Preparing method of superfine/nano tantalum tungsten composite powder and superfine/nano tantalum tungsten composite powder prepared through same
A technology of composite powder and nano-tantalum, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc.
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[0061] The invention provides a preparation method of ultrafine / nanometer tantalum-tungsten composite powder, which includes using fluorotantalic acid solution and tungstate as raw materials, including sol-co-precipitation, hydrogen reduction, alkali metal reduction, and magnesium reduction to remove oxygen. The specific operations The steps are:
[0062] I. Sol-Co-precipitation
[0063] First add the calculated amount of ammonium paratungstate or ammonium metatungstate powder into the fluorotantalic acid solution, and then add 0.1% to 3% of the volume of the fluorotantalic acid solution selected from PEG-400, PEG-600, PEG-1000 and PEG-2000 One or more surfactants, stirred to prepare a sol solution; then, under ultrasonic vibration or stirring, slowly add ammonia water to pH=9-12, let stand and age for 20 minutes to 4 hours, detect and adjust the pH of the solution pH value to the pH value before standing, suction filtration; the precipitate is washed with drum ammonia hot pu...
Embodiment 1
[0081]Example 1 Preparation of Ta-10wt%W Ultrafine / Nanocomposite Powder
[0082] Step 1, sol-co-precipitation
[0083] (1) Weigh 406g of ammonium paratungstate (APT) and dissolve it into a container containing 30L of fluorotantalic acid solution, and add dropwise 300ml of surfactant polyethylene glycol PEG-600, and stir thoroughly for 30 minutes to obtain a sol solution; wherein tantalum fluoride The acid solution is calculated as tantalum oxide, the concentration is 100g / L, and the HF concentration is 1.2mol / L.
[0084] (2) Slowly add concentrated ammonia water (concentration 9.6N) in the sol solution, stir constantly while adding, until the pH=9~10 of solution, stop dripping strong ammonia water, leave standstill after 30 minutes, detect the change of pH value, ensure The pH value of the solution=9~10.
[0085] (3) Use a suction filter to filter the precipitate, and sequentially use 0.3 mol / L drum ammonia hot pure water at 75°C to fully wash and filter the precipitate unt...
Embodiment 2
[0095] Implementation 2 Preparation of Ta-20wt%W Ultrafine / Nanocomposite Powder
[0096] Step 1, sol co-precipitation
[0097] (1) Weigh 916g of ammonium paratungstate (APT) and dissolve it in a plastic bucket containing 30L of fluorotantalic acid solution, add dropwise 300ml of surfactant polyethylene glycol PEG-1200, and stir thoroughly for 30 minutes. A sol solution was obtained; wherein the tantalum fluoride solution was calculated as tantalum oxide, the concentration was 100 g / L, and the HF concentration was 1.2 mol / L.
[0098] (2) Slowly add concentrated ammoniacal liquor (concentration 9.6N) in the sol solution, stir constantly while adding, until the pH value of solution is slightly greater than 9, stop dripping concentrated ammoniacal liquor, leave standstill and detect pH value change after 30 minutes, ensure The pH of the solution was 9.
[0099] (3) Use a suction filtration system to filter the precipitate, and use 40-50°C ammonia concentration of 0.3mol / L dru...
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