A kind of preparation method and application of hfc ceramic precursor
A ceramic precursor and reaction technology, which is applied in the field of preparation of HfC ceramic precursors, can solve the problems of low yield of ultra-high temperature resistant ceramics and low content of ultra-high temperature resistant components, and achieve high ceramic yield and good tolerance High temperature, good solubility effect
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[0026] The preparation method of the HfC ceramic precursor provided by the invention comprises the following steps:
[0027] Add the cyanamide organic compound into the inorganic metal hafnium compound or organic metal hafnium compound solution in the form of solution, heat it to 30-150°C at a heating rate of 0.1-2.0°C / min, and keep it at this temperature for 1-30 hours. Adjust the temperature to 30-160°C, then distill under reduced pressure for 0.5-3 hours to react, and cool to room temperature after the reaction to obtain the HfC ceramic precursor; the molar ratio of the inorganic metal hafnium compound to the cyanamide organic compound is 1:0.1- 10 mixed, or organic metal hafnium compound mixed with cyanamide organic compound at a molar ratio of 1:0.1-10; the inorganic metal hafnium compound is hafnium tetrachloride and hafnium oxychloride.
[0028] The method can improve the ceramic yield when the prepared precursor is used to prepare ultra-high temperature resistant HfC c...
Embodiment 1
[0038] (1) Take hafnium tetrachloride 0.03mol, dicyandiamide 0.03mol;
[0039] (2) hafnium tetrachloride and dicyandiamide are dissolved in acetonitrile;
[0040] (3) Vacuumize and fill the 250ml three-necked flask with agitator, constant pressure funnel and distillation device three times, and then cool the reactor to minus 30°C;
[0041] (4) Add the acetonitrile solution of hafnium tetrachloride into a three-necked flask protected by dry argon, and then add the acetonitrile solution of dicyandiamide into the constant pressure funnel. While stirring, the acetonitrile solution of dicyandiamide is added in the three-necked flask in a dropwise manner;
[0042] (5) After the dropwise addition, the reactor was heated to 50° C. at a rate of 1.0° C. / min, and kept at this temperature for 8 hours;
[0043] (6) Reduce the temperature of the reactor to 30° C., distill under reduced pressure at this temperature for 0.5 hours (vacuum degree 1 kPa), and cool to room temperature to obtain a...
Embodiment 2
[0049] This embodiment includes the following steps:
[0050] (1) Weigh 0.03mol of hafnium dichloride and 0.03mol of dicyandiamide;
[0051] (2) hafnium dichloride and dicyandiamide are dissolved in acetonitrile;
[0052] (3) Vacuumize and fill the 250ml three-necked flask with agitator, constant pressure funnel and distillation device three times, and then cool the reactor to minus 30°C;
[0053] (4) Add the acetonitrile solution of hafnocene dichloride into a three-necked flask protected by dry argon, and then add the acetonitrile solution of dicyandiamide into the constant pressure funnel. While stirring, the acetonitrile solution of dicyandiamide is added in the three-necked flask in a dropwise manner;
[0054] (5) After the dropwise addition, the reactor was heated to 100° C. at a rate of 1.0° C. / min, and kept at this temperature for 8 hours;
[0055] (6) Reduce the temperature of the reactor to 30° C., distill under reduced pressure at this temperature for 0.5 hours (...
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