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Gorkem Yumusak Doctor of Philosophy

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Gorkem Yumusak Doctor of Philosophy Evaluating the Effect of Titanium-Based PVD Metallic Thin Films on Nitrogen Diffusion Efficiency in Duplex Plasma Diffusion/Coating Systems by: Gorkem Yumusak A dissertation submitted in fulfilment of the requirements for the degree of Doctor of Philosophy Department of Materials Science and Engineering AUGUST 2018 ACKNOWLEDGEMENTS Firstly, I would like to express my great appreciation to my supervisors, Dr Adrian Leyland and Prof. Allan Matthews for their encouragement, guidance, support and immense knowledge. I also gratefully thank the Council of Higher Education of Turkey and Marmara University for the financial support to cover all my expenses. Without this financial support, it would be impossible for me to start a PhD study here in the UK. My grateful thanks go Ms Dawn Bussey for her assistance for nanoindentation, Dr Nik Reeves- McLaren for his assistance for various XRD machines, Dr Le Ma, Dr Peng Zeng, and Dr Cheryl Shaw for their assistance in Sorby Centre for electron microscopy, Mr John Lowndes for fixing the PVD equipment. Great thanks also go to my colleagues in the research centre in surface engineering in the University of Sheffield: Ms Lynne Hopkins, Mr. Xiao Tao, Dr Chanon Iamvasant, Dr Xingguang Liu, Dr Chang Liu, Mr. Wei-Yu Chen, Dr Fahima Indeir, Dr Husein D Meshreghi, Mrs Nora Yaakop, Dr Lian Liu and Mr. Jack Cooper. I also want to thank all my Turkish friends in Sheffield for their help, and the memorable time we spent together. Finally, special and deep appreciation to my beloved wife (Cansu Yumusak), my parents (Umit Yumusak, Hulya Yumusak and Gizem Yumusak) and my son (Ali Aras Yumusak born in 22.11.2017) for all their love and encouragement. I would not have completed the PhD study without their grateful support. i ABSTRACT Titanium is a very popular engineering metal due to its outstanding properties, such as low density and high specific strength. However, the wear resistance of titanium is very poor in many industrial environments. Wear-resistant hard coatings can be used to increase the service lifetime of manufactured products, but the effectiveness of these coatings on titanium is sometimes low due to the inadequate load-bearing capacity of the substrate. Therefore, titanium alloys benefit from a substrate strengthening thermochemical diffusion pre-treatment before the Physical Vapour Deposition (PVD) of hard ceramic coatings. In this work, triode plasma nitriding (TPN) has been applied to increase the load-bearing capacity of titanium alloys. It is known that the effective adhesion between PVD hard coatings and titanium alloy substrates can be improved significantly after substrate diffusion pre- treatment. TPN treatments were used in this work because the diffusion of the nitrogen can be achieved more efficiently (than conventional nitriding techniques) at lower temperatures and shorter times, without the need for hydrogen in the gas mixture. Also, the (low) treatment pressure regime allows the coating and diffusion treatment stage to be combined and integrated into the same treatment equipment. Thus, the risk of hydrogen embrittlement is entirely avoided, and the treatment temperatures well below the alloy beta-transus minimise the grain growth (that can reduce the core strength and the fatigue life of the materials). The effectiveness of triode-plasma diffusion treatment can, however, be increased by applying a thin PVD metallic layer on titanium alloy substrates before the plasma nitriding stage. In this context, different compositions of β-titanium coating (stabilised by addition of Nb) were produced on α+β Ti-6Al-4V and β Ti-4Al-10V-22Mo substrate materials; the effect of formation of the β phase in Ti-Nb coatings before nitriding on diffusion treatment efficiency (and on nitride phase formation after TPN treatment at 700oC) was analysed. ii The hardening effect for Ti-Nb coated Ti-6Al-4V substrate was found higher than the other (uncoated and Ti coated) Ti-6Al-4V substrates after 4-hour triode plasma nitriding treatment. On the other hand, the hardening effect for Ti coated Ti-4Al-10V-22Mo substrate was found higher than other (uncoated and Ti-Nb coated) Ti-4Al-10V-22Mo substrates. Besides the hardness results, the wear coefficients of the Ti-Nb coated Ti-6Al-4V, and Ti coated Ti-4Al- 10V-22Mo substrates (after 4-hour triode plasma nitriding treatment at 700 oC) were found approximately 16% and 31% lower (compared to their untreated counterparts) respectively. The enhanced performance of the duplex treated samples suggested that the coating deposition process (prior to diffusion treatments) needs to be optimised for each Ti alloy to attain adequate results. iii TABLE OF CONTENTS 1 INTRODUCTION .......................................................................... 1 1.1 Aims and Objectives ......................................................................................... 2 1.2 Structure of this Thesis .................................................................................... 3 2 LITERATURE REVIEW .............................................................. 5 2.1 Titanium Metal ................................................................................................. 5 2.1.1 Crystal Structure ................................................................................................. 7 2.1.2 Plastic Deformation ............................................................................................ 8 2.2 The Necessity of Surface Engineering for Ti ................................................. 9 2.3 Surface Engineering Methods ....................................................................... 11 2.3.1 Physical Vapour Deposition ............................................................................. 13 2.3.1.1 Evaporation Deposition ............................................................................................................. 13 2.3.1.2 Sputtering .................................................................................................................................. 15 2.3.1.3 Cathodic Arc Evaporation ......................................................................................................... 17 2.3.1.4 Ion Plating ................................................................................................................................. 19 2.3.2 Thermochemical Treatment Methods: Nitriding .............................................. 21 2.3.2.1 Gas Nitriding ............................................................................................................................. 21 2.3.2.2 Laser Nitriding .......................................................................................................................... 22 2.3.2.3 Ion Beam Nitriding ................................................................................................................... 22 2.3.2.4 Plasma Nitriding (Fundamentals) ............................................................................................. 23 2.4 The nitrogen diffusion in titanium and titanium alloys .............................. 26 2.5 The effect of nitriding process parameters on material properties ........... 30 2.5.1 Process Temperature ........................................................................................ 31 2.5.2 Process Time .................................................................................................... 32 2.5.3 Total Gas Pressure ............................................................................................ 32 2.5.4 Nitrogen Partial Pressure .................................................................................. 33 2.5.5 Applied Substrate Voltage ............................................................................... 34 2.6 New attempts to improve nitriding efficiency: The effect of depositing thin α-Ti and β-Ti alloy surface layer coatings on material properties.......... 35 iv 3 EXPERIMENTAL PROCEDURE ............................................. 37 3.1 Production Stages ........................................................................................... 37 3.1.1 Ti and Ti-Nb Coatings ...................................................................................... 37 3.1.1.1 Substrate Preparation ................................................................................................................ 37 3.1.1.2 Deposition Process .................................................................................................................... 38 3.1.2 Triode Plasma Nitriding (TPN) ........................................................................ 40 3.2 Testing Techniques ......................................................................................... 44 3.2.1 X-ray Diffraction (XRD) Analysis ................................................................... 44 3.2.1.1 Glancing Angle X-ray Diffraction (GAXRD)........................................................................... 46 3.2.2 Optical Microscopy (OM) ................................................................................ 46 3.2.3 Scanning Electron Microscopy (SEM) ............................................................ 47 3.2.4 Energy Dispersive X-ray (EDX) Spectrometer ................................................ 49 3.2.5 Nanoindentation Testing .................................................................................. 50 3.2.6 Knoop Hardness Testing .................................................................................
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