Date of Award

Fall 2002

Document Type

Dissertation

Degree Name

Doctor of Philosophy in Electrical Engineering - (Ph.D.)

Department

Electrical and Computer Engineering

First Advisor

Marek Sosnowski

Second Advisor

Roy H. Cornely

Third Advisor

Haim Grebel

Fourth Advisor

Zafar Iqbal

Fifth Advisor

J. K. Hirvonen

Abstract

The goal of this thesis was to provide scientific and technical research results for developing and characterizing tantalum (Ta) coatings on steel substrates deposited by DC magnetron sputtering. Deposition of tantalum on steel is of special interest for the protection it offers to surfaces, e.g. the surfaces of gun barrels against the erosive wear of hot propellant gases and the mechanical damage caused by the motion of launching projectiles. Electro-plated chromium is presently most commonly used for this purpose; however, it is considered to be carcinogenic in its hexavalent form. Tantalum is being investigated as non-toxic alternative to chromium and also because of its superior protective properties in these extreme environments.

DC magnetron sputtering was chosen for this investigation of tantalum coatings on steel substrates because it is a versatile industrial proven process for deposition of metals. Sputter deposited Ta films can have two crystallographic structures: 1) body center cubic (bcc) phase, characterized by high toughness and high ductility and 2) a tetragonal beta phase characterized by brittleness and a tendency to fail under stress. It was found in this work that the bcc Ta coatings on steel can be obtained reliably by either of two methods: 1) depositing Ta on a submicron, stoichiometric TaN seed layer reactively sputtered on unheated steel and 2) depositing Ta directly on steel heated above a critical temperature. For argon sputtering gas this critical temperature was found to be 400°C at a pressure of 5 mtorr. With the heavier krypton gas, this critical temperature is reduced to 350°C.

X-ray diffraction (XRD) was used to investigate the structure of tantalum and nitride films, and the composition of the nitride films was measured by nuclear reaction analyses (NRA), which were used to study in detail the enhancement of the bcc phase of Ta on steel. The scratch adhesion tests performed with a diamond hemispherical tip of radius 200 µm under increasing loads revealed high critical load values for failure (>15 N) for the bcc coatings versus the low load values (<9 N) for the beta coatings. The coating deposited on TaN interlayers on sputter-etched steel had better adhesion than those on steel surface without sputter etching.

The results for this work have demonstrated that by controlling the various process parameters of dc magnetron sputtering, high quality bcc Ta coatings of multimicron thickness with excellent adhesion to steel can be made. An important contribution of this dissertation is in the enhancing an understanding of this process. The impact of this research will be in a number of fields where superior protective castings are needed. These include military applications, electronic components, chemical processing, and others.

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