The Use of Diffraction to Study Fatigue Crack Tip Mechanics Joe F Kelleher1,a, Pablo Lopez-Crespo2,b, Feizal Yusof2,c, and Philip J Withers2,d ISIS, Rutherford Appleton Laboratory, Didcot, Oxfordshire OX11 0QX, UK School of Materials, University of Manchester, Grosvenor Street, Manchester M1 7HS, UK a joe@smartscience.co.uk, b plopezcrespo@gmail.com, c feizal.yusof@manchester.ac.uk, d philip.withers@manchester.ac.uk Keywords: Fatigue, crack closure, residual stress, plastic anisotropy Abstract Simple experimental tests of fatigue life are often insufficient to characterise fatigue behaviour Fatigue crack growth in polycrystalline metals is governed by a number of interacting mechanical effects at the crack tip, such as the deformation inside a plastic zone and contact between the crack faces over part of the loading cycle Typically, results tend to be interpreted in terms of an empirical fatigue law such as the Paris equation, which in itself fails to generalise to different load ratios or multiaxial load cases While extensions to this equation have been used, these are mostly empirical and little to enhance understanding of the fatigue growth mechanisms Recently, the use of diffraction to characterise crack tip stress effects has become increasingly popular In this paper, we consider the opportunities and the difficulties associated with making such measurements by neutron and synchrotron diffraction In particular we examine grain size effects, plane stress/plane strain issues, optimisation of the gauge geometry, measurement of the plastic zone and crack closure effects Introduction The mechanical behaviour of cracked bodies has traditionally been studied largely using analytical and numerical techniques, in which an infinitely sharp crack is assumed to create an idealised stress field that is singular at the crack tip Some efforts have been made to experimentally study the dynamic behaviour of a crack under fracture or fatigue crack growth, but there are experimental difficulties in obtaining information from a sample during a dynamic process like fatigue Full-field surface strain mapping techniques [1] allow comparisons with theoretical predictions, but give no information about the interior of a sample where mechanical behaviour can be quite different [2] Photoelastic methods allow internal examination, but are limited to a narrow range of materials By contrast, diffraction is a valuable means of probing the interior mechanical state of a cracked crystalline body It provides absolute values of elastic strain or stress, whereas external strain gauges measure the total strain, and in some instances it can provide an indication of ‘damage’ or plastic strain from diffraction peak widths Early work used neutron diffraction with millimetre gauge volumes [3], whereas synchrotron diffraction can resolve strains over tens of microns [4] Diffraction measurement of cracks Measurement of the strain fields around a crack tip by diffraction poses challenges for what is otherwise a well-established technique The geometry of the experimental setups used in this work are shown in Fig Following Steuwer et al [5,6], synchrotron diffraction was performed in energy dispersive mode with a fixed 2θ angle of 5º The two detectors (Fig 1a) therefore measure strain in directions close to a pair of perpendicular in-plane directions This arrangement provides high spatial resolution in the in-plane directions, and while the gauge volume is elongated in the sample thickness direction, there is less variation in this direction for common specimen geometries For neutron diffraction (Fig 1b), the neutron beam was directed at a 45º angle to the compact tension C(T) sample surface At the ENGIN-X diffractometer used in this work, two diffracted beams at 90º to the incident beam are measured simultaneously One detector measures the strain parallel to the applied load (crack opening), and the other measures the strain acting normal to the sample surface Second detector: measures strain in crack propagation direction Applied load First detector: measures strain in direction of load Applied load Second detector: measures strain perpendicular to sample surface Incoming white X-ray beam First detector: measures strain in direction of load a) Energy dispersive synchrotron diffraction (ID15A, ESRF) Incoming neutron beam b) Neutron diffraction (ENGIN-X, ISIS) Fig Experimental setups for in situ loading of cracked C(T) specimens for a) energy dispersive synchrotron and b) neutron diffraction Samples As part of larger study investigating crack closure and overload effects, a series of diffraction measurements have been made on C(T) specimens with pre-existing fatigue cracks Here, we report results for two batches of AISI 316 stainless steel with different grain sizes ( Fig 2) Effect of crystallographic peak studied Strain scanning results are well known to be sensitive to the choice of crystallographic peak used, especially where plastic strain is present The suitability of a peak hkl has been shown to be a function of its anisotropy factor, Ahkl ( hk ) (kl ) ( hl ) , (h k l ) (1) which varies from to 1/3 for different peaks In general, peaks with the Ahkl in the middle of this range (e.g 0.157 for the 311 peak) are good choices for strain scanning as these have elastic moduli similar to the macroscale properties and are less sensitive to plasticity-induced intergranular stress [7] Averaging strain over several peaks of different Ahkl further improves accuracy Effect of gauge volume and grain size A sub-millimetre resolution is typically required to capture the highly concentrated strains around the crack tip, at least in the directions extending radially away from the tip Another important factor is the plastic zone size, often approximated by a radius ry K I2 6 y2 , (2) where KI is the applied mode I stress intensity, and y the yield stress In the direction parallel to the crack front (i.e the out-of-plane direction in a C(T) specimen), strain gradients are much lower These arise firstly from the transition from plane stress (surface) towards plane strain (interior) with increasing thickness, and secondly from any curvature (bowing) of the crack front Closure levels can differ substantially between plane stress and strain conditions [8] The narrow incident beams and elongated gauge volumes typically used in high-energy synchrotron diffraction are thus well-suited to strain mapping of C(T) specimens The elongated gauge volume arises from the low 2θ angles that result from the short wavelengths (high energies) needed to penetrate bulk engineering metals [9] The required spatial resolution in either the through-thickness or in-plane directions may thus limit the maximum possible incident beam size 60 mm 15 mm 17.5 mm Scanned area in Fig 32.5 mm Scanned area in Fig 50 µm 50 µm 62.5 mm Fig Optical micrographs of a small and large grained 316 stainless steel used in this study, with the dimensions of the compact tension specimen used and the areas mapped While the gauge volume must be small enough to give adequate spatial resolution, it must be large enough to provide a valid strain value at each measured location The gauge volume should contain enough differently oriented grains to be regarded as mechanically homogeneous and isotropic Furthermore, a representative selection of those grains must be sampled by the diffraction technique used The white beam nature of the energy dispersive (X-rays) and time-offlight (neutrons) methods used here means that several hkl peaks are collected, which helps to provide such a representative selection of differently oriented grains Example strain maps collected using ID15 for different peaks on the large-grained material are given in Fig for a C(T) sample with a crack loaded at 5.16 kN (stress intensity KI = 12.5 MPa m), and mapped with a 300 àmì 300 àm incident beam while rocking ±10º 311 511/333 311 Rietveld refinement 17.5 mm Equally weighted average from 220 to 442/600 peaks -0.0005 0.0005 0.001 Strain 0.0015 0.002 Fig Strain maps for 316 stainless in the loading direction prepared using a Rietveld refinement, an equally weighted average of all peaks, and two example individual crystallographic peaks The schematic crack indicates the approximate position of the crack It was immediately apparent that each of the individual hkl peaks gave a very noisy strain field when considered individually As expected, strain fields derived from several peaks by i) the Rietveld method and ii) an equally-weighted average of several hkl peaks both gave strain fields that were more recognisable as the stress concentration around the crack tip [10] Interestingly, the low-intensity peaks did not give strain maps that were noticeably worse than the high-intensity peaks, suggesting that the statistical accuracy offered by the photon flux was not a limiting factor in the overall validity of the results Rather, as different hkl peaks arise from different grains, a method that considers many peaks is thus increasing the total number of grains that are measured, thereby better approximating the continuum elastic behaviour From strain to stress In many cases elastic strains may be sufficient, for example to compare to models If stress is sought, the normal practice when making synchrotron measurements is to measure two perpendicular in-plane strain components, and convert them to the corresponding stress in the same directions by assuming either plane strain (εz=0) or plane stress (σz=0) Previous finite element modeling of these samples suggests that all but a small zone (~1 mm) around the crack tip is in a state of plane stress In a plane stress state, stress can be found using the relations E x y and y E y x , x 1 1 (2) where σ and ε refer to stress and strain, E and υ are the elastic constants Young’s modulus and Poisson’s ratio (here, 195 GPa and 0.29 respectively), and the x and y subscripts refer to the stress or strain component in two perpendicular in-plane directions The typical synchrotron X-ray strain scanning setup shown in Fig 1a measures perpendicular directions approximately in the plane of the sample, and strain data thus acquired can be converted to stress using this relation However, for experimental setups where one in-plane x and one out-of-plane direction z are measured, such as the neutron diffraction, an alternative plane stress relation may be derived as E z E x x z and y x (3) As σz is zero, the measured εz is merely the Poisson strain from the in-plane stresses σx and σy Monitoring the plastic zone The diffraction peak FWHM provides a measure of the local variation in lattice spacing, such as from the steep elastic strain gradients at a crack tip, or from the plasticity local to the crack (Type III stresses) Plastic strain is also detectable by an ‘anisotropy coefficient’, which shows the extent to which each individual hkl peak strain differs from the average strain of all peaks [7] Fig shows plots of the anisotropy coefficient, the elastic strain and diffraction peak width over an area including the tip and wake of an unloaded ~20 mm crack Anisotropy coefficient Peak width Crack growth direction X Colour scale for plotted values X anisotropy X strain X peak width Y anisotropy Y strain Y peak width 0 0 00 00 00 00 20 66 54 0 0 00 00 00 00 15 62 50 4 0 0 00 00 00 00 10 58 46 0.0075 0.005 0.0025 -0.0025 Loadi ng direct ion Y -0.005 -3 00 39 -2 - 0 00 00 00 05 00 55 43 2 -1 00 51 - 0 00 00 00 48 36 0 00 Anisotropy Strain Peak width Y Peak width X 00 05 Dista nce from crac k face / mm Strain (Rietveld) Average parameter value over crack wake Fig Intergranuar strain as revealed by the anisotropy coefficient in a strain map of a cracked sample, together with an average diffraction peak width An integrated average over the indicated width for each quantity is shown on the right The crack has grown from the left The crack tip is most evident in the elastic strain in the loading direction The peak width and anisotropy coefficient, which relate to accumulated damage and loading history more than the current load state, generally show the crack wake more clearly Fig also includes line plots of these parameters averaged over the path of the crack, revealing how they vary with distance from the crack face The narrow band in which the peak width changes possibly corresponds to a zone Stress in loading direction / MPa Stress in loading direction / MPa of repeatedly reversed plasticity with high accumulated plastic strain; the anisotropy coefficient is sensitive to low uniaxial plastic strains, and may show the larger zone with only tensile plasticity Crack closure The variation in crack tip stresses during a fatigue cycle can be reduced by crack tip closure, retarding crack growth Residual stress measurements are becoming an important tool for the quantification of crack tip closure effects [4,11] Two C(T) samples of the small-grained material were prepared so as to have compressive and tensile residual stresses respectively in the region into which the crack tip was growing Compressive stress at the tip would be expected to encourage crack closure, even if other closure mechanisms such as crack tip plasticity were not present Conversely, tensile residual stress may reduce or prevent crack closure that might otherwise occur by these mechanisms The two samples represent the kinds of residual stress induced closure effects that might arise in a fatigue crack propagating through a stressed component such as a weld Fig shows the measured stress for different gauge volumes in front and behind a crack tip as a function of applied load The plots show both variation with position for different loads, and the variation with load at different positions Strain was measured using neutron diffraction ( Fig 1b), and converted to stress using Eq (3) A square-prismatic shaped gauge volume of mm in the crack propagation direction and mm in the other directions was stepped along several points in the crack propagation direction, at a series of constant loads Applied load / kN 200 0.25 5.83 150 1.2 8.61 2.13 12 3.67 -50 Sample with compressive crack tip residual stress -100 100 -2 10 Position with respect to crack tip / mm Position with respect to crack tip on surface / mm -2 Sample with compressive crack tip residual stress 12 Stress in loading direction / MPa Stress in loading direction / MPa 150 Applied load / kN 1.2 8.61 2.13 12 3.67 100 50 200 0.25 5.83 150 100 -150 200 50 -50 Sample with tensile crack tip residual stress -100 -150 200 150 -2 10 Position with respect to crack tip / mm 12 Position with respect to crack tip on surface / mm -1 100 Fig Stress as a function of position with respect to50crack tip and applied load, for samples 50 with a) 0compressive and b) tensile residual stresses at0 the crack tip Negative positions refer to the crack wake and positive positions refer to intact material ahead of the nominal -50 location of the crack determined from the surface -50 -100 -100 Sample with tensile crack tip residual stress The top applied load (0.25 kN) Both samples -150 two plots include the residual stresses at near-zero -150 6stress8 near10(~1 mm) 12 have a small compressive the crack created by tip2 due to the 6local 8plasticity 10 12 Applied load previous fatigue growth, but / kN behind this the stresses differ by around 150/ kNMPa As the applied Applied load load is increased to 12 kN (25 MPa√m), the local stress for each gauge volume increases in a manner dependent on the position of that volume The ‘zero’ position for the crack tip refers to the crack tip on the sample surface (found by dye penetrant), and internally the crack front had likely bowed to make the crack slightly longer inside Intact material just ahead of the crack tip shows a large change in stress as this is where the applied load is concentrated, while material far ahead of the crack tip experiences less change The steepest gradients of stress vs applied load are at mm from the surface crack tip in the compressively stressed sample, and at mm for the tensile sample – this is possibly the true internal crack tip location The linearity of these plots shows the material here is intact and responding elastically Crack closure is evident in the sample with compressive crack tip residual stress At -2 mm and mm positions, the stress first steeply increases with load and asymptotically approaches zero stress at higher loads, doing so more quickly at -2 mm i.e further behind the surface crack tip The mm and mm positions also show nonlinearity, remaining constant at low loads, then increasing, and then stabilizing again within ± 50 MPa of zero stress Overall, the behaviour is consistent with an ‘unzipping’ mode of crack closure, where the crack first opens far behind the crack tip, with the point of opening moving towards the crack tip with increasing load until the crack is completely open The sample with tensile residual crack tip stress, which would work to counteract closure, shows much less evidence of this effect with the responses being mostly linear Conclusions The strains around a crack tip can be studied using diffraction but careful choice of experimental parameters is needed Even where counting statistics are adequate, there may be microstructural artefacts in the data if the gauge volume is too small As a result, the crack tip stresses, local plastic zone and the effects of closure can all be monitored with careful experiments on sufficiently fine grained materials Crack closure is evident here from in-situ measurements at a series of loads, where ‘upzipping’ behaviour is seen in a sample containing compressive residual stress Acknowledgements For the provision of beamtime, the authors are grateful to the ISIS Pulsed Neutron and Muon Source (expt RB810312) and European Synchrotron Radiation Facility (expt MA-858), in particular the beamline scientists Ed Oliver, Anna Paradowska, Shu Yan Zhang, Axel Steuwer, Matthew Peel and Thomas Buslaps References [1] F Yusof and P.J Withers: J Strain Anal Eng Des Vol 44 (2009), pp 149-158 [2] P de Matos and D Nowell: Int J Fatigue Vol 31 (2009), pp 1795-1804 [3] M.T Hutchings, C.A Hippsley and V Rainey, in: Neutron Scattering for Materials Science, edited by S.M Shapiro, S.C Moss, J.D Jorgensen, Mat Reseach Soc., Boston, MA (1990) [4] A Steuwer, M Rahman, A Shterenlikht et al.: Accepted for Acta Materialia (2010) [5] M Rahman, M Fitzpatrick, L Edwards et al.: Mater Sci Forum Vol 571-572 (2008), pp 119-124 [6] A Steuwer, J.R Santisteban, M Turski, P.J Withers and T Buslaps: J Appl Crystallogr Vol 37 (2004), pp 883-889 [7] M Daymond, M Bourke, R VonDreele, B Clausen and T Lorentzen: J Appl Phys Vol 82 (1997), pp 1554-1562 [8] H Alizadeh, D Hills, P de Matos et al.: International Journal of Fatigue Vol 29 (2007), pp 222-231 [9] P.J Withers: J Appl Crystallogr Vol 37 (2004), pp 596-606 [10] M Daymond and P Bouchard: Metall Mater Trans A Vol 37A (2006), pp 1863-1873 [11] M Croft, V Shukla, N Jisrawi et al.: Int J Fatigue Vol 31 (2009), pp 1669-1677 ... ‘unzipping’ mode of crack closure, where the crack first opens far behind the crack tip, with the point of opening moving towards the crack tip with increasing load until the crack is completely... with compressive crack tip residual stress -100 100 -2 10 Position with respect to crack tip / mm Position with respect to crack tip on surface / mm -2 Sample with compressive crack tip residual... diffraction Samples As part of larger study investigating crack closure and overload effects, a series of diffraction measurements have been made on C(T) specimens with pre-existing fatigue cracks