Materials Research susceptible to these embrittlements. Ni-Cr steels are prone to TE, but its susceptibility to TE, therefore Mo becomes an important alloy element added to steels to minimize the chances of TE occurrence The TE phenomenon can also be named “reversible embrittlement” and “two-step embrittlement” The map in Figure 1 de nes the regions of intergranular and transgranular fractures, according to C and P contents for martensitic steels tempered at low temperatures, showing that the C content necessary to cause intergranular fracture, decreases as the P content . The effect of the P content, has been shown as a result of some research that prove that the P diminish the C solubility in the previous austenite, promoting in this way, the cementite formation The fact that QE being uniformly developed in steels, even if they present low P contents (lower than 0.010 wt. (%)), the rule states that Hyde 10 showed that the embrittlement of quenched and tempered steels may lead to a reduction in the fatigue and endurance limits due to the segregation of P and/or cementite formation in the prior austenite grains boundaries. It has been observed that in super cially hardened steels susceptible to intergranular fracture, which is the case of carburized steels, the exural fatigue may lead to crack nucleation, with size varying from two to four grains in depth, which grows steadily in an elliptical way until the critical size be reached and the nal fracture occurs instantaneously. In these cases, the nucleation was correlated to the cementite formation at the prior austenite grains boundaries, leading to a reduction in the fatigue life by reducing small intergranular fracture zone occurred during the nucleation of a fatigue crack. By analyzing two cemented steels, whose carbon content in the surface was about 1 wt. (%) and P contents were (%). Hyde observed that the fatigue strength had been changed, so the embrittlement affected more signi cantly the fatigue limit (Figure 3). The quenching of high-strength steels to obtain harder martensitic structures is generally expected for high cycle fatigue regime and high wear performance. Nevertheless, this process can introduce microcracking and/or promote intergranular cracking nucleation at the grain boundaries . In a brittle material, the strength of the grains is usually weaker than its interface, therefore cracks nucleate in transgranular way. Even so, with increasing hardening, the strength in the interior of a grain, usually becomes higher than at the interface (boundary), nucleating cracks intergranularly. Corresponding to this mechanism is the intergranular cracking by fatigue in low-carbon prior austenite grains boundaries, weakening them carburized high-resistance steels, a aw may occur intergranularly at the prior austenite grains boundaries, depending on the severity The material investigated in the present work was a SAE 5160 steel, with four different P content and provided as laminated bars thickness and 1000 mm length. Its chemical composition is presented in Table 1. 2.2. Heat treatments Figure 4 presents a schematic owchart indicating the heating treatments performed in the SAE 5160 steel bars, from which Figure 1. Fracture mode due to P and C contents for martensite tempered at low temperatures Figure 2. Location of the intergranular initiation of a fatigue fracture surface of a specimen of SAE 4320 carburized steel Figure 3. Comparison of maximum stress versus number of cycles for steels with different phosphorus contents specimens were removed for hardness, impact toughness and fatigue (S-N) tests. These bars were gradually heated in a continuous two heating zone furnace. The soaking time at the second zone was 15 minutes. All bars, after austenitizing, were quenched in mineral In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel oil and tempered. Basically, three different austenitizing temperatures and three different tempering temperatures were studied for the four different levels of phosphorus studied. The quenching oil was always kept at 66 °C. 2.3. Mechanical tests As mentioned before, the hardness, impact, fracture toughness and fatigue (S-N) tests were performed to investigate the susceptibility of the SAE 5160, with different allowable P content, to the embrittlement quenching and tempering temperatures, to avoid these embrittlements. Rockwell C hardness tests were conducted in a Leco RT-240 made from diamond, according to ASTM E18-04. The hardness values represent an average of 10 measurements, acquired in the width of the surface in each sample. For the impact tests, type A Charpy samples with V-notch were machined according to ASTM E23-04, as shown in Figure 5. The fabrication was performed in a milling machine and the V-notch in a special backed-off cutter machine. The test specimens were removed in the L-S direction, so that the notch was parallel to the width of propagation. The tests were performed in an Instron Wolpert PW30 impact test device, using a 300 J maximum energy capacity and The fatigue tests were performed in a 1 ton nominal capacity Guttman Eccentric Press (used for fatigue tests of at springs). This machine uses a three-point bend device in which the specimen is placed over two points separated by 650 mm span, as shown in Figure 6. The maximum load applied was 1093 kN (corresponding to = 130 MPa in the center of the bar at surface), which corresponds to a load necessary to cause a 25 de ection in the center of the bar. It is important to mention that all specimens, underwent to a shot-peening process on the surface that during test would be under tensile stresses, before they were fatigue- tested, similarly to the procedure for regular leaf springs. The three points fracture toughness tests were performed according to ASTM E1820-06. The load ratio, maximum load and frequency used in the fatigue pre-cracking of specimens were, R 0.1, = 5.5 kN and f = 30 Hz, respectively. A servo-hydraulic MTS810 system was used to conduct the fracture toughness test. As the bar thickness was only 10 mm, the specimens was removed in the T-L direction and three-point bend specimens, SE(B) were used with B = 10 mm; W = 20 mm; a = 80 mm; and f(a/W) = 2.46, as shown in Figure 7. The rate of applied load was 13 kN/min and the crack opening displacement was Initially, two alloys were previously chosen in an attempt to validate the obtained K values. The criterion was the selection of specimens heat treated for the more fragile and more ductile conditions. For validation purpose, it is worthwhile to emphasize that the blade gage restricted the specimen to its thickness (B) = 10 mm. As stated by the ASTM 1820-06 standard, the condition that ,,()2,5 aBWa 2.4. Grain size analysis Samples removed from the bars were prepared according to ASTM E3-08. After the surface preparation, a chemical attack Figure 4. Schematic flowchart of the heating treatment routs for the Figure 5. Table 1. Materials Research Figure 7. Figure 6. Schematic representation of the fatigue test. The dimensions are was performed on the surface of each sample. The chemical attack consisted in a solution of 1.0 g of picric acid, 1.0 mL of chloride acid, minutes. Afterwards, each sample was observed in a Zeiss Axiotech Stemi DV4/DR microscope connected to Graftek Ultimage Optlab software, Version 2.6. The grain size was measured according to 2.5. Fractographic analysis The fracture surface of the broken specimens after impact, fracture toughness and fatigue tests, were observed in a DSM 960 ZE155 scanning electronic microscope. The fracture surfaces have that no undesirable impurity would in uence the analysis. This type of analysis is required to evaluate the micro-mechanism of fractures. As observed in Table 1, except for the P content, the chemical compositions of the four steels are alike. The P content was below the maximum allowable value always. Table 2 shows the values of grain sizes for each condition. The invariability of the grain size was expected since these steels were aluminum killed to avoid large grains. Figure 8 shows the mean hardness values obtained from each steel composition and heat treatment as presented in the ow chart in Figure 4. For the same austenitizing temperature, the hardness values decrease for an increasing tempering temperature, However, 1000 °C. Most hardness values of the tested samples are inside the HRC. For the steel D (0.031% of P) tempered at 530 hardness value was slightly below the minimum value (43 These lower hardness values produced higher impact energy values than those expected for the SAE heat treated for the nominal hardness value (43-48 HRC). Unfortunately, at the highest tempering temperature (530 °C), the furnace did not allowed further reduction the necessary hardness value. Figure 9 shows an overall representation of the absorbed impact energy for all heat treatment conditions, considering the different levels of P investigated. It is observed that, independent of the austenitizing temperature for quenching, lower the P content, higher were the values of absorbed impact energy, especially for the tempering temperature of 500 °C. Also, steel A (0.012 P) austenitized at 850 °C and tempered at 500 °C exhibited the highest value of absorbed impact energy, approximately 400 kJ.m , despite its highest In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel hardness values when compared to the ones obtained at austenitizing According to Reguly tempering temperature, will cause an improvement on the impact toughness, if the phosphorus content is low (0.001 wt. (%)), since it will not develop quench embrittlement. In the case that the P content was low, but developed quench embrittlement after austenitizing at 1100 °C, there was an improvement in the impact toughness when the tempering temperature was high. Reguly , observed also that improvement in the impact toughness values were obtained when the austenitizing temperature was below 1100 °C. As mentioned before, the hardness values of any specimen tempered at 530 °C were not in the required hardness interval HRC), as a consequence the toughness values were overestimated and the fracture surfaces of these specimens were not Figure 10 shows the fractographic images of the Charpy impact specimens tempered at 470 °C for 70 minutes. For Steel D (0.031 wt. (%) P) the intergranular fracture prevails at all austenitizing temperatures, while the intergranular fracture of steel (%) P) occurs only for austenitizing at 1000 °C. The produced a region of mixed fracture (ductile + intergranular) with a dominance of ductile type. The amount of intergranular fracture gradually increases as the austenitizing temperature rises, explaining the gradual drop in the impact toughness values, according to the increase in the austenitizing temperature for both steels B and D for Figures 11 and 12 show images of impact specimens tempered at 500 °C for 64 minutes. In steels A (0.012 wt. (%) P) and C (%) P). Figure 12 features a ductile fracture of steel B (0.017 wt. (%) P) and also a mixed aspect in the specimen from steel D (0.031 wt. (%) P), which shows mostly ductile with only some regions of intergranular fracture. This intergranular portion is compared to specimens from steel B (0.017 wt. (%) P), which display an absorbed impact energy of 240.54 kJ.m Thus, for the austenitizing temperature of 850 °C it is clearly noticed that increasing the P content, the amount of intergranular fracture increased and consequently the value of the absorbed impact energy was reduced. Yet, for those cases of austenitizing temperature of 900 °C, Figure 12 shows the predominance of intergranular fracture for specimens from steel D with high P content (0.031 wt. (%)), and predominance of ductile fracture for specimens taken from steel B with medium P content (0.017 wt. (%)). However, unexpectedly the impact toughness values of both steels were quite similar, i.e., for steels B and D, respectively. P) exhibited a signi cantly larger portion of intergranular fracture than the specimens austenitized at 900 °C. Such fact is evidenced by the fall of approximately 13% in the value of impact toughness when the autenitizing temperature was 1000 °C. On the other hand, the sample of steel D (0.031 wt. (%) P) displayed a fracture surface with predominantly intergranular type. In short, the fractographic analysis agrees the fact that the values of impact toughness of the steels with higher levels of phosphorus are always lower than those with lower levels of P (Figure 9). The large portion of intergranular fracture found in steels with higher levels of P is related to the decrease in the values of absorbed impact energy. It can be inferred that this embrittlement phenomenon is due to the segregation of phosphorus occurred during the respective austenitizing and/or tempering heat treatments, for steels with higher Figure 8. Hardness test results versus tempering temperature for three austenitizing temperatures (TA , TA , and TA Figure 9. Absorbed energy in the Charpy impact test. Comparative image for all conditions studied in this work. Table 2. Grain size ASTM (µm) for each studied condition. Steel A (0.012% P) Obs: --- means that no measurement was made. Materials Research Figure 10. Fracture surface (central part of the fracture) of impact specimens. Steel with 0.017 wt. (%) P (steel B) austenitized at: a) 850 °C; c) 900 °C; and 1000 °C. Steel with 0.031 wt. (%) P (steel D) austenitized at: b) 850 °C; d) 900 °C; and f) 1000 °C. The specimens were tempered at 470 °C for 70 minutes. In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel Figure 11. Fracture surface (central part of the fracture) of the impact specimens. Steel with 0.012 wt. (%) P (steel A) austenitized at: a) 850 °C; c) 900 °C; and e) 1000 °C. Steel with 0.025 wt. (%) P (steel C) austenitized at: b) 850 °C; d) 900 °C; and f) 1000 °C. The specimens were tempered at 500 °C for 64 minutes. Figure 13a shows the Load versus COD curve for steel B According to ASTM E1820-2006, it is observed that the curve for steel B is from Type I, meaning that the value of P is lower than the value . Thus, it is necessary to use the procedure of the 5% secant . Figure 13b shows the behavior of a steel D (0.031 of P) austenitized at 1000 °C and tempered at 470 °C. The Load versus COD curve in this case is from type III, with elastic behavior an indicative of low toughness. Table 3 shows the fracture toughness results for specimens from steel B (0.017 wt. (%) of P) and steel D (0.031 wt. (%) of P). The last line of Table 3 shows the results of a, (W–a) and B, which are be considered the fracture toughness value . It is observed that B did not allowed the obtaining of a valid value of K IC for steel B (austenitized at 850 °C and tempered at 530 °C), therefore it is only. However, for steel D (austenitized at 1000 and tempered at 470 °C), it was possible to obtain K = K only the values of K were used for toughness for these tested conditions. Note that, similarly to the impact test trend with P content, the values of K decreases as the phosphorus level increases. The values of K relates well with the fracture surface results, i.e., steel B, which had a higher value of K mode, while steel D, which had a lower value of K , presented a brittle fracture mode. The fracture surface from steel B, Figure 14, shows a ductile fracture mode, with stable crack growth by coalescence of microvoids, Figure 14b. In this specimen it was also observed a delamination, where the internal faces presents a more brittle aspect, Figure 14c. From Figure 15 it is seen that steel D exhibited a more brittle mode of fracture, with a mixture of cleavage and intergranular types. Such a fracture micromechanism occurred due its highest P content, even considering that it is inside of the allowable range. As previously observed by other researchers to prior austenitic grain boundaries, making the steel to behave in a brittle manner. However, it is not possible to precise in which step it Figure 16 presents the results of the fatigue tests. Note that, for similar heat treatment, there is a spread in the measured values of fatigue life. This scattering could be related to the stress concentrators in the spring surface and/or local changes in mechanical properties, considering that the specimens were directly acquired from bars made on industrial scale. However, besides the austenitizing and tempering temperatures, the values of high cycle fatigue life were not signi cantly affected by the embrittlement caused by a higher level of P, as the heat treatments aimed to produce micro-structures able to provide similar mechanical properties, such as hardness and tensile strength to the specimens, consequently causing a similar high cycle fatigue life. Materials Research Figure 12. Fracture surface (central part of the fracture) of the impact specimens. Steels with 0.017 wt. (%) P (steel B) austenitized at: a) 850 °C; c) 900 °C; and e) 1000 °C. Steels with 0.031 wt. (%) P (steel D) austenitized at: b) 850 °C; d) 900 °C; and f) 1000 °C. The specimens were tempered at 500 °C for 64 minutes. In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel Figure 13. Figure 14. Materials Research Table 3. temperatures and values of load (P Tempering temperature (°C) Yield strength (MPa) Ultimate strength (MPa) K [MPa] (W-a), B, a (mm) Figure 16. Fatigue test results (S-N) performed in the heat-treated samples Figure 15. Fracture surface from steel D (0.031% of P) austenitized at 1000 °C and tempered at 470 °C: a) General view showing the notch, fatigue pre crack Template de Figuras - Materials Research * Fontes Times (Roman), tamanho 8. In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel 3. Hyde RS, Krauss G and Matlock DK. Quench embrittlement: intergranular fracture due to cementite and phosphorus in quenched carbon and Proceedings of the 40 Mechanical Working and Steel Processing Conference . 1998; Warrendale, PA. ISS. p. 921-928. 4. Reguly A, Strohaecker TR, Krauss G and Matlock DK. Quench embrittlement of hardened 5160 steel as a function of austenitizing . 2004; Materials Science and Engineering A . 1999; A273-275:466-470. 6. Zia-Ebrahimi F and Krauss G. Mechanisms of tempered martensite . 1984; 7. Qing-fen L, Li L, Er-bao L, Dong L and Xiu-fang C. Temper embrittlement dynamics induced by non-equilibrium segregation of phosphorus in steel 12Cr1MoV. 8. ASM International Handbook Committee. Failure analysis and prevention. . EUA; 2002; p. 691-692. 9. Krauss G. Deformation and fracture in martensitic carbon steels tempered at low temperatures. 10. Darwish FA, Pereira LC, Gatts C and Graça ML. On the tempered martensite embrittlement in AISI 4140 low alloy steel. Materials Science and Engineering A . 1991; A132: L5-L9. 11. Hyde RS, Krauss G and Matlock DK. Phosphorus and carbon segregation: effects on fatigue and fracture of gas-carburized modi ed 4320 steel. Apple CA and Krauss G. Microcracking and Fatigue in a Carburized 13. Wu R, Freeman AJ and Olson GB. On the Electronic Basis of the Phosphorus Intergranular Embrittlement of Iron. Journal of Materials Resistance. Kunio T, Shimizu M, Yamada K, Enomoto M and Kawada Y. The Role of Prior Austenite Grains in Fatigue Crack Initiation and Propagation in Low Carbon Martensite. Fatigue Engineering Materials Structural . 1979; From the results it is possible to conclude that the P content steel, even if considered P content below the maximum allowable value (0.03 wt. (%)). The effect is more pronounced at lower quenching temperature (850 °C). For higher quenching temperatures 1000 °C), the drop in the impact toughness is smaller. Although, it was not possible to validate the fracture toughness following the ASTM E1820, the K values were able to show a 30% drop in the stress intensity factor value when compared with the energy and stress intensity factor values obtained for the steels analyzed, i.e., higher P content was related to larger percentile of intergranular fracture, as well as with increasing temperature for the values of high cycle fatigue life were not signi cantly affected by the embrittlement caused by higher levels of P. As a nal conclusion, it was noticed that the P content has a recommended that spring steels must have P content as low as Acknowledgements The authors would like to acknowledge Rassini-NHK Automotive for the support and the Materials, Aeronautics and Automotive USP, for granting the use of its facilities. References 1. Fuentes JJ, Aguilar HJ, Rodríguez JA and Herrera EJ. Premature Engineering Failure Analysis 2. : heat treatment and processing principles. Ohio: Materials Park ASM; 1995. Materials Research *e-mail: danilobvc@yahoo.com.br *e-mail: danilobvc@yahoo.com.br In uence of Phosphorus Content and Quenching/Tempering Temperatures on Fracture Toughness and Fatigue Life of SAE 5160 Steel Danilo Borges Villarino de Castro , Jaime Milan Ventura, Cassius Olivio Figueiredo Terra Ruckert, Dirceu Spinelli, Waldek Wladimir Bose Filho Department of Materials, Aeronautics and Automotive Engineering, Engineering School of São Carlos, University of São Paulo (SMM-EESC-USP), Av. Trabalhador São-Carlense, 400, Parque Arnold Schmidt, CEP 13566-590, São Carlos, SP, Brazil Received: May 18, 2010; Revised: November 30, 2010 This study investigates the in uence of quenching/tempering temperatures on the fracture toughness and fatigue life of SAE 5160 steel, considering different phosphorus contents. Quenching and tempering treatments were applied to samples removed from different bars of commercial SAE 5160 steel with different P content. Three different austenitizing temperatures for quenching: 850, 900 and 1000 °C and a constant holding time of 15 minutes were used. The oil temperature for quenching was kept at 66 °C and the tempering conditions were 3 HRC. Therefore, the heat treatments cycles were applied to specimens containing low (0.012 wt. (%)), medium (0.017 wt. (%)) and high (above 0.025 wt. (%)) phosphorus contents, in order to observe the effects of this element on the susceptibility of these content analyzed in this work has caused embrittlement, even in the bars with the lowest P content, leading to intergranular fracture. However, if the nucleation life is taken into consideration, this embrittlement has no effect on the nucleation fatigue life of the component. Keywords: 5160 steel, phosphorus, austenitizing, tempering 1. Introduction It was observed that in the SAE 5160 steel steels used to make springs, the P content may ranges from 0.010 to 0.025 wt. (%). Manufacturers consider that this concentration does not affect the impact and the fatigue performance of this component, which is highly requested in the automotive industry . By knowing the negative effects considering the regular alloying limits content found in the SAE 5160 steel bars, on both: the impact toughness and on the fatigue life. It has been known that low-carbon alloy and plain-carbon steels are susceptible to intergranular fracture along the prior austenite grain boundaries, depending on their chemical compositions and for intergranular fracture for steels with more than 0.5 wt. (%) carbon in low-temperature tempered martensite steels susceptible to intergranular embrittlement phenomenon under as- does not promote intergranular fracture, i.e., this embrittlement phenomenon can occur during the austenitizing or quenching process, . The segregation of atoms of P to the prior austenite grain boundaries (a factor already known in several processes of intergranular embrittlement) and the formation of cementite (Fe C) around prior austenite grains are noticeable The literature has a tendency towards the basic supposition that decomposition increases gradually. Thus, the minimum toughness observed may be referred to tempered martensite embrittlement (TME), which may also be identi ed as “irreversible embrittlement” “one-step tempering embrittlement” or even as “embrittlement at . In the case of high-strength steels, TME is characterized by a signi cant drop in the impact toughness values in temperatures . Researchers have showed that as larger is the drop in impact toughness value (V-notch Charpy impact) in this TME occurs in a tempering interval where the -carbides turn into C) and it mainly takes place in tempered martensitic microstructure. However, it is known that the same is likely to occur certain impurities, such as phosphorus (P), tin (Sn), antimony (Sb), and arsenic (As) . These elements cause embrittlement in the or during the low cooling rate during quenching in this temperature range. The embrittlement degree of steels depends on the impurity degree and the time in which it is kept in this temperature range. The impurities migrate to the grain boundaries during tempering period in the TE range. Relatively small amounts of these elements, as lower as 100 ppm or less have been reported as the cause for TE Other elements are also cited as embrittling agents of TE: silicon (Si), germanium (Ge), selenium (Se), tellurium (Te) and bismuth (Bi). Manganese (Mn) content may cause both, TME and TE, and
Influence Of Phosphorus Content And Quenching Tempering