Effects of Residual Surface Stress and Tempering on the Fatigue Behavior of Ancorsteel 4300 J.J. Williams, X. Deng, and N. Chawla Department of Chemical and Materials Engineering Fulton School of Engineering Arizona State University Tempe, AZ 85287-6006 B. Lindsley, P. King, and K.S. Narasimhan Hoeganaes Corporation 1001 Taylors Lane Cinnaminson, NJ 08077 ABSTRACT In this study, the microstructure, residual stress and fatigue behavior of Hoeganaes’ Ancorsteel 4300 sintered steel were characterized. Samples were tempered at either 205˚C or 315˚C and then machined by low-stress grinding. The effects of residual surface stress (measured by XRD) on the fatigue behavior were studied by either application of a stress-relieving heat-treatment after machining or by polishing away the machined surface. Based on this study, samples tempered at 315˚C had slightly higher fatigue strengths than samples tempered at 205˚C. Although significant compressive stresses were induced by machining on the surface of samples, these residual stresses did not affect the fatigue behavior. Rather, the fatigue behavior was controlled by porosity inherent to these sintered steels. INTRODUCTION The fatigue strength of sintered steels is affected by a variety of factors, such as the amount of porosity and matrix microstructure.1-5 In some studies, the presence of 10% porosity decreased the fatigue strength of steels by 25% to 50%. Additionally systematic studies have shown that pore shape plays an important, yet secondary role in affecting fatigue strength.6,7 For a given level of porosity, steels with spherical pores will possess higher fatigue strengths than steels with irregularly-shaped or angular pores. Surface condition can play a strong role in fatigue strength of both wrought and porous steels. For example, Sonsino et al8,9. have shown that surface rolling and shot-peening can improve fatigue strengths of sintered steels by roughly 20% due to surface densification and the introduction of residual compressive stresses at the surface. In wrought steels, the surface condition, and hence the fatigue strength, is affected by machining. For example, milled tool steel samples have a 35% higher fatigue strength than those machined by EDM, because EDM causes cracking and residual tensile stresses on the surface.10 Finally, for a given composition, tempering can have a strong effect on fatigue strength. Surprisingly few published studies exist on how fatigue strength is affected by tempering. Two such studies have shown that an optimum tempering temperature can increase the fatigue strength by 15% to 30%.11,12 In this study, we have characterized the axial fatigue behavior of Hoeganaes’ Ancorsteel 4300 sintered steel at two tempering temperatures, 205˚C (400˚F) and 315˚C (600˚F). The effects of machining and polishing on the residual surface-stresses (measured by x-ray diffraction) and fatigue strength were also examined. Given its importance in fatigue, the amount and shape of the porosity were also characterized. EXPERIMENTAL PROCEDURE All specimens in this study were synthesized and processed at Hoeganaes Corporation. The nominal composition of the steel is listed in Table I. To achieve this composition, Hoeganaes’ Ancorsteel 4300 powder was mixed with 0.6 wt% graphite. Rectangular specimens were made by uniaxial coldcompaction of the powders at 690 MPa (50 tsi). This resulted in a sample size of roughly 10.5 mm × 10.5 mm × 90 mm (0.4" × 0.4" × 3.5") and a green density of 7.1 g/cm3. The compacts were sintered at 1260˚C (2300˚F) in an atmosphere of 90% N2 – 10% H2 for 30 minutes. Samples were then cooled at a rate of approximately 0.7˚C/s (1.3˚F/s). After cooling, the rectangular blanks were tempered for one hour in air at either 205˚C (400˚F) or 315˚C (600˚F). Axial fatigue specimens were then machined from these tempered blanks using a low-stress grinding technique. Finally, in an attempt to decrease residual surface stresses due to machining, half of the fatigue specimens were given a stress-relieving heat-treatment at 175˚C (350˚F) for one hour. Also, the gage sections of some of the fatigue specimens were polished to a 1µm diamond finish by mounting the sample in a high-speed lathe and manually applying pressure with nylon polishing clothes as the sample rotated. This resulted in a polishing direction that was perpendicular to the direction of the low-stress grinding used to machine the specimens. Fe 95.8 Table I. Nominal Composition of Ancorsteel 4300 (wt.%) C Cr Ni Mo Si Mn 0.6 1.0 1.0 0.8 0.6 0.1 O 0.1 To assess the effects of residual stress on fatigue strength, residual surface stresses along the axial direction were measured at Proto Manufacturing by x-ray diffraction (XRD) using the sin2ψ method. This technique involved measuring the d-spacing of the {211} crystallographic plane versus sin2ψ for 13 unique ψ tilts of the diffractometer. The technique is described in detail by Pineault et al.13 A major advantage of this technique is that the d-spacing of the unstressed material need not be known to obtain absolute strain measurements. The diffractometer had a Cr source (2.291 Å), and the ψ tilts ranged between ±25˚. One measurement was taken from the center of several different specimens to assess the effects that heat-treating, machining and polishing have on the residual surface stress. As porosity plays a significant role in mechanical properties, the amount of porosity, as well as the size and shape of the pores were characterized by optical microscopy and digital image analysis. Crosssections were obtained perpendicular to the compaction direction from the centers of the specimen blanks and polished to a 1µm diamond finish. As aggressive removal rates (such as 600 grit SiC paper or 45 µm diamond paste) caused significant smearing and closing of pores, most of the polishing time was spent at less aggressive removal rates (3 µm and 1 µm diamond paste). Porosity was characterized from three different specimen blanks over a total area of 3.3 mm2, yielding roughly 5000 pores. The resolution of the optical images used in the analysis was 0.6 µm/pixel. To obtain S-N curves, stress-controlled uniaxial fatigue tests were performed at ambient temperature on a precision-aligned servo-hydraulic load frame. Samples were fatigued using a 40 Hz sine wave with a stress ratio of R = -1. The fatigue endurance limit was defined as 107 cycles. The geometry of the fatigue specimens is shown in Figure 1. 3.50 88.9 1.17 29.7 1.17 29.7 0.60 15.2 R, 12.7 0.50 5.1 9.5 Figure 1. Axial fatigue specimen geometry. All units in millimeters, all tolerances are ±0.025mm SAMPLE NAMING CONVENTION Throughout this paper, 205T or 315T are used to indicate that samples have been tempered at 205˚C or 315˚C, respectively. SR is used to indicate samples that have undergone a stress-relieving heat-treatment, whereas NSR is used to indicate samples that have no stress-relieving heat-treatment. Finally, P and NP are used to indicate whether the samples have been polished to a 1µm finish or left in the as-machined state, respectively. As an example, 205T-SR-NP is a sample that has been tempered at 205˚C before being machined, has undergone a stress-relieving heat-treatment at 175˚C after being machined into a fatigue specimen, and has not been polished. RESULTS AND DISCUSSION Microstructure Characterization Figure 2 is a representative optical micrograph of a sample which illustrates the irregular nature of the porosity. The area fraction of pores was measured to be 10.4% ± 0.7%. Analysis of the pore size, circularity, solidity and Feret’s diameter are summarized in Table II. The circularity is defined as: Cp = 4πA/P2 (1) where A is the area and P is the perimeter of a given pore. As the circularity approaches one, the shape of the pore approaches a perfect circle. The maximum Feret’s diameter, also known as the caliper length, Fmax, is the largest distance between two parallel lines drawn tangentially to the edge of the pore (as if pore diameters were measured by a caliper). Another circularity shape parameter based on Fmax, is: CF = π(Fmax)2/4A Figure 2. Optical micrograph of a polished surface illustrating the nature of the porosity (2) This also tends toward one as the pore approaches a perfect circle. This parameter, however, is more descriptive in that the value obtained can be interpreted as the aspect ratio (major axis / minor axis) of an equivalent ellipse. Of course, this parameter is most appropriate when the objects are convex and can be approximated by ellipses. The last shape parameter listed in Table II is the solidity, also known as the convexity. This is the area fraction of an object’s convex hull that is occupied by the object. Thus, a pore that is entirely convex will have a solidity of one. As concavity increases, solidity approaches zero. Table II. Measured Pore Shape Parameters All Pores Largest 2% of Pores Shape Parameter Median Skewness Median Skewness 2 31.3 3.80 451 1.64 Size, µm 8.57 2.16 29.8 1.41 Feret’s Diameter, µm Circularity, CP 0.906 -0.929 0.247 0.816 Circularity, CF 1.83 1.98 2.94 1.09 Solidity 0.940 -1.53 0.617 0.004 Because there is only a very small probability of intersecting a tortuous three-dimensional pore along its largest cross-section, the median solidity and circularity of all intersected pores overestimate the true pore shape. Similarly, the median size parameters underestimate the true median sizes. Beiss and Dalgic6 showed excellent correlation between the Cp of the top 2% of pores and the fatigue strength in sintered steels. Thus, for a more accurate representation of pore shapes, parameters of the largest 2% of all pores are also given in Table III. Optical microscopy of polished surfaces, etched with 2% Nital, show that the microstructure consists primarily of tempered martensite and bainite, with some retained austenite (Figure 3). The difference due to tempering is a coarser bainite in the 315T samples compared to the 205T samples. Figure 3. Optical micrograph of a 205T sample, etched with 2% Nital. Effect of Machining and Tempering on Residual Surface Stress As stated previously, fatigue specimens were machined by a low-stress grinding technique after tempering of the sintered blanks. Examination of the machined surface by optical microscopy revealed a surface porosity of less than 0.2% (compared to 10.4% in the interior), indicating substantial plastic deformation and densification during machining. As shown in Figure 4, low-stress grinding generated a residual compressive stress along the axial direction of approximately -500 MPa (-72.5 ksi). The magnitude of residual stress is expected to be dependent on machining technique, as well as specimen properties such as porosity, strength and surface hardness. For example, Matsumoto et al.14 have shown that AISI 4340 steel machined by turning had a residual surface stress ranging from +200 MPa (+29 ksi) in low-hardness samples (HRC 29) to -530 MPa (-76.9 ksi) in high hardness sample (HRC 53). On the Effect of Stress-Relieving Heat-Treatment on Residual Surface Stress and Fatigue Strength As-sintered Low-stress Grinding 100 0 -100 σ (MPa) surfaces of ground porous steels, Sonsino et al.8 measured residual stresses of -50 MPa (-7.3 ksi) for a soft sample (HV 130) and -100 MPa (-14.5 ksi) for a harder sample (HV 280). In contrast to machining, tempering led to residual compressive surface stresses of less than -100 MPa (14.5 ksi) (Figure 4). Furthermore, no significant difference was observed in the residual stress between samples tempered at 205˚C and those tempered at 315˚C, whether before or after machining. Thus, the residual surface stresses were not sensitive to the subtle changes in phase fractions formed during the two different tempering temperatures of this study. -200 -300 -400 -500 -600 Untempered 205T-NSR-NP 315T-NSR-NP Figure 4. Residual surface stresses along the axial direction due to machining and tempering. Whereas tempering temperature had little effect on the residual stress, substantial compressive stresses were generated by machining. As seen in Figure 5, the 175˚C heat-treatment after machining yielded no significant change in residual stress. Before stress-relief, the average axial surface stress was -507 ± 17 MPa (74 ± 3 ksi) and after stress-relief was -538 ± 39 MPa (78 ± 6 ksi). Furthermore, no difference in fatigue behavior was measured for samples before and after this heat-treatment, whether tempered at 205˚C or 315˚C. This is illustrated in Figure 6 for samples tempered at 205˚C. The plotted lines seen in all figures with S-N data were obtained from linear regression. The difference between the two curves at low cycles – high stress is likely due to an insufficiently small sample size at these levels. 360 Before Stress-Relief After Stress-Relief 100 205T-NSR-P 205T-SR-P 340 0 320 σmax (MPa) σaxial (MPa) -100 -200 -300 280 260 240 -400 220 -500 -600 300 205T-NP 315T-NP Figure 5. Residual surface stresses along the axial direction before and after a 175˚C stressrelief heat-treatment. No significant changes in residual stresses were observed as a result of this heat-treatment. 200 4 10 10 5 10 6 10 Cycles to Failure, Nf Figure 6. S-N curves for samples tempered at 205˚C, with or without a stress-relieving heattreatment. No difference in fatigue behavior was observed due to this heat-treatment. 7 Effect of Surface Polishing on Residual Surface Stress and Fatigue Strength It is important to note, however, that the reduction in residual surface stress did not have an effect on the fatigue strengths (Figure 8). This insensitivity of fatigue strength to residual surface stress is further illustrated in Figure 9 for samples tested at 228 MPa (33.1 ksi). Insensitivity to residual surface stresses is typically seen in materials whose fatigue strengths are governed by large internal defects. For example, a study on high speed tool steels by Meurling et al.15 showed that samples with surface stresses of -350 MPa (50.8 ksi) due to surface grinding had the same fatigue strength as samples with surface stresses of -750 MPa (109 ksi) due to shot-peening. The reason was that fatigue cracks did not originate on the surface, but at large interior inclusions. Several studies on porous sintered steels, including this study, have observed that fatigue cracks routinely originate from just below the surface at either large pores or at localized regions of increased porosity.16-18 Further evidence that fatigue strength in these steels is governed by subsurface porosity is given in Figure 10. The data in Figure 10 are of 205T-NSR-P samples fatigued at 260 MPa (37.7 ksi). As can be seen, the cycles to failure is a function of defect size, which were determine by SEM to be sub-surface regions of distinctly higher porosity. Before Polishing After Polishing 100 0 σaxial (MPa) -100 -200 -300 -400 -500 -600 205T-NSR 205T-SR 315T-NSR 315T-SR Figure 7. Residual surface stresses along the axial direction before and after polishing the surface of machined fatigue specimens. Polishing led to significant reductions in the compressive surface stresses. 360 315T-P 315T-NP 340 320 σmax (MPa) The polishing of sample gage sections, as described in the experimental procedure, yielded a surface that was still significantly denser than the interior. Based on optical microscopy, the amount of porosity on the surface was estimated to be 1% after polishing, compared to 10.4% in the interior and <0.2% on the as-machined surface. Nonetheless, polishing did have a significant effect on the residual axial surface stresses, as seen in Figure 7. The average stress was -522 ± 30 MP a(-7 6± 4 ksi) before polishing and -417 ± 32 MPa (-61 ± 5 ksi) after polishing. 300 280 260 240 220 200 4 10 10 5 10 6 Cycles to Failure, Nf Figure 8. S-N curves for samples tempered at 315˚C, with surfaces in the as-machined state (NP) or with polished surfaces (P). No significant difference was seen in fatigue behavior due to polishing. 10 7 10 5 7 205T 315T 4 Cycles to Failure, ×105 Cycles to Failure, Nf 10 6 3 2 5 10 -600 -550 -500 -450 σaxial (MPa) -400 1 40 -350 Figure 9. Effect of residual axial surface stress on the cycles to failure of samples fatigued at 228 MPa. No significant effect was observed. 60 80 100 Defect Size (µm) 120 Figure 10. Effect of the strength-limiting defect size on the cycles to failure of 205TNSR-P samples fatigued at 260 MPa. Effect of Tempering on Fatigue Strength CONCLUSIONS 360 205T 315T 340 320 σmax (MPa) Since stress-relieving and polishing had no significant effect on the fatigue behavior, Figure 11 combines all data to compare the effects of tempering on fatigue. Two differences exist between the 215T and 315T samples. First, more scatter exists in the 315T samples, as evidenced by the lower correlation coefficient of 0.77, compared to 0.92 for the 205T samples. Second, the 315T samples have a slightly higher fatigue strength of 225 MPa(32.6 ksi) compared to 220MPa(31.9 ksi) for 205T samples. As there was no measurable difference in porosity or surface condition, these differences in fatigue behavior must be due to differences in the microstructural constituents. 300 280 260 240 220 200 4 10 10 5 10 6 10 7 Cycles to Failure, Nf Figure 11. S-N curves for all samples tempered at either 205˚C or 315˚C. Increasing the tempering temperature led to a 5 MPa increase in fatigue strength. Although low-stress grinding generates significant compressive stresses on the surfaces of porous steels, these residual stresses do not affect the fatigue behavior, other than possibly shifting crack initiation from the surface to just below the surface. The compressive residual stresses due to low-stress grinding are known to dissipate rapidly beneath the surface, unlike more energetic techniques such as shot-peening. 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