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Effect of Chemical Structure on Tribological Behavior of Base Oils ABSTRACT EFFECT OF CHEMICAL STRUCTURE ON TRIBOLOGICAL BEHAVIOR OF BASE OILS by Kun Qian Friction and wear cost significant energy and reduce the machine life in engineering applications. Lubricant is widely used to reduce friction and wear with a tribofilm generated on the surfaces during sliding. The tribofilm formation is closely related to the additives and base oils in the lubricants. A commercial lubricant in automobile industry usually contains about 85% base oil and 15% additives. The effect of additives on tribofilm formation has been investigated widely. However, the effect of base oil still needs more investigation. This thesis investigates the effect of different base oils and their chemical composition and structure on tribofilm formation. iii THE EFFECT OF CHEMICAL STRUCTURE OF BASE OILS ON TRIBOFILM FORMATION Thesis Submitted to the Faculty of Miami University in partial fulfillment of the requirements for the degree of Master’s degree by Kun Qian Miami University Oxford, Ohio 2021 Advisor: Dr. Zhijiang Ye Advisor: Dr. Timothy Cameron Committee member: Dr. Mark Sidebottom ©2021 Kun Qian This Thesis titled THE EFFECT OF CHEMICAL STRUCTURE IN BASE OIL ON ZDDP TRIBOFILM FORMATION by Kun Qian has been approved for publication by Department of Mechanical Engineering ____________________________________________________ Zhijiang Ye ______________________________________________________ Timothy Cameron ______________________________________________________ Mark Sidebottom Table of Contents 1. Introduction ……………………………………………………………………………….….1 1.1 Motivation…………………………………………………………………………1 1.2 Problem definition……………………………………………………………........2 1.3 Objective....…………………………………...…………………………………...3 2. Research background…………………………………………………………….….5 2.1 Background……………………...………………………………………………...6 2.2 Base oil……………………...…….….………………………………………...….6 2.3 ZDDP additive…………...…….….……………………………………….……...7 2.4 ZDDP tribofilm………...…….…………………………………………….……...8 2.4.1 Anti-wear function….…………………………………..………...……...10 2.4.2 Structure and element distribution……………………………………….11 2.4.3 Observation and experiment method …………….…………….….…….12 3. Methods……………………………………………………………….………….….13 3.1 Sample preparation.…….….……………………………………………....…….13 3.2 Friction experiment.…….….……………………………………………....…….14 3.3 Analysis method.…….….……………………………………….………. ….….17 4. Result & Discussion ……………………………………….……………………….19 4.1 Types of ZDDP additive ………………………………………….……….…….19 4.2 Secondary alkyl group ZDDP ……………………………….…………….…….20 4.2.1 General load effect…………………………...…………………….…….20 4.2.2 Various base oil group………………………………….………….……..22 4.2.3 Various on different load…………………….…………………….….….23 4.2.4 Temperature effect ………………………………………………...…….26 4.2.5 Wear track under Electron microscopy ………………………………….27 4.3 Primary alkyl group ZDDP …………………………………………….….…….27 4.3.1 General load effect ………………………………………………. ….….29 4.3.2 Temperature effect…………………………………………...…….…….34 4.3.3 Wear track under Electron microscopy……………………….………….35 4.3.4 Surface morphology………………………………….……………….….37 5. Conclusions………………………………………………………………………….41 6. Appendix………………………………….……………………………………...….46 6.1 MATLAB code 7. Reference…………………………………………………………………..….…….43 iii List of Table 1. Phosphor and sulfur concentration in engine oil …………………………………………9 iv List of Equation 1. Hertzian contact model…………………………………………………………..21 v List of Figures 1. Rtec Multifunction tribometer rotation stage ………………………………..……4 2. Two type of Zinc Dialkyldithiophosphates (ZDDP)……………………….….…..7 3. Cross-section of wear track under TEM…………………………………….……..8 4. ZDDP tribofilm formation under AFM at different period…………………....…..9 5. Wear track under various temperature in ZDDP tribofilm formation……....……10 6. Different base oil mix with two type of ZDDP lubricant sample …………..…....13 7. Demonstration experiment and equipment ...…………………………….….…...15 8. Temperature versus time under different power output……………………..……16 9. COF plot for two type of ZDDP……………………………………………....….19 10. COF under 10N load for long period….………………………………….…...….20 11. Steady state COF for secondary ZDDP…………………………………….….…21 12. Weight present of chemical structure in base oil samples... ……………….…….22 13. Secondary ZDDP with different base oil under different load …………….…….23 14. Secondary ZDDP with different base oil under 10N and 20N …………….…….24 15. Secondary ZDDP with different base oil under 20N and 40N …………….…….25 16. Thermal film formation after 120 °C test …………………………………….….…26 17. Group 5 with secondary ZDDP under various temperature……………….….….27 18. SEM and EDS image for group 5 with secondary ZDDP under 10N……….…...28 19. SEM and EDS image for group 5 with secondary ZDDP under 20N……….…...29 20. Steady state COF for primary ZDDP………………………………………..……30 21. Primary ZDDP with different base oil under different load ……………….…….31 22. Comparison between secondary and primary ZDDP under different load….……32 23. Primary ZDDP with different base oil under 10N and 20N ……………….…….33 24. Primary ZDDP with different base oil under 20N and 40N ….…………….……34 25. Group 2 with primary ZDDP under various temperature…………………………35 26. SEM and EDS image for group 5 with primary ZDDP under 10N……………….36 27. SEM and EDS image for group 4 with primary ZDDP under 20N……………….37 28. Wear track for primary ZDDP with group 5 under 10N load……………….……38 29. Wear track for primary ZDDP with group 5 under 20N load……………….……38 30. Wear track for primary ZDDP with group 5 under 40N load……………….……39 vi Acknowledgements I would like to express my gratitude to my advisors Dr. Zhijiang Ye and Dr. Timothy Cameron for supporting my masters study and research. Their patient guidance helped me in all the research time and thesis writing. Besides my advisors, I would like to thank the Dr. Mark Sidebottom for encouragement, insightful comments and help on research. Thanks to my friends in the Tribology Research Group, Xiaoyun Fan and Holden Rittenhouse-Starbuck, for helping with the experiments and equipment adjustment. Thank you, also, to Dr. Mark Devlin, of Afton Chemical Corporation, for providing the base oils and ZDDP additives, the great support and the useful discussions of research. vii Chapter 1: Introduction 1.1 Motivation Friction and wear play a significant role in the modern world, often dominating the energy transport behavior of many engineered systems with sliding contact. Contacting interfaces are typically regarded negatively, often resisting the flow of thermal and electrical energy or irreversibly converting useful mechanical work into heat, plastic deformation and wear. Indeed, such concern is financially justified, as some estimates attribute ~$200 billion/year in losses to friction and wear in the US alone [1,2,3]. Friction always resists relative motion and contributes to wear, which directly affects the lifetime of parts. Ways to achieve friction reduction include, reducing the normal load, improving surface finish, and applying lubricant. The former two ways are less cost effective, so lubrication is the most common way to reduce friction. Three general forms of lubrication include solid (dry), liquid, and gas (vapor) phase. Dry lubricants are often used under high temperature or low pressure with low humidity working conditions and vapor lubricants can only be applied under extremely low load [4,28]. Liquids have fewer restrictions under typical conditions, which makes liquid lubrication the most widely used form. The common usage of liquid lubricant is often seen in machines, such as automobiles. Liquid lubricants also provide other functions, such as heat removal and scavenging dirt or wear debris, which the other forms of lubrication cannot achieve. The use of liquid lubricants to reduce friction can be traced back to early civilization with water or plant oil used in machines and mechanisms [5]. In the 1900s, petroleum-based lubricants were developed, which had great performance achieving friction reduction. However, achieving friction reduction is not always enough. Wear and oxidation are other parameters that have great impact on the lifespan of machines [6]. Thus, additives to improve anti-friction, anti-wear, and anti- corrosion performance, as well as other functions, are typically added to base oil. Zinc dialkyldithiophosphates (ZDDP), which have extraordinary anti-wear and anti-oxidation functions, are one of the remarkable additives used in the automobile industry. After the 1940s, most commercial lubricants in US had ZDDP additives [7]. The mechanism of its excellent anti- wear performance was found to be due to chemical reactions that occur during stressed contact between surfaces with lubricant. These chemical reactions form a solid film up to a few hundred nanometers thick, referred to as a tribofilm, on the sliding surfaces [7,8]. This tribofilm is constantly being generated and worn off, which prevents direct contact between the two surfaces. This gives ZDDP excellent anti-wear performance [7]. However, drawbacks of ZDDP were discovered later. The phosphorus in ZDDP harms the environment and the ZDDP formed tribofilm is microscopically rough, which increases the coefficient of friction. It is important to understand the characteristic of ZDDP tribofilm and to optimize its properties to reduce friction while maintaining strong anti-wear performance. 1 1.2 Problem definition The objective of this thesis is to investigate the effects of different base oils on ZDDP tribofilm formation and analyze the tribolfilm properties on 52100 steel. The behavior and condition of ZDDP tribofilm formation
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