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Plasma-assisted synthesis and physical chemical characterization of titanium nitride films

Technical Report ·
OSTI ID:5312357

TiN films synthesized by radio-frequency plasma-assisted chemical vapor deposition onto M2 tool steel were investigated. TiCl/sub 4/ with NH/sub 3/ or with H/sub 2/ and N/sub 2/ were used 0.2 to 1.0 torr. Film composition, structure, and mechanical properties were strongly influenced by chlorine concentration within the filsm and at the film-substrate interfaces. Chlorine concentration in the films decreased with increasing deposition temperature. A transition from an amorphous zone one morphology, to a fine-grained zone T morphology, to a highly crystalline zone two morphology with (200) preferred orientation was observed with increasing deposition temperature. Films formed at temperatures lower than 400/sup 0/C exhibited poor mechanical properties. At 400/sup 0/C and above, film adhesion was influenced by initial deposition conditions. Films formed from TiCl/sub 4/ and NH/sub 3/ had low scratch adhesion test critical loads, with fracture occurring at the interface. Auger analysis of scratch tracks created in vacuum revealed a high interfacial chlorine content. IN contrast, films synthesized with H/sub 2/ and N/sub 2/ exhibited higher scratch adhesion test critical loads, with fracture within the film. Auger depth profilng revealed no chlorine accumulation at the interfaces of H/sub 2/-N/sub 2/-based films. Early film growth was accompanied by TiN islands. A plasma was essential for TiN synthesis from TiCl/sub 4/, H/sub 2/, and N/sub 2/. The chlorine concentrations of titanium carbonitride films, synthesized in a plasma with the addition of CH/sub 4/ showed greater variation at fixed deposition temperature than those of pure nitride films. The use of an organometallic source, titanium tetrakis dimethylamide, Ti(N(CH/sub 3/)/sub 2/)/sub 4/, resulted in the formation of carbonitride powders. 140 refs., 88 figs

Research Organization:
Lawrence Berkeley Lab., CA (USA)
DOE Contract Number:
AC03-76SF00098
OSTI ID:
5312357
Report Number(s):
LBL-24584; ON: DE88007365
Country of Publication:
United States
Language:
English