Method for preparing zinc oxide nano hollow spheres by caustic corrosion reaction

A technology of zinc oxide nano and hollow spheres, which is applied in the field of nanomaterials, can solve problems such as uneven size of zinc oxide hollow spheres, blank nano-hollow spheres, complex washing process, etc., and achieve large size controllability and shape controllability, The effect of stable shape and simple process route

Inactive Publication Date: 2008-09-03
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are a few reports on the research of zinc oxide hollow nanospheres, there is almost no new mechanism for preparing hollow nanospheres. The main preparation mechanism is the Oswald ripening mechanism, and most of them use complex organic processes.
[0003] Proposed by Li et al. to use coordination copolymers as reactants to prepare zinc oxide hollow nanospheres, the washing process is complicated (Li.Z.Q.; Xie.Y.; Xiong Y.J.; Zhang.R.New J.Chem.2003, 27, 118) Zeng et al. proposed to use zinc powder as raw material to synthesize zinc oxide hollow spheres by oxidation-reduction reaction (Liu.B.; Zeng.H.C.J.Am.Chem.Soc.2004, 126, 16744), Yan et al. proposed to use basic zinc carbonate to make The precursor prepared zinc oxide hollow spheres through the aging mechanism (Yan, C.L.; Xue.D.F.J.PHys.Chem.B.2006, 110, 11076), and the obtained zinc oxide hollow spheres were not uniform in size and agglomerated severely

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  • Method for preparing zinc oxide nano hollow spheres by caustic corrosion reaction
  • Method for preparing zinc oxide nano hollow spheres by caustic corrosion reaction
  • Method for preparing zinc oxide nano hollow spheres by caustic corrosion reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] First prepare solution A: 4.39g Zn(Ac) 2 2H 2 O was dissolved in 100 mL of deionized water and dissolved under stirring at 400-600 rpm. At the same time, solution B: 5M concentrated ammonia solution was prepared. Zn(Ac) in A solution 2 After stable dissolution and complete transparency, add solution B dropwise under magnetic stirring at 400-600 rpm until PH=11.5-14. Due to the addition of ammonia water, solution A immediately produces a white precipitate. With the gradual addition of ammonia water under magnetic stirring, the white precipitate dissolves rapidly and forms a stable Zn(NH 3 ) 4 2+ of ammonia solution. The resulting Zn(NH 3 ) 4 2+ 10 mL of ammonia solution was added to 60 mL of absolute ethanol, then transferred to a 100 mL Teflon tube, and reacted at 180°C for 12 hours to obtain white zinc oxide nanosphere precipitates. Repeat washing with deionized water and absolute ethanol three times each, and finally vacuum-dry at 60° C. for 2 hours. figur...

Embodiment 2

[0034] First prepare solution A: 4.39g Zn(Ac) 2 2H 2 O was dissolved in 100 mL of deionized water and dissolved under stirring at 400-600 rpm. At the same time, solution B: 5M concentrated ammonia solution was prepared. Zn(Ac) in A solution 2 After stable dissolution and complete transparency, add solution B dropwise under magnetic stirring at 400-600 rpm. Due to the addition of ammonia water, solution A immediately produces white precipitate. With the gradual addition of ammonia water under magnetic stirring, the white precipitate dissolves rapidly. Formation of stable Zn(NH 3 ) 4 2+ of ammonia solution. Continue to add solution B dropwise until pH=11.4 to get Zn(NH 3 ) 4 2+ 10 mL of the solution was added to 60 mL of absolute ethanol, transferred to a 100 mL Teflon tube, and reacted at 180°C for 12 hours to obtain a white precipitate. Repeat washing with deionized water and absolute ethanol three times each, and finally vacuum-dry at 60° C. for 2 hours. Figure 5 ...

Embodiment 3

[0036] First prepare solution A: 1.76g Zn(Ac) 2 2H 2 O was dissolved in 100 mL of deionized water and dissolved under stirring at 400-600 rpm. At the same time, solution B: 5M concentrated ammonia solution was prepared. Zn(Ac) in A solution 2 After stable dissolution and complete transparency, add solution B dropwise under magnetic stirring at 400-600 rpm. Due to the addition of ammonia water, solution A immediately produces white precipitate. Under magnetic stirring, with the gradual addition of ammonia water, the white precipitate dissolves rapidly, forming a stable Zn(NH 3 ) 4 2+ The ammonia solution is Zn(NH 3 ) 4 2+ (Ac) 2 . Continue to add solution B dropwise until pH=11.4 to get Zn(NH 3 ) 4 2+ 10 mL of the solution was added to 60 mL of absolute ethanol, transferred to a 100 mL Teflon tube, and reacted at 180°C for 12 hours to obtain a white precipitate. Repeated washing with deionized water 3 times, then washing with absolute ethanol 3 times each, and fin...

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Abstract

The invention provides a method for preparing zinc oxide nanometer hollow spheres in caustic corrosion reaction. The method is mainly characterized in including using the solution of Zn(Ac)2 as the initial reactant first, adjusting the pH value to 11.5-14 by adding ammonia, using ethanol as the solvent, finally forming the nanometer hollow spheres in the hydrothermal reaction between Zn(NH3)4<2+> and excessive ammonia at a high temperature. The entire reaction has simple material, easy operation, no need for any complex instrument processing, convenience and rapidness, which is a method of rapidly preparing the zinc oxide nanometer hollow spheres. The obtained hollow spheres have narrow size distribution and good dispersibility with an external diameter of 600 nm and an internal diameter of 200-300 nm. The caustic corrosion reaction is adopted to synthesize zinc oxide nanometer hollow spheres in the method, thus agglomeration phenomenon caused by an aging machine is obviated, complex operation steps of organic reaction synthesis, contamination and disturbance to objective material zinc oxide caused by the complex operation steps are obviated. The method is obviously characterized in high production rate, rapidness, easiness, convenient operation, low cost and environment friendliness.

Description

technical field [0001] The invention relates to a method for preparing zinc oxide nanometer hollow spheres, more precisely, to a method for preparing zinc oxide nanometer hollow spheres through alkali corrosion reaction, and the prepared hollow spheres can be used in biomedicine, gas-sensing and light-emitting devices. It belongs to the field of nanomaterials. Background technique [0002] Zinc oxide is a functional material with a wide range of uses, and is widely used in important industrial and technical fields such as biomedical carriers, gas-sensitive components, and light-emitting devices. The basis of the application of zinc oxide materials lies in their unique physical properties, such as the spectral properties of the material, energy band properties, etc. In particular, the energy spectrum bandgap of ZnO is affected by its shape, size and structure. In recent years, a large number of studies have focused on the preparation of ZnO nanocrystals with different shapes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82B3/00
Inventor 高濂陈志涛
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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