Synthesis Of Mesoporous TiN Powder Via Ammonia Reduction Nitridation Reaction

Mesoporous titanium nitride?TiN?has been used as supercapacitor and catalyst support due to its electrochemistry performance.The preparation of mesoporous TiN powder with excellent performance is one of research hotspots.Therefore the mesoporous TiN powder was systhesized by reduction-nitridation reaction based on the hydrolytic sol-gel?HSG?and nonhydrolytic sol-gel?NHSG?process.In reduction-nitridation reaction based on the HSG process,the powders with a mixture of anatase and rutile phase and low activity were obtained when reduction nitridation temperature was 700?.Powders were Ti O phase after reduction nitridation at 800?;For reduction-nitridation reaction based on NHSG process,powders were anatase phase and had relatively high activity when reduction nitridation temperature was 700?.Powders became Ti?N,O?phase reduction nitridation at 800?.TiO₂ powders were converted to TiN as the reduction nitridation temperature increasing.In comparison,the morphology of mesoporous TiN powers systhesized by NHSG combined with the ammonia reduction technique had high pure and smaller grain size.The optimum process parameters for the synthesis of mesoporous TiN powder by ammonia reduction-nitridation reaction based on NHSG process were as follows: the gelation temperature was 110?,suitable gelation time was 38 h,reasonanle calcining temperature was 600?,ammonia flow was 800ml/min,holding time was 2h and heating rate was 1?/min.The BET specific surface area and electric capacity of high purity mesoporous TiN powders obtained 71.342 m2/g and 164F/g.The TiN powders synthesised by adding F127 and P123 were disordered mesoporous.Furthermore,ordered mesoporous TiN powders were synthesized by further adding cyanamide,whose lattice constants was 4.2135?.The TiN powders with spherical particles had high surface area?97.462m2/g?,small average pore diameter?14.2nm?and narrow pore size distributed between 5nm and 40 nm.The TiN powders had good square resistance capacitance of electric double layer and its electric capacitywas 213F/g.