High pressure liquid phase synthesis method of titanium nitride nanopowder
A technology of nano-powder and high-pressure liquid phase, which is applied in the direction of nitrogen compounds, chemical instruments and methods, nanotechnology, etc., can solve the problems of difficult control of the reaction process, high reaction temperature, high energy consumption, etc., and achieve low production cost and high reaction efficiency The effect of low energy consumption and high purity
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Embodiment 1
[0033] refer to figure 1 , a titanium nitride nano powder high-pressure liquid phase synthesis method, comprising the following steps:
[0034] Step A: Using toluene as a reaction aid, add liquid ammonia to the toluene, after the liquid ammonia and toluene are separated into layers, add titanium tetrachloride to the toluene and carry out a chemical reaction at -34°C and 0.2MPa. Washing is performed after the reaction is completed to obtain a titanium nitride precursor; wherein, before the chemical reaction starts, the mass ratio of titanium tetrachloride, liquid ammonia, and reaction aid is controlled to be 1:2:6.
[0035] Step B: Calcining the titanium nitride precursor obtained in step A under a nitrogen protective atmosphere, the calcination temperature is 400°C, and the calcination time is controlled at 150min, and finally titanium nitride nanopowder is obtained. After testing, the titanium nitride nanopowder The average particle size of the body is 40nm, and the average ...
Embodiment 2
[0039] A high-pressure liquid phase synthesis method of titanium nitride nanopowder, comprising the following steps:
[0040] Step A: Using toluene as a reaction aid, add liquid ammonia to the toluene, after the liquid ammonia and toluene are stably separated, add titanium tetrachloride to the toluene and carry out a chemical reaction at -20°C, 0.3Mpa, Washing is performed after the reaction is completed to obtain a titanium nitride precursor; wherein, before the chemical reaction starts, the mass ratio of titanium tetrachloride, liquid ammonia, and reaction aid is controlled to be 1:4:2.
[0041] Step B: Calcining the titanium nitride precursor obtained in step A under a helium protective atmosphere, the calcination temperature is 800°C, and the calcination time is controlled at 60 minutes, and finally titanium nitride nanopowder is obtained. The average particle size of the powder is 70nm, and the average grain size is 20nm.
Embodiment 3
[0043] A high-pressure liquid phase synthesis method of titanium nitride nanopowder, comprising the following steps:
[0044] Step A: Using toluene as a reaction aid, add liquid ammonia to the toluene, after the liquid ammonia and toluene are separated into layers, add titanium tetrachloride to the toluene and carry out a chemical reaction at -10°C and 0.4MPa. After the reaction is finished, washing is performed to obtain a titanium nitride precursor; wherein, before the chemical reaction starts, the mass ratio of titanium tetrachloride, liquid ammonia, and reaction aid is controlled to be 1:3:5.
[0045] Step B: The titanium nitride precursor obtained in step A is roasted under an argon protective atmosphere, the roasting temperature is 1000 ° C, and the roasting time is controlled at 60 minutes, and finally titanium nitride nanopowder is obtained. The average particle size of the powder is 200nm, and the average grain size is 60nm.
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