Colloquium 19-20 April 2011 Institute for Microstructural and Mechanical Process Engineering: The University of Sheffield INTRODUCTION The authors gratefully acknowledge the Ministry of National Education of Indonesian Government and Institut Teknologi Nasional Bandung for their financial support The microstructure evolution of hot work tungsten tool steel during conventional heat treatment M. Nurbanasari, P. Tsakiropoulos, and E.J. Palmiere Hot work tungsten tool steels (Group H) are developed to meet the industrial need for materials with good mechanical properties for forming operations at high working temperature. These steels are highly alloyed specially with tungsten and chromium which affects the volume fraction and nature of the carbides. The critical issue of these steels is the low toughness. They are prone to brittleness at normal working temperatures and are inclined to distort during hardening process. The carbides of these steels are very brittle and do not dissolve in austenite by heating. A choice of heat treatment process and their parameter must be considered. The potential of these steels is: Resistance to deformation at the elevated working temperature. High hot hardness, High compressive strength Wear resistance at elevated temperatures Resistance to heat checking Good machinability in the annealed condition AIM To provide data that would allow the design of tool steels with a balance of satisfactory hardness and toughness. STRATEGY Select heat treatment parameters that give combination of satisfactory hardness and toughness Investigate phase transformations during conventional heat treatment process HOT WORK TUNGSTEN TOOL STEELS 1. The main alloying elements are strong carbide formers [3] 2. Choice of proper heat treatment processes [3] 3. Create secondary hardening (SH) during heat treatment process Table 2: The chemical composition of investigated hot work tungsten tool steels (%wt): cavity 10 10 10 Fig 10 :Heat treated sample Austenizing temperature of both tool steels : 1100, 1250 o C First and second tempering temperatures respectively of both tool steels: 650, 750, 800 o C Conventional heat treatment process Fig 11: Schematic of heat treatment process AIM AND STRATEGY OF PROJECT THE STRENGTHEN OF TOOL STEEL REFERENCES HARDNESS AND XRD RESULT CONCLUSIONS MICROSTRUCTURE EXPERIMENTAL PROCEDURE Fig 12: Tempering curve of H21 472 226 214 422 247 236 0 100 200 300 400 500 600 650 700 750 800 850 Hardness (VHN) Double tempering (DT) temperature ( o C) austenising temp 1250 oC austenising temp 1100 oC 413,1 300,5 285,4 257,7 254,5 235,0 0,0 100,0 200,0 300,0 400,0 500,0 600 650 700 750 800 850 Hardness (VHN) Double tempering (DT) temperature ( o C) austenising temp 1250 oC austenising temp 1100 oC Fig 13 : Tempering curve for H23 Table 3: Hardness of as cast and as quenched condition The as quenched hardness of H23 is lower than as cast because of absence of martensite The hardness of both tool steel decreased with higher tempering temperatures because the carbide size became bigger The hardness increased during tempering process due to secondary carbides produced at this condition Higher austenizing temperatures increased the hardness of tempered samples, due to the higher dissolution of M 6 C in the austenite matrix as cast as quenched (Tg 1100 o C) as quenched (Tg 1250 o C) H21 483 574 536 H23 356 265 284 Hardness (VHN) Type of tool steel As cast condition Fig 15: SE image of cast H21 Type position V Cr Fe W phase H21 matrix 0.6±0.4 4.8±1 92±1.5 2.7±0.5 ferrite carbide 1.5 4.6 64.7 29.3 M 6 C H23 matrix 1.1±0.6 13.5±1 79.9±1 5.5±2 ferrite Carbide 1 3.9 21.2 49.5 25.3 M 6 C Carbide 2 2.5 16.2 52.2 29.1 M 6 C Table 4: EDS analysis of as cast steels (%wt) Fig 16 : SE image of as cast H23 Heat treated condition The primary carbide for both tool steels was M 6 C and was dominantly located along the grain boundaries the differences between the composition of the carbides and matrixs refer to the levels of W, Cr, V and mainly Fe Fig 18 : The microstructural changes of heat treated H21 (etchant 98 % picric acid + 2% HCl) 1. G.A Roberts. G.Krauss, Kennedy. 1998, Tool Steels, 5 th edition, ASM, Metals Park, Ohio. 2. G.F. Vander Voort., E.P. Manilova., J.R Michael. 2004, A Study of Selective Etching of Carbides in Steels, Micros. Microanal. 10(suppl 2), 76-77 3. LS.Kremnev. 2008, Alloying Theory and Its Use for Creation of Heat Resistant Tool Steels and Alloys”, Material Science and Heat Treatment, Vol.50, 18-27 4. M. Kroneis. 1979, Tungsten in Steel, in: Proc.1 st International Tungsten Symposium, Stockholm, Mining Journals Books, Ltd, London, 96-107 code position V Cr Fe W phase A1 matrix 0.7 4.0 83.3 12.0 martemper Carbide 1 1.5 3.1 28.4 67 M 6 C Carbide 2 1.1 4.1 46.0 48.8 M 6 C D6 matrix 0.7 13.4 78.8 7.1 ferrite Carbide 1 2.6 10.8 47.8 38.8 M 6 C Carbide 2 3.0 38.1 42.3 16.6 M 7 C 3 Carbide 3 3.1 40.0 38.4 18.5 M 23 C 6 Fig 19: BSE images of D6 Fig 20: SE images of A1 Table 5: EDS analysis of some heat treated samples (%wt) • The highest hardness the H21 tool steel was 472 VHN and of the H23 tool steel was 412 VHN with austenizing temperature 1250 o C and double tempered 650 o C • After double tempered process, some of the carbides were still networked and mainly located along the grain boundaries • The primary carbide for both tool steel was the M 6 C and after heat treatment the M 7 C 3 and M 23 C 6 were found in the H23 tool steel as secondary carbides DH1 :Tg 1250 o C , quenched D1: Tg 1250 o C, quenched, DT 800 o C D2: Tg 1250 o C, quenched, DT 750 o C D3 : Tg 1250 o C, quenched, DT 650 o C DH2 :Tg 1100 o C , quenched D4: Tg 1100 o C, quenched, DT 800 o C D5: Tg 1100 o C, quenched, DT 750 o C D6: Tg 1100 o C, quenched, DT 650 o C • The morphology of carbides in H23: M 6 C (FCC structure): round, rod, square, irregular M 7 C 3 (hexagonal structure): square and irregular M 23 C 6 (FCC structure): square and irregular • The distance between the carbides increased in their higher austenizing temperature • The morphology of M 6 C (FCC structure) in H21 was mostly round, irregular • After double tempering, the carbides still made a network but were less interconnected than in the cast structure • Higher austenizing temperature increased the volume fraction of the retained austenite in the as quenched condition AH1: Tg 1250 o C , quenched A1: Tg 1250 o C, quenched, DT 800 o C A2: Tg 1250 o C, quenched, DT 750 o C A3: Tg 1250 o C, quenched, DT 650 o C AH2: Tg 1100 o C , quenched A4: Tg 1100 o C, quenched, DT 800 o C A5: Tg 1100 o C, quenched, DT 750 o C A6: Tg 1100 o C, quenched, DT 650 o C Fig 9 : As cast ingot (a,b,c) and dimension of ingot in mm and sample position taken for chemical analysis and as cast microstructure (d) 1: sample taken for chemical analysis (centered 30 mm from the bottom and 120 mm from the top (size: 10x10x10 mm) 2:sample taken for as cast microstructure (size: 10x10x10mm) Fig 17:The microstructural changes of heat treated H23 (etchant:Groesbeck’s: MC and M 23 C 6 carbides are not etched and M 7 C 3 – M 6 C in blue or yellow [2]) Fig 14 : Diffraction pattern of as cast and heat treated H21 (a) and H 23 (b) tool steel (b) (a) code phase JCPDS code phase JCPDS code phase JCPDS M 6 C : Fe 3 W 3 C 41-1351 M 7 C 3 : (Cr,Fe) 7 C 3 5-720 g retained 52-512 M 23 C 6 : Cr 23 C 6 85-1281 Ferrite (a) 54-331 6-696 martensite 44-1292 Fig 3: Hot Forging die (H23) [1] Fig 4: Die casting die (H21) [1] Fig 5: Vacuum Remelted Hot Work Tool Steel (BOHLER W403 VMR) Fig 1: Classification of tool steel (AISI) Fig 6 : Schematic heat treatment process for tool steel Fig 7: Secondary hardening mechanism during tempering process Fig 2: Schematic effect of tungsten on hardness [4] • The main eutectic carbide in the microstructure of both tool steel was Fe 3 W 3 C • The as quenched H21 tool steel contained Fe 3 W 3 C and martensite and the quenched H23 contained ferrite, g retained , FeW 3 C 3 and (Cr,Fe) 7 C 3 • After second tempering, the X-ray analysis of H23 confirmed the presence of undissolved Fe 3 W 3 C, (Cr,Fe) 7 C 3 , Cr 23 C 6 and ferrite meanwhile for H21 only Fe 3 W 3 C with tempered martensite as matrix Why double tempered ? Fig 8: Microstructural changes during tempering process Chemical composition analysis using XRF method Casting of material into 4 ingots (Vacuum induction furnace and slow cooling) SH (a) (b) (c) (d) 75 10 70 120 mm Top of ingot cavity 10 30 120 285 cavity 2 top bottom bottom top steel denotation Position C Si Mn P S Cr Mo Ni W V Co H21 Top 0.24 0.33 0.25 0.023 0.022 3.18 <0.02 0.3 7.7 0.43 <0.02 Bottom 0.27 0.32 0.25 0.028 0.022 3.13 <0.02 0.3 7.43 0.42 <0.02 H23 Top 0.33 0.49 0.36 0.014 0.029 12.35 <0.02 0.4 12.3 1.16 <0.02 Bottom 0.36 0.49 0.36 0.014 0.032 12.33 <0.02 0.4 12.47 1.16 <0.02 matrix matrix matrix matrix matrix matrix