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The Effect of Restoration Process on the Mechanical Behavior of Ultrafine Grain Size Nb-Ti Steel Processed by Warm Rolling and Sub and Intercritical Annealing Hezio Rosa Silva Gustavo Gonçalves Lourenço Luciana Helena Reis Braga Dagoberto Brandão Santos Federal University of Minas Gerais - UFMG - Brazil FVA Concepts Review Ferrite grain size refining increases both mechanical strength and toughness of steels Low carbon content enhances good welding characteristics Mechanical Behavior of High Strength Steels FVA Historical Review Development through the years Dr. D. Ponge – Max Planck Inst. FVA Introduction %C Nb, V, Ti %Mn stable precipitates enhances welding microstructure control Controlled rolling with accelerated cooling refined ferrite (σe )HSLA : 350 to 850 MPa = 3(σe)carbon steels without alloying automotive industry pipe lines for low temperatures operations plates for the naval industry FVA Objectives Evaluate the restoration process in refinement of ferrite in low C-Mn steel microalloyed with Nb and Ti. Produce ferrite grain size of about 1m with different microstructural constitution: Besides ferrite and MA constituent, a combination of: Ferrite + dispersed cementite particles FVA Experimental Procedure Chemical Composition (%) -----------------------------------------------------------------C Mn Nb Ti 0.11 1.41 0.028 0.012 Following steps: Specimens reheated at 900°C and then ice brine quenched; Specimens reheated at 740°C, submitted to warm rolling at 700°C, with three equal pass reductions and then air cooled; The annealing schedule was employed on all specimens at temperatures of 550ºC or 800ºC for different times, and after the soaking time the samples were air cooled. FVA Experimental Procedure T (°C) 900°C – 30 min 740°C – 30 min 800°C Ac3 Ac1 Three pass of 20% reduction each 550°C Times: 5, 30, 60, 120 min Time (min) Final microstructure revealed by nital 2% and LePera etching. Ferrite grain size and volume fractions were determined using image analyzer software and the ASTM standards. Vickers microhardness measured using a 0.3 N (300 gf). Tensile tests and sub-size Charpy impact tests at -20ºC FVA Results and Discussion Ice brine quenching of non-deformed samples Temperature (ºC) To obtain a metastable microstructure to increase the ferrite nucleation rate during the warm rolling and in the subsequent annealing. 900ºC Quenching Ar3 800oC 740oC Ar1 550oC Warm rolling Annealing Time (s) Nital Etched, MO 50m FVA Results and Discussion Ice brine quenching of non-deformed samples Temperature (ºC) The mean prior austenite grain sized was about 10.1 m. 900ºC Quenching Ar3 800oC 740oC Ar1 550oC Warm rolling Annealing Time (s) Picral Etched, OM 50m FVA Results and Discussion Warm Rolled Microstructure Temperature (ºC) Microstructure highly deformed due to the work hardening during warm rolling, and presents islands of martensite over a ferritic matrix. 900ºC 800oC Ar3 740oC Ar1 550oC Quenching Warm rolling Annealing Time (s) Nital Etched, MO 20 m FVA Results and Discussion Warm Rolled Microstructure Rolling temperature was not enough to start recrystallization; The austenite formed in the ferrite grain boundaries. Temperature (ºC) 2% nital etched, SEM micrographs 900ºC Quenching 800oC Ar3 740oC Ar1 550oC Warm rolling Annealing Time (s) FVA Results and Discussion Intercritical and Subcritical Annealing Temperature (ºC) 550ºC, 300 s – OM and SEM respectively, nital 2% etched 900ºC Quenching 800oC Ar 3 740oC Ar 550oC Warm rolling 1 Annealing Time (s) 7200 s FVA Results and Discussion Intercritical and Subcritical Annealing Temperature (ºC) 800ºC, 300 s 900ºC Quenching 800oC Ar 3 740oC Ar 550oC Warm rolling 1 Annealing Time (s) 800ºC, 7200 s FVA Results and Discussion Intercritical and Subcritical Annealing Two types of ferrite grains were observed: polygonal ferrite grains which were formed on cooling from annealing temperature; ferrite sub-grains formed as a result of recovery and recrystallization of deformed grains. Some ferrite grains with cell dislocation structure in which recovery took place are also present; As soon as austenite become homogeneous, it has sufficient time to coalesce, providing larger MA islands. FVA Results and Discussion Intercritical and Subcritical Annealing 300 s 7200 s 550ºC 800ºC OM, LePera etched FVA Results and Discussion Intercritical and Subcritical Annealing Some elongated grains with high dislocation density; Observed: Islands and blocks of MA in the final microstructure; Minor constituents present were granular bainite and pearlite; Carbides prevail for subcritical annealing, while MA for intercritical annealing. 220 MA HV 10 210 8 200 6 190 4 180 2 0 170 0 20 40 60 80 100 120 Microharness Vickers, HV Volume Fraction of MA, % 12 Fv(800ºC) for MA practically suffers no variation with the annealing time. Annealing Time, min FVA Results and Discussion Mechanical Behavior As the annealing time increases, the hardness and tensile strength decreases… Microharness Vickers, HV 220 215 210 205 200 195 190 185 180 175 170 0 20 40 60 80 100 Annealing Time, min 120 Yield Strength - Tensile Strength, MPa o 550 C o 800 C Warm rolled sample YS - 550ºC TS - 550ºC YS - 800ºC TS - 800ºC 700 600 500 400 300 (a) 0 1000 2000 3000 4000 5000 6000 7000 Annealing Time, s FVA 8000 Results and Discussion Mechanical Behavior …whereas the average ferrite grain size increases continuously. 550ºC 800ºC 4.0 Ferrite Grain Size, m 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 0 20 40 60 80 100 120 Annealing Time, min Result of the competition between three processes taking place: I - recovery and recrystallization of ferrite; II - grain growth of recrystallized ferrite grains; III - austenite formation and their grain growth during intercritical annealing FVA Results and Discussion Mechanical Behavior The beginning of the recrystallization can be observed by an inflection in the curve of hardness versus annealing temperature at approximately 550ºC. As warm rolled Microhardness Vickers, HV 280 260 Microhardness values for specimens annealed during 1800 s at different temperatures. 240 220 200 180 160 0 100 200 300 400 500 600 700 Temperature, ºC FVA Results and Discussion Mechanical Behavior 550ºC 800ºC 30 Total Elongation, % 28 26 24 22 20 18 16 14 12 10 0 1000 2000 3000 4000 5000 6000 7000 8000 Annealing Time, s The MA constituent formation is responsible for lower yield strength of the samples annealed at 800ºC as the same way that happen in DP steels. The higher ductility for samples annealed at 800ºC can be explained in the same way. FVA Results and Discussion 550C 800C 74 Mechanical Behavior 72 Impact Energy at -20ºC, J 70 68 66 64 62 60 58 56 0 1000 2000 3000 4000 5000 6000 7000 8000 Annealing Time, s The MA constituent formation is responsible for low energies of the samples annealed at 800ºC. Annealing at 500ºC led to an increase in strength, but low values for absorbed energies. FVA Conclusion The mean ferrite grain size obtained was between 1.3 and 3.8 µm, respectively, for the highest and lowest annealing times, respectively. Reaching the maximum level of refinement about 87% with an initial austenitic grain size of 10.1 µm. The microhardness has changed from 175 to 220 VHN, that shows the influence of austenitic grain size prevail about MA volume fraction. There was an improvement of 20% on mechanical properties in comparison to initial sample (hot rolled – 187 VHN). FVA Conclusion The quenching from 900ºC led to the formation of a martensite homogeneous microstructure. The results indicates it is possible to project an alloy with tensile strength near by 630 MPa for a 300 s annealing at 550ºC or a lower value for a 7200 s annealing (570 MPa). For annealing at 800ºC these values are lower. FVA Conclusions The low carbon steel has been subjected to warm rolling followed by intercritical and subcritical annealing. The results have shown the significant refinement of ferrite grain structure and corresponding improvement in mechanical properties. The optimum combination of strength and ductility has been achieved in samples subjected to 900ºC austenitizing, quenching and then 0.66 reduction during warm rolling and 60 min annealing at 800ºC. FVA Conclusion The ferrite grain refinement led to an increase by 20% in mechanical properties compared to industrially hot rolled steel. This was accompanied by similar improvement in ductility and work hardening behaviour. FVA Special Thanks To Your attention Aknowledgements Conselho Nacional de Desenvolvimento Científico e Tecnológico CNPq Project FVA number: 400609/2004-5 FVA