A method for producing titanium nitride and titanium carbonitride by two-stage reduction nitriding
A technology for titanium carbonitride and titanium nitride, which is applied in the field of preparation of titanium nitride and titanium carbonitride, can solve the problems of decreased product purity, difficulty in industrialized production, slow solid solution process, etc., and achieves uniform particle size and easy Industrial production, fine-grained effect
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Embodiment 1
[0018] The present invention analyzes pure TiO 2 , carbon black (99.85wt%) as raw material, according to TiO 2 : C molar ratio is 1:1.6, and then use a mortar to mix the prepared raw materials evenly; put the mixed raw materials into a high-temperature furnace, and heat them to 1400 °C at a heating rate of 5 °C / min under argon flow ℃, keep it warm for 4 hours, and then drop to room temperature to get TiC x o y Precursor, the measured carbon content is 6.12wt%, and the oxygen content is 17.35wt%. Taking the preparation of TiN as an example, according to the reaction formula Add 6.90wt% carbon, mix evenly by ball milling at 200rpm for 3 hours; put the mixed raw materials into a high-temperature furnace, heat to 1800°C at a heating rate of 5°C / min under nitrogen flow, keep it warm for 2 hours, and then lower it to room temperature to obtain a titanium nitride product with a carbon content of about 0.23wt%, an oxygen content of about 0.48wt%, a nitrogen content of about 21.93w...
Embodiment 2
[0020] Embodiment 2 is basically the same as Embodiment 1, the difference is:
[0021] By TiO 2 :C molar ratio is 1:2, heated to 1500°C at a heating rate of 5°C / min under argon flow, kept for 1 hour, and then lowered to room temperature to obtain TiC x o y Precursor, the measured carbon content is 10.48wt%, and the oxygen content is 11.90wt%; to prepare TiC 0.5 N 0.5 For example, according to the reaction formula Add carbon to 8.16wt%, and mix evenly by ball milling at 400rpm for 6 hours; put the mixed raw materials into a high-temperature furnace, heat up to 1700°C at a heating rate of 5°C / min under nitrogen flow, keep it warm for 4 hours, and then lower it to room temperature , to obtain TiC with a carbon content of about 9.66wt%, an oxygen content of about 0.42wt%, a nitrogen content of about 11.27wt%, and a particle size of less than 1 μm 0.5 N 0.5 product. The XRD analysis showed that the product phase was TiC 0.5 N 0.5 , without other phases; SEM showed that th...
Embodiment 3
[0023] Embodiment 3 is basically the same as Embodiment 1, the difference is:
[0024] By TiO 2 :C molar ratio is 1:1.8, heated to 1600°C at a heating rate of 5°C / min under argon flow, kept for 4 hours, and then lowered to room temperature to obtain TiC x o y Precursor, the measured carbon content is 8.48wt%, and the oxygen content is 14.40wt%; to prepare TiC 0.3 N 0.7 For example, according to the reaction formula Add 8.11wt% carbon, mix evenly by ball milling at 300rpm for 4 hours; put the mixed raw materials into a high-temperature furnace, heat to 1600°C at a heating rate of 5°C / min under nitrogen flow, keep it warm for 8 hours, and then lower it to room temperature , to obtain TiC with a carbon content of about 5.75wt%, an oxygen content of about 0.48wt%, a nitrogen content of about 15.64wt%, and a particle size of less than 1 μm 0.3 N 0.7 product. The XRD analysis showed that the product phase was TiC 0.3 N 0.7 , without other phases; SEM showed that the finally...
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