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A Study of Nitrogen-Containing, High Manganese Austenitic Stainless Steel Coatings Deposited by Sputter PVD

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A Study of Nitrogen-Containing, High Manganese Austenitic Stainless Steel Coatings Deposited by Sputter PVD A study of nitrogen-containing, high manganese austenitic stainless steel coatings deposited by sputter PVD By: Lynne Hopkins A thesis submitted in partial fulfilment of the requirements for the degree of Doctor of Philosophy The University of Sheffield Faculty of Materials Science and Engineering July, 2019 ABSTRACT The use of nitrogen as an alloying element in steel is either limited to small quantities (<2 wt% / 7. 5 at%) in bulk materials, where it is used primarily as an austenite stabiliser and mechanical/tribological property enhancer, or introduced in much larger quantities (e.g. 38 at%) in thermochemical surface engineering treatments – where it is used to create a hard, corrosion-resistant diffusion layer of typically 20-30 μm depth, commonly referred to as “Expanded austenite” or “S-phase”. This study examines the effects of nitrogen incorporation in a high-manganese austenitic stainless steel (Staballoy AG 17), at levels that lie between these two extremities with the intention of improving the mechanical and wear properties without compromising the inherent high resistance to corrosion which such alloys possess. Thick, dense and featureless coatings of austenitic-manganese steel containing different levels of interstitial nitrogen were deposited by reactive magnetron sputtering in an argon-nitrogen plasma. The resulting microstructures, characterized by XRD, SEM/EDX, nano-indentation, and fracture analysis were found to exhibit a texture and a small nitrogen gradient across their thickness. With increasing nitrogen content, the hardness was observed to increase and the morphology changed. Moreover, changes in nitrogen content were found to have a more profound effect on the coating properties than any of the process parameters evaluated, the results of which are presented. Excessive nitrogen resulted in the precipitation of Mn4N, apparently avoiding chromium sensitisation. Finally, since the deposited coatings were characterized by high compressive stresses, the stresses involved and the failure modes observed are discussed. i ACKNOWLEDGEMENTS I truly appreciate the opportunity to work on this project given by: my supervisors – Dr Adrian Leyland and Prof Allan Matthews; Dr Glen Cassar and Dr Ann Zammit; and the European Research Council that funded the research. I would also like to express my most sincere gratitude to Dr Adrian Leyland for his invaluable insights, guidance, supervision and support throughout the research. The help and assistance given by Ms Dawn Bussey with nano-indentation, Dr Nik Reeves McLaren with the XRD technique and Dr Le Ma, Dr Cheryl Shaw and Dr Peter Korgul with the SEM/EDX equipment is very much appreciated. Special thanks go to Mr John Lowndes, who gave invaluable technical support on the PVD equipment. I am also grateful to my colleagues and (mostly) former members of the RSCE group Dr Gorkem Yumusak, Dr Xingguang Liu, Mr David Brown, Dr Xiao Tao, Dr Chang Liu, Dr Wei-Yu Chen and Dr Hussein Meshrghi. I would also like to offer sincere thanks to the University of Malta, department of Metallurgy & Materials Engineering staff, particularly Dr Glen Cassar, Prof Joseph Buhagiar and Dr Ann Zammit, for providing use of and assistance with the equipment at the University of Malta. Special thanks go to my friends in Sheffield, most especially Ms Hande Özbayraktar, for being like a sister to me; and Mr Nikola Tanov, for not only being a friend, but also for helping me with his experience on SEM/EDX. Finally, I would like to thank my beloved parents for their support – both moral and financial – and my husband Dr Emir Avcioglu, for his love and endless support, without which, I would not have completed my PhD. ii CONTENTS ABSTRACT .......................................................................................................................... i ACKNOWLEDGEMENTS ......................................................................................................ii LIST OF FIGURES .............................................................................................................vii LIST OF TABLES ................................................................................................................ xi CHAPTER 1: INTRODUCTION .............................................................................................. 1 1.1 Introduction ................................................................................................................ 1 1.2 Aims and objectives ................................................................................................... 3 1.3 Thesis layout .............................................................................................................. 4 CHAPTER 2. NITROGEN IN STAINLESS STEEL ..................................................................... 5 2.1 Stainless steel ............................................................................................................. 5 2.1.1 Introduction ......................................................................................................... 5 2.1.2 Classification of steels ......................................................................................... 5 2.1.3 Stainless steel ....................................................................................................... 6 2.2 Nitrogen alloying of steels ....................................................................................... 12 2.2.1 Nitrogen in bulk ................................................................................................. 12 2.2.2 Surface treatments ............................................................................................. 14 CHAPTER 3: PVD AND PROPERTIES OF DEPOSITED COATINGS ........................................ 19 3.1 PVD processing ........................................................................................................ 19 3.1.1 Introduction ....................................................................................................... 19 3.1.2 Sputter deposition .............................................................................................. 21 3.1.3 Magnetron sputtering ......................................................................................... 24 3.1.4 Unbalanced magnetron sputtering ..................................................................... 25 iii 3.2 Process parameters ................................................................................................... 28 3.2.1 Base pressure ..................................................................................................... 28 3.2.2 Working pressure ............................................................................................... 28 3.2.3 Reactive sputtering ............................................................................................ 30 3.2.4 Target power ...................................................................................................... 32 3.2.5 Pulsed magnetron sputtering ............................................................................. 34 3.2.6 Target-to-substrate distance ............................................................................... 38 3.2.7 Substrate bias ..................................................................................................... 38 3.2.8 Substrate pulsed bias ......................................................................................... 39 3.2.9 Substrate temperature ........................................................................................ 41 3.3 Coating Characteristics ............................................................................................ 43 3.3.1 Structure-zone models ....................................................................................... 43 3.3.2 Coatings from alloy or compound targets ......................................................... 47 3.3.3 Stress .................................................................................................................. 47 3.3.4 Adhesion ............................................................................................................ 54 3.4 Sputtering of austenitic stainless steel coatings ....................................................... 55 CHAPTER 4 – EXPERIMENTAL EQUIPMENT AND PROCEDURES ......................................... 63 4.1 Materials used .......................................................................................................... 63 4.2 Substrate preparation ................................................................................................ 64 4.3 Coating deposition .................................................................................................... 65 4.3.1 Deposition apparatus ......................................................................................... 65 4.3.2 Equipment preparation ...................................................................................... 67 4.3.3 Deposition procedure ......................................................................................... 68 4.4 Analytical techniques ............................................................................................... 69 4.4.1 X-Ray diffraction ............................................................................................... 70 4.4.2 Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) ..........................................................................................
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