Metastable phases, 304 stainless steel, Sputter depsoited coatings, Mechanically milled powders, Transmission electron microscopy, Three dimensional atom probe


Study of the metastable phases obtained by non-equilibrium processing techniques has come a long way during the past five decades. New metastable phases have often given new perspectives to the research on synthesis of novel materials systems. Metastable materials produced by two non-equilibrium processing methods were studied for this dissertation- 304-type austenitic stainless steel (SS304 or Fe-18Cr-8Ni)+aluminum coatings produced by plasma enhanced magnetron sputter-deposition (PEMS) and nanocrystalline Ti, Zr and Hf powders processed by mechanical milling (MM). The objective of the study was to understand the crystallographic and microstructural aspects of these materials. Four SS304+Al coatings with a nominal Al percentages of 0, 4, 7 and 10 wt.% in the coatings were deposited on an SS304 substrate by PEMS using SS304 and Al targets. The as-deposited coatings were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and three-dimensional atom probe microscopy (3DAP). Surface morphology and chemical analysis were studied by SEM. Phase identification was carried out by XRD and TEM. The microstructural features of all the coatings, as observed in the TEM, consisted of columnar grains with the columnar grain width (a measure of grain size) increasing with an increase in the Al content. The coatings had grains with average grain sizes of about 100, 290, 320 and 980 nm, respectively for 0, 4, 7 and 10 wt.% Al. The observed grain structures and increase in grain size were related to substrate temperature during deposition. XRD results indicated that the Al-free coating consisted of the non-equilibrium ferrite and sigma phases. In the 4Al, 7Al and 10Al coatings, equilibrium ferrite and B2 phases were observed but no sigma phase was found. In 10Al coating, we were able to demonstrate experimentally using 3DAP studies that NiAl phase formation is preferred over the FeAl phase at nano scale. During mechanical milling of the hexagonal close packed (HCP) metals Hf, Ti and Zr powders, unknown nanocrystalline phases with face centered cubic (FCC) structure were found. The FCC phases could be either allotropes of the respective metals or impurity stabilized phases. However, upon MM under high purity conditions, it was revealed that the FCC phases were impurity stabilized. The decrease in crystallite size down to nanometer levels, an increase in atomic volume, lattice strain, and possible contamination were the factors responsible for the transformation.


If this is your thesis or dissertation, and want to learn how to access it or for more information about readership statistics, contact us at

Graduation Date



Suryanarayana, Challapalli


Doctor of Philosophy (Ph.D.)


College of Engineering and Computer Science


Mechanical, Materials, and Aerospace Engineering

Degree Program

Materials Science and Engineering








Release Date

May 2010

Length of Campus-only Access


Access Status

Doctoral Dissertation (Open Access)