Method for preparing gold nano microgranule powder
An ultra-fine particle and nano-gold technology, which is applied in the field of preparation of nano-gold ultra-fine particle powder, can solve the problems of increased cost, complicated process, difficult removal of passivating agents, etc.
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Embodiment l
[0028] In a beaker containing 10ml of 6.3mmol / L PVP ethanol solution, add 4.2ml of 0.59mmol / L chloroauric acid aqueous solution, then add 5ml of double distilled water, fully stir and cool in an ice bath, and add dropwise under rapid stirring 0.2mol / L sodium hydroxide aqueous solution 0.3ml. The molar ratio of PVP to gold is 26:1, the molar ratio of sodium hydroxide to gold is 24:1, and the molar ratio of methanol to water is 1:1. Then transfer to a 100ml round bottom flask, install a reflux device, heat and reflux with full power microwave (output power 750W) for 5 minutes to obtain a purple gold sol, cool at room temperature, and the absorption peak of the ultraviolet-visible absorption spectrum is 542nm. Vacuum rotary evaporator evaporation and drying A powdery product was obtained.
Embodiment 2
[0030] In a beaker filled with 10ml 3mmol / L PVP ethylene glycol solution, add 0.2ml of 17.8mmol / L chloroauric acid aqueous solution, then add 10ml of double distilled water, fully stir and cool in an ice bath, quickly stir and drop Add 0.11ml of 0.2mol / L sodium hydroxide aqueous solution. The molar ratio of PVP to gold is 8:1, the molar ratio of sodium hydroxide to gold is 6:1, and the molar ratio of methanol to water is 1:1. Then transfer to a 100ml round bottom flask, install a reflux device, heat and reflux with full power microwave (output power 750W) for 5 minutes to obtain a blue gold sol, cool at room temperature, and the absorption peak of the ultraviolet-visible absorption spectrum is 592nm. Vacuum rotary evaporator evaporation and drying A powdery product was obtained.
Embodiment 3
[0032] In a beaker containing 4.9ml of 24mmol / L PVP methanol solution, add 4ml of 0.59mmol / L chloroauric acid aqueous solution, then add 5ml of anhydrous methanol, fully stir and cool in an ice bath, add 4.7ml dropwise under rapid stirring 4mmol / L sodium hydroxide aqueous solution. The molar ratio of PVP to gold is 50:1, the molar ratio of sodium hydroxide to gold is 8:1, and the molar ratio of methanol to water is 1:1. Then transfer to a 100ml round-bottomed flask, install a reflux device, heat and reflux with full-power microwave (output power 750W) for 10 minutes to obtain purple gold sol, cool at room temperature, and the absorption peak of the ultraviolet-visible absorption spectrum is 556nm. Evaporate and dry in a vacuum rotary evaporator to obtain Powdered product. The average particle size of gold powder is 17nm. The maximum and minimum particle size deviation is ≤5nm.
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