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.
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[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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