Low temperature controllable preparation method of double metal oxide semiconductor nanocrystalline sol

Abstract

The invention relates to a low temperature controllable preparation method of double metal oxide semiconductor nanocrystalline sol, which belongs to the technical field of the preparation of the semiconductor nanocrystalline. The method comprises the following steps of: dissolving two soluble metal inorganic salts into water; adding aqueous alkali dropwise in the water under a stirring condition;adjusting pH value to neutral to obtain white precipitate; filtering and washing after standing and ageing; dissolving the obtained filter cake in the solvent again and then performing ultrasonic dispersion; adding peroxide dropwise for dispergation under a condition of ice-bath and stirring and performing reflux heating at the temperature of 95 DEG C to obtain metal peroxide sol; and transferring the sol to a high-pressure reactor to crystallize at the temperature of between 100 and 200 DEG C to obtain the double metal oxide semiconductor nanocrystalline sol. In the preparation method, the double metal oxide semiconductor nanocrystalline sol is prepared by binary composite peroxide; the sol crystalline grains which are prepared under the appropriate reaction condition have small size andcontrollable crystal form and appearance; and the preparation process avoids the addition of surfactant and does not need high-temperature calcination. The produced sol has wide application prospect in the fields such as indoor air purification, sterilization, bacteriostasis, mildew prevention, photoelectricity conversion, sensors and the like.

Description

Technical field [0001] The invention relates to a low-temperature controllable preparation method for preparing bimetal oxide semiconductor nanocrystalline sol from a binary composite peroxide, and belongs to the technical field of semiconductor nanomaterial preparation technology. Background technique [0002] In recent years, bimetal oxide semiconductor materials have attracted great attention of researchers due to their special properties in light, electric field, and magnetic field. Double metal oxide semiconductor materials have greatly improved the performance of single semiconductors, and broadened the discovery of new materials and the application of semiconductor materials. At present, the preparation of bimetal oxide semiconductor materials usually adopts chemical vapor precipitation method, sol-gel method, thermal oxidation method, impregnation-sintering method, etc. For example, Hiroaki Uchiyama et al. prepared rutile (Ti 1-x Sn x )O 2 , And pure TiO 2 In comparison,...

AI Technical Summary

Problems solved by technology

Rutile type (Ti 1-x sn x )O 2 , with pure TiO 2 In contrast, its light absorption and photocatalytic properties have been improved, but high-temperature calcination requires high equipment requirements, which is not conducive to large-scale production (Hiroaki Uchiyama and Hiroaki Imai. Crystal growth of metastable rutile-type Ti x sn 1-x o 2 solid solutions in an aqueous system: Chem.Com., 2005, 6014-6016)

Fernando Fresno et al. used the inverse microemulsion method to prepare (Ti 1-x sn x )O 2 , studied the preparation of different molar ratios of Ti and Sn and different calcination temperatures (Ti 1-x sn x )O 2 gas sensitivity, but the disadvantage is that there is a relatively serious phase separation, which limits its practical application (Fernando Fresno, David Tudela, Juan M.Coronado, Javier Soria.Synthesis of Ti 1-x sn x o 2 Nanosized photocatalysts in reverse microemulsions: Catalysis Today 143 (2009) 230-236)

At present, the problems existing in the preparation of double metal oxide semiconductor materials by traditional methods, especially the preparation of double metal oxide semiconductor sols are: the difference in hydrolysis rate of the two-phase components is large, and phase separation is prone to occur; and the prepared double metal oxide semiconductor sol It is difficult to control the grain size, crystal form and morphology, which restricts the value of its practical application. In recent years, researchers have begun to explore the use of a two-component precursor to overcome the difference in the two-phase hydrolysis rate.

Guangqiang Lu et al first used Zn(NO 3 ) 2 ·6H 2 O, Mg(NO 3 ) 2 ·6H 2 O and polyacrylic acid to synthesize bimetallic polyacrylate precursors, and Zn was obtained by high-temperature calcination 1-x Mg x O powder, but the price of polyacrylic acid is high, the whole production process is cumbersome and the conditions are harsh (Guangqiang Lu, Ingo Lieberwirth, and Gerhard Wegner. A General Polymer-Based Process To Prepare Mixed Metal Oxides: The Case of Zn 1-x Mg x O Nanoparticles: J.AM.Chem.Soc.2006.128:15445-15450)