Preparation method of iron molybdenum oxide (II) nanocube

A technology of nano-cubes and ferrous molybdate, which is applied in the direction of nanotechnology, chemical instruments and methods, and iron compounds, can solve the problem that monoclinic ferric molybdate materials are difficult to obtain a regular shape structure, and achieve easy-to-large Large-scale industrial production, uniform particle size distribution, and high operational controllability

Inactive Publication Date: 2015-06-17
CHINA UNIV OF MINING & TECH
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Problems solved by technology

[0003] Aiming at the deficiencies of the prior art, the present invention provides a simple preparation method of a ferrous molybdate nano-cubic structure material, which solves the problem that it is difficult to obtain a regular shape structure for a monoclinic ferric molybdate material

Method used

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  • Preparation method of iron molybdenum oxide (II) nanocube
  • Preparation method of iron molybdenum oxide (II) nanocube
  • Preparation method of iron molybdenum oxide (II) nanocube

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: a kind of ferric molybdate ( ) preparation method of nano-cubic structure material, using liquid phase synthesis technology to prepare iron molybdate ( ) nanostructure comprising the steps of:

[0022] (1) The iron source is ferrous salt, selected from ferrous chloride hydrate (FeCl 2 4H 2 O), ferrous oxalate hydrate (FeC 2 o 4 2H 2 O), hydrated ferrous nitrate (Fe(NO?)? 6H?O), hydrated ferrous sulfate (Fe 2 SO 4 ·7H 2 O) or ferrous acetate hydrate (Fe(CH 3 COO) 2 4H 2 O);

[0023] Molybdenum source is hexavalent molybdenum salt, selected from sodium molybdate (Na 2 MoO 4 ), ammonium molybdate ((NH 4 ) 2 Mo 2 o 7 , (NH 4 ) 2 Mo 4 o 13 , (NH 4 ) 6 Mo 7 o 24 4H 2 O, (NH 4 ) 4 Mo 8 o 26 ), or molybdic acid (H 2 MoO 4 ·H 2 o).

[0024] Add the iron source and the molybdenum source in a molar ratio (1.5-3): 1 to the alcohol-water mixture of sodium acetate and polyvinylpyrrolidone with a mass percent concentration of 0.3-2.0%,...

Embodiment 2

[0033] Embodiment 2: iron molybdate ( ) Preparation and structural characterization of nanocubes;

[0034] Take 0.56 g ferrous sulfate hydrate (Fe 2SO 4 ·7H 2 O) and 0.25 g sodium molybdate (Na 2 MoO 4 ) into the container, add 25ml ethylene glycol and 15ml distilled water, add 0.2 g polyvinylpyrrolidone (PVP) and 0.2 g sodium acetate, mix and stir evenly; transfer the mixed material to a closed pressure-resistant reaction vessel, and React at 200°C for 20 hours. Then cool to room temperature, open the airtight reaction vessel, filter with Buchner funnel, and wash with deionized water to obtain a dark brown powder product. The product was identified as monoclinic β-FeMoO by Bruker D8 ADVANCE X-ray powder diffractometer with Cu Kα rays (wavelength λ= 1.5418?, scanning step speed 0.08° / s). 4 ( figure 1 ), which matches the JCPDS card standard value No. 22-0628, and is mixed with a very small amount of α-FeMoO 4 (JCPDS No: 22-1115).

[0035] Cubic phase iron molybdate...

Embodiment 3

[0036] Embodiment 3: get 0.36 g ferrous oxalate hydrate (FeC 2 o 4 2H 2 O) and 0.25 g sodium molybdate (Na 2 MoO 4 ) into a container and add 25 ml ethylene glycol and 15 ml distilled water, add 0.2 g polyvinylpyrrolidone (PVP) and 0.2 g sodium acetate, mix and stir evenly; transfer the mixed material to a closed pressure-resistant reaction vessel , reacted at 180°C for 20 hours. Then cool to room temperature, open the airtight reaction vessel, filter with Buchner funnel, and wash with deionized water to obtain a dark brown powder product.

[0037] The obtained ultrafine powder is monoclinic β-FeMoO 4 (JCPDS No. 22-0628), good crystallinity; composed of nanoparticles with an average particle size of about 90 nm.

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Abstract

The invention relates to a preparation method of an iron molybdenum oxide (II) nanocube, and belongs to the preparation of an iron molybdenum oxide nanometer material with a regular shape. The method comprises the following steps: adding an iron source and a molybdenum source into a sealed pressure resistant reaction container according to the molar ratio of (1.5-3) to 1, using an ethanol and water mixing liquid as a solvent, respectively adding sodium acetate which accounts for 0.3-2.0% of the mass of the ethanol and water mixing liquid and polyvinylpyrrolidone to be used as auxiliary agents, uniformly stirring and mixing, and reacting for 8 to 40 hours at the temperature of 100 to 250 DEG C. The iron molybdenum oxide (II) nanocube is firstly prepared by the one-step liquid phase method; the used raw material is low in price, and easy to obtain; the preparation step is simple, and the operation controllability is high; the single crystal with uniformly distributed particle size and proper particle size is obtained, and the large-scale industrial production is facilitated. As the nanocube has the large specific area and regular surface shape structure, the nanocube is widely applied to the fields of new energy lithium iron cells and catalytic optics. The method is applied to the fields of optics, electrics, energy storage and catalyzing.

Description

technical field [0001] The invention relates to the preparation of ferrous molybdate nanometer material with regular shape, in particular to a preparation method of ferrous molybdate nano cube. Background technique [0002] As a member of the field of inorganic functional materials, metal molybdate nanomaterials are widely used in optics (Chem. Eur. J., 2007, 13, 746), magnetism ( J. Am. Chem. Soc., 2008, 130, 13490), catalysis (Chem. Commun., 2009, 1565), electrochemical energy storage (J. Mater. Chem. A, 2013, 1, 9024) and other fields have Wide range of applications has aroused great concern of material scientists. As we all know, the shape, structure and size of materials seriously affect the physical and chemical properties of materials. Therefore, it is necessary to tailor and modify materials accordingly. This is the great challenge that materials scientists are currently facing. For an important member of the molybdate system, iron molybdate is no exception, especi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/00B82Y40/00
Inventor 鞠治成邢政
Owner CHINA UNIV OF MINING & TECH
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