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Corrosion Behavior of Titanium Based Ceramic Coatings Deposited on Steels (Korrosionsverhalten Einer Auf Stahl Abgeschiedenen Keramikbeschichtung Mit Titanbasis)

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Corrosion Behavior of Titanium Based Ceramic Coatings Deposited on Steels (Korrosionsverhalten Einer Auf Stahl Abgeschiedenen Keramikbeschichtung Mit Titanbasis) Corrosion Behavior of Titanium Based Ceramic Coatings Deposited on Steels (Korrosionsverhalten einer auf Stahl abgeschiedenen Keramikbeschichtung mit Titanbasis) Der Technischen Fakultät der Universität Erlangen-Nürnberg zur Erlangung des Grades DOKTOR-INGENIEUR vorgelegt von Frau. Dipl.-Ing. Rania Ali Erlangen- 2016 Als Dissertation genehmigt von der Technischen Fakultät der Universität Erlangen-Nürnberg Tag der Einreichung: 11.12.2012 Tag der Promotion: 13.11.2015 Dekan: Prof. Dr. Peter Greil Berichterstatter: Prof. Dr. Sannakaisa Virtanen Prof. Dr. Andreas Roosen Acknowledgements: One of the joys of completion is to look over the journey past and remember all the friends and family who have helped and supported me along this long but fulfilling road. First of all I would like to express my heartfelt gratitude to my supervisor, Prof. Dr. Sannakaisa Virtanen. This thesis would not have been possible without her help, support and patience. She unconditionally and readily shared her knowledge and offered support, providing me with valuable insight and many ideas for the research. I would also like to thank my examining committee, Prof. Dr. Andreas Roosen, and Prof. Dr. Nadja Popovska-Leipertz, Prof. Dr. de Ligny, who provided encouraging and constructive feedback. I am very thankful to my friends and colleagues, Dr. Manuela Killian, Dr. Emad Alkhateeb, Dr. Florian Kellner, Dr. Florian Seuss, Dr. Leonhard Klein, Dr. Hanadi Ghanem, Dr. Giorgia Obigodi-Ndjeng, for always being there and ready to share their experience with me over my PhD period. I also thank Prof. Dr. Patrik Schmuki for giving me the possibility to carry out my thesis at LKO. I appreciate all my colleagues and friends who have helped me with surface analysis and technical stuff. Also many thanks to the LKO staff, particularly, the corrosion group, who enabled me to enjoy every day during this research process. Special thanks go to Mr. Hans Rollig and his family. You have been like surrogate family sheltered me over the years. I would like to thank my parents, my sisters and brothers. Without their love and support I would have not completed this road. Finally, I would like to thank my husband, Ghadeer Diab. He was always there cheering me up and stood by me through the good times and the bad times. Dedicated to: My small family, my beloved husband, and my little angel, my daughter Leah You are the sunshine of my life… Abstract Titanium based ceramic films are increasingly used as coating materials because of their high hardness, excellent wear resistance and superior corrosion resistance. Using electrochemical and spectroscopic techniques, the electrochemical properties of different coatings deposited on different steels under different conditions were examined in this study. Thin films of titanium nitride (TiN), titanium diboride (TiB2), and titanium boronitride with different boron concentrations (TiBN-1&2) were deposited on stainless steel and low carbon steel by chemical vapor deposition using the hydrogen reduction of TiCl4, BCl3 and N2 at a reduced pressure of 600 mbar and a temperature of 900°C. The factors evaluated were the substrate material, the coating composition, the boron content, the thickness and the boron content. Different alternating current and direct current electrochemical methods (corrosion potential screening, potentiodynamic techniques at low scan rate and electrochemical impedance spectroscopy) were used to study the electrochemical behavior of the different coated steels in different electrolytes at ambient temperature. The porosity of the deposited coatings which is essential for the estimation of the corrosion resistance of coated components was also measured. Results showed that different coatings deposited on different steels have different morphologies and crystal structures and consequently different corrosion resistance. The resistance to corrosive attack of the coatings deposited on stainless steel was relatively poor for TiN, better for TiBN-1&2 and best for TiB2. On coated low carbon steel, TiB2 showed the worst corrosion resistance, followed with TiN and TiBN-1 with relatively better resistance; TiBN-2 was the best. Thicker TiBN-3 with higher boron content deposited on low carbon steel was tested in simulated soil solution, simulated seawater and 1 M HCl. The corrosion resistance was also evaluated with immersion tests. The effect of different temperatures (15, 35, and 45°C) was evaluated. ii Finally, applied cathodic protection and interrupted cathodic potential measurements were also carried out. To elucidate the corrosion protection mechanisms of the coatings, coating morphology, chemical composition and crystal structure was studied by different characterization techniques before and after corrosion testing. Results showed that coating with good corrosion resistance has to meet the following requirements: fine and dense structure with low porosity, good adhesion to the material substrate. Surface analyses indicate that the coatings do not only offer a physical barrier which protects the substrate material from aggressive species, but also oxidize to form an oxide passive layer on the coating surface, which consists mainly of titanium oxide and titanium oxynitride. This layer enhances the corrosion protection due to its chemical inertness; it also fills the cracks existing on the surface and decreases the number of pathways which allow the electrolyte to penetrate into the underlying substrate. It is also shown that coatings with nano-crystal structure, and intermixed phases with different crystal orientation, as TiBN-3 on low carbon steel, can provide a superior corrosion protection in neutral test solution up to 90 days immersion days. In acid medium, the coating is less protective due to the dissolution of the oxide layer. Applying cathodic protection was found to decrease the protection effect of the coating due to the reduction of the oxide film. Interrupting the applied cathodic potential leads to coating damage and peeling off due to hydrogen embrittlement and the reduction and reformation of the oxides filling the cracks which leads to chipping off of the deposited coating. iii Zusammenfassung Titan basierte keramische Beschichtungen werden mit zunehmender Häufigkeit wegen ihrer hohen Härte, guten Abriebresistenz und überragender Korrosionsbeständigkeit verwendet. Mittels elektrochemischer und spektroskopischer Untersuchungen wurden in dieser Arbeit die elektrochemischen Eigenschaften unterschiedlicher Beschichtungen auf unterschiedlichen Stählen und mit unterschiedlichen Beschichtungsbedingungen evaluiert. Dünne Filme aus Titannitrid (TiN), Titanborid (TiB2) und Titanboronitrid mit variierender Borkonzentration (TiBN-1&2) wurden sowohl auf Edelstahl als auch auf kohlenstoffarmem Stahl mittels chemischer Gasphasenabscheidung aufgebracht. Dabei wurden TiCl4, BCl3 und N2 unter reduziertem Druck (600 mbar) bei einer Temperatur von 900°C reduziert. Das Substratmaterial, die Beschichtungszusammensetzung, -dicke und der Borgehalt wurden ausgewertet. Um das elektrochemische Verhalten der unterschiedlichen, beschichteten Stahlproben in verschiedenen Elektrolyten bei Raumtemperatur zu prüfen, wurden unterschiedliche elektrochemische Methoden mit Wechsel- oder Gleichstrom angewandt (Screening des Korrosionspotentials, potentiodynamische Techniken mit geringer Rasterfrequenz, elektrochemische Impedanzspektroskopie). Die Porosität der abgeschiedenen Beschichtungen, welche im Hinblick auf die Bestimmung der Korrosionsbeständigkeit der beschichteten Komponenten essenziell ist, wurde ebenfalls bestimmt. Die Messungen zeigten, dass unterschiedliche Beschichtungen auf unterschiedlichen Stählen unterschiedliche Oberflächenstrukturen und Kristallstrukturen aufweisen, was wiederum in einem unterschiedlichen Korrosionsverhalten resultiert. Die Beschichtung von Edelstahl mit TiN wies relativ geringe Resistenz gegenüber korrosiven Angriffen auf, TiBN 1&2 wiesen bessere Beständigkeit auf, am besten schnitt TiB2 ab. Auf kohlenstoffarmem Stahl wiederum zeigte TiB2 die schlechteste Korrosionsbeständigkeit, gefolgt von iv TiN und TiBN-1, welche im Vergleich stabiler waren; TiBN-2 zeigte die besten Resultate.Dickere Beschichtungen mit erhöhtem Borgehalt (TiBN-3) auf kohlenstoffarmem Stahl wurden in künstlicher Bodenlösung (simulated soil solution), künstlichem Meerwasser und 1M HCl getestet. Die Korrosionsbeständigkeit wurde auch mittels Tauchtests evaluiert. Der Einfluss von Temperatur (15°C, 35°C, 45°C) auf die Korrosion wurde ebenfalls untersucht. Schlussendlich wurden kathodischer Schutz und kathodische Potentialmessungen durchgeführt. Um den Mechanismus der Korrosionsprotektion aufzuklären, wurden die Oberflächenbeschaffenheit, chemische Zusammensetzung und Kristallstruktur der Beschichtungen mit verschiedenen Untersuchungsmethoden vor und nach den Korrosionsbeständigkeitstests bestimmt. Die Ergebnisse lassen den Rückschluss zu, dass für gute Korrosionsbeständigkeit folgende Voraussetzungen notwendig sind: feine und dichte Struktur mit geringer Porosität und gute Substratanhaftung. Oberflächenanalytische Untersuchungen legen nahe, dass die Beschichtungen nicht nur eine physische Barriere gegenüber aggressiven Medien darstellen, welche das Substrat schützt, sondern auch durch Oxidation stabilen Passivfilme auf ihrer Oberfläche ausbilden, welche hauptsächlich aus Titandioxid und Titanoxynitrid bestehen. Diese Schicht erhöht den Korrosionsschutz wegen ihrer chemischen Inertanz, füllt gleichzeitig auf der Oberfläche vorhandene Risse
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