A kind of preparation method of rare metal boride
A rare metal, boride technology, applied in the direction of metal boride, boron/boride, etc., can solve the problems of process energy consumption, high cost, product purity decline, difficult industrial application, etc., to improve the reaction conversion rate and crystallinity. Good, high conversion rate
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Embodiment 1
[0028] Take 1.2kg of tantalum oxide, 0.6kg of boron carbide, and 0.6kg of metal aluminum powder, mix them evenly, put them into the mold, press them at 70MPa and 120°C for 20min, put the formed sample blocks into the roasting furnace, and vacuum them. After inhalation, the mixed gas of hydrogen and argon with a hydrogen concentration of 2% was introduced at a rate of 1L / min, and the temperature was raised to 600°C at a rate of 2°C / min. After 60 minutes, cool down to room temperature at a cooling rate of 5°C / min. After the product is crushed and sieved, the obtained powder product is mixed with H + Dilute nitric acid with a concentration of 1mol / L was mixed at a solid-to-liquid ratio of 1:10, leached in a water bath at 60°C for 30 minutes and then filtered, and the filter residue was washed and dried to constant weight to obtain tantalum diboride powder. The product XRD pattern is attached figure 1 shown.
Embodiment 2
[0030] Take 1.6kg of tungsten trioxide, 0.5kg of boron oxide, and 0.4kg of tin powder, mix them evenly, put them into the mold, press them at 20MPa and 100°C for 20min, put the formed sample blocks into the roasting furnace, and vacuum them. After inhalation, a mixed gas of hydrogen and argon with a hydrogen concentration of 10% was introduced at a rate of 1.2L / min, and the temperature was raised to 1000°C at a rate of 5°C / min. After continuing to keep warm for 30 minutes, cool down to room temperature at a cooling rate of 5°C / min. After the product is crushed and sieved, the obtained powder product is mixed with H + Dilute hydrochloric acid with a concentration of 1.5mol / L was mixed at a solid-to-liquid ratio of 1:10, leached in a water bath at 80°C for 30 minutes and then filtered, and the filter residue was washed and vacuum-dried to constant weight to obtain ditungsten pentaboride powder. The product XRD pattern is attached figure 2 shown.
Embodiment 3
[0032] Take 0.6kg of chromium carbide powder, 1.2kg of boron oxide, and 0.1kg of metal aluminum powder, mix them evenly, put them into the mold, press them at 70MPa and 120°C for 20min, put the formed sample block into the roasting furnace, and vacuum After purging, feed a mixed gas of hydrogen and argon with a hydrogen concentration of 10% at a rate of 1 L / min, raise the temperature to 500 °C at a rate of 10 °C / min, keep warm for 360 min, and then continue to heat up to 1600 °C at a rate of 40 °C / min. After 90 minutes of heat preservation, the temperature was lowered to room temperature at a rate of 5°C / min. After the product is crushed and sieved, the obtained powder product is mixed with nitric acid: hydrochloric acid at a ratio of H + Dilute hydrochloric acid with a concentration of 3 mol / L was mixed at a solid-to-liquid ratio of 1:5, leached in a water bath at 60°C for 180 minutes, filtered, and the filter residue was washed and dried to constant weight to obtain tantalum...
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