A large amount of white precipitates appeared in the solution. After continuing to stir for 20 minutes, the mixture was separated by suction filtration. The solid powder was washed with distilled water several times and dried at 120°C to obtain a white fibrous powder.

[0024] X-ray diffraction proves that the white powder is pure orthorhombic molybdenum trioxide; scanning electron microscope characterization shows that the sample is composed of nanowires with a diameter of 250-300nm and a length of 30-40μm, and the electron diffraction pattern show...

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Abstract

The invention discloses a method for preparing an orthorhombic phase molybdenum trioxide nano wire, which is characterized in that molybdate, molybdic acid or molybdenum trioxide is dissolved in aqueous solution with quadrol concentration of 0.2-6 mol / L to cause the mol ratio of molybdenum atom and quadrol to be 1:1-6; and then strong acid solution with hydrogen ion concentration of 0.5-3.0 mol / L is dropwise added under the condition of stirring till the pH value is within 4 to 5; the solution is unceasingly stirred for 10 to 30 min; then the white precipitation is sucked, filtered, washed and dried to obtain white orthorhombic phase single crystal nano wires with the diameter of 100 to 400 nm and the length of 10-40 Mum. In the method, the raw materials are easily obtained; the needed device is simple; the technique is convenient; the reaction can be finished in an hour in the normal temperature and pressure; the method is safe and easy to be controlled; the productive rate reaches more than 99 percent; the mother solution can be reused; and the method is applicable to large-scale industry production.

Description

technical field [0001] The invention belongs to the technical field of preparation of molybdenum trioxide nanometer materials, in particular to a liquid-phase chemical preparation method of orthogonal phase molybdenum trioxide nanowires under non-solvothermal conditions. Background technique [0002] Molybdenum trioxide nanomaterials have important applications in the fields of catalysis, optics, sensing, and electrochemistry due to their small size, large specific surface area, and high reactivity. Molybdenum trioxide mainly has three crystal phases: orthorhombic, hexagonal and monoclinic, among which the orthorhombic molybdenum trioxide is a thermodynamically stable phase, so it is the most widely used. The existing methods for synthesizing orthorhombic molybdenum trioxide nanowires mainly include electrospinning, chemical vapor deposition, template method, and solvothermal method. However, these methods have the disadvantages of complex operation process, numerous steps,...

Claims

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Application Information

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IPC IPC(8): C01G39/02
Inventor 倪小敏郑化桂戚邦华廖光煊
Owner UNIV OF SCI & TECH OF CHINA
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