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Corrosion Fatigue: Type 304 Stainless Steel in Acid-Chloride and Implant Metals in Biological Fluid

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Corrosion Fatigue: Type 304 Stainless Steel in Acid-Chloride and Implant Metals in Biological Fluid 76-9939 BOWERS, Davtd Francis, 1937- CORROSION FATIGUE: TYPE 304 STAINLESS STEEL IN ACID-CHLORIDE AND IMPLANT METALS IN BIOLOGICAL FLUID. The Ohio State University, Ph.D., 1975 Engineering, metallurgy Xerox University Microfilms, Ann Arbor, Michigan 48ioe CORROSION FATIGUE: TYPE 304 STAINLESS STEEL IN ACID-CHLORIDE AND IMPLANT METALS IN BIOLOGICAL FLUID Dissertation Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University by David Francis Bowers, B.S., M.S. Metallurgical Engineering The Ohio State University 1975 Approved by (dviser Department of Metallurgical Engineering Reading Committee: Dr. Mars G. Fontana Dr. Frank Beck Dr. John P. Hirth To My Wife and Daughter TABLE OF CONTENTS Page ACKNOWLEDGEMENTS.......................................... iv VITA........................................................ vi LIST OF TABLES............................................. viii LIST OF FIGURES... ...................... x INTRODUCTION.................. .. ......................... 1 I. LITERATURE SURVEY..................... 4 1.1 Concepts and Theory of Fatigue Crack Growth.. 4 1.2 Fracture Mechanics Approach to Crack Growth in Engineering Structures..................... 18 1.3 Effect of Microstructure on Fatigue Cracking Growth................................ 24 1.4 Mechanical Variables in Corrosion Fatigue.... 41 1.5 Environmental Interaction with Fatigue Crack Growth.................................... 59 II. EXPERIMENTAL DETAILS................................ 92 2.1 Test Apparatus and Specimen Design........... 93 2.2 Test Material................................... 109 2.3 Test Procedure..................... 112 III. EXPERIMENTAL RESULTS AND DISCUSSION................118 3.1 Polarization Properties of Type 304 Stain­ less Steel in 5NH2SO4 and IN NaCl.............119 3.2 Corrosion Fatigue Crack Propagation in Air and at Open Circuit Potential................. 122 3.3 Corrosion Fatigue Crack Growth at Applied Potential....................................... 128 ii Table of Contents (Continued) Page III. 3.4 Metallography and Fractography............... 131 3.5 Environmental Mechanisms Involved in the Corrosion Fatigue Behavior................... 138 IV. CONCLUSIONS . 144 APPENDICES A. A Review of the Literature Concerning Metallurg­ ical Invesitgations and Related Studies of Surgical Implant Materials........................ 147 B. The Corrosion Fatigue Behavior of Biomedical Alloys.............................................. 306 BIBLIOGRAPHY 379 ACKNOWLEDGEMENTS A very special thanks is rendered to my employer, Dr. R.W. Staehle whose constant efforts provided the research grants to financially support my education and thesis work during the past five years. His dedication to professional duties will never be forgotten as this example provides the necessary impteus for me and fellow co-workers to always strive for professional excellence both academically and in research. I express my best wishes for his continued success in the future. In addition, I offer my thanks to Professors Fontana, Beck and Hirth for their suggestions and comments. The following persons are gratefully acknowledged for their prompt assistance: Mr. R. Farrar for the photography and S.E.M. fractography; Mr. R. Justus and his assistants for machine shop work; Mrs. E. Orwig for typing this manuscript. My grateful thanks is offered to the National Science Foundation and the Electric Power Research Institute who provided the financial support for my thesis work. iv No words can express the gratitude in my heart for the great personal sacrifice my wife and daughter sustained during these past five years. I sincerely hope they will receive the rewards so richly deserved in the years to come. v VITA May 8 , 1937......................... Born-Birmingham, Alabama 1959................................. B.S. Metallurgical Engr'g, University of Alabama, 1959-1965........................... Project Engineer and Supervisor, Ross Meehan Foundry, Chattanoaga, Tenn. 1959-1967........................... U.S. Army Reserve; Platoon Leader-169th Engr Bn. Co. Executive Officer- HQ, 101st Engr. Combat Battelion. 1965-196 6 .............. ............Research Assistant, Dept. of Metal. Eng., Univ. of Wisconsin, Madison, Wise. 1966.... ........................... M.S., Metal En., University of Wisconsin, Madison, Wis. 1966-1970. ......................... Plant Metallurgist, Dayton Malleable Iron Co., Columbus, Ohio. 1970-1975.......................... Research Assistant, Dept. of Metal En., Ohio State University. PUBLICATIONS "The Corrosion Fatigue Behavior of Biomedical Alloys, be published 1975, Journal of Biomedical Research FIELDS OF STUDY Major Field: Metallurgical Engineering Studies in Electrochemistry and Corrosion: Professors M. G. Fontana, R. W. Staehle Studies in Thermodynamics, Kinetics and Process Metallurgy Professors G. R. St. Pierre, R. A. Rapp Studies in Physical Metallurgy Professors G. W. Powell, J. P. Hirth J. W. Spretnak vii LIST OF TABLES Table I - Procedures used in photo-fabrication technique. Table II - Test material chemical composition and mechanical properties. Table III - Geometrical multiplying factors for each (—) ratio of 5 mil crack length increments. APPENDIX A Table IV - Classification of Metals to Implant Locations and Functions. Table V - A.S.T.M. Chemical Composition and Mechanical Properties of Implant Metals. Table VI- Standard E.M.F Series of Metals. Table VII - Galvanic Series of Some Commercial Metals and Alloys in Seawater. Table VIII-Anodic Back E.M.F. (A.B.E.) of Metals in Equine Serum. Table IX - Predicted Electrolytic Crevice Corrosion Resist-, ance Table X - Relative Crevice Corrosion Resistance of Metals and Alloys in Seawater. Table XI - Comparison of Bone Strength to Intramedullary Fixation Devices. Table XII- Effect of Alloy Composition on SCC Resistance as Measured by Fracture Toughness. viii Table XHE-Examples of Test Results in Measuring Material Resistance to SCC. Table XIV - Results of Visual Examination and Weight Measurements For SCC Specimens. Table XV r Results of Fatigue and Stress Corrosion Tests for Pacemaker Electrode Materials. Table XVI - Strength Reduction Factors and Fretting Fatigue Limit. Table XVII - Statistical Evaluation of Metal Performance in Implant Applications, APPENDIX B Table XVHI— Composition of Lactated Ringer's Solution. Table XIX-Fatigue Specimen Processing Procedure. Table XX- Chemical Composition and A.S.T.M. Specification for Test Materials. Table XXI-Mechanical Properties and A.S.T.M. Specifications for Test Material. Table XXn-Heat Treatment and Processing of Fatigue Specimens. LIST OF FIGURES Figure 1 Sequence of crack opening and closing under the repeated loading cycle 0 to or. Figure 2 Notation for crack growth theory. Figure 3 Comparison of crack growth theory parameters to those of LEFM. Figure 4 Kj values for various crack geometries. Figure 5 Effect of thermal aging on fatigue crack growth of type 304 and 316 stainless steel. Figure 6 Effect of grain size on fatigue crack growth of 309 stainless steel. Figure 7 Crack growth rates for marazing and stainless steels. Figure 8 . Comparison of fatigue crack growth in weld and parent metal of type 304 composition. Figure 9 Comparison of fatigue crack growth of type 308 weld and type 304 basemetal at 800°F. Figure 10 Influence of cold work in fatigue crack growth of type 304 at 800°F. Figure 11 Fatigue crack morphology in cast (CF-8 ) stainless steel. Figure 12 The effect of frequency on fatigue crack growth of type 304 at 1100°F. Figure 13 Idealized crack growth of type 304 at 1000°F. x Figure 14 Design curve for the effect of cyclic frequency on type 304 stainless steel at 1000°F. Figure 15 Fatigue-crack propagation behavior of type 304 stainless steel at 75°F over a frequency range of 0.067 to 6.7 H2 * Figure 1.6 S.E.M. of fracture surfaces of specimens exposed to different hold times in loading. Figure 17 Logarithmic plot of fatigue crack length vs strain cycles for type 304 stainless steel. Figure 18 Effect of cyclic stress ratio on fatigue crack growth of 304 at 1000°F. Figure 19 Same as Figure 17 but plotted as a function of effective stress intensity. Figure 20 AK vs da/dN for 18/8 austenitic steel using Frost and Pook's analyzing crack growth. Figure 21 Types of fatigue crack growth behavior. Figure 22 Effect of humidity on crack growth rates in type 304 stainless steel at room temperature. Figure 23 Potential-pH diagram of iron-water system based on the oxides of iron. Figure 24 Corrosion fatigue crack growth rate versus frequency for nickel-base superalloy. Figure 25 Growth rates of fatigue cracks in 12% chromium steel as influenced by frequency, environment and heat treatment. Figure 26 A schematic diagram of the superposition model. Figure 2 7 Superposition model prediction for a slow frequency. Figure 28 Metallographic photos of fatigue cracking of type 304 in active and passive range MgCl-2 environment. Figure 29 S.E.M. photographs of the same specimens shown in Figure 27. Figure 30 Photomicrographs and S.E.M. photos of specimen exposed to SCC conditions in MgCl2 . Figure 31 Photomicrograph and SEM photos of specimens exposed to superimposed cyclic loading on SCC conditions in MsCl2 * Figure 32- Same as Figure 30 but cyclic loading imposed at higher frequency. Figure 33 S.E.M. surface area photograph of the specimen shown in Figure 31. Slip line impingement at grain boundaries is shown. Figure 34 Effect of applied current on corrosion
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