MECHANISMS OF ENVIRONMENTALLY-INFLUENCED FATIGUE CRACK GROWTH IN LOWER STRENGTH STEELS by SUBRAMANIAN SURESH B. Tech., Indian Institute of Technology, Madras (1977) M.S., Iowa State University (1979) SUBMITTED IN PARTIAL FULFILLMENT OF THE REQ UIREMENTS FOR THE DEGREE OF DOCTOR OF SCIENCE at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY May 1981 0 Massachusetts Institute of Technology, 1981 re- redacntedr Signature of Autho r e)rtment of Mechanical, Engineering May 7,9 1981 Ce rti fi ed by / /Signature reaactea Robert 0. Ritchie I C so / s UPe Accepted by Signature redacted Chairman, Archives MASSACHUSETTS INSTITUTE OF TECHNOLOGY OCT 29 1981 U1BRARES Department Committee i - - MECHANISMS OF ENVIRONMENTALLY-INFLUENCED FATIGUE CRACK GROWTH IN LOWER STRENGTH STEELS by S. SURESH Submitted to the Department of Mechanical Engineering on May 7, 1981 in partial fulfillment of the requirements for the Degree of Doctor of Science in Mechanical Engineering. ABSTRACT been traditionally have steels strength Lower of presence the in brittlement to em considered to be immune steels, strength lower on work In this thesis hydrogen gas. it is clearly demonstrated that contrary to conventional where wi sdom, there are two regions of fatigue crack growth crack in accelerations cant causes signifi hydrogen gas influences Environmental propagation rates compared to air. these two regimes are sh own to be governed by entirely in different mechanisms. In particular, in the near -threshold regi on of fatiguo than 10 smal 1 e r rates (growth propagation crack mm/cycle) , it is seen that with refere nce to a moist air are growth rates crack near-threshold environment, dry helium, are ga s and in accelerated in dry hydrogen marginally decelerated in di stilled water and remain the are results surp rising Such same in wet hydrogen. "oxide-induced termed pproach a new a of terms in interpreted several crack closure" which is seen to be con si stent with in Evidence . al observations hitherto unexplained experiment using ind iirectly obtained support of this model has been analyses of fracture surface spectroscopy and ESCA Auger ferri tic-ba i ni tic, in ferritic-p earl itic,, oxide deposits steels. Direct fully bainitic, and fully martensitic is provided with evidence for oxide-induced crack closure of variable Effects aid of ultrasonic techni ques. the amplitude lo ads, in the form of block underload cycles below are explained based on this mechanism and their threshold, to the impl ications are noted with pa rti cul ar reference Environmental influences measurement of fatigue threshold s. strength steels are in the near- threshold region of lower The consequences compared wi th those in an alumi num alloy. of this work are examined in the light of the effects near o f not only various environments, but also such threshold ratio, load as factors and microstructural mechanical and grain si ze. trength s frequency, Th esi s Su pervi sor: Title: Robert 0. Ritchie Associ ate Professor Department of Mechanical Engi ni eei ng ii - - ACKNOWLEDGEMENTS It is my pleasure to than k for Professor R.O. Ritchie me to enjoy the challenges of research. motivating His dedication and achieveme nts have constantly of source a been I sincerely thank him for his inspiration. encouragement, stimulating ideas, and close friendship. I am very grateful for R.M . Latani sion to Professors D. M. Parks and their e nthusiastic p articipation in this work and many valuable comments and suggestions. Thanks are due to Mr. Palmer J. Lewis and Dr. I.G. of Lockheed Palo Alto Research Laboratories, Mr. Martin, Mr. M.I.T., Dr. Lindley of England, R.E. A. A. Rudolph, and Mr. M.Kurkela, Joshi of Perkin-Elmer, Electricity Central and Dr. Generating of T.C. Board, for their help during the course of this work. I am also very thank ful Mr.D.DeLonga for to Professor their assistance J.H.Williams with and ultrasonic measurements. The information, facilities by Lockheed Missile and and materials provided Company, Rockwell Space International Science Center, Westinghouse RID Center, NASA-AMES Research Center, and Surface Sciences Division of Perkin-Elmer are gratefully acknowledged. iii - - The support and friendship of my office-mates, both past and present, are sincerely appreciated. Finally, I wish to thank my parents and who, my sister despite 12000 miles of separation, have constantly kept my spirits high through their weekly letters. - - iv TABLE OF CONTENTS Page No. i ABSTRACT....................... ACKNOWLEDGEMENTS............... ii TABLE OF CONTENTS.............. iv LIST OF FIGURES................ LIST OF TABLES................. viii NOMENCLATURE................... ix I. INTRODUCTION............... 1.1 CONCEPTUAL BACKGROUND. 1.2 SCOPE OF PRESENT WORK. ........... 2. N.. 7 MATERIALS AND EXPERIMENTAL PROCEDURES.... 2.1 MATERIALS............. ............ 2.2 EXPERIMENTAL PROCEDURE .... ......... 9 9 19 3. TWO REGIMES OF HYDROGEN-IND 24 4. AN EXPLANATION FOR ENVIRONMENTAL EFFECTS NEAR THRESHOLD ............................................... 51 5. EVIDENCE SUPPORTING OXIDE-INDUCED CRACK CLOSURE.......... 70 6. INFLUENCE OF UNDERLOADS NEAR THRESHOLD .................. 79 7. THRESHOLD BEHAVIOR IN DIFFERENT ALLOY SYSTEMS............ 91 8. CONCLUDING REMARKS ...................................... 102 9. CONCLUSIONS AND SUSUGGESTIONS FOR FURTHER RESEARCH....... 109 REFERENCES................................................... 115 APPENDIX..................................................... 121 LIST OF FIGURES Schematic variation of fatigue crack growth rate with the stress intensity range in steels, showing primary crack growth mechanisms. Fig. 2.1 Optical micrograph of SA542 Class 3, 174 mm thick base plate at a)surface, b)quarter thickness ( T), and c)mid-thickness ( T) locations (2% nital etch). Fig. 2.2 Transmission electron micrograph of SA542-3 steel showing globular Cr 2 3 C 6 and needle-shaped Mo 2 C particles. Fig. 2.3 Micrograph showing the structure of BA2021 alloy; white globular particles are CuAl 2 Fig. 2.4 Hydrogen permeation cell. Fig. 3.1 Influence of frequency on fatigue crack growth rate in SA542-3 steel tested at R = 0.05 in moist air and dry hydrogen. Fig. 3.2 Influence of load ratio R on fatigue crack growth rate in SA542-3 steel tested at 50 Hz in moist air and dry hydrogen. Fig. 3.3 Schematic showing regimes of hydrogen-assisted crack growth commonly observed in lower strength steels. Fig. 3.4 Fractography of fatigue crack growth in 24 Cr-lMo steel at 50 Hz in moist air and dry hydrogen gas (R = 0.3). Fig. 3.5 Schematic illustration of the possible steps involved in the embrittlement of steels by gaseous hydrogen atmospheres. a is the maximum principal stress as a function of distance xyyahead of the crack tip. Fig. 3.6 Basic types of corrosion fatigue crack growth behavior defined in ref. 26. a) true-corrosion fatigue, b) stresscorrosion fatigue, and c) mixed behavior. Fig. 3.7 Effect of load ratio on the near-threshold fatigue behavior of SA542-3 steel. Fig. 3.8 Fatigue crack propagation in SA542-3 steel tested at R = 0.05 and 0.75 (50 Hz) in moist air and dry hydrogen. Fig. 3.9 Fatigue crack propagation in bainitic SA542-3 steel tested at R = 0.05 in environments of moist air, water, dry and wet hydrogen and helium. Fig. 3.10 Fractographs of near-threshold fracture surfaces of SA542-3 steel from tests in air, water, dry hydrogen and dry helium environments. . Fig. 1.1 - - vi Fig. 4.1 Bands of corrosion deposits visible on near-threshold fatigue fracture surfaces tested in moist air at a) R = 0.05 and b) R = 0.75. Fig. 4.2 ESCA analysis of crack tip corrosion debris in SA542-3 steel showing the presence of predominately Fe 0 ' 2 3 Fig. 4.3 Measurements of oxide thickness as a function of crack length and crack growth rate for SA542-3 steel tested in moist air and hydrogen gas at R = 0.05 and 0.75. Fig. 4.4 Idealizations of oxide wedge inside near-threshold crack. Fig. 4.5 Correlation between oxide thickness and cyclic CTOD. Fig. 4.6 Variation of threshold stress intensity parameters with load ratio. Fig. 4.7 Nomenclature for stress intensity parameters at threshold and their variation with load ratio R (after Schmidt and Paris). Fig. 5.1 Schematic showing the location of transducers on the compact tension specimen for ultrasonic testing. Fig. 5.2 Variation of receiver signal with stress intensity. Fig. 5.3 Schematic showing receiver signal output for uncracked, saw-cut and fatigue-cracked specimens. Fig. 6.1 Nomenclature of different parameters used to describe the underload interactions near threshold. Fig. 6.2 Crack length versus the number of cycles showing the effects of underloads. Fig. 6.3 Variation of cyclic CTOD, oxide thickness d, and crack growth rate with stress intensity range and a scheme for finding the critical underload stress intensity range. Fig. 7.1 Variation of crack growth rate with stress intensity range in SA516 steel tested in moist air and dry hydrogen environments Fig. 7.2 Variation of crack growth rate with stress intensity range in X-60 pipeline steel in moist air and dry hydrogen environments. Fig. 7.3 Fatigue crack propagation behavior of BA2021 alloy in moist air, dry hydrogen, distilled water and hydrazine environments. Fiq. 7.4 Variation of excess oxide thickness with crack length in BA2021 allov. - - vii Fig. 8.1 Schematic showinq the differerent modes of crack closure in steels. Fig. 8.2 Variation of threshold stress intensity range with yield strength in several classes of steels. Fig. 8.3 Fatigue crack growth behavior of Cr-Mo-V steel in moist air and vacuum at 550'C (ref. 12). Fig. Al Schematic showing a typical deDth comoosition orofile of Fe3, 01, and Cl peaks. Fig. A2 Schematic showing oxide formation on crack faces and the excess oxide thickness. - - viii LIST OF TABLES Table No. 2.1 TITLE Page Chemical composition, heat treatment, ambi ent temperature mechanical properti es of SA542-3 steel. 10 2.2 Plate Chemistries of SA516, X-60 steels and 2021 aluminum alloy. 15 2.3 Ambient temperature mechanical properties of SA516, X-60, and BA2021 alloys. 17 3.1 Conditions for onset of hydrogenassisted crack growth in SA542-3. 29 4.1 Threshold data for 24 Cr-lMo steels. 63 6.1 Results of variable amplitude tests involving effects of underloads on near-threshold growth rates. 84 Threshold data for SA516 and X-60 steels. 95 7.1 - - ix NOMENCLATURE a crack length a* crack length over which retardation occurs CH local hydrogen concentration at point of maximum dilatation ahead of crack tip Co equilibrium hydrogen concentration in unstressed lattice d excess oxide thickness measured on fracture surface da/dN fatigue crack growth rate per cycle (da/dN)B baseline fatigue crack growth rate at AKB fatigue crack growth rate following initial underload (da/ dN D diffusion coefficient for hydrogen permeation E elastic modulus h initial h final asperity height K linear elastic stress intensity factor (Mode I) Kn plane strain fracture toughness Kmax maximum stress intensity during fatigue cycle 0 asperity height minimum stress intensity during fatigue cycle transition maximum stress intensity K Iscc threshold stress intensity for environmental attack half the distance between location of peak oxide layer and crack tip x - - N number of cycles N* number of cycles over which retardation occurs n' work hardening exponent (cyclic) R load ratio (K t time T absolute temperature ) RO /K . max min universal gas constant partial molar volume of hydrogen in iron (2 cm 3 /mole) x hydrogen permeation distance ahead of the crack tip ACTOD cyclic crack tip opening displacement AK alternating stress intensity range (Kmax AKB baseline alternating stress intensity range AKff effective stress intensity range AK threshold stress intensity range for. crack growth (measured) AKth actual threshold stress intensity range AKU alternating stress intensity range at underload AKUC critical value of underload stress intensity range Kmin ) - AU F1reduction in cohesive strength due to hydogen F_ ftrue fracture strain GO hydrostatic tension TVr monotonic yield strength AK transition stress intensity range in mid-growth regime poisson's ratio INTRODUCTION 1 1.1 CONCEPTUAL BACKGROUND design Modern approaches to against fatigue failure involve the application of linear elastic fracture mechanics and take int consideration th at all engin eering are The useful flawed. lif e span of such components, then, is estimated from the number 0 f cycles or time to the largest assessed undetected ba ed Because the of approach in attempted on to a crit cr ac k increasing propagate ical size which is mechanics fractu re esign, a large t components considerations. of this "defect tolerant" use number of i nvestigators characterize t he fa tigue cra ck growth behavior of many engi eering material s in terms of such variables mean stress forth. as frequency, mic rostr uctu r e, environment, and so Al though a major portion generated have of thes e data has been for the mid-growth reg ime o f cr ack growth (growth rates typi cally in excess of 10- 5 mm/cy cl e) , da ta there has been a rapidly growing extremely low growt h rates (less than 1o-6 rm/cycle or of the one intensity rang e below la tti ce fa tigue spac ing per c ycl e pertaining to where the stress approaches a so called threshold value , of for ) order need which cracks remain dormant or grow at experimentally undetectable rates (1). -2- The of use in essential data threshold been to found be applications as large scale nuclear and such coal conversion pressure vessels, turbine shafts, turbine alternator rotors, and acoustic fatigue of welds in blades, gas has circuitry nuclear in systems reactor high where frequency, low amplitude loads may be present (1). It is now well known from available the crack growth rates are sensitive to several mechanical that and microstructural variables, such as mean stress /Kax ), ratio (characterized by R= K, monotonic frequency, forth. with and cyclic yield A recent review of the effects be found in Ref. the 1. propagation load of size, cyclic strength, and so these variables The various mechanisms associated of fatigue cracks are shown 1.1 for the near-threshold regime as in Fig. schematically or prior stress history, grain size, grain boundary composition, crack can information well as for higher growth rates. The effect of behavior of environment materials, some controversy. information in influences near threshold. has resulted in near-threshold fatigue however, has remained a subject of First available on of the all, there very little literature on environmental Even this limited extent of data contradicting inconsistent descriptions. is interpretations and 10~2 10~4 PRIMARY MECHANISMS REGIME B I NON - CONTINI. UM MECHANISM S CONTINUUM MECHANISM (striation growth) large influence of: Ilittle influence of: i. microstruc ture ii. mean stres s i. microstructure ii. thickness iii. environmen 11 KC FINAL IFAILURE N X Imm/min d dN B z 2 -C C STATIC MODE" MECHANISMS I -6 large influence of: "-I lat tice spacin g Iiii. certain combinations of environment,meon per cycle stress 8frequency A1 10-8 1mm/hour (cleavage, intergranular 8 fibrous large influence of: i. microstructure ~ 0 ) N I m Wc C(A K)' REGIME E E 0 - - REGIME A ii. mean stress 1mm/day iii. thickness Ilittle influence liv. environment aT U of: 1mm/week THRESHOLD A Ko log A K Fig. 1.1 Schematic variation of fatigue crack growth rate with the stress intensity range in steels, showing primary crack growth mechanisms. -4- Fatigue tests on low carbon steel pressure vess el crack propagat ion decrease threshold AK 0 in hydrogen gas c ompared threshold near rates was fatigue proc esses involving ev en no embri ttl explained though air. 5-7), conventional corrosion threshold (1,3 4). nuclear press u re of corrosion em brittlement The results of are fatigu e Paris and with the inconsistent (vi z., mechanisms metal corrosion as well as hydrogen path suggested embrittlement) in fluence p recise mechanism f or hydrogen however, active or dissolution This hydrogen ement was suggested (4) . co-workers c onsiderable and in te rms of conventiona 1 hydrogen arguments, normalized the presence of d ehumidified in humi d tu and sho w significant acce leration in (3) steel (2) for environmental ef fects near For ex ampl e , data on A533 B 1ow strength v essel s tee 1 (5) tested in air and distilled wate r show no va ri ati on in threshold be havior with change in envi ronmen t for tests at a frequency tes ts Threshold 0f 160 Hz. on a low strength steel did not reveal an y appreciable ch ange in behavior among envi ronment s of air distilled wate r, and gaseous hydrogen of u nspeci f ied purity Results threshold air and although h igh in str ess dry and strength intensity wet argon D6ac steel showed that th e range values were u nchanged in atmospheres at 100-374 Hz, near- threshold growth rates were mar g inal ly 1ower in dry argon compared to air (8). There is al s o the added -5- complication of a seemingly more severe environment actually reducing the near-threhol d growth rates compared to air. and Seth higher (9) repored reduced near-threshold growth rates and AK 0 values in steam than in air at 1000 C. On the other hand, several studies have found vacuum increases the thresholdK0 compared to air. data on high purity heats of tempered E24 steel Cr Tu stainless martensitic have clearly demonstrated steels (En that the that Threshold (10) and 13% 56 and FV 520b) near-threshold (11), growth rates are decreased and threshold AK 0 values are increased in vacuo compared to re-welding has behavior (1). air. The possibility of crack flank been suggested as a partial reason for this The results of Skelton and however, show that in zero-tension loading it Haigh (12), is possible to propagate cracks in vacuum at much lower values of AK than the threshold values in air. It is evident from the above that conventional corrosion fatigue mechanisms do not explain the wide variety of near-th reshold environmental influences on in the literature. Also arguments embrittlem ent are inconsistent with the that low based steels on traditional cited hydrogen notion strength steels are relatively immune to hydrogen attack at low stress values. Moreover, the purity levels of the vacuum and inert gases used in different studies are too -6- different to allow any reasonable comparisons. has been speculated for Although a number of years th at corrosion deposits on crack faces might play some role in the it rates of crack growth, determining no quantitative anal ysis has yet been carried out to substantiate the exact natu re of this clear that influence. In with light of the above discussions, the limited extent of it is information avai lable in the literature, it mechanistic interpretations for environmental threshold stress proposed thus is not possible intensity far, is to levels capable make of i nfluences at that and viable any no providi ng model, possible explanations for the experimental observations. The purpose of this work is data base for the effect of to establish environments a reliable in the near threshold fatigue crack growth regime of low strength steels and to develop a mechanism to explain the influences near threshold of not only various environments, mechanical and microstructural size, load ratio, and so forth. but also such factors as strength, grain -7- 1.2 SCOPE OF PRESENT STUDY In the present study, it is clearly demonstrated that the signifi cant influence o f environments in the mid-growth and in the propagation near-threshol d are (chapter 3). closure" h as termed approac h been devel oped experi mental ne ar-thre s hol d ratios, reduced in compared to moi st dry which hydrogen in an d 0f enhan ces cl osure pressu re vessel hel ium is role of consistent at are as (such low load significantly water or air) such as h ydrogen or helium) corros io n excess crack be t hat rates growt h envi ronments oxide-induce d crack fatigue i s seen It to the crack in a 1ow strength pressure env ironments due to the f ormati on faces shown obs ervations (cha p ter 4). ex pl ain c osure. to deposits crack The significance of th reshold near - vessel steel . crack "ox ide-induced to environment near threshold a nd is with fatigue of by entirely di fferent mechanisms governed A new regions corrosion t es ted in air, water, steels noted. In particular, a characteriza tion of crack flank oxide de po0 sits is made using X-ray photoe lectron Evidence spectroscopy su pporti ng the concepts closure is p rovi ded in chapter 5. observations are highlighted and of spectroscopy. 0 xide-induced crack The consequences of these with p articular reference to the measurement of near-threshold data for Au ger and an explanation the effect of underloads on fatigue crack growth at low -8- stress intensities is given (chapter 6). environmentally-affected threshold strength pressure vessel steel different classes behavior 7). Further, surface mechanical, patterns additional intensities low in 2021 aluminum alloy contributions to crack resulting from varying are discussed in light of the morphology microstructural, commonly the low strength steels, viz., SA516 and of closure at low stress fracture of are c ontrasted with those X-60 pipeline steels, as well as in a (chapter The mechanisms for and observed envi ronmental at near-threshold behavior levels (chapter8). It is hoped that cl earer insight the into corrosio n fatigue crack which w ill material s form with results the of mechanics growth at this and work provide mechanisms ne ar -threshold of levels the basis for alloy design procedures for greater i nfl uenc ed fracture. resistance to environmentally -9- 2 MATERIALS AND EXPERIMENTAL PROCEDURES 2.1 MATERIALS low The strength investigation is a steel in used the pressure vessel &4Cr-1Mo present steel, namely ASTM A524 Class 3 (he reafter referred to as SA5 42-3) which is a ca ndidate materi al for coal conve rsi on app I i cati ons. thick section of thi s steel heat (Lukens 370 7) no. mm from Westinghouse Research and Developme nt chemi ca 1 compositio n tr eatment, heat Center . the and tempera ture mechanica 1 proper ties of this stee 1 Tab le 2.1. thickne ss, as used than shown mi crosc opy s tudies molybde num micros truc ture The bai ni ti c wit n I ess (13). was with a size of approximately 140 mm x 300 m m x 175 obtai ne d in A carbide 3%lo in polygonal Fig. showed of the 2.1. as - rec e i ved steel, SA516 condition. listed a re SA5 42- 3 wa s fully 1errite presence of at cent er a nd chromium particles (Fig. For c omparison purposes, three additional plain C -Si ambi ent Transmission electr on (Cr, C. and Mo 2C) f or th e environmental The 2. 2) alloys we re fatigue crack growth studies. Grade 70, was Microstructures studied of in A t he this pipeli ne steel w ere f ound to be 30% pearlite and 70% ferrite, with an average grain si ze of about 35pm-. The X-60 pipeline steel -10- TABLE 2.1 Chemical compositi-m, heat treatment, and ambie;t tm-perature mechanical properties of SA542-3. i) Base Plate Chem.;try C Mn 0.12 0.45 Si N__i 0.21 0.11 Cr Mo 2.28 1.05 Cu 0.12 p S 0.014 0.015 Heat Lukens Heat #3707 ii) As-received Heat Treatment a) Austenitize 5 1/2 hr at 954*C b) Temper 8 at 663 0 C c) Stress Relieve 15 hr at 593 0 C 22 hr at 649 0 C 18 hr at 663 0 C hr water quench -11- TABLE 2.1 iii) (continued) Ambient Temperature as-received Mechanical Properties (mean values) Yield strength (MPa) 496 7 U.T.S. Elongation Reduction in Charp* K Impact Area Energy (2Pa) (2) (%) (J) 610 17 25 77 197 18 Computed from ,J.. -neasurements; For dehumidifie. hydrogen at 138 kPa pressure For 45 mm gau0e length K Iscc (1Par) 295 >85 -12- Fig. 2.1 Optical micrograph of SA542 Class 3, 174 mn thick base plate at a)surface, b)quarter thickness (4 T), and c)mid-thickness ( T) locations (2% nital etch). -13- Fig. 2.2 Transmission electron micrograph of SA542-3 steel showing globular Cr 2 3 C 6 and needle-shaped Mo 2C particles. -14- was obtained from Science International Rockwell Center. Metal 1ography of the samples revealed a fine, equiaxed grain structure (approximat ely 10pm ferrite. The al ong the of direction the b anded in the longitudinal direct ion . structure, i .e. In appl icat ions, addition, an aluminum alloy u sed in aerospace namely, "ba nded" with crack growth spec imens were m achi ned so that the crack propagated ferrite diameter) in British Alumi num 2021 wi th a c op per content of about 6.4%, was investigate d material in produc ed was prese nt the ingo t as show n microstructure, in F ig. 2.3, The plate th e British Aluminum by A1 can Company and rolled to plate b y work. Pl a te Company. The is characterized by a distribution of globu lar part ic e s of CuAl 2 phase, which are This mate rial also contains located on grain boundarie S. 0.15% Cd which precipitates. acts for 10h. in a a he at agent for the 0' treatment at 529'C for 5h., gly col sol u tion, and dup lex aging at 163*C plus 171 0 C for 12h. temperature nucl eati ng Prior heat tre atment of the 19 mm thick plate consisted of solution quenching as The com p 0 si tions, and ambient mechanic 1 properties of SA516 , X-60 and BA 2021 alloys are given in Tables 2.2 and 2.3, respectively. -15- U. 0 - 10 0 fftk~2 Micrograph showing the structure of BA2021 alloy; white globular particles are CuAl 2 . Fig. 2.3 ,A-m 16- TABLE 2.2 Plate Chemistries Material C 0.23 ISA 516 Mn Si 1.2 0.25 Grade 70 Composition of X-60 steel plate, weight percent 0.147 Va Mn = 1.4 Cu = 0.049 p = 0.008 Nb = 0.047 S = 0.012 AZ = 0.029 Si = 0.255 Co = 0.014 Cr = 0.008 Mg Mo = 0.240 Ca c = 0.004 0.003 = 0.010 P S 0.006 0.019 -17- TABLE 2.2 (continued) Chemical analysis of 2021 aluminum alloy, weight percent Si = 0.1 Sn = 0.06 Fe = 0.17 Zn = 0.03 Cu 6.4 Ti = 0.05 Mn 0.32 Zr = 0.18 0.005 Cd = 0.15 Mg < V = 0.09 -18- TABLE 2.3 Ambient Temperature Mechanical Properties. Yield Material Strength Ultimate Strenguh Elongation K (MPa) (MPa) (%) SA 516 327 496 28 233 X-60 386 552- 418 489 8.5 r20 * 2021 AZ 25 mm gauge length ** Computed from Jc measurements (MPa m) -19- 2.2 EXPERIMENTAL PROCEDURES Fat igue crack propagation 12 .7 with mm cri ter ion the 50k N under pla st ic zone sizes did not c Yc lic that contr ol . in temperatu re mo ist Tes ts performed ai r pct (30 H ydrogen gases. clamped onto sieves sm all ring o- and were sealed system involving cold tr a ps, and heat bakeable lines (14). techni ques achie ved using DC electrical cap a ble of detec ting changes in crack length of the ord er of 0.0 1 mm. measured atmospheres puri f i cati on Crack growth moni toring wa s potential hydrogen th e test p i ece, where gas purity was obtained using an extensiv e molecular humidity), relative hel i um and ambient at co nducted wer e maintained at 138 kPa pres s ure in a were Testing was a nd high p urity d ehumi dified distilled water, chamber based In stron el ectro-s e r vo-hydra ul ic machines operating lo ad helium performed compact specimens machined in the T-L exceed 1/ 15 of tes t piece t hi ckness. on were Plane strain conditions were maintained orientation. on thick experiments N ear-t hreshold growth rates oad-she ddi ng under (decreasing stress intensity) condit ions, wit h the th resho 1Ld L'defined in terms of a mm/c ycle. g rowth of rate 10- maximum For decreasing load conditions, at each 1 oad level the crack was propagated a distance at least fo ur times th e size of the maximum plastic zone size formed a t the previou s load level. rates above 10-0 mm/cycl e were measured Growth at constant load -20- amplitude. Full experimental details have been described elsewhere (1,3,4). Characterization fracture surfaces was performed controlled PH I Model 550, ESCA on deposits usi ng ESCA/scanni ng fatigue a fully computerAuger spectometer. on fr actu r e surfaces a nd at 25 A depth studies ion sputter-e tchi ng) of corrosion of SA542-3 (after were conducted on the fracture surfaces SA516 and a luminum 2021 s amples. By comparing the resul ti ng ESCA s urvey spectra with standard spectra, the compositi on of the surfa ce oxide was deduced. the exten t of ox idat ion, obtained depth correspon ding rates tantalum oxide standard. The on io n argon sputtering yields from Veeco Brochure V60 and Physical Electronics 0 and Fe Auger monitore d were for iron oxide an d aluminum oxide were estimated u si nq the data (14). profiles compos ition as a funct ion o f Auger sputte ring time, calibrated using a k nown thi ckn ess o f (atom/ion ) To determine and their peaks, as amplitudes well From this informat ion, thicknes s fracture surface Auger sp ectrosc opy measurements detail in the Appendix. C peaks, were measured as a function of sputter time. of as an estimate of the oxide debris was obtained. are discussed in greater -21- Experiments to measure the rate of SA542-3 in procedures of Kurk el a and develop ed technique electrochemical the utilized by L atan ision (15 ), in 2.4 Fig. permeation De vana than and S tachurski cell the on based schematic diagram of the hyd roge n permeati on shown transport hydrogen (16). is used The mat erial unde r investigation is made a bi-electrod e i n the f orm of a membr ane (about 1.5 thickness) entry) of and anode c1amped an d ( in be tween both solutions experiment by (hydrogen An el ectr olyte solu tion of O.1N H2 S0 4 is used in the cat hode half-cell m inimize To the cathode mm hyd rogen e xit) hal f-cell s exposing 1.27 cm the surface ar ea. half-cell. A ar e the de-aerated and 0.1N NaOH in the anode effects of oxygen reduction, prior bu bbling nitroge n gas. the during and to Hy drogen charging is controlled by a ga lvanostatic ci rcuit whic h insures that the cathodic charging resistance and current not the is cell a functi on of the external resistanc e. is Hydrogen adsorbed into the membrane and d iffuses th rough to the other The anodic side of the sp ecimen is side. at maintained a constant potential versus a satu rated calo mel electrode by a potentiostat so th at the concentration of hydrogen surface side, it is zero. 0n that Thus, when hydrogen emerges at t he anodi c is immedi ately oxidized and the current thereby is a direc t meas ure of the permeation rate. sure that the oxidation of hydrogen is the sole g enerated To make reaction, C ATlHODE SIDE -Electto- E me It Polenliostal qSi clptW IR A Ga A mmele Gas -Gas input output Gas input N2 N2 *recorder Colomel electrode N) Deta 0 - in pPb i rei P.1 e lectrode %.ucim Iu coutr n terl electro2de n probeio 5on Idion soIN drainn ~2 To i he grips of ANODE SIDE on Instron Externalt e auae machine Power supply Fig. 2.4 HYDROGEN PERMEATION CELL K -23- the anodic side is plated with palladium to suppress the oxidation of iron (this has behavior). The permeation no effect current on is el ectrometer and recorded on chart paper. were carried out at room temperature. the permeation measured All by an experiments -24- TWO REGIMES OF HYDROGEN-INDUCED CRACKING 3 Lower strength steels, yield with typically below 1 000 MPa, hav e traditional immune to em brittlement i to be relatively hydrogen gas, a notion which has persisted K Iscc stress threshold inte nsities cracking under su stained load ing. strength values been considered the presence of ue to their high ydrogen-assi sted for However from the initial results obtained in this work on low stren, h steels, it has become evident th at such stee ls may be susce ptible to marked hydrogen-assisted cracking un der cy clic Ioa ding at stress The ambi ent temperature KIs Xc in fatigue cr ack pro pagation beh av i or of SA542- 3 is shown well below . intensities 3. 1 Figs. pressure for en vi r onments of dehumi d ified (0.5 frequencie s Fig. 3.2 and gaseo us to 50 Hz) or hydrogen and load rati 3.1 shows t he effect of fr equency at 3 .2,. the effe ct of load ra 0.05, and Fig. of 50 Hz. fatigue It is apparent tha t crack propagation signi fican t incre ases in moist ambi ent air cra ck oist air and low a range (0.05 to 0.75). load ratio are two where dry hydrogen rat es regions examined in the f 0 llowing sections. in these of causes compared as shown schematically in Fig. characteri stics o f hydrogen effects of o at a frequency there growth of to 3.3. The regimes are 5 6 7 8 9 K) 20 20 0 30n An I I 2 /4 Cr - I Mo STEEL ';n AC~ - -2 4 ) AK ( k sif 3 SA 542 Class 3 R = 0.05 Ambient Temperature 50 Hz air V 2 HzJ (30% RH) A 50 Hz S Ol I0 0 VV Environment Frequency * E -cc 2 5 Hz dry 2 Hz hydrogen (138 k Pa) 1-5 0 VIr 0.5 Hz 1-4 A L4 ai -6 0) U c N o di* z .0 aa -8 - 010 ci ,'- -3 0 le a0 0 00 0 I lattice 0 spacing per cycle 0 0 air 10 0 -9 10 Threshold AK 0 0 10 RI 81 I 3 4 Fig. 3.1 4 5 I I 6 7 I I I 8 9 10 20 30 ALTERNATING STRESS INTENSITY,AK (MPaVm) 40 50 Influence of frequency on fatigue crack growth rate in SA542-3 steel tested at R = 0.05 in moist air and dry hydrogen. 60 0 A K ( k si 4F) 2 3 4 5 I I N L) 7 8 9 10 20 I I I I I I 30 40 | | 50 I 10-4 21/4 Cr- I Mo STEEL 3 z E0-4 } 0.7 5 0 V H 2 (R=0.05) SA 542 Class 3 Frequency = 50 Hz, Ambient Temperature R 0.05 moist K -* x vx H (R= 0.3) air V A 00.* A0 -5 10 of 0.05 0.3 x x H 2 (R=0.5) 0.5 0.75 . 0.05 (0.5 Hz) 2 VA 00 ".0. H H2 000 jf *0 10 1 -6 > RO 0 10-4 F-6 0 7 0 z '0 0 5 6* *0 H2 H 10 I 10 of 0 I lattice spacing per cycle 0 Air 0 a : a 0 o -61 cr -7 0 1 . 0 9 -8 10 13 Air H2 R=0.75 a R=0.05 1-9 I 2 Threshold AKO 14 3 I~ 4 5 6 7 8 9 10 20 ~I I 30 40 ALTERNATING STRESS INTENSITY, AK (MPaVi) Fig. 3.2 Influence of load ratio R on fatigue crack growth rate in SA542-3 steel tested at 50 Hz in moist air and dry hydrogen. - E 6 - 1 -2 50 60 0 I 10-2 decreasing v increasing R AIR (independent of v and R) - E E -o 4- -6 10 increasing R 0-8 T HYDROGEN GAS Kmax m AIR *AKo(H 2 )j AKO(air) log AK Fig. 3.3 Schematic showing regimes of hydrogen-assisted crack growth commonly observed in lower strength steels. I I -28- REGIME excess of causes enhancements to compared air. growth in the r ates times) 20 ma x (roughly at lo wer AK levels with provide d t he frequency is 3.2), o n R). below a critical value (dependent and load ratio have absolutely propagation 20 value,' termed present case), i.e. increasing load ratio (Fig. crack to up These accelera tions s eem to occur at an approximately constant Kmax MPa/-m in the pre sence o f g aseous hydrogen 10-5 mm/cycle), in rates propagation (crack In the mid-growth regime ( MID-GROWTH no How ever, frequency 0n effect the for tests condu cted in mo ist 3.1 summarizes the Knax fatigue air. Table values for different freque ncies and load ratios obtained for tests in h ydrogen. The sudden hydrogen is transition observed to to a result in rate growth higher from cha nge a in a predomin ately transg ranul ar to a predomi nately i nte rgranular fracture in Fig. is at stress i ntens ity values of around K 3.4. F nax as shown The c haract eristic fractu re in ai r,. however, pred omi na tely t ransgr anular with sp oradic i nte rgranuiar both below a nd abo ve KT This effect of hydrogen max also app ears to be reversi ble in the sen se that rem oving the facets, hydrogen envi ronment durin g the test, val ues above KT max resul ts in at stres s intensity up to 20 times de crease in growth rates, whereas re-introducing hydrogen leads to an -29- TABLE 3.1 Conditions for Onset of Hydrcgen-Assisted Crack Growth in SA542-3 Frequency K K (Hz) (MPa/M) 0.05 50 no effect 0.01; 5 no effect 0.05 2 21.8 22.9 0.05 0.5 21.2 22.3 0.30 50 15.3 21.9 0.30 5 14.4 20.6 0.50 50 11.8 23.6 -30- AIR HYDROGEN AK= 14 MPa.iFi~ AK= 20MPa./m- AK= 25 MPa /i- Fig. 3.4 Fractography of fatigue crack growth in 24 Cr-lMo steel at 50 Hz in moist air and dry hydrogen gas (R = 0.3). -31- acceleration in propagation rates by a similar magnitude. Although many mechanisms have been for the hydrogen embri ttl years proposed ement of steels, such as the the Pf ei l-Troi ano-O ri ani de cohes ion models (18) and p res sure (19 model Zappfe is unlikely that one s ingle theory it can provide a c ompl ete under standing of the prob 1em. precise of mechanisms the over (Since embrittl ement are in most hyd rogen cases unknown, particul arly in low strength stee ls, w e imply here by mechanisms which hydrogen e nters the lattice and fracture). promotes some degradati on in resistance to Fo r high strength steels, h oweve r, decohesi on theories appea r to provide at least a part ial d escription of observed behav ior, monoto nic for both cy cli c and in such as H 2 0 and H 2 S. at mosph eres, "hydrogen-producing" loading Such models propose that hyd rogen is ad sorbe d f rom the gas phase, or evolved by reactive electroc hemi c al surface at the re a ction freshly on tip, thereby entering the crack und er the lattice and being trans porte d, (20) , driving force of the stress gradient, to the region of maximum dilation ahead of the crack tip where place presumably (Fig. 3.5). point of by some form embrittlement (Unlike b ehavi or ahe ad of a blunt maximum takes a red u cti on in cohesion at interfaces notch, the dil atati on ahea d of a sharp crack may be very close to the crack tip, i .e. crack of tip opening displacement. of the order of twice the Accordingly, in this latter 0y yy elastic /plastic stress distribution crack tip region 00 gaseous H2 2 embrittlement ~ F1 x o eg ion 4 Gas Phase Transport 2 . Physisorption 3 . Chemisorption (dissociation) 4. Solution in Metal Lattice (hydrogen entry) 5. Hydrogen Transport in Lattice I Fig. 3.5. Schematic illustration of possible transport processes involved in the embrittlement of ferrous alloys by gaseous hydrogen environments. IIC -33- critical case, the process may involved event rather in at occur the some embrittlement microstructu rally significant characteristic distance ahead of the crack tip). reduction in cohesive strength (a can be assumed to ) The be proportional to the local concentration of hydrogen at this point, where CH C0 is the unstressed = Co - exp(% /ROT) equilibrium iron (3.1) concentration lattice, the v hydrogen in iron, a0 the hydrostatic constant, of partial in the molar volume of tension, T the absolute temperature and hydrogen R. (2). the gas Such models are consistent with an increasing susceptibility to hydrogen embrittlement with increasing material hydrogen enrichment factors (CH /Co ) strength (21), are an since exponential function of the hydrostatic tension. The mechanistic aspects of hydrogen-induced cracking in lower strength steels, on the other hand, are still unclear. Classical decohesion models they predict only (18,21) marginal pose a problem since enrichment factors due to the small magnitude of the hydrostatic tension in lower strength materials. For external environments, classical models (19), where hydrogen is assumed to accumulate internal are also voids in pressure within molecular form and exert gas pressures, inappropriate since internal pressures cannot -34- proposed tha t hyd rogen a nner unspecified Beachem has hydrogen. of pressure external the exceed in deformation assists some and thereby promotes fracture, whi ch is after consistent wi t h observations of reduced flow stresses (22 hydrogen ato m s ) charging . disl ocations, and t0 importance the embri ttlement undefined at t his time (23 ). (24,25) hav e precis e interaction between the However, of clearly iron alloys, remains of studies Recent me tallographic may hydrog en that indicated al though the enhance nucleation an d growth of m icrovoids at internal surfaces strength low it bu t steels, is no t known whether such fatigue, "micro-decohesiv e" mechanisms are impor tant during where a complete mechanistic ba sis for crack growth the absence of environmental ef fects, is sti I1 strength a bainitic pressure vessel load marked ratio/freq uency with coincident a growth crack fatigue Hydrogen-assisted in even in , lack ing. low the in steel is characterized by depen dence, often is fractur e mode change from predo mi nantly transgranul ar to intergranul ar cracking, and occurs above critical Km. Many autho rs cracking in which is smal 1 value, KTmax have observ ed higher streng th ratio/frequ ency dependence, The (Fig. phenom enon, 3.6b) (26), referred has when Kmax compared to KIscc' hydrogen- assisted similar steels, a with identi cal load exc eeds Kscc (26-29). to as "stress corrosion fatigu e" been interpreted in terms of a I I (c ) ) (b) (a Og gressiveI agg ressive a ggressive z 0 "0 inert inert inert U E'I 0 EI log AK Fig. 3.6 Basic types of corrosion fatigue crack growth behavior: (a) true corrosion fatigue; (b) stress corrosion fatigue; (c) s.c.f. and t.c.f. combined. (after McEvily and Wei,1971). I -36- superposition (27) or process competition (28) load hydrogen-induced cracking and pure of sustained fatigue mechanical Reaction kinetic studies (20,30) indicate that components. such environmentally-induced cracking can be attributed to a mechanism of hydrogen embrittlement, Specifically, it reactions at the crack tip. in gaseous hydrogen rate-limited by atmospheres this appears crack growth that rate-limiting step involves chemisorption of hydrogen atoms, whereas environments, surface in water is limited by the oxidation of freshly exposed iron surface at the crack tip (20,30). Similar kinetic studies (30) in a lower strength steel (SA542-2) have shown that hydrogen-assisted cracking in this regime (i.e. chemisorption rate-i imited by KT aiso ) is max for crack growth i n ga seous hydrog en, and the above acceleration i n growth rates has been attr ibu ted to hydrogen embrittlement mechanisms (altho ugh the these mechanis ms for lower streng th s teel s In of view for fracture study, it the are uncertain). presence of a pred omi na ntly in tergranular hydrogen- assisted is preci s e nature of not c ra ck ing unreasona bl e to in t he presume present that the embrittlement mechanism involves hydrogen- induced decohesion at grain bou ndari es, strength steel s (18). similar to that observed in high -37- data In terms of macroscopic growth rate behavior, the in 3.1 and 3.2 indicate that an effect analogous to Figs. stress corrosion fatigue takes place in the mid-growth rates 6 10- (above mm/cycle) in lower strength steels, with the very notable exception that it well occurs at stress intensities T KIscc below i.e. at where no such hydrogen Kmax < KIscc embrittlement would normally result under sustained purely This suggests some synergistic interaction loading. than additive or mutually-competitive interactions) and environment growth. thus continuously providing that the role is felt a freshly basic some through However, rather than occuring of cyclic loading is simply to maintain tip, between fatigue contributions to crack mechanical in embrittlement mechanism, it change (rather sharpened crack exposed metal surface there for hydrogen to adsorb. One is now faced with a terminology problem of nature the characteristic since hydrogen-assisted growth observed, with its fracture mode ratio frequency/load and dependence, conforms to stress corrosion fatigue (c.f. 3.1 with Fig. effect clearly in lower occurs "below KIscc ". 3.6b), yet strength been termed "true corrosion fatigue" differ from steels the below KIscc has (26,31,32) , as shown in 3.6a, yet the characteristics of clearly Fig. Conventionally, such environmentally-assisted fatigue behavior Fig. the the present those depicted in this figure. effect It is -38- apparent that the commonly termi nol ogy (26,31 ,32) "above used steel s, strength high KIscc for corrosio n fatigue, whil st perhaps provi ding si mple a nd u seful ci assi fication insensiti ve 11 below and lower str engt h materials. s train-rate for be misl eading for can This fol lows from the fact that in such d uctile alloys, the st ress intensities nec essary for the onset of such hydrogen-ind uced cracking loading for ( embrittle ment) K Iscc9 i.e. this . First, ax as fatigue b y Ford (33) and strength high threshold s be can be steels should o ut for aqueous corrosion Daws on a nd Pelloux such (3 4), tha t K Iscc env ironmental dy nami c Second, K Iscc since stressed under fixed-load (i.e.cyclic) measurements or ri si ng-load critical event for determining the KIscc p rot ective In expected straining are condit ions, often fact, environment oxide by under the or fra cture of, scale previ ously formed at the crack pre-crack i ng test and threshold may often simpl y in volve hydrogen permea ti on through, tip. be on test pieces prev iousl y pre-cracked in air, performed the lower not be tak en as material const ants for a under reduced condition s. provided point ed particul ar alloy/environmental syst em, and can to and cyclic sustained Two r easons ). hydrogen are more str ain-r ate sensitive c ompared to steels str ength und er different are (from and in the employing conditions on side-grooved specimens, Shaw actual hydrogen fixed di splacement (35) has recently -39- signifi cantly that demonstrated approaching Kx mat lower KIscc lo w er values, can be measured in values, strength steels includin g 2 k Cr-Mo al 1 oy s. Thus, an it is reasonable to regard the value of in intensity stress threshold effective which threshold in KIscc steels (26), yet max as fatigue for embrittlement gaseous hydrogen-induced cracking by hydrogen mechanisms, KT is nominally equal to the sustained load is high rate-insensitive strain in the less than KIscC considerably present lower strength steels. strength hydrogen of role (The in influencing fatigue crack growth at near-threshold levels is to considered be largely of independent conventional hydrogen embrittlement mechanisms as discussed later in this chapter). Similar environmental embrittlement mechanisms. onset of the above a in or threshold as titanium alloys. environmentally-assited constant place in Dawson and Pelloux refer to their environmental fatigue systems, alloy where contribution to cracking involves active path corrosion in addition to, corrosion for fatigue crack growth for the mid-growth regime in aqueous environments for a number of the proposed maximum stress of, hydrogen (34), in fact, AKscc for aqueous However, since the crack growth intensity occurs (K max ) corrosion been have (33,34) arguments -40- (independent of R) for the present case of gaseous envi ronements (Table it is preferable to define the 3.1), envi ronmental threshold in terms of than a parti cular alternating perhaps worth noting here that who a value, ra ther intensity. I t is Kmax stress certain (2,36- 39), authors have exam ined fatigue crack propagation behavior ov er a limited range of growth rates, have this hydrogen environm ental threshold fatigue crack growth. interpr eted mistakenly as threshold fo r no the AK0 in As shown by the data and 3.2, this is clearly erroneous, since AK Figs. 3 .1 thresholds are generally an order of magnitude smaller. Finally, the question arises as to the reason existence of environmental an for the th res hold stress intensity ) for a hydrogen embrittlement con tribution to fatigue (KT max From the present da ta, the value of KT crack growth. max and and 3.2) 3.1 appears dependent upon frequency (Fig S. hydrogen pressure (discussed lat er independent of load ratio (Table are consistent the critical embrittlement stress is intensity Such hydrogen Thus, abo ve and observations which predomi nant with a c ritical tip. concentrati on hydrostatic stress and the lattice). 3 .1). 7), with modelling stu dies (18,21) which equate hydrogen ahead of the crack critical Chapter in by Fro m (I CH) hydrogen increasing Eq. hydrogen solubility of (3.1), this is dependent upon the concentration in the the hydrogen pressure, an -41- expected earlier onset of hydrogen-assisted growth is to be (this is shown to be true in Chapter7), whereas the similar least consistent with the kinetic asp ects rf q ualitatively there b e ing sufficie n t time for t he considered several processes in terms of t ce This critic al st ep the step competition betwe en principally i nvol v ing t he 3.5) (I Fig. in critical hydroge n embrittleme nt process t0 occur. can be at 3.1) is effect observed with decreasing frequency (Fig. tr anspo rt rate of hydrogen ads 0 r ption at t he crack tip, its into th e lattice, an d the rate of formation of fresh surfa ce as the crack grows. dismissed qui ckly diffusion hydrogen permeation 0f these, transport rate- 1 imiting a as hydrogen d ata. Us i ng step simpl y sampl es of 2 cm/sec. fr om (1 7), o ur a yie 1 ded SA542-3 of rough ly diffusion coeffici ent for hydroge n permeation (D) 5x10 - 7 be electro-c hemi c al the techni que of D evanath an and Stachurski measurements on un str es sed can Us ing the simple relation for the dis tance x for hydrogen diffusion into the lattice in time t, namely, (3.2) implies that hydrogen will permeate through the distances roughly 4 and 40pm during frequencies of 50 and 0.5 Hz, respectively. several times one lattice cycle, Since this by for is larger than the crack advance per cycle, and furthermore actual diffusion rates may be in excess of this -42- due to dislocation aided transport in stres sed (23,40) samples, hydrogen transport can clearly not be considered as rate-limiting noted above, co-workers more detailed (20,30) kinetic equate chemisorption of hydrogen hydrogen the crack t hreshold for the analogous effect of an environmental fatigue in aqueous T frequency dependence on K max the interaction between environments or hydrogen for the where , is assumed to be a function the of rate of oxide r upture at the crack tip, the rate of passivation and dissolution to gase ou s for tip and step rate-limit ing the at Wei by studies as Related arguments have been advan ced atmospheres. corrosion However, for the frequency range studied. rate the metal the bared surface at production of (33,34,41). NEAR-THRESHOLD In the where REGIME near-threshold growth increasing threshold the regime smaller rates are load ratio of crack than results in propagation, 10-6 a mm/cycle, decrease in AK0 up to a certain load ratio value, beyond which it is load ratio-independent, as shown in Fig. 3.7 for moist air environment over a range of R values from 0.05 to 0.75. The most growth is seen pronounced in the effect of hydrogen on crack near- threshold regime, where the presence of dry gaseous hydrogen enhances the fatigue crack AK (ksi'-In) 2 I 1022 - 7 8 I I 910 I I 20 30 30 20 150n 40 40 I 100 0 0 0 0 o R v - 6 I SA 542 Class 3 Frequency = 50 Hz Moist air 23*C, 30% RH - -o I 5 I 2 1/4 Cr- IMo STEEL 0 z 4 I -- E E 3 00 0.05 0.30 0.40 0.50 -5 00 00 0 0 0.75 0P o 00 0 z 0 0v N I 0 d- c 0 -6 0 A A A _0 0 40 I lattice V z 0 00 2 0 0 spacing per cycle V 0 510 0 a a: R=075o o R=O.4 vR=0.3 'R=0.05 Th reshold AKO -8 10 1 A AR=0.5 4I 2 3 i 4 i | 4 | | I I 5 6 7 8 _ 9 I . 10 20 I-9 30 ALTERNATING STRESS INTENSITY, A K(MPavri) Fig. 3.7 600 . U_ 0 2 . -7 10 z 0 AA 106 -7 00 Effect of load ratio on the near-threshold fatigue behavior of SA542-3 steel. 40 50 LA.) -44- by rates propagation orders of magnitude and two to up 30% decreases the threshold str ess intensity range by up to moist to compared influence signifi cant This air. hydrogen is o bserved only at low load rat ios, and there of is and hydrogen at high R valu es the helium ( little differ ence between near threshold growth rates in air 3.8). Fig. Although in dry g rowth rate s are lower compared to moist crack air in the mi d-growth regi o n of crac k it propagation, is seen in the n ear-thre shol d regi me tha t the presence of a dry inert gas act ually ac cel era tes growth rates by over an order of magnitude compar ed to mo ist ai r, the threshol d moist air bei ng 24% h igher comp ared t o helium. a hand, water dis till ed env i ronme nt A Ko value humid air, w hilst fractionally w et above re sults hydrogen On t he other leads to a marg inal deceleration in near thresh old crack growth threshold AK 0 in rates, a that mea sured in a t hreshold 3.9). At these in behavior simi lar to t hat of moist a ir (Fig. low stress in tensi tie s, the fractur e mode with is predo mi nantly transgranul ar with ev idence of some i ntergranular se paration 3.10). (Fig. are not maximum The pr oportion of in te rgranular facet s, which see n at R=0 .75, of typic ally increases wi th increasing 30-40% at AK decreasing to zero above AK=20-25 MP Hz, where abr upt observed in accelerations in z 15 MPa /i, AK to a before (at a frequen cy of 50 g rowth rates are not hydrogen or water) in air, water, and hydrogen AK (ksi friT) 3 4 5 6 7 8 9 10 I I I I I I 20 30 40 50 I - n2 2 1 21/4 Cr-I Mo STEEL SA 542 Class 3 Frequency = 50Hz, Ambient Temperature R 1 3 104 S U 0. .E .* 0 S0 10 air (30% RH) 5 0 - z 10-4 0 -) ~0 0.05) dry hydrogen 0.75i (138 k Pa) 00 1-) -6 10 7 0 0-5 0 L.. 10 03100 0 l0 C o C.D I) 7 0 I3 vu S S 0 H2 -7 6 Air 0 0 0 8 N spacing per cycle R=0.05 1?0 H2 R=0.75 I lattice * M a 0 I 0 0 0 0 0 10- 8 Air _ a 1- 9 Threshold AK 0 2 3 4 1 1 . 0 I 5 6 7 {{ | 8 9 10 I I I I 20 30 40 50 ALTERNATING STRESS INTENSITY, AK (MPa/m) Fig. 3.8 Fatigue crack propagation in SA542-3 steel tested at R = 0.05 and 0.75 (50 Hz) in moist air and dry hydrogen. 60 A K ( ksi /In) 3 -2 10 5 II 4 6 I 7 8 T I 20 1 9 10 I1 30 40 50 _ I 21/4 Cr- I Mo STEEL E -3 E 10 -4 10 SA 542 Class 3 Frequency = 50 Hz, R =0.05 Ambient Te mperature z -- air (3( -5 10 % RH) --- dry hy irogen (138 kPa) -74 0 a distille d water 0 dry heli urn (138 kPa) o wet hyd rogen (138kPa) 10 6 00 0 S00 ~0 6 ----- E 0_ 0 -0 / - 0 0 to-8 3 4 5 0 4 6 -8 10 -- Air 0 dry H 2 I lath ce spaci ng per cyycle H2 0 10- 9 wet H2 Threshold AKO 1 U l I I 7 8 9 10 20 I 30 I 40 . 0 -7-.-. -* (9 10 5 z He 0 0 1 41-- 000 50 60 ALTERNATING STRESS INTENSITY, AK (MPa/im) Fig. 3.9 Fatigue crack propagation in bainitic SA542-3 steel tested at R = 0.05 in environments of moist air, water, dry and wet hydrogen and helium. -47- Fig. 3.10 AIR HYDROGEN HELIUM WATER Fractographs of near-threshold fracture surfaces of SA542-3 steel from tests in air, water, dry hydrogen and dry helium envi ronments. -48- environments. Little evidence of such facets was seen in helium tests. The significant influences of hydrogen near threshold have also been interpreted previously as possible effects of (1,4). Although conventional corrosion fatigue mechanisms (i.e. in the case embrittlement hydrogen mechanisms of hydrogen environments, hydrogen embrittlement mechanisms) have been suggested the earlier, mechanisms had not been explained. has exact nature of such work In the present it become obvious that such models are not consistent with the near-threshold data observed and with the existing data in the literature. First, although there is a significant of influence at low load ratios near threshold, there is little hydrogen effect of hydrogen at high load ratios. as Arguments well as models based on hydrogen embrittlement do not explain as to why hydrogen near - deteriorates fatigue threshold resistance only at low load ratios. Second, the accelerations in ultra-low crack growth rates in the presence of hydrogen are not accompanied by any apparent change mid-growth in regime. fracture At low mode, load as ratios, growth rates are similar in hydrogen and proportion of was seen in the near-threshold helium where the intergranular fracture is different, whereas -49- in the proportion of intergranular fracture is similar rates are different (Fig. growth the where hydrogen and air 3.10). Third, strength have (42,43) recent studies shown that high which are known to suffer marked h ydrogen s teel s, embrittleme nt even under static loading co nditions, s how acceleratio n in near-t hreshold presence of hydrogen. growth is This behavior conventiona 1 corrosion fatigue arguments. not to the due rates explai ned by Most impor tant of AK 0 the pr esent study h as shown that the threshold all, no in dry helium for the low strength steel unde r investiga tion to AK in humid air an d similar t o be below th e threshold hydrog en. significant compared to moist air environment dry hydrogen causes growth rates near-threshol d in increases behavior si milar to that water whereas Moreov er, wet hydrogen leads to th reshol d , in that in moist air. Also, di stilled results in a marginal reduction in ultra low growth rates compared to air. The above observations clearly conventional question role of corrosion fatigue mechanisms, such as hydrogen embrittlement and active path corrosion (metal on the dissolution), environmentally-affected near-threshold crack growth. A new approach termed "oxide-induced crack closure", which has been developed in this thesis work, is seen to be consistent -50- with the observed effects of environments and is presented in the next chapter. near threshold, -51- 4. AN EXPLANATION FOR ENVIRONMENTAL EFFECTS NEAR THRESHOLD It was demonstrated in the previous chapter that conventional corrosion embrittlement explanations fatigue concepts involving hydrogen mechanisms for might near offer environmental rates, such arguments are seen threshold. viable effects inconsistent at the following mechanistic higher growth with the behavior A new model, based on crack closure due to the oxide debris on fracture surfaces, in while paragraphs and is the presented influences environmental and mechanical factors in the low growth regime are described of rate using the concepts of this mechanism (44-46). During fatigue crack growth, the crack tip, surroundi ng elastic material cl osure of the the tress propagati on , effective value, due to the restr aint of and on this residua l of intensity AK eff (=K intensity phenomenon range loading AK (=K max -K c2 cycle approaches the a respons ible range, from a nominal value the s tretch The result o f this is some , ). and the nominal -K re ducti on for crack for to mi n However,, max load rati 0 is raised, the crack remai ns open porti on plastically crack faces may occ ur at p ositive I oads of the loadi ng cycle (47). in is . at strained material as a an the 1 arger effective stress val ue. This by which crack tip stress intensity range values -52- are reduced fracture our due residual to surfaces occurs contact of is known as crack closure, or in "plasticity-induced terminology, and stretches crack closu re" (44,46-48). Al though it has long been k nown that the role of closure the near-threshold regime of crack growth could in be quit e significant no (1,49), has been carried out . phenome non detailed study of the It has become apparent in this wo rk, however, that by cons idering the closure arising crack from not only the resid ual effects plastic stretches in the wake of the crack, but also the enlarged excess oxide debris on the crack flanks, a mechani sm for environmental effects near th reshold could be derived. Fracture surfaces obtained after threshold tests show bands of corrosion products examination of such surfaces reveal thickest in specimens analysis Macroscopic that the oxide layer relatively at high load ratios (Fig. information obtained from X-ray (ESCA) them. 4.1). insignificant Comparison of photoelectron spectroscopy with standard spectra for iron oxides show that deposits present on the surfaces are predominantly (Fig. 4.2). is tested in moist environments at low load ratios and is found to be of proportions on often Actual oxide function of crack length (and thickness thus a measurements, function of Fe 2 03 as a growth -53- AK 0 = 7.7 MPa notch M AKO= 3.1 MPoj s - notch b R= 005 Fig. 4.1 R=075 Bands of corrosion deposits visible on near-threshold fatigue fracture surfaces tested in moist air at a) R = 0.05 and b) R = 0.75. -54- 11 7 1 CAuger 6 OAuger 5 Wj 1 | -- Fe2p1 / 2 Fe2P 3/ 2 4 Z 3 T eAuger Ols Cis Fe3s NI\s 0 -1000 1 -800 -600 BINDING Fe3p 2p 1 1 -400 -200 ENERGY, EV 2P3/2 1 0 Fe 203 2 P1/2 - 6 - 51 L 2k -740 -724 BINDING -708 -716 ENERGY, EV -700 SA542-3 steel ESCA analysis of crack tip corrosion debris in showing the presence of predominately Fe 2 03 . Fig. 4.2 -732 -55- rate) a re shown in Fig. 4.3, estimated using Ar+sputtering analysis in the Auger spectrometer. (Details of the oxide thicknes s measurements using Auger spectroscopy can be found in Appen di x). It is apparent that the oxide thicknesses are inversely related to the crack growth rate, an d are at a maxi mum close to AKo of . 0.2 In moist air the maximum t hickness is of the order pm hydrogen. at R=0.05, compared 0.liam in than less to (Even after intensive pur if ic ation of gas streams some residual traces of moisture rem ai n in the system which, aided by formation a fretting in mechanism, some in re su lt dehumidified environm en ts ). At R=0.75 thicknesses in either environment ar e an order of smaller. It is also found th e that oxide , oxide ma gni tude oxide background deposits obtained by exposing a fres hly bared surface of the same material to the same laboratory ai r environment for the same length of time as the duration of a threshold te st roughly 50A to 150A in thickness the substantial oxide formation similar to the whi c h is amount of oxide formation at higher grow th rates. fatigue process. This Clearly at n ear-threshol d stress intensities at low load ratios resul ts f rom some the are asp ect of proce ss h as been descr ibed as "fretting oxidation", where plastici ty-i nduced crack closure (47) and Mode II displacements (50) fracturing and compacting of the oxi de lead scale to ab rasi on, at lo w load E 3 2 1/4 Cr-I Mo STEEL 0.2 -SA 542 Class 3 Ambient Temperature (23*0C) U) Frequency iu z air (R=0.05) 50 Hz 0 0 0 air (R =0.75) 10-5 E 10-6 E z 10~7 - Threshold- 0 10- 0 0 1 2 3 4 5 6 7 8 CRACK LENGTH (mm) Fig. 4.3 9 10 11 Measurements of oxide thickness as a function of crack length and crack growth rate for SA542-3 steel tested in moist air and hydrogen gas at R = 0.05 and 0.75. -57- ratios, to yield local heating, new zones of exposed surface and hence more corrosion rates oxidation (46,51). The lack of visible deposits at high load ratios and at higher growth (Fig. 4.1) is certainly consistent with this promoting crack mechanism. MODEL TO COMPUTE CLOSURE K DUE TO OXIDE DEPOSITS The signifi cance of oxide closure, i.e. the where cyclic crack layers in tip displacements are small, at near-th reshold levels, can be estimated by means of following simple crack, shown in Fig. model. Consider first an idealized 4.4a, wher e the excess oxide layer taken to be a ri gid wedge of co nstant thickness d, along the crack length a distan ce 2Z behind the Assuming only is extending crack tip. a mechanical cl 0 sure phenomenon arising from the presence of the excess oxid e debris on the crack and ignoring pla sticity and hys teresis effects, calculations based on elastic integral (53) superposit ion equations (52) using Barenblatt faces singular or the Westergaard s tress function yiel d a closure stress intensity value at the crack tip (54) dE Kcz where d is x=O the (4.1) 42) maximum excess oxide thickness, 2z the -58- y i===, I dl so X - e- 24 (a) C 00/2 Kfra/o-y E -0.50 OXIDE PROFILE d /2/ -0.02 -0.25 r (Kmax/my )2 I-- 2t --a4 (b) Fig. 4.4 Idealizations of oxide wedge inside near-threshold crack. -59- behind the tip corresponding to the thickest oxide location formation and E/1- -2 the effective Young's modulus in plane strain. 2 z c in be obtain ed from scanning of estimate An el ectro n mi croscopy of fati gu a liquid ni tr ogen after cycl ing at threshold tip for SA542-3 steel roo t square numerical a pm. It dependenc e in air (R=0.0 5) of thic knes s oxide 2 in of 1 1A Eqn. MPaVin. 0.1 pm, KcZ For tests at R=0 .05 a ), the exact W ith 2 = 2 pm, and 4.3), an d = 0.2 pm (Fi g. found to be estimate of the closure stres s intensity K 4.5 the sho uld be noted t hat b ecause of v alue becomes less critical). maximum From was found to be . between 1/2 to 5 AKO levels. the 1ocati o n of the oxid e peak behind such microg raphs, crack in open broken specimens, h ydroge n, where d = in dry is estimat ed to be about 2.3 MPa /m. Thus the predicted d ifference in cl osu re stress int ensi ti es for moist to air and dry hydrogen near- thr eshold condit ions, due the presence of oxide debris, is of order 2 MP a/m, a pproximately equal the AK, values for to th e difference in ob served thresh old two e nature of t plasticityenvironment crack face influence o levels, ironmen ts (Fig. 3.1). Thus despite the crude model and the a ssumption tha t duced it closure are the ide ntical levels in is clear tha t corrosion d eposits formed of both on at the thicknes ses measured have a significant closure stress intensities at near-threshold where crack tip displacements are small1. -60- of the situation A more realistic idealization (55) in shown where Fig in SA542-3 steel on superimposed mo ist the mea sured oxi d e profile, for the ai r (Fi g. 4.3), is for a solid of crack opening profile as determi ne d from y ielding finite element sol uti o n, Shih's for monotonic . loading using J2 maximum R =0 .05 at strain hardeni ng exponent n'=0 .1), small-scale is deformation theory (56). thickness oxide By comparing the wi th the normalized crack opening COD/(K ) ( 2 /Ea , as a function of normalized max y /cr )2 ), it is again t ip (r/(K distance from the crack max y C ar ise from the can apparent that significant cra k closure displacement presence of su b-micron corros ion deposits. Ho wever, because of uncertantie s associated wi t h the location o f the oxide thicknes s behind the cr a ck tip at nature of cont act between the oxide profile from the crack AK faces, with the exact and by Purushothaman and al so was derived in of the in terference between mating fracture surfaces. In th eir surface roughness model the have Tien (57) , where an estim ate of the closure stress intensity Kck terms the are not feasible at present. Approximate calculations for closure levels performed with ox ide peak to the c rack tip, more rigorous calculations of Kcz been maximum for fatigue crack cl osure, influence of fracture surface undulation is considered, such that h = h0exp (cf) .( (4.2) -61- where h0 and h are length dimensions describing and final fracture surface roughness, the and initial the true fracture ductility representative of the stress state of the crack tip. a(h-h0 ), the ahead By equating the change in asperity height where a is an unknown constant less than unity, crack tip opening displacement, estimates of Kcz were derived. The model does not, incidentally, incorporate role crack of crack (50), growth influence the extent of interference which will (58). markedly However, despite this and uncertainties in the empirical CTOD expression the and constant a, this simple model does yield reasonable (57). estimates of KCP Thus, at the associated with small crack tip near-threshold opening fatigue displacements crack growth, it appears that crack opening or closing loads can be both the tip Mode II displacements characteristic of near-threshold in to by the presence surface roughness. assume more of foreign Whereas importance debris and by fracture oxide-induced with enhanced regard to closure will environemental effects, surface roughness-induced crack closure may well be significant known to in have coarser-grained superior microstructures, which are near-threshold crack resistance and rougher fracture surfaces (59-61). growth -62- Comparisons of the maximum excess computed cyclic crack different 2 4 Cr-lMo of cl as s es derived f ro in Sh ih's pressure calcul ations parameter s are o f similar Despite 4.5). sputterin g measu rements and one suggests in physically when environme nts, The at on this t his varia t ion differen t AK0 in cease will load wet for model, thresho 1d f or te sts in on e vac U o the for rationale appealing AK and to eff dry ratios, and with varying yield str ength a re consiste n t with this mechanism. based Au ger become s wedged-closed, such that it tends to zero. F i g. and computations, ACTOD existence of a t hreshold, i n that the crack propagate ) the two the in uncertainties inherent 0 4.1 (Table magnitude (5 6), strain that at the thresho ld stress intensity (AK reveal stee is, vessel plane for for ACTOD) displacements opening with 4.3), (Fig measurements Auger from threshold, at thickness oxide not would except to expect perhaps Further, at find a smaller CTODs w here , for example, r ughness-induced closure may play a role. masked Wh ile i nterpretati 0 ns of such a result may be by rewel ding effect '5 , the vacuum data of Cooke et al (10) and Skelton and Haigh (12) on medium strength steels do not in fact show a well-defined threshold. -63- Table 4.1. Threshold Data Environment Steel for 2tCr--1M o Steels R cyclic ___________ j(MPa ) (ijm) (jim) (iym) SA542-3 moist air 0.05 7.7 0.18 0.31 0.20 a-500.Pa) moist air 0.75 3.2 0.03 0.78 0.01 dry H2 0.05 5.2 0.08 0.14 0.09 dry H2 0.75 3.3 0.03 0.83 0.01 dry He 0.05 6.2 0.11 0.20 0.10 water 0.05 7.8 0.18 0.32 0.25 SA542-2 moist air 0.05 7.1 0.11 0.17 0.12 ayz769MPa) moist air 0.75 2.8 0.02 0.41 - __ max dry H2 0.05 4.6 0.04 0.07 0.04 dry H2 0.75 2.8 0.02 0.38 - __ Max. dry He 0.05 4.9 0.05 0.08 0.04 dry He 0.75 2.7 0.02 0.35 - ___ Oxide Thic kre ,s CTOD 0 SA542-2/ T690 moist air 0.05 8.6 0.19 0.34 0.16 a -Y575MPa) dry H 2 0.05 6.9 0.12 0.22 0.11 dry He 0.05 7.1 0.13 0.23 0.11 Plane strain values defi ned as 0.50 (AK 0.50 (Kmaxo /aYE) - maximum where 0 /2'E) - cyclic, and y , AK 0 and Kmax,o are the cyclic and maximum threshold stress intensities, a' and a y are the cyclic and monotonic yield strengths, and E is the elastic modulus. -64- 21/4 Cr -I Mo Steels 0.21 . SA542-3 e SA542-2 A SA542-2/T690 A 6 0 A cm, 0.\ 4-. 0 0~ 0' 0 0.1 0.2 maximum excess oxide thickness,d (AL m) Fig. 4.5 Correlation between oxide thickness and cyclic CTOD at 6KO -65- From the above results and that in dry environments is it discussions, such as dehu midified hydrogen or helium (where the availabil i ty of moistu re is less to an d environments) humid high load smaller), the at closure due to plasticity is excess r estricted. oxide debris is closure due to corrosion de b ris is stress intensity range resul ting threshold atmospheres. In v a lue values other lar ger air, not to thickness of such cases, the the and effective hence to the humid w 0 rds, near-th reshold crack growth hydrogen compared because of h ydrogen em brittlement per se, but moist air. measurements, influences formation compared lower due to a smaller amount of closure in opposed compared ratios (where smal ler, is are In rates are accelerated in th e presence of to clear threshold gaseous hydrogen as This is co nsistent with the oxide t he observ ation that hydrogen only at low load ratios and beha vior the fact that there is no c hange in c haracteristic fracture mode. The influences threshold (44). values of also load ratio follow and from strength on the such closure concepts The variation of the measured threshold AK0 values in both moist 4.6. Low load ratio threshold values are apparently greater compared residual to air and hydrogen environments is shown in Fig. those plastic at higher stretches load and ratios because of the the resulting -66- 10 8 SA 542 Class 3 Frequency = 50 Hz e mojit &ar(23*C,30%RH) 8_ K6 o dry hycregen (138kPa) CL Y w< 00 -- 4- 04 u WO z 0.2 0 2 0.6 0.4 0.8 1.0 C,, -12 C,) W E C;o 8 -P 4 8 00 - 0 0.2 0 0.4 0.6 0.8 1.0 LOAD RATIO, R = Kmin/ Krr. . Fig. 4.6 Variation of threshold stress intensity parameters with load ratio. -67- plasticity-induced this closure is closure enhanced further crack oxi de-induced by However, above a envi ronments. dry to compared In moist environments, closure. crack these critical R value (about 0. 58 for SA542- 3 steel), both c1osure modes The nomencl ature load rat io or environment. intensity stress ratio ar 4 .7 positive open crack a intensity a fatigue crack is a constant. Kc9, necessary to ,is threshold At low load ratios higher than those plasicity-induced for higher closure in load dry (Kmin are apparently where the meaured threshold values AK0 ), stress ), necessary to propagate AKeff(=Kmax -Kcz range, Kc a that assumed is It effecti ve the that and (49). intensity, stress threshold for and thei r variation with load paramet ers shown in Fig. minimum and the re is no influence of minim ized are ratios of because environments and both platicity-induced closure and oxide-induced closure in moist is seen that the maximum stress intensity it value corresponding to threshold = Kcz KOmax +AK . is no a constant, K mi is greater than becomes equal to K to same. at which the minimum stress intensity R value of corresponding Kc closure and hence the measured and the actual threshold alternating stress intensity values are the The i.e. However, at high load ratios, where the minimum stress intensity there AK 0 is , environments, , i.e. the R , is the critical load transition from a ratio constant Koe max -68- K AKth (A) Kmax - 4 4 Ki Kmin 4 T IM E Ln Ko Kma I Kmin= cI (B) LKth K 'I, ' IRcl 1.0 R Kmax KC Komax (C) AKth I-R Kmax IRcl R 1.0 Fig 4,7 : Nomenclature for stress intensity parameters at threshold and their variation with load ratio R (after Schmidt and Paris) behavior to a constant important AK , -69- R-independent behavi or. to note from Fig. 4.6 that R The fact that is corre sponding to moist air and hydrogen enviro nments is about respectively. It 0.6 and 0 .3, this critical load ratio is higher in moi s t ai r than in hydr ogen is indicative of higher closure loads due to enhanced ox ide debr is formatio n. Finally, the reduction in increasing material strength hydrogen in ultra-high consistent with threshold and values with and the la ck of an effect of strength steels (1) may also be this model, since plasti city-induced crack closure would be expected to be reduced in materials AK0 further, fretting higher strength damage from oxide debris would be somewhat less severe on the harde r fracture surface of a high strength material. Results of a number of studies show evidence supporting the oxide-induced crack closure model. Such data, along with measurement of closure using ul trasonic techniques discussed in the next chapter. are -70- 5. EVIDENCE SUPPORTING OXIDE-INDUCED concepts Evidence in support of the of oxide-induced an be readily fo und in the literature. closure crack CRACK CLOSURE The idea of corrosion deposits form in g in cr ack s and influencing subsequent growth example, threshold results for enti rely not is behavi or ve ssel pressure have been found to show so mewhat high er steel water than in air near-threshold (6,46). Tu a nd Seth new. (9) and For rotor AK0 values in slower report rat es i n se veral rotor steels tested growth at 100 0 C in the seemingly more ag gressive environment of a f act they attribute to a number of steam compared to air; factors including crack tip cor rosi on deposits. In fact, observation of corrosion de bri s has traditionally provided a means to detect and monitor the gro wth under show clearly incipient conditions in m any aircraft components service Studies by Swanson and Marc us (51) of that the 63) as well as Benoit amount of dif fusi on oxide in to far greater than that abs ence of crack growt h. ) (64 reveal that in et al and that the mat eri al in the pre senc e of moist envi ronments duri ng fatigue is (62). phe nomenon of enlarged oxide formation is a result of th e fa ti gu e process itself the flaws c rack growth i n th e same enviro nment in the Resul ts 0 f h um id Mahulikar and environments di spl acements on the faces of fatigue specimens Marcus resi dual are higher compared to those in vacuum due to the build up of oxides on -71- fracture faces. explain in Fatigue data by Nordmark and Fricke (65) crack arrest during fatigue of 7475 alumi num alloys sump water using arguments Skelton and Haigh (12) deposits. of crack tip corrosion interpret their results of lowered AKO values in vacuo and at R=-1 in Cr-Mo-V steels at 550 C terms in of reduced crack tip opening dis placements from shea r lips and oxide-filling become of the crack. has clear that several hitherto unexplained ex perimental observati ons cited in the literature (and briefly in It chapt er described be understood ba sed on the c oncepts of 1) can crack closure induced by corrosion deposits. The on results environmental effects near-thres hold region of crack prop agation previous chapt er) oxide-i ndu ced clearly crack closure. supp ort in the (presented in the the concepts of The fact that with reference to moist a ir, near-threshold growth rates are accelerated in dry hydro gen and dry helium and marginally decelerated in distilled water while hydrogen the point corrosion showing the same behavior in wet may b e somewhat surprisin g (and unexplainable from of view fat igue of arguments mechanisms). based However, on conventional these results cl earl y demonstrate that the si gni f icant role of environment near th reshold de pends princ i pal ly on the availability of moi stu re and not on the embritt 1i ng tendency of any specific envi ronmental species. This behavior is obvious from the -72- result that while dry crack hydrogen accelerates growth rates by up to 20 times, wet hydrogen leads to a threshold behavior similar to moist air. on near-threshold SA387, Class 2, Grade 22 steel Recent data (66) specimens taken from the heat-affected as well as the weld moisture is responsible for thick oxide (and formation. not In oxygen) this near-threshold pressure growth similar to those in rates dry air zones have vessel shown that steel, the in dry oxygen are found to be and dry hydrogen are and significantly higher than those in moist air. Actual procedures measurements Williams of of and closure crack DeLonga techniques developed by Frandsen et al usin g (67) (based (68)) are the on the de scri bed below. MEASUREMENT OF CLOSURE USING ULTRASONIC TECHNIQUES Near-threshold crack using cl osure ultrasonic waves(68). phenomenon was studied Compact tension specimens were prepared by conducting thresh old tests in moist air and hydrogen environments length, frequency i.e. of about 2 MHz, and by pre-cracking to the same crack 26 mm were specimen and were received at schematically in Fig. dry 5.1, Ultrasonic waves, with a transmitted at one edge of the the opposite end as shown while the specimen was mounted -73- ULTRASONIC GENE RA TOR TRANSMITTER CT LOAD SPECIMEN RECEIVER OCLLOCOPE Fig. 5.1 Schematic showing the location of transducers on the compact tension specimen for ultrasonic testing. -74- specimen was subjected intensity values (slightly above to the K ze ro values max thresholdAK0 of 7.7 MP a/in at R=0.05). signal load. The corresponding to stress loads from ra nging the of on the testing machine for application to 8.5 [A Pa1/m about corresponding to the The amplitude 0f the to the specimen was kept a constant and transmitted the transmitted outpu t from the receiver was mon itored an oscilloscope. T h ere no variation in the receiver was signal up to a certai n load level beyond whi ch t here was a This is due to the fact the sig nal amplitude. in decrease with that as the crack sta rts to open, a of arno unt lesser the signal is transmitted to the receiver leadin g to a reduction in th e signal s i gna 1 After a gradual de crea se, reciever amplitude agai n reached a constant v al ue . droppe d then were ampl itud e. repea tability. to There the zero level to The loads check for was no noticeable difference between the receiver signals for increasing and decreasing loads. The variation of against the stress conducted on specimens values receiver output signal intensity factor for fatigue cracked to is plotted closure threshold in both air and hydrogen atmospheres (Fig.5.2). seen that there is no steep decrease in the receiver implying so that the crack does not open all rather observation gradually. of Bachmann This is and Munz in AK0 It is output at once, but does agreement (69) tests with the that crack surfaces -75- MOIST AIR (R=O.05) IR -5 - a: DRY HYDROGEN (R=O.05) - w MOIST 1n - '-I W- AIR(R=0.5) 3 w u w - 15 X Z 201 - o, Ai ,- INCREASING K O,AO - DECREASING K SIGNAL FREQUENCY = 2 MHz 251 0 2 4 6 8 , STRESS INTENSITY Fig. 5.2 10 12 KI (MPaJ/n) Variation of receiver signal with stress intensity. -76- can remain in contact 1local ly, be considered open. fully for the c rack c losure obtained, it while globally the crack Although no precise estimati on stress intensities, of the c losure K values threshold coul d KcZ be is observed that the stress intensi ty levels at which the recei ver output signal order can in air and value decreases is of the (roughly equal to K levels at hydro.gen). The most importa nt observati on of these tests is that crack opening occurs at a higher sti ress i ntensity value for com pared aiir moist the specimen tested in to that tested in hydrogen, confirmi ng the occurrence of increased crack closure near threshold due to oxide deposi To check the validity of the closure addi ti onal experiments were conducted. signal wa s the same (Fig. 5.3), with a saw cu t equal and output wi th and this hydrogen. the constant Al so, a in length to the crack length of the fat igue-cr acked specimens showed receiver in as that obtained with no load on the specimens thresho 1d- tes ted in air specimen variation whi 1e the applied loads were increased from zero to th reshol d 1evel s output two When a specimen with no fatigue crack was te sted there was no receiver tests, increasing no change 1oads. in the However, the amplitude of the output signal for the case of the specimen was much smaller than the initial saw cut output amplitudes of the uncracked and the precracked specimens. -77- UNCRACKED SPECIMEN _j AIR (R =0.05) H 2 (R=0.05) AIR (R =0.5) SPECIMEN 0 Fig. 5.3 WITH SAW-CUT LOAD Schematic showing receiver signal output for uncracked, saw-cut and fatigue-cracked specimens. -78- The tests conducted that using ultrasonic waves indicate the closure loads for threshold tests in moist air are higher than uncertainties those involved of the fact that locally in the dry hydrogen. of Because the in using this technique and because crack surfaces may be in contact (similar to the growing region of Hertzian contact) while macroscopically the crack may remain closed, a closure load cannot be meaningfully estimated. single -79- INFLUENCE OF FATIGUE UNDERLOADS NEAR THRESHOLD 6 Transients in growth rate behavior or overloads attributed stresses blunting cycli c (70,71) , hardening (72) ,crack strain (73), and plasticity-induced closure such phenomena these studies where mechanisms such as Since (47). sheets thin plane stress conditions, essentially under (70,71,74-76), with performed been have tip to airframe components many of common are compressive residual as mechanisms such single spectrum loading sequences have been various to by induced plasticity-induced closure crack can be predominant (47). In this work, however, the role of loading under fully Specific ally, the ed so-cal is considered (AKO) certai n loading standard load near-thr eshold example, of spectra, shedding blo ck intensi ty stress (1). amplitude strain con ditions is examined. plane influence threshold variable in procedures the occ ur within laborato ry during (1 ,77) for measuring growth rates at low s tre ss intensi ties. since measurement of such the for no cr ack growth Such underl oad s may and below cycling ne ar -thresh old For crack growth a t conventional frequencies ca n b e so time consuming, it or is often necessary to interrupt the test, "parking" where overnight presumably no by say stopping at aAK level below the thresholdAK0 damage can occur. Where such -80- interruptions have been transients crack growth behavior in reported behavior for nominally , result often after the interruption is initially from behavior before unexplained (78), and very different identica 1 conditions. In the present work, the influence of periodic cycling at AK levels below the threshold AK0 fatigue is examined on near-threshold crack propagation in SA542-3. rate behavior is rationalized in The tr ansient growth terms of oxide-induced crack closure. The examined of influence under variable constant AK cycling sequences illustrated in Fig. near-threshold levels , amplitude loading was using load (R=0.05) After load shedding 6.1. cracks were grown for 1 -1.5 whereupo n a (AK mm at a s ub-threshold AK underload (15 level ( ) constant baseline AK 1evel to AK U) was a pplied for 2.7 x 106 AKB baselin e original level. serie s A performed for baseline levels of AKB underloads (below AK0 length (a) the retur ned hrs at 50 Hz) , bef ore condit ions were 4 - versus numb er of cycl es (N) sequence, the 6.1), namelv (da/dN)B (da/dN)s of AKU = 8.3 the initial of - number the were 10 MPa/iKn, with 7.5 MPa/I. From crack dat a moni tored during following p arameters were defined (Fig. the baseli ne crack growt h rate at AKB, crack grow th rate at AKB of cycles at LKB before growth rates to tests following the underload period, and a and N*representing the crack and cycles returned length following the underload period to their original baseline -81- H- constant Cr) z R=0.05 LJ 0L CT) Ile Vl) AKB AKU AKS LUJ Hn +-27x 106cycles+ (a) AKB - E - N Cr LU - d-- dN) B ---+ z AKU E da N8 dN /S dN JB N NUMBER OF CYCLES (b) Fig. 6.1 Nomenclature of different parameters used to describe the underload interactions near threshold. -82- value (da/dN)B' of Effects near-threshol d sub-threshold crack underloads growth between 8.3 and 10 MPaiii (R ) on at baseline AK B level s rates a re =0. 05 ) < AK (AKU shown in Fig.6.2. Data pertinent to this figure i n term s of paramete rs defined in Fig. growth 6.1 are listed in Tabl e was cycles, ever affected. Little AKU = 4 MPa/iii (Fi g. AKB = 10 MPaVi at AKU = 6.5 MPaii had growth at AKU = 9 MPa/i underloads AKU = gr owth crack underload of a smal 1 4.2b). (Fig. be 1ow and 10 underload periods, initial slower MPai cases apparen t after an rates growth influence at Fig. on crack Appl i cation of cycl ic the resul ted however, ( 8.3 underload Simi 1 arly, underl 0ad cycling decelerations in subsequent bas eli ne between was crack cert ain in base line 6.2a). only was e ffect on fractionally 7.5 MPa/i, no Although du ri ng t he 2.7 x 106 detected subsequenct severely 6.1 . threshold in growth at significa nt 6.2c-f) . AK B at rates Following t he grow th rates were up to 5 tim es than pre-underload base line rates, w ith retardatio ns experienced over crack growth i ncrements a* (equivalent up 0.3 to mm to several times the maximum pl astic zone siz es at AKB ). Thus periods of underload cycles beneath the , AK 0 threshold where presumably no crack growth damage can occur, can give rise to transient retardations in near-threshold crack -83- A K = 10 -- a- 4 2 2.3 - -+10 MPa / 22.4 3 x 1O~ 6 mm/cycle 22.2 22. 1 - - 3 x 10-6mm/cycle 22.0 21.9 0 4 AK=9- 6.5- 22.8 - 0 8 I 282 278 I 286 9 MPaGV' 8x l~7 mm/cycle 22.7 10- 6 mrn/cycle 22.6 23.2 282 12 I 294 288 - E E 6 0 AK 8.3 -- 7.5 -+e-8.3 MPa y 42xxlO- mm/cycle 23.0 0 3 S24.0 -AK=9-7.5 --- 9MPa 303 20 4 30 20 10 M- 10 7 mm/cycle ).5x 24.06 253. B 24. 6 12 906. x 28 6. 5 Fig. 6.2 10 280 mm /cycle i- x -/mm/cycle 285 290 Number of Cy cle s (N x 104) Crack length versus the number of cycles showing the effects of underloads. TABLE 6.1 Test 'No. a B~~ U 10 10+ 4 96.5 8.3 d 9 + 7.5 - 9 e 9.5 7.5 7.5 8.3 + 9.5 10+7.5+i0 (mm/cycle) d( x-6 1 x 10 + +8.5 +2 (mm) N, (no. of cycles) 0.01 1.5 x 10 x 10 0.008 1.5 x 104 x 10~7 0.1 8.0 x 10 5 0.14 6.5 x 105 x 10 7 1 2.5 x 10 6 +6.5x 3 x 10- 6 a 3 x 10J 4 x 10~7 +1.4 1 x 10- 6 _____I____________ f dKB . 3 9 c S on Near-Threshold Growth 1.2 x1 6 0.3 5.0 x 105 - of Variable Amplitude Tests involving Effects of Underloads (AKU ) Results I CO 4:11 .2 0_________I x1 0.24 10 15 -------------- -85- growth rates over distances comparable wi th several maximum plastic zone dependin g sizes, both on the the magnitude baseline of and the retardation under - load stress i ntensi ty ranges applied. It has been shown that, certai n in circumstances, below the threshold stress intensity AKO can retard cycling subsequent near-threshol d crack growth rates, somewhat ana logous to found to posses s failure. Howev er, whereas strain phenomenon well know n effect of "coaxing" the where smooth specimens cycled below the often a improved coaxing fatigue re sistance has been limit to are fatigue attributed to aging effects (79), a mechanism for the influence of sub-threshold underloads is presented below in terms of oxide-induced crack clos ure arguments. It was shown thicknesses from the chapter that oxide propagat e equals displacement (ACTOD). AKB threshold is approached oxide thickness measurements it was inferred thickness baseline previous levels as t he that cracks would not oxide the increase with decreasing growth rates and hence with decreasing AK and in and the when the pulsating crack Thus for particular underload AKU, it maximum excess tip opening combinations follows that if excess oxide thickness d formed at baseline AKBis less the ACTOD at underload AKU then the application of the than of sub-threshold underload cycles, while not generating fatigue -86- per se, can result in further oxide formation due to damage Thus fretting oxidation mechanisms. level AKB baseline following underload cycling, one the retardation initial might expect in this instance some the to returning on in growth rates due to the increa sed crack closure loads crack from the extra oxide deposits formed at AKU larger than the underload ACTOD, underload the on the excess oxide thickn ess d at AK B is already hand, other If, . the of then little effect cycling would be expected since during the latter period the crack would be effectively wedged-closed thereby limiting further oxidation. This c once pt is illustrated in variation cr ack of thi ckness oxi de measured pul sating growth crack (d) and tip cyclic CTOD a the where 6.3, experimentally (da/dN), rates Considering first the situation o f MPaVi, Fig. underload computed is values basel i ne plotted. 0f A KB 10 the oxide thi ckness gener ated at thi s le ve1 h as been measured to be app rox imately 0.11 pm (Fig. underload of 4 MPa/m AKU ACTOD is ro ughly 0 .05 thickness, such is the crac k enhanceme nt in oxide-induce d crack the exi sti ng remains c los ed. closure, , observations (Fig. an oxide With no th eref 0 re, underload of 4 MPa/im would b e expected to have 1 ittl on growth ra tes at 10 MPav/im When applied, t h e c orre s pondi ng pm, smaller than tha t 6 .3) an e effect in accordance with exper imental 6.2a and Table 6.1). an underload of AKU= 7.5 MPa/m is applied at Conversel y, when AKB= 10 MP a/f, -2 2 1/4 Cr-I Mo STEEL 0.7 Z42 -3 10 C lass 3 Freq uency = 50 Hz, Ambient Temperature Air (30% RH), R=0.05 Calculated ACTOD 0.6 .- 0.5 *& - E da/dN E 10-5 0.4 0 z ~0 0 -10.3 I-) -6 10 - lattice S pacing p er cycle 0.2 Measured d -7 10 0.1 AKuc AKO -08 2 4 6 8 AK 8 10 20 30 40 A K (M Pa v/r) Fig. 6.3 I 0 . _0 E Variation of cyclic CTOD, oxide thickness d, and crack growth rate with stress intensity range and a scheme for finding the critical underload stress intensity range. 0 50 I -r-0 ('_ underload ACTOD is now roughly 0.17 pm, larger than the the existing (baseline) oxide thickness, such that some oxide growth can occur. With the resulting enhancement in oxide-induced crack closure, the 7.5 mpa be expected rates at AKB (Fig to cause some It also follows level, e effect. bel ow which underl oad retardation in growth from discussion this that whi ch underloads ca n remains crac k ACTOD is clo sed, corresponds to an underloads at 7.5 (Table AK,= 9 MPav'm AKU= 7.1 MPavm, rates underloa d MPa/mi ca n S0 .11ptm), level of AK U =6 MPa/m. lead underloads at 6.1). Similarly fo r where critical un derload whereas to 4 MPa/-m crack sub sequent h ave Iy by ro ugh ly five lev el time s, negl i g ible effects are ap parent fol lo wing underlo ads 6.5 MP av/-i AKUC by (Fig. 6.2b and 6.2d). Using Fig. 1ittl grow th under loads at 7.5 MP a/m are seen to initial the less than the existing oxid e th ickness this growth have whe re i.e. For crack growth at AKB = 10 MP a/m (where d effect each This corresponds to an underloa d AK U level the retard ati ons at a critical u nderload stress intensity (d). Hence results 6.2. range (AKUC ) would exi st below 1 i ttl would Similar arguments are applicable to the other results in Fig. r initial underload /m 10 NPa VF consistent with experimental = 6.2f and Table 6.1). basel i ne further e at becomes reduce whereas at at 6.3, values of can be esti mated graphically for any baseline AKB level, simply fol 1 owing the direction of the arrows i n equating -89- oxide thickness (d) to AKB . However, AKU crack closure is important ACTOD oxide-induced that recognizing at at only at low stress intensities where crack tip d isplacements are deposits corrosion and of the same size scale, it is likely to apparent that sub-threshold underl oads are (proportional rapidly i ncreases k levels, the corresponding ACTOD increasing With r ates. growth near - threshold on effect an have only so to AK 2 ) that further oxid ation during the underload would be negligible in comparison. has been shown that near-threshold Thus, in summary, it growth crack fatigue suffer can following underload cycling (at the same load to Such crack growth threshold. the generated oxide enhanced from result ret ardations transient rati o) below retardations are reasoned crack induced closure during the underload, provided that the underload ACTOD is large enough to allow further close numerical correspondence between oxide The grow th. \'CTOD and cr ack flank oxide thickness data, however, could be considered somewhat in view of the uncertainty in the two e stimates. fortuitous But conceptually such data are totally of explanation experimental the with consistent an observations in terms of oxide-induced crack closure. In terms of recommended procedures for thresh old (77), fatigue such crack closure growth concepts measuring and threshold could have AK near values important -90- Current practices for threshold determination consequences. utilize c rack grow th (load-shed ding) monitoring an d/or under decreasing AK increasing conditions, continuous ly involvi ng variable amplitude 1oading. generally minimize taken to crack gro wth considerat ions. be too rapid retardation determi nation threshold may avoid and in that a "parking" overnight at AK levels below yield simi lar premat ure retardations. plasticity tests, the growth rate s determined incre asi ng AK. In this si gni f icant tha t material s which unde r aqueou s this str ess behavi or contri buti on regar d, are say by may More over, where oxide conditions may be somewhat different f rom under factor threshold, induced cl osure is s ignificant, one might e xpect threshold in K to further interrupting is premature from It is now apparent that important hence resulting thus Care descent a AK v ery that decreasing those it near AK determined is perhaps, susceptible to corrosio n cracki ng are oft en likely to show (77,80) from possibl y refl ect ing a differing oxide induced crack closure arising from the presence of sub stanti al crack fl ank corrosi on deposits. -91- 7. THRESHOLD BEHAVIOR IN DIFFERENT ALLOY SYSTEMS It was in shown oxide-induced crack pressure of that the grow rates eels. vessel th ree in aracteristics classes teels lower strength alloy are di scussed in the li intensity r ange It two other as well as an aluminum pipeline SA516 for presure (0.14 gas at load rati os of 0.15 and 0.75. of this steel obtained by Wachob and pressure in t of crack clos ure phenomena. environments of moist air and low hydrogen different 7.1 shows t he v ariation of crack growth rate with Fig. stress (6.9 Nelson stee in MPa) dry Fa ti gue data in (37) high MPa) h ydro gen are also plotted in Fig. 7.1. is observed that si mi 1a r to the behavior observ ed in case of SA542-3, the pipeline steel of crack growth, namely, the unde rgoes also significant accel erati ons in propagation rates regions of thi s c hapter, the In near-thresho 1d crack growth of concepts readily explain environmental closure influences at ultra- low types 4 Chapter in the two the mid-growth and the threshold regimes. In obtained the in Nelson (37) similar. studies mid-growth the present region, study the as crack growth data well as by Wachob and f or environment of moist air are found to be The difference in the testing frequency in the two does not appear to result in any significant 2 t072 t4~ [ 3 4 5 AK (ksil/in) 6 8 7 9 10 20 30 40 50 SA 516 Grode 70 Pipeline Steel z 1-4 Ambient temperature E E 0oz ' R 015 0.15 0.75 dry hydrogen (0.14MPo) o 0.15 0 15 laboratory air dry hydrogen (6.9MPa) o o * 0 0.75 Environment rnoist air (30% RH) Reference present study Hz) present study f50 high pressure H2 (0.15) 10 .111 6 00e (50Hz) Wociob and (0 Nelson (0.1 -OHz) 0 A~ * * .0 -6 10 >' low pressure H 2 and air (015) - A 1,0 z 0; -6 76, 90 83 0 0 0 spacing 0 H2 E air ---- ,) (0.75) 0 _ H 2 (0.15) 0 t 2 3 per cycle 8-air (0.15) -69 b 4 I lottice ' - 0 -8 L Threshold AK, 5 6 7 8 9 10 2 0 30 40 50 60 ALTERNATING STRESS INTENSITY, AK(MParmn) Fig. 7.1 Variation of crack growth rate with stress intensity range in SA516 steel tested in moist air and dry hydrogen environments -93- in fatigue be havior. differences (This on the influence of low pr essure critical in the frequency mid-growth inferred and the information hydrogen i mply the for a ny effect of low pr essure hydrogen regime is below 0.1 Hz) . It can be from these resul ts t hat increasi ng the pressure of hydrogen from 0.14 MPa to acceleration in 6.9 MPa g rowt h crack leads to value of 11 MPa/'m (co p a r ed to a KTmax of1 for low strength This SA542- 3). the of influence about 20 MPa/m effe ct of consistent with the previo usly presented that considerable rates wit h a relatively low K ax 3) that pressure is arg ument (Chapter hydrogen in accelerating crack velocities at growth rates above 10 -5 mm/cycle is due to a hydrogen embr ittlement mechanism. In the threshold environmental regime influences seen for in crack the case growth, the of SA516 are similar to those in SA542-3 for both low and high load ratio values. Also, comparison of the results obtained on SA516 in the present study and in Ref.37 crack shows no variation in growth rate with a change in frequency from 0.1 to 50 Hz above a information growth on rate crack of 10- mm/cycle. growth rates near-threshold for high pressure hydrogen or frequencies lower than 50 available for SA516. Unfortunately, Hz are not -94- The fatigue crack steel in 7.2. Fig. other pipeline X-60 In this case also, behavior similar to that of lower strength steels is observed. classes 7.1 shows the fracture surface oxide SA516 and X-60 pipeline steels both of behavior and hydrogen environments is shown in air moist growth Table values thickness in for It is noted that (81). at low R ratios the thickness of excess oxide on crack faces is several times greater at ultra-low growth rates than that observed at higher growth rates or load ratios. From the above results, it can be that inferred the explanation for environmenta 1 effects based on oxi de-induced closure is several consistent classes of low s trength steels, i.e., (ferritic-bainitic) , SA542-2 (fully (banded bainitic), ferritic) observ ations experimental with SA516 (fully martensitic) (ferritic-pearlitic) SA542-3 and X-60 IN 2021 ALUMINUM ALLOY To contrast the behavior near-threshold environmental in lower strength steels, influences were investigated in 2021 aluminum alloy which is used in aerospace (40% SA387-2-22 steels. THRESHOLD BEHAVIOR (82). in applications Fatigue crack growth rates were measured in moist air RH), dry distilled low-pressure water, and (0.14 hydrazine HPa) gaseous (N2 H 4 ), hydrogen, over a range of 10-3 EIT E A K (k sijIW) 8 9 10 7 I 6 I 5 4 IXI 3 I 20 30 I X-60 PIPELINE STEEL Frequency: 50 Hz, Ambient Temperature U E z 10-4 10-5 Environment R 0 0.1 )moist A 0.5 (30% R.H.) 0 0.1 dry hydrogen aa oir A ( 138 k Pa) 0 0 0 10-6 A0 < I00-5 PAO 4, 911 U z 0 0 ba b 0 0 0 C 6 z e * 1Q O <0-6 0 I lattice 0 spacing per cycle 0 RR0.5 Air 0 *-R (.1, 10-i 7 R =0.1 =0.1 H2 10-8 Air a Threshold A KO I I 3 4 5 6 7 8 9 I 10 I 20 I 30 ALTERNATING STRESS INTENSITY, AK(MPaViF) Fig. 7.2 Variation of crack growth rate with stress intensity range in X-60 pipeline steel in moist air and dry hydrogen environments. -96- TABLE 7.1 Threshold data for SA516 and X-60 steels Steel Environment R CTOD AK cyclic SA516 (a - 327 MPa) moist air 0.15 7.2 0.24 0.57 0.45 moist air 0.75 3.5 0.07 1.8 0.06 0.15 5.7 0.15 0.36 0.1 9 0.32 0.68 0.28 0.1 5.9 0.14 0.29 0.1 dry H 2 X-60 (a m 386 MPa) pm - lPalm rr Jm max Max. excess oxide thickness moist air dry H 2 A -97- growth frequecy Hz and a load ratio of 0.1 (Fig. 9 exces s of 10-J mm/cycle, acce 1erate Na H4 the 7. 3). a At water distill ed rates wh ile the growth crack at . and of rate s in growth 10~ 7 mm/cycle to 10-2 mm/cycle) (from rates presence of hydr 0 gen similar g as results cra ck grow th rates The increase in growth ra tes due tho s e in a ir. to in to IN 2 H4 seems to be the result of attack of NH 3(form ed due to of dissociation on effect of wa te r, appears with Cu in the its wh ile the mat enial, mode, fractu re characteristic be a resul t of hydrogen embrit tilement pr ocesses to (commonly ob serv ed in s everal (83,84)). It is classes acceleration mid-growth re gime at KT max KIscc (82,85). aluminu m alloys that j ust lik e the be ha vior in observed lower streng th steels, 2021 al umi n um significant of in al 1 oy also growt h c ra ck un dergoes rates the in than values considerably smaller In the near-threshold region of crack growth, however, moist air, dry hydrogen and distilled water environments are found to analysis moist air result of the has predominantly fracture threshold in identical fracture surfaces behavior (82). (Fig. shown values. ESCA surfaces obtained from tests in identified Al2 03 threshold the surface film to be Auger spectroscopy study of the 7.4) by reveals lower that strength unlike the steels, the excess oxide thickness on the crack faces of aluminum alloy ) AK(ksiin 3 2 10*' 4 5 6 7 I I I I'~- 8 9 10 20 1 II'IIIIII BA 2021 ALUMINUM ALLOY R=0.1, FREQUENCY =9Hz, 25 0 C - 0 o moist oir (-40 % RH) * dehumidified hydrogen (115kPo) 0 a distilled water 0 0 a o hy dro z ini Cf' 0 a0 a 0f 0 1- 6 0 0 C-) C-) 0 0 E 10 A A I . A 0 0 10 0 0 a. -10 I 0 V.4D~ -. ~ '-3 pc. cy'cie I I 2I Threshold AKO I I I 3 4 5 6I 7I 8I , I 9I 10 I I I t~ I I 1 ALTERNATING STRESS INTENSITY FACTOR, AK(MPa/-) Fig. 7.3 Fatigue crack propagation behavior of BA2021 alloy in moist air, dry hydrogen, distilled water and hydrazine environments. 1 1 1 I 1 20 3 -7 I I I I I (I) U) SA542 -3 (50Hz) --A2021 (9Hz) Ambient temperature moist air (30-40%RH) R = 0.05 - 0.1 z - E 0.2 w - - I I I I I I SA542 -3 A-202 I (H 2 0, 9Hz) 0.11 0 0 - O-- - r - I. A4_2021 0 10-5 E 10-6 E E 10-7 Threshold 0 'a ) 10~8 . .. , ,. ./ Fiq. 7.4 2 . 3 . 4 5 6 7 8 I 9 I 10 I 11 CRACK LENGTH (mm) Variation of excess oxide thickness with crack lenth in BA2021 allov, ana SA542-3 steel. -100- tested in moist environments is about the same at all growth rate levels . will Altho ugh it based concl usi ons on this be to Sre mature make any extent of data, it limite is all clear that oxide-in duced crack closu re may not occur in the alloy capa bl e that rea dily aluminum though even thickening of the o xide film at thre shol d occur readily fo rming of just A pl ausibl e explanation for this behavior may oxides. be are that systems because aluminum the oxide forms oxides, AK values may not fo rmed on the fracture surfaces is so tena cious that it is di ff icult to activate mech ani sm fretting at hydrogen has been k nown to crack growth in controversy on the investigators higher influence of a alloys. on on near-threshold all oys. lower effects Ho wever, there is some w ater of Gaseous stresses. in sign ificant aluminum observed have many While thresh old val ues and near-t hresh old growth rates in water than in air for some aluminum all oy s, as have aluminum beha vi or fatigue thresh old low a result of and have interpreted such conve nti onal corrosion mec hani sms have found no di ffE rence betwee n threshold water a nd moi st in certa in cl asses o f aluminum all oys is probably du e to the corrosion a fact that, from the (83 behavior 0 thers ai r at This convent ional mechanisms point of view, moist air itself may be a severe environment. -101- In this light, recent results Vasudevan (86) reveal the obtained by inconsistent behavior o f aluminum alloys. W h ile Bucci near-threshold their studies si gni fi can tly more oxide growth at threshold were found explain limited s uch results extent susceptibi lity of to It has not been possible of publishe on information environmenta 1 limited formation such alloys. i nformation at to in alumi n um alloys because only very influences at growth rat es is currently availa b le, despite the use oxide be the same at all growth rate to levels in a 7075-T7 alloy. showed AK0 levels than at higher growth rates in a 7075 I- T6 alloy, the excess thicknesse s and their ultra-low widespread However, it can be said even with the that the mechanism of thick oxide threshold in alum Ii num alloys may be different from that in low strength steels and may depend not only on the mechan ical and metallurgical properties of the material, but also on the properties of the oxide. -102- 8. CONCLUDING REMARKS The present study has clearly demonstrated the that of corrosion products on crack faces significantly presence influences the fat igue behav ior of lower streng th steel s small int ensi ty ran ge values. stress At this po int, it is pertinent to consi der other forms of crack clos ure that the excess fracture surface r oughne ss (57,60 (87) cannot be ign ored. that there is near-threshold a stro ng gr owth Mode rat es. pr esent component II closure ( 87) de scri be d in increased thres hold for the si gni fi cant rol e nea r threshold di ffe rent envi ronments and load ratios grain strength (1,4,11,91). of ab ove (and schematically shown in (88) en able u s t 0 envi sage possible as AK locations The se different mecha nisms 8.1) factors at This implies that a rougher Fig. other m orphology and irregular because of the d isc rete c ontact at several along the crack le ngth crack on Th e work of Davidson (50) has shown fracture surface w ould r esu lt values debris oxide the possi bib ity of crack closure ari sing from faces, crack are Si nce fracture morph ology may of importance near threshol d. be of the same siz e scal e as at size but exp lanations of not only also of such (1,4,61,87,89,90) and yield No Closure Oxide Induced Closure Roughness- Induced Closure Kmin C Kmax (V AKeff Km x- Kmin Fig. 8.1 Schematic showin steels. Ak' ~V ef- 'max -v 'CI eff = K max -v K the differerent modes of crack closure in CI -104- The variati on of measured threshold steels The (1,48). decreasing less from fre tting surfaces (60). in strength plasticity-induced limited closure (44-46), or perhaps smoother fracture Certainly higher strength retardatio n less increased of values may simply result from reduced crack AK0 closure, arising (48), role with classes of 8.2 for several strength is shown in Fig. yield values AK 0 steels show far in crack growth following single positive overload cycles (92), a phenomenon often explained in terms of crack closure arguments. The role of finer grain si ze in AK 0 may again values closure from 1es s is explanation simply fracture be similarly a result of reduced crack surface roughness. far often less than it sizes a grain diameter. verification of t hese ideas is in but most near instances AK 0 lacking, is inter esting to note that, similar to the role of of 1 owe r strength beneficial a nd coarser microstructures in reducing nea r-thr eshold grow th rates are generally far evident, an Quantitative moist enviro nment s seen in the present work, the effects Such more appealing than those based on inherent mi crostructu ral r easons where p lastic zone are decreasing an d often non-existent observation which strongly crack closure (46). suggests less high load ratios, an at a prominent role of (ksi) ay 100 50 0A 10 200 250 I I i Threshold Data for Steels at R=0-0.05 ambient temperature air N AA A 10 8 N0 A 00 V aAA 2 1/4 Cr 11Mo 0 - 8- 150 N%'%I VI 12 4 o- m- W - R * o * martensitic bainitic y pearlitic (< 20% ferrite) U 0 austenitic duplex (ferrite + martensite) A ferritic (<20% pearlite) A SA 387 (bainite + < 40% ferrite) 0 SA 542 -3 (bainite) o SA 542-2 (martensite) 1 1 2 0 0 Fig. 8.2 200 400 * M 4 0 '.""" """ ."" """ '".. 0 I I 1200 1000 800 600 YIELD S.TRENGTH, o-y (MPa) 2 1400 1600 Variation of threshold stress intensity range with yield strength in several classes of steels. 1800 -106- interpreted Overload effects on crack growth have been based on crack phenomena (73). to attempted closure as well as crack tip blunting rationalize effect of oxide deposits on the near-threshold growth rates by means of crack blunting tip Such an interpretation certainly seems plausible arguments. because the values have (93,94) Similarly some investigators of threshold AK from predicted the increased crack tip radius (calculated from the procedures of Kreager and Paris (95)) due to oxide formation appear be reasonably close to and crack one is AK 0 values. the actually measured While it is not known at this point whether to both blunting closure occur at ultr-low growth rates and which more ultrasonic predominant, techniques the results (Chapter 5) obtained clearly using indicate a prominent role of crack closure. It can also be inferred that the results this work may also shows in possibly explain the behavior seen in vacuum and the existence of a 8.3 presented threshold in steels. the threshold behavior of a Cr-Mo-V Fig. steel tested in air and vacuum at 550 0 C (from the studies of Skelton Haigh (12)). It is observed from definite threshold exists for vacuum Although a number of the existence a workers (see ref.1) threshold value for no crack growth in values, of such figure that no this at a and high R ratio. have reported a steels at threshold lower could R be II -107- x 7-0 LOW R (0.2 5) HIGH R (0.7) E E /0 10-6 0 ,0 I LATTICE SPACING dz ,a" 0 CYCLE~ VACUUM (R=0.7) - 1 10Hz 10-8 4 | 5 I . I I I I, , I , I 10 , I I I 15 I 20 AK (MPa/in~) Fig. 8.3 Fatigue crack growth behav ior of Cr-Mo-V steel in moist air and vacuum at 5500C (ref. 12). -108- to attributed rewelding crack plasticity-induced (1), closure, and surface roughness-induced closure. hi gh of a threshold at that shows clearly load the ratios in The absence "good" a vacuum of threshold values in existence steels in seemingly d ry environments may merely be due to combined effects of oxidation, fracture morphology, and the residual stresses. In summary, it is clear that concepts of crack closure are of paramount im portance to fatigue crack growth behavior at near-threshold 1evels although may closure mech ani sms the At lo w stress closur e mechanisms originate fr om the fact that crack cyclic such very different from the pl asti cit y-induced be closure originally proposed by Elber (47). intensities, of tip opening are displacements of a size comparable with fra cture surface roughness a nd the thickness of corrosion debris within the crack. their speculative These ideas, despite nature, clearly suggest that si gni fi cant influences in fatig ue crack propagation may arise s imply due to a mechanical co ntact of fractured faces, rather than any inherent metallurgical rea sons. profound influence the direction which should be taken for the design of on alloys with This role increased may have resistance fatigue crack propagation at near-threshold growth rates. a to -109- CONCLUSIONS AND SUGGESTIONS FOR FURTHER RESEARCH 9. a Based on of study corrosion temperature ambient fatigue crack growth in SA542-3 pressure vessel low strength steel, X-60 pipeline steel steel, SA516 2021 and aluminum alloy, the following conclusions can be made: Lower 1. strength steels significant undergo in fatigue crack propagation rates due to the accelerations presence of hydrogen gas in mid-growth regime (growth in excess near-threshold mm/cycle) as mm/cycle) (growth region at threshold for loading. 10 of stress hydrogen-assisted far below cracking in than smaller rates intensities as well rates the under the 10- 6 KIscc sustained Mechanisms for the influence of hydrogen in these two regimes are entirely different. 2. abrupt In the mid-growth regime of crack propagation, in crack growth rates which depend on accelerations frequency, load ratio, and hydrogen pressure, are associated with to a be characteristic intergranular fracture mode and seem specific containg/producing enhanced crack to gaseous environments. growth embrittlement" mechanisms. rates hydrogen It result and appears from hydrogen that such "hydrogen -110- 3. 1evel s, At near-threshold growth below 10 -0 mm/cycle, in dry gaseous hydrogen and hel i um are larger rates than those compared to moist air and w et hy droge n by two orders approximately of magnitude , with 40% higher in air. near-threshold rates propagation thres hol d On in AK0 the up values other di still e d to hand, water are marginally lower compared to those in air. 4. Contrary to in propagation the the behavior a ssociated mid-growth characteristic fracture mode for regime, crack with there env ironmental is no inf1 uences near threshold. 5. The corrosion tested at ambient products temperature formed that crack growth observed at the the specimens have been identified using ESCA analysis to be predominantly Fe 2 03 found in in steels. It oxide thicknesses are inversely related to rates. The thickest oxide formation at high load that ratios or on specimens of the same material exposed to the same environment for same length time. is near-threshold growth rates at low load ratios in moist environments and is several times larger than observed is of -111- 6. Environmental explained based on influences intensity but to due are growth According to this model, low rates are accelerated in hydrogen per embrittlement compared to air, not because of hydrogen se, threshold the concepts of a new mechanism termed "oxide-induced crack closure". stress near reduced amount of crack closure resulting from less oxide debris formation on crack surfaces. 7. with Concepts of oxide-induced observed effects fracture morphology, behavior and of and load closure are ratio, environment consistent strength on level, near-threshold are in accord with observations that further growth rates Despite the normal uncertainties involved in oxide inert environments accelerate near-threshold compared to distilled water. 8. it can be inferred that the exces s measurements, thickness oxide deb ri s on the crack flanks is roughly of the order of the cycli c crack tip open ing displacement at the threshold. 9. Measurement ultrasonic of techniques closure cl early amount of closure in moist air even though be made. It spontaneous near using threshold demonstrate the increased to dry hydrogen, compared precise meas urement of closure loads could not is also seen that crack opening may phenomenon, but a rather gradual not be a process with crack surfaces remaining i n contact locally, while globally -112- the crack can be considered fully open. 10. Block intensities underload below the cycles subsequently magnitude of the underload resumed effect stress at growth rates when baseline being 'KB critically cycling levels, the dependent upon (Au ) and baseline (AKB ) stress intensities. This behavior appears to be oxide-induced consistent crack closure. baseline load with the arguments of The lack of such crack growth retardation effects for certain and alternating threshold can result in significant transient retardations in initial is at combinations of underload levels is found to occur when pulsating crack tip displacements at the underload are smaller than the existing excess oxide thicknesses. 11. debris, In addition to mechanisms generated sources of enhanced crack by corrosion closure from fracture morphology and roughness may arise at near-threshold because their size scales are comparable to levels crack tip displacements. 12. that Near-threshold data in 2021 aluminum alloy reveal the concepts of oxide-induced crack closure may not be valid in all the forming oxide materials films. that are capable of readily Thick oxide formation at low growth rates may depend on how tenaciously the oxide is attached to the fracture surfaces. 113- SUGGESTIONS FOR FURTHER RESEARCH 1. levels Thick oxide formation at low R values has threshold been found behavior to significantly understood and further AKeff influence of lower strength steels. kinetics of such an oxidation process are and the However, the still not fully needs to be conducted to research elucidate the mechanism of excess oxide debris formation. 2. Fatigue results on aluminum alloys concepts show that the of oxide-induced closure are not applicable to all materials. The mechanism for thick surface film formation under threshold fatigue conditions and its dependence on the properties of the oxide itself 3. appears It environmental possible interactions influenced by surface film corrosion mec hanisms effects may be alloys, which and operative. are need to be studied in detail. being at that in threshold may not be solely effects and that other chemical For material s, some example, developed for conventional and metallurgical aluminum-lithium extensive use in aerospace appl ication, readily form hydrides on exposure hydrogen. It would to be interesting to study the effect of hydrides on th reshold fatigue behavior and to investigate the process of oxide formation and the resultant closure, if any , i n these all1oys due to the combined effects. -114- 4. steps Although information regarding the rate-limiting for hydrogen embrittlement mechanisms associated with the mid-growth regime is becoming available, further studies on chemical reaction kinetics and hydrogen diffusion are required to substantiate the currently-known concepts. 5. Arguments of crack closure near threshold arising from fracture surface roughness and irregular morphology are conceptually currently appealin g, yet no quantitative information Further available. research is is needed to closure as substantiate these con cepts. 6. wel 1 The implicati ons of the as di f ference roughness-in duced in thre shold oxide-induced closure mechanisms are that the A K0 values for different env ironments (and stre ngth levels and grain sizes) is due to a p ure mechanical clos ure phenomenon. it is possible con siderations t hat may met allurgical factors. phi losophies is needed be grain more A In the light of this, size and important environmental than various systematic approach to aid design -115- REFERENCES Met. Reviews, 20, 1979, p. 20 5 R.O. Ritchie, Int. 2. H.G. Nelson, Proc. Second Int. Cong. on Mech. Beh. Mat., 1976, Americ an Society for Metals, p.690. 3. C.M. Moss, S.M. Thesis, M.I. T., 1979. 4. R.O. 5. P.C. Paris, R.J. Bucci, E.T. Wessel, W.G. Clark, and T.R. Mager, ASTM STP 513 , 1972, p.141. 6. R.J. 7. R.J. Bucci, P.C. Paris, R.W. Hertzberg, R.A. and A.F. Anderso n, ibid, p.1 25. Sch mi dt 8. J. Mautz and V. Weiss, ASTM STP 601, 1976, p. 154 9. L.K.L. Tu and B. B. Seth, J. Test. Eval., 6, 1978 p.66. Ritchie, Me t. . 1. Sci., 11, 1977, p.368. . Clark, and P.C. Paris, ibid, p. 141. Bucci, W.G. 10. R.J. Cooke, P.E. Irving, G.S . Bo oth, Eng. Frac. Mech. , 7, 1975, p .69. 11. T.C. Lindley and C.E. Richar ds, CEGB Note No. RD/L/N 135/78, 1978. 12. R.P. Skelton and J.R. Haigh, Mater. 1978, p. 1 7 13. R.G. Baker and J. Nutting, J. Iron Steel Inst., 1959, p.257. 14. G.F. 15. A. Joshi, private communication, Perkin-Elmer, Surface Sciences Division, Mountain View, California, 1980. 16. M. Kurkela and R.M. Latanision, Corrosion Laboratory Report, M.I.T., 1980. 17. M.A. Devanathan and Z. Stachurski, 270A, 1962, p. 9 0 18. R.A. Oriani and P.H. Josephic, Acta Met., 22, 1974, p.1065. and C.J. Engr., 36, . Sci. Be evers, Zamiski, S.M. Thesis, M.I.T., 1980. Roy. Soc., . Proc. -116- 19. C. Zappfe and C. Sims, 20. G.W. Simmons, P.S. Pao, and R.P. Wei, 9A, 1978, p.1147. 21. W.W. Gerberich and Y.T. Chen, p.271. 22. C.D. 23. J.P. Hirth, Met. Trans., 24. H. Cialone and R.J. Asaro, Met. Trans., p.367. 25. R.A. Oriani and P.H. Josephic, Acta Met., 27, p. 9 9 7 26. A.J. Mc Evily and R.P. Wei, Corrosion Fatigue: Chemistry, Mechani cs, an d Microstructure, Proc. NACE Conf., Storrs, Conn. 1971, p.381. 27. R.P. We i and J.D. p.25. 28. I.M. Austen and P. McIntyre,, Me t. Sci., 29. K. H irano, Y . Kobayashi, H. Kobayashi Fa ti gue '81, Proc. SEE Conf., Warwick 1981 , p.87. 30. R.C. Brazill, G.W. Simmons, and R.P. We i, J. Eng. Tech., (Trans. ASME Series H ), 101, 1979, p. 1 2 9 31. M.O. Speidel, M.J. Blackburn, T.R. Beck, and J.A. Feeney, Corrosion Fat igue: Chemistry, Mechanics, and Micr 0structure, Pr oc. NACE Conf., Storrs, Conn., 1977, p.324. 32. D.A. Meyn, 33. F.P. Ford, Mechanical Behavior of Materials, 2, Proc. 3rd Int. Conf., Cambri dge, eds. K.J. Miller and R.F. Smith, Pergamon Press,, 1979, p. 4 3 1 34. D.B. Dawson and R.M.N. Pel 1 oux, Met. Trans., 5A, p.723. 35. B.J. Shaw, unpublished work, Pittsburgh, PA, 1980. Trans. AIME, 145, 1941, p.225. Met. Trans., Me t. Trans., 6A, 1975, 43 7 . Beachem, Met. Trans., 3A, 1972, p. 11A, 1980, p.861. 10A, 1979, . 1979, Res. Stds., 9, 1969, 13, 1979, p.420. and H. Nakazawa, Westbury House, Mat. . Landes, Mater. . Met. Trans., 2A, 1971, p.853. 1974, Westinghouse R&D Center, -117- H.G. Nelson, Effects of Hydrogen on Behavior of Materials, eds. A.W. Thompson and I .M. Bernstein, AIME, New York, 1976, p.602. 37. H.F. Wachob and H.G. Nelson, Proc. 3rd Int. Conf. on Hydrogen, Jackson Lake, eds. A.W. Thompson and I.M. Bernsstein, AIME, Newyork, 1981. 38. T.R. Mager, D.M. Moon, and J.D. Landes, J. Press. Vess. Tech. (Trans. ASME Series J), 99, 1977, p. 2 3 8 39. W.A. Bamford and D.M. Moon, Corrosion '79, Proc. NACE Meeting, Houston, NACE, 1979. 40. J.K. Tien, A .W. Thompson, I.M. Bernstein, and R.J. Met. Trans., 7A, 1976, p.8 2 1 41. F. P. Ford and T.P. Hoar, Microstructure and Design of Al loys, 1, Proc. 3rd Int. Conf. Strength of Me tals and Al loys, Cambridge, The Metals Society, 1973, p.4 6 7 42. J. Toplosky, S.M. Thesis, M.I.T., 1981. 43. P.K. Liaw, S.J. Hudak, and J.K. Donald, Proc. 14th National Symposium on Fracture Mechanics, UCLA, June 1981. 44. R.O. Ritchie S. Suresh, and C.M. Moss, J. (Trans. ASME Series H), 102, 1980, p.1 9 2 45. A.T. 46. S. Suresh, G.F. Zamiski, and R.O. 1981. 47. W. Elber, ASTM STP486, 48. S. Suresh, G.F. Zamiski, 1981 (in press). 49. R.A. Schmidt and P.C. 50. D.L. 51. D. Benoit, R. Namdar-Tixier, 45, 1980, p.1 52. G.L. Barenblatt, in Advances i n Applied Mathematics, Academic Press, New York, VII 1962, p.55. . 36. . . , Ri chards Eng. Mat. . Tech., 463 Ritchie, Met. Trans., 12A, . 280 and R.O. Ritchie, ASTM STP 755, Fat. Eng. Mat. ASTM STP 536, 1973, p.7 9 . Paris, Struct., 3, 1981, p.229. and R. Tixier, Mat. Sci. Eng., . Davidson, 1971, p. 1980, p. . Stewart, Eng. Frac. Mech., 13, -118- 53. H.M. Westergaard, J. App. Mech. 66, 1939, p.49. 54. K. Tada, P.C. Paris, Cracks Handbook, Del 55. S. Suresh, D.M. Parks, and R.O. Ritchie,, Fatigue Th resholds, Proc. 1st Int. Conf., Stockholm, Sweden, EMAS Publ. Ltd., Warley, 1981. 56. C.F. Shih, J. Mech. Phys. Solids, 29, 1981. 57. S. Purushothaman and J.K. Tien, i n Strength of Metals and Alloys, ICSMA5 Conf. Proc., P. Ha asen et al, eds., Pergamon Press, New York, 2, 1979, p.1267. 58. R.O. Ritchie, Fati gue Thresholds, Proc. 1st Int. Conf., Stockholm, Sweden, EMAS Publ. Ltd., Warley, 1981. 59. C.J. Beevers, Met. Sci., 14, 1980, 60. I.C. Mayes and T.J. Baker, in Micromechanisms of Crack Extension, The Metals Society, London, 1981. 61. G.T. Gray III, A.W. Thompson, J.C. Wi lliams, and D.H. Stone, Fati gue Th resholds, Proc. Int. Conf., Stockholm, Sweden, EMAS Publ ishers, Warley, 1981. 62. R.E. Lewi s, private communication, Lockheed Palo Al to Research Labs, Palo Alto, Californ ia, 1980. 63. J.W. Swanson and H.L. Marcus, Met. Trans., p.291. 64. P. Mahulikar and H.L. 2, 1980, p.245. 65. G.E. Nordmark and W.G. p.66. 66. R. Fuquen-Molano and R.O. M.I.T., Cambridge, 1981. 67. J.H. Williams II and D. DeLonga, M.I.T., Cambridge, 1981. (Trans. ASME Series A), and G.R. Irwin, Stress Analysis of Research Corp., 1976. 4 18 Marcus, Fat. Eng. Fricke, . p. 9A, 1978, Mat. Struc., J. Test. Eval., 6, 1978, Ritchie, unpublished research, private communication, -119- 68. 3.D. Frandsen, R.V. 11, 1975, p.345. 69. V. 70. H.F. Hardrath and A.J. McEvily, Proc. Crack Prop. Symp., Cranfield, England, 1961, p.1 71. J. Schijve and D. 72. R.E. Jones, Eng. Frac. Mech., 5, 1973, p. 5 8 5 73. J.R. Rice, ASTM STP 415, 1967, p. 2 4 7 74. E.F.J. von Euw, R.W. Hertzberg, 513, 1972, p.2 3 0 75. J. Willenborg, R.M. Engle, and H.A. Hood, Tech. Mem. 71-1-FBR, 1971. 76. D.E. Wheeler, J. Bas. Eng., (Trans. ASME Series D), 94, 1972, p.181. 77. R.J. Bucci, Proc. ASTM E-9/E-24 Symp. on Fatigue Crack Growth Measurement and Analysis, Pittsburgh, 1979. 78. G.A. Miller, S.J. Hudak, and R.P. Wei, J. Test. Eval., 1, 1973, p.524. 79. J.F. Knott, Fundamentals of Fracture Mechanics, Butterworths, London, 1973. 80. R.J. Bucci, Proc. ASTM, 1981. 81. Rockwell International Report to NASA-AMES, 1980. 82. S. Suresh, I.G. Palmer, and R.E. Lewis, manuscript under preparation, Lockheed Palo Alto Research Labs, 1981. 83. J.A. Feeney, J.C. McMillan, and R.P. Wei, Met. Trans., 1A, 1970, p.1 7 4 1 84. J.C. Radon, Met. Sci., 13, 1979, Frac. Mech., 11, 1979, p. 6 1 . Bachmann and D. Munz, Eng. Buck, Int. J. Fracture, . Inman, and 0. . . . Broek, Aircr. Eng., 34, 1962, p.3 1 4 . and R. Roberts, ASTM STP . 13th National Symp. Fracture Mechanics, 411 . p. -120- 85. M.O. Speidel, Stress-Corrosion Cracking of Aluminum Alloys, The Ohio State University, 1975. 86. R.J. Bucci, A. K. Vasudevan and K. Bretz, unpublished work, Alcoa Research Labs, Alcoa Center, 1981. 87. N. Walker and C.J. Beevers, Fat. 1979, p. 1 3 5 88. R.O. 89. J. Masounave and J.-P. p.165. 90. W.W. Gerberich and N.R. Moody, ASTM STP 675, 91. 0. Vosikovsky, 92. G.J. Petrak and J.P. 1975, p.2 0 6 93. F.P. Ford, unpublished work, Schenectady, New York, 1981. 94. J.C. Radon, C.M. Branco, and L.E. Culver, Int. J. Fracture, 12, 1976, p.467. 95. M. Creager and P.C. Paris, Int. J. 1, . Eng. Mater. Struc., Ritchie and S. Suresh, Met. Trans., 12A, 1981. 10, 1976, . 1979, p.2 9 2 Frac. Mech., 11, 1979, p.959. Gallagher, J. Eng. Mater. Tech., 97, . Eng. Bailon, Scripta Met., General Electric Co., Fracture, 3, 1967,1 p.247. - 121 APPENDIX AUGER SPECTROSCOPY STUDY OF OXIDE DEPOSITS Ch aracteri zati o n of surfaces 550 was Scanning Auger 01 of profiles the monitor were Fe3 Depth composition obtained using Ar The composition of C1 was also measured sputter-techniques. to spectrometers. and as PHI Model 590 as well done using PHI Model fracture on deposits oxide the A typical depth pr esence of hydrocarbons. composition profile is shown in Fig. Because of count peaks plotted against the sputtering time. sputter the difficulties ass ociated with the calibration of rate by a preparing thickness known tantalum oxide standard was for used of Auger the with Al, oxide, a iron Since calibration. there is no currently-available standard procedure, the time the taken for the 01 composition profile to drop from to a value which is half of the peak minus the steady-state level, was arbitrarily defined as the sputter from the time. oxide were Also, rates calibrated with the tantalum oxide sputter rates standard using this procedure, the corresponding iron peak using estimated sputtering yields (atom/ion) from the Veeco data for on argon ion Brochure V60 and Physical Electronics (15). Using a beam voltage of 5kV, ion and sizes of electron beam respectively (for PHI Model roughly 200 and 20pm, 550), and rastering rates of 180 Fe 3 CI 0I w a- C PC Fe3, 01, and Cl peaks. - - 123 Hz (X-directi on) and 30 Hz (Y-direction), obtained for several sputter times were fracture surfaces. The sputter time mul tiplied by the modifi ed sputter rate provides an estimate of the extent of oxidati on. Simple calculations oxidizes of FeO. Thus showed to 2.13 cc of Fe 2 03, Similarly 1 cc of Al that a cubic cm of Fe 2.07 cc of Fe 3 0 4 , and 1 .76 cc results in 2 cc of Al2 03 the oxide thickness measurements represent rough ly the total excess material inside the c rack (assuming thicknesses on each crack face), as sh own in Fig. A2. equal 124 - - B I / Oxi d e I Unoxidized Steel Fig. A2 Oxidized Steel Schematic showing oxide formation on crack faces and the excess oxide thickness.