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Method for preparing single-phase polycrystalline bismuth molybdate by using solid-phase reaction method and application

A solid-state reaction method, bismuth molybdate technology, applied in the direction of single crystal growth, single crystal growth, polycrystalline material growth, etc., can solve the problems of long time consumption, low yield, unsuitable for large-scale production, etc., and achieve the preparation process Simple, Inexpensive Effects

Inactive Publication Date: 2012-02-08
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, crystallization needs to be calcined at 400-700°C, and it is difficult to obtain single-phase products
High-quality bismuth molybdate single crystal samples are commonly obtained by electrolysis of Bi 2 o 3 -MoO 3 Obtained by molten salt (Xiong Rui et al., J.Mater.Sci.Technol., 2006, 22(4):487-490.); but this method takes a long time and has low yield, so it is not suitable for large-scale production

Method used

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  • Method for preparing single-phase polycrystalline bismuth molybdate by using solid-phase reaction method and application
  • Method for preparing single-phase polycrystalline bismuth molybdate by using solid-phase reaction method and application
  • Method for preparing single-phase polycrystalline bismuth molybdate by using solid-phase reaction method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Bismuth powder (purity 99.999%) and molybdenum trioxide (purity 99.5%) are mixed in a molar ratio of 1:5, and a total of 2 g is mixed in a mortar.

[0024] (2) Place the well-mixed mixture in a 100ml stainless steel ball mill tank, vacuumize it, and fill it with argon protection; the mixture and agate balls are mixed in a mass ratio of 1:20, and 10ml of absolute ethanol (analytical grade, mass Score greater than 99.7%), ball milling with 450 rev / min rotating speed for 40 hours.

[0025] (3) The ball-milled powder is washed with absolute ethanol (analytical grade, mass fraction greater than 99.7%), dried, pressed into tablets (20 MPa), and calcined in a vacuum atmosphere at 700° C. for 10 hours.

[0026] (4) adopt XRD to carry out phase analysis to final product and find: sample crystallization is good (results such as figure 1 shown); EDS analysis shows that the ratio of Bi and Mo elements is about 0.14:1 (the results are as follows figure 2 shown); comprehensive...

Embodiment 2

[0029] (1) Bismuth powder (purity 99.999%) and molybdenum trioxide (purity 99.5%) are mixed in a molar ratio of 1:5, and a total of 2 g is mixed in a mortar.

[0030] (2) The mixture was pressed into tablets (20 MPa), and calcined in a vacuum atmosphere at 700° C. for 10 hours.

[0031] (3) XRD was used to analyze the phase of the final product, and it was found that the product was impure and had many impurity phases; it indicated that mechanical ball milling was very critical for the solid-phase synthesis of single-phase bismuth molybdate.

Embodiment 3

[0033] (1) Bismuth powder (purity 99.999%) and molybdenum trioxide (purity 99.5%) are mixed in a molar ratio of 1:5, and a total of 2 g is mixed in a mortar.

[0034] (2) Place the well-mixed mixture in a 100ml stainless steel ball mill tank, vacuumize it, and fill it with argon protection; the mixture and agate balls are mixed in a mass ratio of 1:20, and 10ml of absolute ethanol (analytical grade, mass Score greater than 99.7%), ball milling with 450 rev / min rotating speed for 40 hours.

[0035] (3) The ball-milled powder is washed with absolute ethanol (analytical grade, mass fraction greater than 99.7%), dried, pressed into tablets (20 MPa), and calcined in a vacuum atmosphere at 680° C. for 10 hours.

[0036] (4) XRD was used to analyze the phase of the final product, and it was found that the sample crystallized better, but the single-phase property was worse than that of the product calcined at 700°C for 10 hours; it shows that choosing an appropriate calcination temper...

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Abstract

The invention discloses a method for preparing single-phase polycrystalline bismuth molybdate by using a solid-phase reaction method and application. The method comprises the following steps of: mixing bismuth powder and molybdenum trioxide according to a molar ratio of 1:5; ball-milling obtained mixture under inert gas atmosphere; and cleaning, tabletting, calcining and sintering to obtain the single-phase polycrystalline bismuth molybdate after ball-milling. The single-phase polycrystalline bismuth molybdate has a structural formula of Bi0.27Mo2O5 and shows semiconductor behavior at 160-300K. In the invention, the single-phase polycrystalline bismuth molybdate polycrystal is prepared by a method for combining mechanical ball-milling and solid-phase sintering; and the method has the advantages of simple preparation process, low cost, no environmental pollution, yield of over 90 percent and suitability for large-scale production.

Description

technical field [0001] The invention relates to the preparation of inorganic chemical raw materials, in particular to a method and application for preparing single-phase polycrystalline bismuth molybdate by using a solid-state reaction method. Background technique [0002] Ternary molybdate has abundant physical phenomena such as superconductivity and charge density wave. Among the trivalent cation molybdates, bismuth molybdate has received special attention due to its wide applications in photocatalysis, ionic conductors, acousto-optic materials, photoconductivity, and gas sensing (Song N et al., J. Catal 2005, 236: 282-291; Cruz A et al., Catal. Today, 2007, 129: 194-199; Xie H et al., Mater. Chem. Phys., 2008, 110: 332-336.). The preparation of bismuth molybdate mostly adopts solid phase reaction method, co-precipitation method, sol-gel method and hydrothermal method (Thang L M et al., Catal.Today.2008, 131:566-571; Li Honghua et a1., Mater . Chem. Phys., 2009, 116: 134...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B28/02C30B29/32
Inventor 乐松严振升
Owner JINAN UNIVERSITY
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