The studies of nodular graphite cast iron early stages austempering

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1 ARCHIVES of FOUNDRY ENGINEERING Published quarterly as the organ of the Foundry Commission of the Polish Academy of Sciences ISSN ( ) Volume 8 Issue 4/ /4 The studies of nodular graphite cast iron early stages austempering A. Krzyńska a, *, M. Kaczorowski b a Institute of Materials Processing, b Institute of Mechanics and Design Faculty of Production Engineering, Warsaw University of Technology ul. Narbutta 85, Warszawa, POLAND *Corresponding author. address: krzynska@wip.pw.edu.pl Received ; accepted in revised form Abstract The results of early stage of ductile cast iron austempering are presented. The aim of the investigations was to look closer into the structure mechanical properties relationships of this very attractive cast material. The experiment was carried out with enriched with Cu EN-GJS grade ductile iron. The specimens were first solution heat treated 1 hour in 910 o C and then isothermally quenched for different time in molten tin at the temperature 275 o C. The mechanical properties of as cast and heat treated specimens were tested to evaluate tensile R m and yield strength R p, 0.2 and elongation A 5. Additionally hardness measurements were carried out using Brinell- Rockwell method. Structure of the specimens both as cast and after austempering was studied using conventional light microscopy. Moreover, scanning electron microscopy (SEM) was applied for fracture surface observations. It was concluded that short time low temperature austempering lead to formation martensitic microstructure characterized by very high hardness with almost zero ductility. The lack of ductility make the material very sensitive to any structure defects which work as a stress concentrators which strongly influence the strength of heat treated ductile iron specimens. Keywords: ADI, Heat treatment, Structure, Properties 1. Introduction Since 1985 when ADI was discovered it is one of the most promising iron - carbon cast alloys [1]. This is due to specific combination of high tensile and fatigue strength, toughness and wear resistance compare to the other grades of cast iron [1,2]. The most surprising example is the truck wheel made from ADI which is lighter than that from Al cast alloy [3]. The unique mechanical properties are obtained applying relative simple heat treatment involving austenitizing at the temperature o C followed by isothermal quenching at the temperature range of o C. The ADI microstructure depends on heat treatment parameters, especially temperature and time of austempering and consists of three main components: ferrite, austenite and sometimes some amount of martensite. This is very well known fact often meet in the literature in form of schema illustrating the relative proportion each component depends on time of austempering [4-6]. However it is very difficult to find in the literature the results of systematic investigations concerning the microstructure evolution during isothermal quenching of ductile cast iron. The aim of this elaboration is to present our studies directed into find out what is happening in nodular graphite cast iron while austempered at relative low temperature, especially at early stages of the austempering process? ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008,

2 2. Experimental procedure The chemical composition of ductile iron selected for the study is given in Table 1. Table 1. Chemical composition in weight % Chemical composition C Mn Si P S Cr Ni Cu Mg The specimen were cut from YII type casting. From them 4mm diameter tensile strength mini-specimens were prepared. The samples were solution heat treated 1h at 900 o C and then isothermally quenched in molten tin at the temperature 275 o C for 5, 10, 15, 30, 45 and 60 minutes. After heat treatment the specimens were grinded to remove surface layer thickness of 0.1mm, which we expected to be decarburized while solid solution heat treated. The specimen were tensile tested using Instron 1115 to evaluate yield strength R p,0.2, tensile strength - R m and elongation - A 5. For each heat treatment parameter three specimens were used. Except tensile test, Brinell hardness measurements were carried out. In this case 2.5mm steel ball loaded 35s with force F = 187.5N was used. For microstructure investigations light and scanning electron microscopy (SEM) were employed. Microstructure observations were carried out on metallographic specimens prepared using conventional grinding and polishing which were etched with 4%HNO 3 solution in C 2 H 5 OH. The microstructure was observed in Olympus IX-70 light microscope using different magnifications and observations mode. The SEM investigations were performed in LEO 1030 scanning electron microscope working at U = 20kV, using secondary electrons (SE). In this case fracture surfaces of the tensile test specimens were studied. the graphs, where the mechanical properties of as cast ductile iron were given, the tensile, yield strength and elongation after 5 min. austempering time is much lower than that as cast ductile iron. It should be noted that at the same time hardness reach a maximum value. R0,2 & Rm [MPa] Elongation A 5 [%] ,0 3,5 3,0 2,5 2,0 1,5 1,0 0, Austempering time [min] R0.2 Rm 2. Results 2.1. Mechanical testing The results of mechanical testing are given in Table 2. c. 0, Austempering time [min] Table 2. Results of mechanical testing Mechanical properties Austempering R p, 0..2 R m [MPa] A 5 [%] time [min] [MPa] HB As cast The results of mechanical testing collected in Table 2 were converted into graphs depicted in Fig. 1. As can be seen from s Brinell Hardnes Austempering time [min] Fig. 1. The changes of mechanical properties as a function of austempering time: a - tensile and yield strength, b elongation, c Brinell hardness 88 ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008, 87-92

3 2.2. Structure investigations Metallography Fig. 2 illustrate an example of typical microstructure of as cast ductile iron. Fig. 3. The microstructure of 5 min austempered ductile iron: a x200, b x1000 Fig. 2. The microstructure of as cast ductile iron: a x50, b x500 As can be seen from Fig.2 the microstructure of as cast ductile iron consists of nodular graphite precipitates embedded in almost pure pearlite matrix. However it should be mentioned that apart from nodular shape graphite some amount of degenerated form - vermicular graphite precipitates were identified. Moreover, in spite of machining the aim of which was to remove decarburized skin formed during solution heat treatment at 900 o C, very thin (0.05mm) ferrite layer was identified. In Fig.3 the microstructure of 5 min. austempered ductile iron is depicted. In this case, very fine dark color needles of martensite are clear visible. The details matrix of morphology is much better visible at higher magnification (Fig.3b). In space between needle like martensite and bainitic ferrite precipitates white areas are observed. The sequence of micrographs in Fig.4 shows the evolution of the ductile iron microstructure with time while austempered at the temperature 275 o C. In all micrographs very fine needle like microstructure of matrix is observed. It looks that amount o white areas which represent carbon stabilized austenite is decreasing with austempering time increase. It should be noted that these austenite pool are located mainly at the boundary of eutectic cells, which were showed in Fig.5. ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008,

4 c. d. Fig. 5. The microstructure of austempered ductile iron: a small magnification (x50) of 45min ADI showing distribution of eutectic cell boundaries where untransformed austenite is located, b the pool of carbon stabilized austenite in the same specimen observed at higher magnification (x1000) SEM observations e. Fig. 4. The microstructure of ductile iron after: a 10, b -15, c -30, d- 45 and e 60 minutes of austempering (x500) In Fig.6-8 the example of fracture surfaces of tensile tested specimens are presented. In Fig.6 the morphology of fracture surface of as cast ductile iron is depicted. The surface morphology is characterized with cleavage planes around graphite nodules which is typical for conventional ductile cast iron. The cleavage planes are 100 type crystallographic planes in BCC ferrite, which is like an envelope ( bull eyes ) around graphite nodules (Fig.6). The fracture surface of 5 minutes austempered ductile iron (Fig.7) differs from that showed in Fig 6. Although in this case the morphology of fracture surface is also typical for brittle material but it is characterized rather with intergranular mode of fracture than cleavage. The last micrographs show the fracture surface of 45 minutes austempered ductile iron (Fig.8). As could be expected some evidence of matrix plasticity are observed. These are the dimples which are characteristic feature for ductile materials. Depend on degree of ductility the dimple are more or less deep [7]. Considering elongation of the specimens being studied in these 90 ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008, 87-92

5 investigations we are not surprised that the depth of the dimples is not fascinating. Fig. 7. The fracture surface of 5 ductile iron after 5 min austempering at 275 o C Fig. 6. The fracture surface of as cast ductile iron- Fig. 8. The fracture surface of 5 ductile iron after 45 min austempering at 275 o C ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008,

6 3. Discussion Among the results we obtained in this study, most interesting looks to be these for 5 minutes austempering at the temperature 275 o C. First of all it is surprising that the tensile strength after short time austempering is substantially (200MPa) lower than for as cast ductile iron. Moreover, the material 5 minutes heat treated had the ultimate yield strength the same as tensile strength. It follows from this that there is no strain hardening in the specimen, what is proved through almost zero elongation (Table 2). On the other hand the hardness is maximum value for 5 min. isothermal aging at 275 o C (Fig.1c). The very rough analysis suggests that such behavior of short time austempered ductile iron is caused by extremely brittleness of the specimens. It has been confirmed by metallography investigations (Fig. 3) where needle of martensite are clear visible. However, if look closer into details of microstructure showed in Fig. 3b, we see a lot of untransformed austenite being the white matrix for martensite (Fig.9) at higher magnification (Fig.5b). Lack of the TEM observations make impossible to discuss the problem more deeply, but these are planed in future and probably will confirm the suggestion concerning the reason of extremely high hardness and brittleness of ADI in very early stage of austempering. 4. Conclusions On the basis of the experimental results including mechanical testing and structure investigations, following conclusion can be proposed: 1. The isothermal quenching at the temperature 275 o C lead to formation of moderate mechanical properties ADI. 2. Five minutes austempering lead to formation of ADI with microstructure consisting of needle like martensite in austenite matrix. 3. This ADI is characterize by very high hardness and relative low ultimate yield and tensile strength compare to that of as cast ductile iron. 4. One of the reason of very high hardness are probably residual stresses caused by martensite formation not relaxed during short time austempering at relative low temperature. 5. The practical lack of ductility of short time austempered ductile iron causes extremely brittleness of ADI making it very sensitive to stress concentration which could be involved by degenerated graphite precipitates, discontinuities, hard particles and other microstructure imperfections. References Fig. 9. The magnified fragment of microstructure showing needle of martensite in white austenite matrix This is a little surprising because austenite with FCC structure should promote ductility of short time austempered ductile iron. Nothing like this is observed in this case so it looks to us that, another reason of very high hardness and brittleness, except martensite precipitates, might be the residual stresses caused by rapid quenching, not accommodated during very short time austempering. Increase of austempering time at the temperature Ta = 275 o C allow strain relaxation and proceeding the processes of decomposition of super-cooled austenite, which according to Taran and coworkers [8], can be described as follows: a Stage I : γ(cγ o ) α + γc(γ supersaturated ) b Stage II : Stability of two phase (α + γc(γ supersaturated )) structure c Stage III: γc(γ supersaturated ) α + (ε or Fe 3 C) carbides Since the relative low temperature and short time we expected that processes taking place in stage - I can occur only. The another conclusion which can be drawn from metallographic observations is, that carbon stabilized austenite is located mainly at the eutectic cell region what is clear visible at small magnification (Fig.5a) and confirmed in micrograph taken [1] J.F. Janowiak, R.B. Gundlach, Development of Ductile Iron for Commercial Austempering, AFS Trans., 86 (1983) 377. [2] The Solrelmetal Book of Ductile Iron, RIO TINTO&Titanium INC., Montreal (Quebec) Canada, [3] [4] B.V. Kovacs: Heat Treating of Austempered Ductile Iron, AFS Transactions, 99 (1991) [5] M. Kaczorowski, A. Krzyńska, The mystery of ADI, Archives of Foundry Technology, vol. 7 (2007) [6] M. Kaczorowski, A. Krzyńska, The study of mechanical properties of structure of austempered ductile iron (ADI), Proc. 4 -th Int. Conf. on Advances in Production Engineering, APE 07, Warsaw, June 2007, [7] Metals Handbook, Ninth Edition, vol. 12 Fractography, ASM International Metals Park, Ohio, USA, [8] Ju.N. Taran, K.I. Uzlow, A.I. Kucow, Theoretical and practical aspects of ductile iron austempering, Proc. Int. Conference Ductile Iron the Chance of Polish Foundries Development, Kraków, June (1996), chapt.6, pp (in Polish). [9] M. Kaczorowski, D. Myszka, On the differences between mechanical properties and structure of ductile iron castings Austempered using conventional and direct method, Int. Journal for Manufacturing Science & Technology, vol. 7 No. 1 (2005) ARCHIVES of FOUNDRY ENGINEERING Volume 8, Issue 4/2008, 87-92

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