A monodisperse flower-like globular mos 2 Preparation method of powder
A flower-shaped, monodisperse technology, which is applied in the direction of nanotechnology, nanotechnology, structural parts, etc. for materials and surface science, can solve the problems of not being easy to obtain, difficult to control the preparation process, and cumbersome process, and achieve low cost of raw materials , Uniform particle size and controllable steps
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Embodiment 1
[0022] (1) Weigh 0.196g ammonium molybdate and 0.076g thiourea according to the Mo:S element molar ratio of 1:1, dissolve ammonium molybdate in 50mL deionized water to obtain solution A, and dissolve thiourea in 21.5mL B Diol to make Solution B.
[0023] (2) In the solution A that step (1) makes, drip ammonia solution and adjust its pH value to be 9, make solution C, in the solution B that step (1) makes, drop 1mL concentration and be 95% Diamine solution, prepared solution D, sealed the prepared solution C and solution D respectively, stirred for 30 minutes, then mixed solution C and solution D, stirred for 30 minutes to prepare a mixed solution.
[0024] (3) Pour the mixed solution prepared in step (2) into the reactor and seal it, transfer the reactor to the microwave reactor, set the microwave power to 200W, the heating rate to 5°C / min, and raise the temperature to 180°C for 6 hours , after the reaction was completed, it was cooled to room temperature to obtain a suspensi...
Embodiment 2
[0027] (1) Weigh 1.235g ammonium heptamolybdate and 0.655g sodium sulfide according to Mo:S element molar ratio of 1:1.2, dissolve ammonium heptamolybdate in 20mL deionized water to prepare solution A, dissolve sodium sulfide in 46.6 mL diethylene glycol to obtain solution B.
[0028] (2) Add dropwise sodium hydroxide solution to the solution A made in step (1) to adjust its pH value to 12 to make solution C, and add 5 mL dropwise to the solution B made in step (1) with a concentration of 95%. n-Butylamine solution, prepared solution D, sealed the prepared solution C and solution D respectively, stirred for 120 minutes, then mixed solution C and solution D, stirred for 120 minutes to prepare a mixed solution.
[0029] (3) Pour the mixed solution prepared in step (2) into the reactor and seal it, transfer the reactor to the microwave reactor, set the microwave power to 500W, the heating rate to 20°C / min, and heat up to 200°C for 1 hour , after the reaction was completed, it wa...
Embodiment 3
[0032] (1) Weigh 0.628g ammonium tetramolybdate and 0.331g thioacetamide according to Mo:S element molar ratio of 1:1.1, dissolve ammonium tetramolybdate in 25mL deionized water to prepare solution A, and dithioethyl Solution B was prepared by dissolving the amide in 25 mL of glycerol.
[0033] (2) Add potassium hydroxide solution dropwise to the solution A prepared in step (1) to adjust its pH value to 10 to obtain solution C, and add 2.5mL solution dropwise to the solution B prepared in step (1) with a concentration of 95 % triethylamine solution to prepare solution D, seal the prepared solution C and solution D respectively, stir for 60 minutes, then mix solution C and solution D, and stir for 60 minutes to prepare a mixed solution.
[0034] (3) Pour the mixed solution prepared in step (2) into the reaction kettle and seal it, transfer the reaction kettle to the microwave reactor, set the microwave power to 400W, the heating rate to 10°C / min, and raise the temperature to 19...
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