The pyrolysis of cross‐linked polycarbosilanes, polysilanes and polysilazanes in an ammonia atmosphere to 1473 K yields amorphous, low‐carbon silicon nitride powders. The efficacy of carbon removal is independent of the polymer's structure or functionality but is partially dependent on the initial cross‐linking temperature. The amorphous silicon nitride powders partially crystallize to α‐Si3N4 by 1773 K.
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