Method for prehydrolysis preparing core-envelope type inorganic nanocrystalline - silicon dioxide composite grain
A technology of inorganic nano-composite particles, applied in the field of inorganic chemistry, can solve the problems of low yield of core-shell inorganic nano-crystal-silicon dioxide composite particles, adverse effects on the physical and chemical properties of nano-crystals, particle aggregation, etc., and achieve colloidal dispersion The effect of improved ability and chemical stability, simple and easy preparation method, and narrow particle size distribution
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Embodiment 1
[0012] Example 1 Fe 3 o 4 Preparation of nanocrystals
[0013] Take 0.5647 g FeCl 3 ·6H 2 O and 0.2077 g FeCl 2 4H 2 O, dissolved in 10ml of deoxygenated high-purity water, added to 60ml of ammonia water with a concentration of 7% under strong stirring, and reacted in a 50°C water bath for 30 minutes. After the reaction is completed, use a 0.1T permanent magnet to separate the black solid from the reaction solution, and wash the obtained solid with deoxygenated high-purity water for 3 to 5 times to obtain Fe with a particle size of 8 to 12 nm. 3 o 4 Nanocrystalline. Fe 3 o 4 nanocrystalline sol. Produced Fe 3 o 4 The concentration of the nanocrystalline sol is about 4mg / ml.
Embodiment 2
[0014] Embodiment 2 Preparation of Au nanocrystals
[0015] 1.2 ml of 80% tetrakishydroxymethylphosphonium chloride (THPC) was dissolved in 100 ml of water. Add 45.5ml of water, 1.5ml of 0.2M NaOH aqueous solution, 1ml of the above THPC solution into a 100ml three-necked flask, and add 4ml of 50mM HAuCl under vigorous stirring 4 The aqueous solution is reacted at room temperature for 30 minutes to obtain a gold nanocrystal sol with a particle diameter of 2-3 nm. The concentration of the prepared Au nanocrystalline sol is about 0.8mg / ml.
Embodiment 3
[0016] Example 3 ZnS: Preparation of Mn nanocrystals
[0017]Add 20ml of water, 25ml 0.1M Zn(Ac)2 into a 100ml three-necked flask, and pass nitrogen gas for 15 minutes, then add 0.870ml mercaptopropionic acid (MPA), 0.75ml 0.1M Mn(Ac)2 and pass nitrogen gas for 3 minutes, use Adjust the pH of 4M NaOH solution to 10.3, and pass nitrogen gas for 15 minutes, and weigh 0.3827g Na2S·9H 2 Dissolve O in 5ml of water, quickly inject it into a three-neck bottle and react for 15 minutes, stop the nitrogen flow, stir in the air for 6 hours, filter it with a filter membrane of φ0.25μm, and put it into the reflux device for reflux for 2 hours (starting with boiling) , after natural cooling, stir and age overnight. Centrifuge at 8000rpm / min for 15 minutes, take the supernatant, heat to boiling, airtightly cool to room temperature. Add ethanol to wash twice, and centrifuge at 8000 rpm / min for 5 minutes to obtain a white precipitate, which is dried in a vacuum desiccator to make a powder. ...
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