A kind of preparation method of stibnite nanocrystal
An antimony lead silver and nanocrystal technology is applied in the field of preparation of multi-component sulfide nanocrystals, which can solve problems such as great influence on products, and achieve the effects of no special equipment requirements, low production cost and simple process.
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Embodiment 1
[0023] In this example, silver diethyldithiocarbamate is used as a precursor, and Ag is prepared by segmental heating in a reflux system. 3 Pb 2 Sb 3 S 8 compound, the specific process is.
[0024] 1) Weigh 5mmol of sodium diethyldithiocarbamate and 5mmol of silver nitrate, dissolve them in 20mL of distilled water, and gradually add the silver nitrate solution dropwise to the sodium diethyldithiocarbamate solution under magnetic stirring, and react After the end, the resulting precipitate was filtered, washed alternately with water and ethanol twice, and dried at 50° C. for 6 hours to obtain a silver diethyldithiocarbamate precursor.
[0025] 2) Weigh 1.5mmol silver diethyldithiocarbamate precursor, 1mmol lead acetate, 1.5mmol antimony trichloride, and add them to a mixture consisting of 20mL octadecene, 5mL dodecyl mercaptan and 2mL oleylamine solvent, stirring evenly to form a mixed reaction solution.
[0026] 3) Transfer the obtained mixed reaction solution to a three-...
Embodiment 2
[0029] In this example, silver diethyldithiocarbamate is used as a precursor, and Ag is prepared in a slow one-step heating mode in a reflux system. 3 Pb 2 Sb 3 S 8 compound, the specific process is.
[0030] 1) Weigh 5mmol of sodium diethyldithiocarbamate and 5mmol of silver nitrate, dissolve them in 20mL of distilled water, and gradually add the silver nitrate solution dropwise to the sodium diethyldithiocarbamate solution under magnetic stirring, and react After the end, the resulting precipitate was filtered, washed alternately with water and ethanol three times, and dried at 50° C. for 6 hours to obtain a silver diethyldithiocarbamate precursor.
[0031] 2) Weigh 1.5mmol silver diethyldithiocarbamate precursor, 1mmol lead acetate, 1.5mmol antimony trichloride, and add them to a mixture consisting of 20mL octadecene, 5mL dodecyl mercaptan and 2mL oleylamine solvent, stirring evenly to form a mixed reaction solution.
[0032] 3) Transfer the obtained mixed reaction sol...
Embodiment 3
[0035]In this example, silver ethyl xanthate is used as the precursor of the reaction, and Ag is prepared in the reflux system by segmented heating mode. 3 Pb 2 Sb 3 S 8 compound, the specific process is.
[0036] 1) Weigh 5 mmol of sodium ethyl xanthate and 5 mmol of silver acetate, dissolve them in 20 mL of distilled water, slowly mix the silver acetate and sodium ethyl xanthate solution under magnetic stirring, filter the obtained precipitate after the reaction, and Wash twice with water and ethanol alternately, and dry at 50°C for 6 hours to obtain a silver ethyl xanthate precursor.
[0037] 2) Weigh 1.5mmol ethyl xanthate silver precursor, 1mmol lead acetate, 1.5mmol antimony trichloride, and add them to a mixed solvent consisting of 20mL octadecene, 5mL dodecanethiol and 2mL oleylamine, Stir evenly to form a mixed reaction solution.
[0038] 3) Transfer the obtained mixed reaction solution to a three-necked flask, install a reflux system, and gradually raise the tem...
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