Method for preparing rod-like zinc oxide nano-crystals

A technology of zinc oxide nanocrystals and zinc oxide nanocrystals, which is applied in the field of preparation of rod-shaped zinc oxide nanocrystals, and can solve the problems of unfavorable environmental protection, difficult size control, complicated process, etc.

Inactive Publication Date: 2012-11-28
XIAN UNIV OF TECH
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Problems solved by technology

[0008] The purpose of the present invention is to provide a method for preparing rod-shaped zinc oxide nanocrystals, which solves the problems in the prior art that the process is generally complicated, the product shape is uneven, and the size is not easy to control. The problem that the introduction of chemical compounds is unfavorable to environmental protection

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  • Method for preparing rod-like zinc oxide nano-crystals
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  • Method for preparing rod-like zinc oxide nano-crystals

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preparation example Construction

[0026] The preparation method of the rod-shaped zinc oxide nanocrystal of the present invention is implemented according to the following steps:

[0027] Step 1. Add 0.001~1mol / L ammonia aqueous solution to 0.001~1mol / L zinc salt aqueous solution dropwise at room temperature ≤25°C to pH=7~8, and control the dropping rate at 2~4mL / min. After 0.5~1h of reaction, washing with water and centrifugation to obtain amorphous zinc hydroxide;

[0028] Step 2. The amorphous zinc hydroxide obtained in step 1 is prepared into a dispersion system of 0.001 to 1 mol / L, then a potassium hydroxide solution of 0.001 to 1 mol / L is added, and the molar ratio of the mixed solution is controlled to be KOH:Zn(OH) 2 =1: (0.5~6), the pH of the mixed solution is controlled to be 14; the mixed solution is then subjected to constant temperature reaction at 75~95°C for 2~8h, and the obtained precipitate is washed with water, centrifuged, and dried at 40~100°C for 8~8 hours. After 24 hours, rod-shaped zinc...

Embodiment 1

[0035] 0.15mol / L ammonia solution was added dropwise to 0.5mol / L zinc sulfate (or hydrated zinc sulfate) aqueous solution at room temperature (≤25℃) to pH=7, the dripping rate was controlled at 2mL / min, and the reaction was sufficient for 0.5 After h washing, centrifugal separation obtains amorphous zinc hydroxide; The obtained amorphous zinc hydroxide is dispersed in deionized water to make a dispersion system of 1 mol / L, and then the potassium hydroxide solution of 1 mol / L is added (mol ratio is Zn( OH) 2 : KOH=1:2), the pH of the solution is about 14, the obtained mixed solution was reacted at a constant temperature of 95°C for 2h, the obtained precipitate was washed with deionized water, centrifuged, and dried at 80°C for 16h to obtain rod-shaped zinc oxide nanocrystals. . Its scanning electron microscope photos such as figure 1 As shown, the XRD diffraction pattern is as figure 2 shown.

Embodiment 2

[0037] Add 0.001mol / L aqueous ammonia solution dropwise to 1mol / L zinc chloride aqueous solution at room temperature (≤25℃) to pH=8, control the dropping rate at 3mL / min, fully react for 1h, wash and centrifuge to obtain Amorphous zinc hydroxide; the obtained amorphous zinc hydroxide is dispersed and prepared into a dispersion system of 0.3 mol / L with pure water, and then a potassium hydroxide solution of 0.001 mol / L is added (molar ratio is Zn(OH) 2:KOH=1:6), the pH of the mixed solution system was about 14, and further reacted at a constant temperature of 80°C for 4h, and the obtained precipitate was washed with purified water, centrifuged, and dried at 65°C for 14h to obtain rod-shaped zinc oxide nanocrystals. Its TEM electron microscope photos such as image 3 As shown, the photoluminescence spectrum is as Figure 4 shown.

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Abstract

The invention discloses a method for preparing rod-like zinc oxide nano-crystals, comprising the following steps of: step 1, adding dropwise ammonia-water solution to zinc salt aqueous solution at the room temperature, and after thorough reaction, performing washing using water and centrifugal separation, thereby obtaining amorphous zinc hydroxide; and step 2, preparing the amorphous zinc hydroxide obtained through the step 1 into a dispersion system and then adding potassium hydroxide solution, arousing a constant-temperature reaction of the mixed solution, washing the obtained sediments using water, and centrifugally separating and drying the sediments, thereby obtaining the rod-like zinc oxide nano-crystals. The product prepared by the method disclosed by the invention is the rod-like zinc oxide nano-crystals which are small in size, large in specific surface area, obvious in nanometer effect, and excellent in properties such as photoluminescence, photocatalytic degradation and the like; and the method is simple in preparation process, high in yield, free of needs of any template or special substrate and any chemical additive, free of pollution, and low in energy consumption.

Description

technical field [0001] The invention belongs to the technical field of inorganic functional materials, and relates to a preparation method of rod-shaped zinc oxide nanocrystals. Background technique [0002] Nanomaterials exhibit exotic properties that are different from conventional bulk materials due to their surface effects, small size effects, and macroscopic quantum tunneling effects. Therefore, it has become a research and application hotspot at home and abroad. Zinc oxide nanocrystals are a new type of high-function fine inorganic products. With the reduction in size, they show many special functions in optics, magnetism, mechanics, electricity, etc., making them useful in functional ceramics, electronics, photoluminescence, etc. , photocatalytic degradation, biomedicine, ultraviolet shielding and many other fields have great application value and cause great research enthusiasm. The morphology and size of zinc oxide nanocrystals have a huge impact on its performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82Y30/00
Inventor 张卫华夏培康张博华
Owner XIAN UNIV OF TECH
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