UDK 621.78:620.178.3 ISSN 1580-2949 Professional article/Strokovni članek MTAEC9, 48(6)959(2014) FATIGUE-LIFE ENHANCEMENT OF SHEETS MADE OF 34CrNiMo6 STEEL POVEČANJE ODPORNOSTI PROTI UTRUJANJU PLOČEVIN IZ JEKLA 34CrNiMo6 Jan Džugan, Zbyšek Novy, Martina Marešova COMTES FHT Inc., Prümyslovä 995, Dobfany, Czech Republic jan.dzugan@comtesfht.cz Prejem rokopisa - received: 2013-10-04; sprejem za objavo - accepted for publication: 2014-01-27 Currently available and well-known materials can obtain superior properties when treated with special procedures. Nowadays special treatment procedures are efficiently developed with the use of physical simulators. Physical simulators allow a treatment optimization for small-scale laboratory samples that can be subsequently transferred to real production processes. There is always a need for a successful transfer of knowledge from small-scale laboratory experiments to a real production of, for example, metal sheets. In the current paper the previously developed thermomechanical procedures for the 34CrNiMo6 steel under laboratory conditions are applied to the metal-sheet production. Very promising properties of the bulk-material samples processed in a physical simulator were obtained; the challenge was to obtain similar properties of real metal sheets by transferring the laboratory procedure to a metal-sheet production process. Several previously developed thermomechanical procedures were applied to the metal-sheet production. The sheets exhibit a very good combination of the tensile strength exceeding 1500 MPa and the elongation reaching 10 %. The fatigue strength was investigated in all the considered states and a comparison of the materials treated with various thermomechanical procedures was carried out. Keywords: thermomechanical treatment, fatigue, steel, metal sheets Razpoložljivi in dobro poznani materiali, obdelani s posebnimi postopki, lahko pridobijo posebne lastnosti. Ti postopki obdelave se danes razvijajo s fizikalnimi simulatorji, ki omogočajo optimiranje obdelave majhnih laboratorijskih vzorcev, rezultati pa se lahko kasneje prenesejo v realno proizvodnjo. Kljub temu vedno obstaja potreba po uspešnem prenosu iz laboratorijskih eksperimentov na majhnih vzorcih v realno proizvodnjo, kot je primer kovinskih pločevin. V tem primeru so bili predhodno laboratorijsko razviti termomehanski postopki za jeklo 34CrNiMo6, uporabljeni pri proizvodnji pločevine. S fizikalnim simulatorjem so bile dobljene zelo obetajoče lastnosti osnovnega materiala, izziv pa je bil dobiti podobne lastnosti realnih pločevin s prenosom laboratorijskih postopkov v proizvodnjo. Pri proizvodnji pločevin so bile uporabljene številne vrste predhodno razvite termomehanske obdelave. Pločevine imajo dobro kombinacijo natezne trdnosti nad 1500 MPa, raztezek pa dosega 10 %. Pri vseh upoštevanih stanjih je bila preizkušena odpornost proti utrujanju in opravljena je bila primerjava materialov po različnih termomehanskih obdelavah. Ključne besede: termomehanska obdelava, utrujanje, jeklo, pločevine 1 INTRODUCTION 2 HEAT TREATMENT This work is a part of a currently running project The material of interest underwent several heat dealing with the material-property improvement using a treatments. Following the previous investigation, the special treatment. The material of interest in the present influences of the two main parameters on the resulting case is the 34CrNiMo6 steel The material investigatedis material properties were investigated: the cooling rate widely used for heavily loaded parts such as rotors or during quenching and the impact of the subsequent crank shafts. This material is generally used in bulk annealing. Two cooling mediums were used, oil and nitrogen gas. The procedure of applying oil was per- form. Investigations leading to an optimization of the material properties for bulk applications were per- formed1,2. The results obtained were very good and thus formed with the use of a furnace. The procedure the investigations are extended also to thin-sheet appli- of applying nitrogen was carried oui,in a special vacuum cations, where a high strength with a certain degree of furnace using nitrogen treatment. The nitrogen cooling available plastic deformation is of high demand at pre- was carried out at a pressure of 6 bar. The applied sent3,4. The input material for the study included the cooling rate for nitrogen was roughly between oil and sheets with a thickness of 1 mm rolled from a diameter air' thus slower than inthe first case of cooling. The sam- bar 60 mm. Several heat-treatment procedures were ples were quenched in both above-mentioned ways and a applied and the resulting mechanical properties and half of the each batch of the samples was subsequently microstructures were observed. Special consideration annealed. Detailed information on the heat-treatment was given to the fatigue strength for the obtained mate- conditions can be found in Table 1. rial states in the current case. 3 TENSILE TESTS Tensile tests according to CSN EN ISO 6892-1 were performed at room temperature. Standard flat specimens with a gauge-section width of 12.5 mm and a gauge length of 50 mm were tested. Three samples were tested for each material condition. Prior to the testing, the specimen dimensions were measured and the original gauge length for the elongation A5 determination was marked on each specimen. After the test, the yield stress Rp = 0.2 and tensile strength Rm were determined. The final gauge length was also measured after the test and the elongation after fracture A5 was evaluated as well as the uniform elongation at the tensile strength Ag and the cross-section reduction Z. The records of the tests can be found in Figure 1. The evaluated material properties are summarized in Table 2. The samples quenched in oil generally exhibited slightly higher strength values than the samples treated in nitrogen. It can also be seen that there is a significant Figure 1: Examples of tensile-test records for the considered heat-treated states Slika 1: Primeri krivulj pri nateznem preizkusu za uporabljena toplotno obdelana stanja Table 1: Heat-treatment-regime overview Tabela 1: Pregled uporabljenih vrst toplotne obdelave Figure 2: Specimen for fatigue tests Slika 2: Vzorec za preizkus utrujanja difference in the tensile-strength value between the nitrogen-quenched samples with and without annealing. The values for the annealed samples are lower by about 150 MPa, while the other tensile-test parameters are almost identical. In the case of the oil-treated samples, a very small decrease in the tensile strength is found between the annealed samples and the samples without annealing. The annealed samples exhibit an improvement in the other parameters. The yield stress is especially improved, by almost 150 MPa. 4 FATIGUE TESTS High-cycle fatigue tests were performed on the experimental batches with a magnetoresonant testing machine. The tests were run in the force-control mode at room temperature. The geometry of a test piece is shown in Figure 2. The test frequencies were about 120 Hz. The fatigue strength was evaluated as the intersection of the line fitted to the measured data with the line representing 1 ■ 107. The evaluated high-cycle fatigue-strength values are summarized in Table 3. The obtained fatigue curves are shown in Figure 3. The results obtained point out a significant difference in the fatigue strength between the Sample Normalizing Quenching Annealing °C Hold Cooling medium °C Hold Cooling medium 1 860 °C/vermikulit 850 20 min nitrogen - - - 2 860 °C/vermikulit 850 20 min nitrogen 200 120 min air 3 860 °C/vermikulit 850 20 min oil - - - 4 860 °C/vermikulit 850 20 min oil 200 120 min air 5 860 °C/vermikulit 850 20 min nitrogen — — — 6 860 °C/vermikulit 850 20 min nitrogen 200 120 min air Table 2: Tensile-test results Tabela 2: Rezultati nateznih preizkusov Treatment Rp0.2 (MPa) ReH (MPa) ReL (MPa) Rm (MPa) Ag (%) A50 (%) Z (%) 1 1173.8 939.4 295.3 1615.9 3.4 4.3 32.8 2 1183.8 1208.7 283.8 1461.3 3.5 4.6 33.0 3 1164.8 1170.7 269.3 1665.0 3.9 5.1 10.8 4 1308.7 1272.0 275.2 1648.8 4.4 5.5 12.9 5 1193.2 946.4 305.6 1626.7 2.6 5.0 41.5 6 1226.8 606.3 273.0 1546.8 4.1 5.3 39.4 5 METALLOGRAPHY Metallographic investigations were performed in order to assess the obtained microstructures for all the considered material states. The standard preparation of metallographic samples was done. The samples were observed with a light microscope and investigations at Figure 3: High-cycle fatigue curves for the materials investigated Slika 3: Krivulje visokocikli~nega utrujanja preiskovanih materialov oil- and nitrogen-quenched samples. The difference is about 100 MPa in favor of the oil-treated samples. The difference between the samples with and without annealing is not significant in the cases of both sample treatments. The highest fatigue strength can be found for the annealed oil-treated samples. Table 3: Results of high-cycle fatigue tests Tabela 3: Rezultati preizkusov visokocikli~nega utrujanja Material Fatigue strength (MPa) 1 235 2 250 3 335 4 355 5 230 6 235 ^^ V - 20kU -^xs.ees , Swm . •;jjjl2 35 SC! Figure 5: Microstructure after regime 2 (SEM) Slika 5: Mikrostruktura po režimu 2 (SEM) 20ky yi 000 10 m ^ Et Figure 4: Microstructure after regime 1 (SEM) Slika 4: Mikrostruktura po režimu 1 (SEM) Figure 6: Microstructure after regime 3 (SEM) Slika 6: Mikrostruktura po režimu 3 (SEM) s Figure 7: Microstructure after regime 4 (SEM) Slika 7: Mikrostruktura po režimu 4 (SEM) higher magnifications were carried out with a scanning electron microscope. The obtained microstructures for all the applied regimes are shown in Figures 4 to 9. The microstructure of the sample that underwent quenching in nitrogen is shown in Figure 4. The micro-structure consists of fine martensite with original Figure 8: Microstructure after regime 5 (SEM) Slika 8: Mikrostruktura po režimu 5 (SEM) Figure 9: Microstructure after regime 6 (SEM) Slika 9: Mikrostruktura po režimu 6 (SEM) carbides, which were not dissolved in austenite before the hardening, The length of the martensite plates seems to be between 5-10 pm. The average diameter of the undissolved carbides is about 0.4 pm. There is no fine-carbide dispersion precipitation in the microstructure after the hardening. Figure 5 depicts the microstructure of the nitrogen-quenched and annealed sample. A microstructure very similar to that of the previous nitrogen-quenched sample can be found. It includes fine martensite und undissolved carbides. Additionally, very fine, needle-like carbide particles that almost create a network structure can be found. The microstructure after oil quenching (regime 4), including martensitic needles without carbides is shown in Figure 6. A very fine precipitate seems to be present in the oil-quenched sample after quenching followed by annealing. This microstructure is depicted in Figure 7. Fine martensitic grains with fine needle-like particles that almost create a network structure around the original austenitic grains after the treatment with regime 5 are shown in Figure 8. The average diameter of the undis-solved carbides is 0.5 pm. A very fine-grained martensitic microstructure with a very low presence of undissolved carbides obtained after the treatment with regime 6 can be seen in Figure 9. 6 RESULTS AND DISCUSSION Sheets with a thickness of 1 mm were rolled from a diameter bar 60 mm. Normalizing, quenching and tem- pering processes were consequently performed on the sheets. Two variants of quenching were performed, hardening in oil and hardening in nitrogen gas under a pressure of 6 bar. A metallographic analysis, quasistatic tensile tests and high-cycle fatigue tests were realized on the experimental material. The metallographic analysis shows that quenching in oil is faster than in pressure nitrogen gas 6 bar. The mixture of martenzite and bainite occurred after the quenching in nitrogen, while pure fine martensite is visible after the oil quenching. The annealing after both variants of quenching caused a precipitation of very fine, needle-like carbides. The samples after the quenching in oil exhibit higher yield strength, higher tensile strength and higher fatigue strength in comparison with the samples after the quenching in nitrogen. This result is expected as the martensitic samples after the oil quenching have higher strength properties. A drop in the tensile strength was found after the annealing at 200 °C for the samples quenched in nitrogen. On the other hand, the oil-quenched samples exhibited no drop in the tensile strength after the annealing, and their yield strength increased by almost 150 MPa. The fatigue strength was also found to be higher for the oil-quenched samples than for the nitrogen-quenched ones. 7 CONCLUSION A laboratory preparation of ultra-high-strength sheets from the 34CrNiMo6 steel was achieved. The sheets with a thickness of 1 mm, a tensile strength above 1650 MPa and fatigue strength of 350 MPa were produced. A standard phenomenon was observed when the tensile-test properties and the fatigue strength obtained after the mild quenching in nitrogen were lower than in the case of the faster oil quenching. The tempering at 200 °C caused a further enhancement of both the yield strength and the elongation of the oil-treated material. Excellent attained properties of the investigated sheets allow further possibilities for a mass reduction of the heavy-loaded sheet constructions, for example, in the automotive industry. Acknowledgment This paper includes the results obtained within project ED2.1.00/03.0077 - West-Bohemian Centre of Materials and Metallurgy (2011-2014, MSM/ED). 8 REFERENCES 1 J. Dzugan, Z. Novy, P. Konopik, P. Motycka, Improvement of fatigue properties of 34CrNiMo6 steel by controlled thermomechanical treatment, Proc. of the conference Metal 2010, Roznov pod Radho-stem, Czech Republic, 2010, 421-426 2 J. Dzugan, Z. Novy, M. Sosnova, Improvement of fatigue life of 34CrNiMo steel by thermomechanical treatment, Advanced Materials Research, 264-265 (2011), 1725-1730 3Z. Novy, J. Dzugan, P. Motycka, M. Donatova, J. Dlouhy, Fatigue life improvement of metal sheets made of 34CrNiMo6 steel with the use of physical simulator, Proc. of the conference Metal 2011, Brno, Czech Republic, 2011 4 J. Dzugan, Z. Novy, P. Motycka, J. Martinkova, P. 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