화학공학소재연구정보센터
Thin Solid Films, Vol.247, No.2, 169-177, 1994
Effect of Oxygen and Carbon on the Formation and Stability of A-15 Crystal-Structure Chromium Thin-Films
The effect of oxygen and carbon impurities on the crystal structure, chemical binding states and phase transformation of r.f. sputter-deposited Cr thin films was investigated. It was found that when the O and C concentrations in the films were each within the range of 8-15 at.% (total impurity concentration between 15 and 30 at.%) the crystal structure of the Cr films was cubic A-15. Body-centered cubic (b.c.c.) Cr films formed when the total impurity concentration was <15 at.% or >30 at.%. The binding energy states of Cr, O and C were identical in the A- 1 5 and low-impurity b.c.c. Cr films. Cr and O were found to be predominantly in an elemental or unbound state while the binding energy of C was indicative of a chromium carbide compound. Studies of the A-15 to b.c.c. Cr phase transformation were done by vacuum annealing samples for 1 h at temperatures in the 200-500-degrees-C range. Characterization of the annealed Cr films demonstrated that the transformation occurred without a measurable change in either the atomic concentration or the binding energy states of the elements in the films. X-ray diffraction studies of the A-15 --> b.c.c. phase transformation indicated that complete transformation of A-15 Cr into b.c.c. Cr required an annealing temperature between 400-degrees-C and 500-degrees-C. Differences in the annealing temperature required to fully transform A-15 Cr into b.c.c. Cr were attributed to differences in impurity concentration among the as-deposited films; the higher the impurity concentration in the film, the higher the temperature need.ed to completely transform an A-15 structure into a b.c.c. structure. Vacuum heat treatments of 25 nm thick Cr films done in situ in a transmission electron microscope revealed that the A-15 to b.c.c. transformation occurred by nucleation and growth of b.c.c. particles from the A-15 matrix. Therefore, it was concluded that Cr films with an A-15 crystal structure are an impurity-locked, metastable phase that transforms into a b.c.c. crystal structure at T/T(m) almost-equal-to 0.3 by a nucleation and growth mechanism.