TY - JOUR
T1 - Novel zirconium nitride precursor
T2 - Synthesis, decomposition pathway, and pyrolysis of [(CH3)3Si]2NH·ZrCl4
AU - Narula, Chaitanya K.
AU - Allard, Lawrence F.
PY - 1998/8
Y1 - 1998/8
N2 - The reaction of hexamethyldisilazane with zirconium tetrachioride furnishes an adduct, [(CH3)3Si]2NH·ZrCl4, which is soluble in dichloromethane. The decomposition of [(CH3)3Si]2NH·ZrCl4 proceeds with the elimination of trimethylchlorosilane and hydrogen chloride and is complete at 600°C. The resulting powder is amorphous zirconium nitride which is highly susceptible to hydrolysis and oxidation. The pyrolysis of the precursor in a dynamic vacuum or ammonia atmosphere at 600°C and subsequent sintering of the powder at 900°C furnishes crystalline zirconium nitride. Transmission electron microscopy of the powder shows that the particles are coated with a thin zirconium oxide layer. Crystalline zirconium nitride powder, free from zirconium oxide impurities, is obtained if the sintering is carried out at 1075°C.
AB - The reaction of hexamethyldisilazane with zirconium tetrachioride furnishes an adduct, [(CH3)3Si]2NH·ZrCl4, which is soluble in dichloromethane. The decomposition of [(CH3)3Si]2NH·ZrCl4 proceeds with the elimination of trimethylchlorosilane and hydrogen chloride and is complete at 600°C. The resulting powder is amorphous zirconium nitride which is highly susceptible to hydrolysis and oxidation. The pyrolysis of the precursor in a dynamic vacuum or ammonia atmosphere at 600°C and subsequent sintering of the powder at 900°C furnishes crystalline zirconium nitride. Transmission electron microscopy of the powder shows that the particles are coated with a thin zirconium oxide layer. Crystalline zirconium nitride powder, free from zirconium oxide impurities, is obtained if the sintering is carried out at 1075°C.
UR - http://www.scopus.com/inward/record.url?scp=0001650586&partnerID=8YFLogxK
U2 - 10.1039/a802864h
DO - 10.1039/a802864h
M3 - Article
AN - SCOPUS:0001650586
SN - 0959-9428
VL - 8
SP - 1881
EP - 1884
JO - Journal of Materials Chemistry
JF - Journal of Materials Chemistry
IS - 8
M1 - 8/02864H
ER -