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University of Cincinnati UNIVERSITY OF CINCINNATI Date:___________________ I, _________________________________________________________, hereby submit this work as part of the requirements for the degree of: in: It is entitled: This work and its defense approved by: Chair: _______________________________ _______________________________ _______________________________ _______________________________ _______________________________ MECHANISTIC INVESTIGATION OF RUBBER-BRASS ADHESION: EFFECT OF FORMULATION INGREDIENTS A dissertation submitted to the Division of Research and Advanced Studies of the University of Cincinnati in partial fulfillment of the requirements for the degree of DOCTORATE OF PHILOSOPHY (Ph.D) in the Department of Materials Science and Engineering of the College of Engineering October, 2005 by Pankaj Y. Patil M. S., University of Cincinnati, Cincinnati, OH, 2003 B.Tech, Laxminarayan Institute of Technology, Nagpur University, India, 1999 Committee chair: Prof. William J. Van Ooij ABSTRACT It is very customary to use adhesion-promoting resins in the belt compounds’ formulation to enhance the adhesion between rubber and brass-coated steel cords. Conventionally, two-component adhesion-promoting resins, i.e., HexaMethoxy- MethylMelamine (HMMM) + Resorcinol Formaldehyde (RF) precondensed resin, are commonly used in the tire industry to enhance the initial and aged adhesion between rubber and brass-plated steel cord. However, one-component adhesion-promoting resins were developed in an attempt to eliminate resorcinol from the formulation of belt compound. This study was undertaken to unravel the role of these newly developed one-component resins in enhancing the initial as well as aged adhesion performance. Initial experiments were conducted using a squalene liquid rubber modeling approach in the laboratory to study the effect of resins on the chemistry of the vulcanization reaction and their effect on the adhesion interface. Based on the GPC, SEM/EDX and TOF-SIMS data, a mechanism was proposed to explain the possible role played by resins in the improvement of initial and aged adhesion performance between rubber and brass-coated steel tire cords. Actual natural rubber compounds were later cured to confirm the proposed mechanism derived from the initial squalene-based studies. The proposed mechanism based on squalene studies, which theorized the possible migration of resins towards the rubber-brass interface, was found to be unfeasible in the actual natural rubber compounds, primarily because of the substantial increase in the molecular weight of the rubber matrix. Thus, a new approach was undertaken and the effect of resins on the mechanical properties of the cured natural rubber compounds was studied. Similarly, the initial, heat and humidity aged adhesion studies were performed using these natural rubber compounds. The effect of resin incorporation on the crosslink density distribution was studied using C-13 NMR analyses of the cured rubber compounds. In order to understand the effect of resins on the rubber-brass adhesion interface, brass-plated steel cords and highly polished brass coupons were sulfidized against the natural rubber compounds. The cured rubber was removed using a unique approach, i.e., ortho dichlorobenzene solvent cleaning method. The sulfidized brass cords were tested for their corrosion-resistance properties using electrochemical (DC polarization) techniques. Furthermore, the effect of resins on the crystal structure of copper sulfide adhesion layer was understood by analyzing the sulfidized brass coupons using synchrotron source grazing incidence angle X-ray diffraction (GIXRD) method. A better understanding of the effect of one-component resins on the rubber-brass bonding was achieved. Based on the results obtained in this research work, a new mechanism of action for the one-component resins is proposed that explains the effect of these resins in improving the rubber-to-brass adhesion performance, especially after aging. iii PREFACE The experimental work on this project began in the year 2000. The primary goal behind undertaking this research project was to unravel the role of adhesion- promoting resins (one-component resins) mechanistically in imparting durability to the rubber-brass bond in tires during aging conditions. To understand the effect of these adhesion-promoting resins on the curing chemistry of the rubber compounds, a popular squalene modeling system was chosen as an initial approach. However, real rubber compounds were later cured to study the effect of various formulation ingredients on the mechanical properties of the cured rubber compounds. Furthermore, the effect of formulation ingredients on the corrosion-resistance properties of the sulfidized brass-plated steel tire cords, cured in different rubber formulations, was also studied. Finally, the effect of formulation ingredients on the crystal structure of the copper-sulfide interfacial layer was determined. A new mechanism that explains the role of the adhesion-promoting resins in enhancing the durability of the rubber-to-brass adhesion during aging conditions is proposed based on this research work. Given the variety of subject areas that are covered in this dissertation and to maintain the coherency of the document, the literature survey of the corresponding subject areas will be discussed in the corresponding chapters and a conventionally practiced approach of dedicating one chapter exclusive to the literature survey was not chosen in this work for brevity. This dissertation is a compilation of the research work that was published in the following papers: I. Pankaj Y. Patil and W. J. van Ooij, "Mechanistic study of the role of one- component resins in rubber-to-brass bonding", Rubber Chemistry and Technology, Vol. 77, 891 (2004) II. Pankaj Y. Patil and W. J. van Ooij, "Mechanism of improved aged rubber-to- brass adhesion using adhesion promoting one-component resins", Rubber Chemistry and Technology, Vol. 78, 155 (2005) III. Pankaj Y. Patil and W. J. van Ooij, "Mechanism of adhesion degradation of rubber-to-brass plated steel cords", Journal of Adhesion Science and Technology, Vol. 18, No. 12, 1367 (2004) IV. Pankaj Y. Patil and W. J. van Ooij, "Crystallographic study of copper sulfide adhesion layer using synchrotron source grazing incidence X-ray diffraction(GIXRD)" - Scheduled for publication in 'Rubber Chemistry and Technology', Vol. 79, Mar-Apr 2006 The timeline of the experimental work in this project is in the same chronological order in which the papers are listed above. vi OUTLINE OF THIS DISSERTATION The outline and a brief description of this dissertation conducted in the order research work were based on the following chapters. The Chapters 2, 3, 4 and 5 are published papers. The work described in this dissertation involves many diverse subjects, e.g., polymers, corrosion, ceramics etc. Therefore, in an effort to make the document more coherent, certain departures have been made from the traditional format of Literature Survey → Experimental → Results and Discussion → Conclusions. A general introduction of the rubber-brass bonding and use of adhesion promoters is presented in Chapter 1. The results and the proposed adhesion mechanism based on the initial squalene studies are presented in Chapter 2. Chapter 3 summarizes the experimental work done on understanding the effect of adhesion-promoting resins on the mechanical properties of natural rubber cured compounds. A new approach of testing the corrosion-resistance properties of the sulfidized brass cords after sulfidizing them in different rubber formulations is discussed. In Chapter 4 the corrosion-resistance property imparted by the sulfide film formation on the brass-plated steel cord is investigated in details. The sulfidized tire cords were obtained from the squalene study and also from the real tires. Real tires were made to verify and correlate the results obtained from the squalene study in terms of the corrosion-resistance properties of the sulfidized cords. A concept of different type of CuxS inter-reacted rubber-brass layer formation as a function of different formulation ingredients is discussed. In Chapter 5, to verify the crystal structure of the CuxS inter-reacted rubber-brass layer, formed as a function of different formulation ingredients, GIXRD analysis of the mentioned layer on the highly polished and sulfidized brass coupons was performed. The results and a new mechanism are discussed. In Chapter 6, a mechanism for the possible generation of H· atoms through the catalytic cleavage of N-H bond present on the one-component resin molecules is discussed. To explain the role of these H· atoms in hindering the amorphous-to- crystalline transformation of the rubber-brass interfacial CuxS bonding layer, resulting in a durable rubber-brass bond after aging conditions, a newly proposed unit cell model for the non-stoichiometric CuxS layer and the effect of H· atoms on the CuxS lattice is discussed at the end of this chapter. Chapter 7 summarizes the findings in this work Chapter 8 suggests the scope for future work viii To my Family ACKNOWLEDGMENTS It is very challenging for me to write this section since I find it really hard to express my gratitude in just some words, i.e., just words will not suffice for me to express my heartfelt gratitude towards all the individuals behind the success of this work. Nevertheless, first and foremost, I am immensely grateful to my advisor, Professor William J. van Ooij, for giving me the opportunity to work on this project, for
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