Boron-containing polycarbosilane and preparation method thereof
A carbosilane and metal technology, which is applied in the field of boron-containing polymetallic carbosilane and its preparation, can solve the problems of difficult inside fibers, uneven distribution of B elements, large diffusion resistance of B elements, etc., and achieves simple reaction steps and reaction conditions. Simple, mild reaction conditions
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Embodiment 1
[0044] Example 1, see figure 1 :
[0045] The invention provides a boron-containing polymetallocarbosilane and a preparation method thereof, comprising the steps of:
[0046] 1) Inactivation of polymetallocarbosilane: Take 350g of polyzirconium carbosilane and 650g of xylene and put them into a medium 2L high-pressure reactor, first replace the air in the reactor with high-purity nitrogen, and then inject a pressure of 0.3 0.8L of high-purity ammonia gas at MPa, close the reactor, heat up to 350°C and keep it warm for 5h, then cool to room temperature;
[0047] 2) One-time solvent extraction: remove a small amount of precipitate in the reactant solution to obtain solution G1, remove the solvent in solution G1, and obtain 336g of dark brown solid, which is the inactivated polyzirconium carbosilane A1, and A1 is measured The mass content of chloride ions is 0.15%;
[0048] 3) Adding boron to polymetallocarbosilane: put 88g of A1 sample, 29g of dimethylamine borane (DMAB), and...
Embodiment 2
[0051] Example 2, see figure 2 :
[0052] The invention provides a boron-containing polymetallocarbosilane and a preparation method thereof, comprising the steps of:
[0053] 1) Polymetallocarbosilane inactivation and adding boron: Take 350g of polyzirconium carbosilane, 21g of dimethylamine borane (DMAB), and 851g of xylene into a medium 2L high-pressure reactor, and first replace the reactor with high-purity nitrogen Then, 0.8L of high-purity ammonia gas with a pressure of 0.3MPa was introduced into the reactor, the reactor was closed, the temperature was raised to 160°C for 2.5 hours, and then heated to 350°C for 2.5 hours, and then cooled to room temperature;
[0054] 2) Solvent removal: remove a small amount of precipitate in the reactant solution to obtain solution G3, remove the solvent in solution G3, and obtain 54 g of dark brown solid, which is to deactivate polyzirconium borocarbosilane A3 after adding boron, and measure The mass content of chloride ion obtained ...
Embodiment 3
[0056] Example 3, see Figure 3 to Figure 4 :
[0057] The present invention provides a method for preparing composite carbides of boron-containing polymetallocarbosilane, comprising the following steps: heating 2 g of boron-containing polyzirconium carbosilane prepared in Example 1 under an Ar atmosphere, and raising the temperature at 2° C. / min to 1600°C and keep it warm for 1h, then lower the temperature at 10°C / min to obtain about 1.2g of gray-black solid.
[0058] Adopt XRD to carry out measurement, the result shows as image 3 As shown, diffraction peaks appear at 2θ angles of 33.05°, 38.35°, 55.36°, and 66.01°, which coincide with the characteristic peaks of face-centered cubic ZrC; The characteristic peaks of center-cubic SiC coincide; diffraction peaks appear at 25.21°, 32.64°, and 41.69°, which are consistent with those of hexagonal ZrB 2 The characteristic peaks match, proving that the obtained solid is SiC ZrC ZrB 2 Complex.
[0059] Since the atomic numbers o...
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