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Materials and Design 21 2000.

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Effect of cooling rate on dendrite arm spacing DAS/ , eutectic cell count ECC/ and ultimate tensile strength UTS/ of austempered chilled ductile iron
Joel HemanthU,1
Department of Mechanical Engineering, Siddaganga Institute of Technology (S.I.T.), Tumkur-572 103, Karnataka, India Received 4 June 1999; accepted 12 July 1999

Abstract This paper presents the results obtained and the deductions made from a series of microstructural studies and strength tests involving austempered chilled ductile iron which was sand cast using a variety of end chills metallic, non-metallic, water-cooled and sub-zero, respectively.. The effect of cooling rate on the dendrite arm spacing, eutectic cell count and the ultimate tensile strength were evaluated. It was found that the ultimate tensile strength is highly dependent on the rate of chilling which determines the dendrite arm spacing and the eutectic cell count of the material. Attempts were also made in this paper to explain these effects and to correlate the UTS with DAS and ECC. Moreover, it was found that UTS decreases as DAS increases and UTS increases as ECC increases. 1999 Elsevier Science Ltd. All rights reserved.
Keywords: Chill; Austemper; Ductile iron

1. Introduction Chills are used by the foundry engineer for the production of quality castings w1x. The use of chills in molds results in controlled directional solidication and forms the required temperature gradient which assists in effective feeding. They also increase the feeding efciency of risers and minimize the formation of hot spots. In recent years austempered ductile iron has attracted much attention because of its high strength, good shock resistance and a high capacity for deforma-

Tel.: q91-816-282-990; fax: q91-816-282-876. Dr Joel Hemanth obtained his B.E. and M.E. degrees in Mechanical Engineering, M.B.A. degree in Personal Management from University of Bangalore and Ph.D. degree from University of Mysore, India. He is currently the Professor of Mechanical Engineering at Siddaganga Institute of Technology, Tumkur, Karnataka, India. Currently he is reading his Post Doctoral studies and his area of research is Metallurgical Sciences.
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tion. However, ductile iron solidies in a pasty manner and is prone to unsoundness. Unsoundness or porosity in castings of this metal is caused by its poor feeding characteristics. However, the distributed microporosity caused by insufcient feeding during solidication can be minimized more effectively by the use of chills which in turn increases strength of ductile iron and renes microstructure due to variation in DAS and ECC. Hemanth et al. w2x concluded from their investigation that the inuence of a higher cooling rate during solidication is normally responsible for superior properties of chilled cast iron. For a metallurgist, there is sufcient information available on the DAS and ECC of ordinary cast iron cast using sand molds. However, there is a dearth of information on the DAS and ECC and the effect of these two on the strength of austempered chilled ductile iron cast using various types of metallic and nonmetallic chills including water-cooled and sub-zero chills. This has led to a series of experiments to nd the

0261-3069r00r$ - see front matter 1999 Elsevier Science Ltd. All rights reserved. PII: S 0 2 6 1 - 3 0 6 9 9 9 . 0 0 0 5 2 - 7

J. Hemanth r Materials and Design 21 (2000) 1 8

effect of DAS and ECC on the strength of various types of austempered chilled ductile iron. The reason behind the selection of this series of austempered chilled ductile iron for the present investigation is that a wide range of UTS values can be obtained with different DASs and ECCs. Moreover, using such a chilling technique, a low-grade iron can be converted into one of the superior qualities depending on the mode of solidication and hence the DAS and ECC. 1.1. Past research 1.1.1. Chilling of cast iron The inuence of very high cooling rates in producing ne structures offers the possibility for the future development of high-strength cast alloys w3x. The undercooling of a melt to a lower temperature increases the number of effective nuclei relative to the growth rate, the latter being restricted by the rate at which the latent heat of crystallization can be dissipated w4x. The rening effect of an enhanced cooling rate applies both to primary grain size and to substructure. Thus, there is a marked effect upon dendrite arm spacing and eutectic cell count over a wide range of cooling rates. The effect of chills on the solidication characteristics of cast iron has been studied by Bishop et al. w5x. Berry w6x showed the importance of time on the solidication of castings. The eutectic solidication starts at certain locations and continues by radial growth with the simultaneous separation of graphite and austenite from the melt. Furthermore, the lower the temperature of formation i.e. the greater the amount of under-cooling., the ner is the graphite formed. Sun and Loper w7x showed that intensive super-cooling both constitutional and thermal. in front of the chilling interface results in the development of cellular dendritic growth of the graphite into a form recognized as exploded graphite. The microstructures of gray iron and ductile irons are determined by cooling rate, composition, nucleation and growth conditions prevailing during solidication and the transformation behavior of austenite during cooling through the critical temperature range w8x. The dendritic structure in cast irons may be signicantly rened by selected additions to the melt. The effect of this renement is to increase the number of cells and to reduce the spacing of the dendrite arms of the austenite dendrites w9x. 1.1.2. Dendrite arm spacing and eutectic cell count Dendrite arm spacing in alloys that solidied dendritically have been investigated by Alexander and Rhines w10x, Michel and Bever w11x and Howard and Mondolfo w12x. Results of these investigations are in general agreement. Pande et al. w13x concluded from their investigation that secondary dendrite arm spacing can easily be related to cooling rate. Baker w14x observed

that both fracture toughness and tensile strength of cast iron decreased linearly with increasing eutectic cell size. Suzuki and Kayama w15x concluded from their investigation that conrmation of graphite nucleation out of residual graphite is by means of eutectic cells and the eutectic cell number is an index to nucleation frequency. Thus cell growth conforms to and is superimposed on a dendritic structure that solidies rst. The dendritic structure that solidies hosts the cells and therefore can have a major effect on cell nucleation and growth w16x. Ruff and Wallace w17x showed that, by increasing the eutectic cell count, the effective span and stress concentration effect of the graphite can be reduced and hence improve the tensile strength. A suggested classication of cell size has been dealt with in detail by Dawson and Oldeld w18x. 1.1.3. Solidication, structure and austempering of ductile iron Solidication of ductile iron was examined in detail by Dumpy and Pellini w19x. They found that a large number of small graphite nodules were formed at the beginning of the eutectic arrest and counts showed their number is xed at the start of eutectic freezing. The principal factor is the structural role played by spheroidizing elements when incorporated in the graphite lattice and their effects on the kinetics of growth w20x. The results of unstinted efforts by various researchers in the development of ductile irons include different microstructures viz. pearlite, austenite, martensite and bainite. Of course, the bainitic ductile iron with high strength and toughness has added new directions to the already popular ductile iron family w21x. The morphology of bainite and techniques for producing bainitic ductile irons, structure property relations, etc., have also been studied during recent years w22x. The demand for a tougher, harder and stronger matrix led to the development of bainitic matrix and such a matrix can be developed through a heat treatment known as austempering, in which the matrix is transformed from austenite to bainite directly without entering the martensitic stage at any time w23x. The benecial use of this heat treatment has encouraged many researchers to apply it to ductile iron so that it could become a tougher, more wear resistant and stronger material w24x. Ductile iron subjected to an austempering treatment is often referred as austempered ductile iron ADI. in most international forums. 1.2. Rele ance of the research Ductile irons have the potential to replace other materials in many signicant engineering applications. The requirements concerning safety and reliability are always on the increase and therefore the effect of dendrite arm spacing and eutectic cell count on tensile

J. Hemanth r Materials and Design 21 (2000) 1 8 Table 1 Chemical composition of the ductile iron tested Element Amount %wt.. C 3.42 Si 1.8 Cu 1.5 Mg 0.05 Mn 0.41 S 0.04 P 0.08 Fe Balance

strength is ever more crucial when ductile iron is chilled using various types of metallic and non-metallic chills including water-cooled and sub-zero chills. Because there are presently no published data on this topic, the present research is intended to ll the void.

Table 2 UTS and microstructure at the chill end. of castings chilled using various chills a Specimen Chill used UTS MPa. 287.24 311.43 346.67 362.69 Microstructure

2. Experimental procedure 2.1. Production of the material Ductile iron specimens of the composition shown in Table 1 were cast at 1440 C in the form of ingots using different types of chills. They shall henceforth be designated as specimens A, B, C and D as shown in Table 2. Apart from the usual alloying elements such as Si, Mn, S and P, copper was also added to improve machinability as well as to act as a grain rener. The molds for plate type castings 225 = 150 = 25 mm AFS standard. were prepared using silica sand with 5% bentonite as binder and 5% moisture. The melts were carried out using a medium frequency coreless induction furnace. A base metal analysis, generally of 3.42% C and 1.8% Si, was produced and superheated to 1500 C prior to tapping into a pre-heated 20-kg

A B C D
a

Si-Carbide Steel Water-cooled Sub-zero

8% Cem in bainite 31% Cem in bainite 56% Cem in bainite 71% Cem in bainite

Austempering temperature: 300 C; austempering time: 3 h. Note: Cems cementite.

capacity hand shank containing nodularizing alloy Mg. using the sandwich technique. Prior to casting, an inoculating addition Ferro-Si to promote uniform structure. and other alloying elements were stirred into the molten metal using a graphite spoon. The treated metal was poured directly into the mold at a temperature of 1440 C. Fig. 1 shows the diagram of the mold used for producing the various ingots cast with water-cooled and liquid nitrogen cooled copper chills specimens C and D.. The same type of mold was also used for other specimens specimens A and B. except that no liquid

Fig. 1. Mold used for producing chilled ductile iron.

J. Hemanth r Materials and Design 21 (2000) 1 8 Table 4 DAS, ECC and UTS of sub-zero chilled ductile iron along the length of the casting a Specimen location distance from chill end, mm. 25 chill end. 75 125 175 225 riser end.
a

Table 3 DAS, ECC and UTS of water-cooled chilled ductile iron along the length of the casting a Specimen location distance from chill end, mm. 25 chill end. 75 125 175 225 riser end.
a

DAS m. 3 5 6 10 10

ECC cellsrcm2 . 165 151 108 93 102

UTS MPa. 331.60 280.17 255.14 248.35 258.23

DAS m. 1 1 7 9 9

ECC cellsrcm2 . 185 174 108 95 101

UTS MPa. 364.63 298.34 254.64 255.35 263.43

Austempering temperature: 300 C; austempering time: 3 h.

Austempering temperature: 300 C; austempering time: 3 h.

was passed through the chills. The molten alloys were cast in the mold and were cooled from one end by the chill. In the case of water-cooled and liquid nitrogen cooled chills arrangements were made to circulate water at 23 C. and liquid nitrogen at y60 C., respectively, through the copper chill. Austempering comprised of two stages, viz., heating the plate castings to the austenizing temperature of 950 C followed by rapid quenching and holding in a salt bath maintained at a temperature of 200 400 C for different time intervals. 2.2. Microstructural examination and strength testing The specimens for microstructural and strength stud-

ies were taken all along the length of the casting. Microstructural studies to observe dendrite arm spacing were done on nely polished specimens using a scanning electron microscope and a Neophot-21 optical microscope under different magnications. Various etchants were tried but Nital 2%. proved to be the best and therefore used. Eutectic cell count measurements were carried out on polished specimens at low magnication 5 = . using Steads reagent as the etchant. Tensometer specimens were prepared for strength testing using an Instron testing machine. and the tests were performed in conformance with American Foundrymen Society AFS. standards.

Fig. 2. Relationship between UTS and DAS for different specimens austempering temperature: 300 C; austempering time: 3 h..

J. Hemanth r Materials and Design 21 (2000) 1 8

Fig. 3. Relationship between UTS and ECC for different specimens austempering temperature: 300 C; austempering time: 3 h..

3. Results and discussions Table 2 shows the experimental results of the strength tests done on castings using various chills each 25 mm thick. as well as the microstructures observed. To show the typical relationship between DAS, ECC and the UTS shown in Figs. 2 and 3. along the length of the casting from the chill end to the riser end, these values for specimens A, B, C and D are listed in Tables 3 and 4, respectively. 3.1. Microstructural examination The differences in associated graphite, its randomness and matrix structure for various specimens are shown in Figs. 4 and 5. Fast cooling produces ne and

highly oriented dendrites, while slow cooling produce large and coarse dendrites. Therefore solidication over a temperature range is the primary requirement for dendrite growth. Primary austenite dendrites readily grow from the liquidus down to the eutectic temperature. Growth of dendrites may also continue concurrently with the eutectic as the temperature decreases through the eutectic range to the solidus. Thus, undercooling in case of water-cooled and sub-zero chilled ductile iron may lead to longer dendrites and higher interaction. Hence the eutectic cells solidify around these austenite dendrites and in this manner the entire microstructure is affected by the number and size of the dendrites. Primary austenite dendrites were observed in all the specimens tested Figs. 6 and 7., with variations in

J. Hemanth r Materials and Design 21 (2000) 1 8

Fig. 4. Microstructure of specimen C cast with water-cooled chill; austempering temperature: 300 C; austempering time: 3 h; magnication: 500 = ..

Fig. 6. Dendrite arm spacing of specimen C cast with water-cooled chill; austempering temperature: 300 C; austempering time: 3 h; magnication: 1000 = ..

pattern occurring as a result of differences in the rate of cooling. For each specimen, the structure of the dendrites was analyzed by determining the dendrite arm spacing, the average dendrite length, the dendrite interaction and the directionality. Marked changes were also seen in the graphite morphology as the rate of cooling was varied using different types of chill. Primary austenite dendrites would be expected to develop within each of the castings produced in such a manner that their solidication is dependent on the rate of under-cooling. For ductile iron of hypoeutectic composition selected for the present investigation, because of the cooling provided during solidication, it is believed that the dendrites form prior to nucleation and growth of the eutectic. The eutectic then completes solidication by lling in the areas surrounding the dendrites. The resulting structures of transformed primary austenite dendrites traverse a number of eutectic cells, which contain both graphite and transformed eutectic

austenite. However, in the present investigation, the observed formation of primary dendrites prior to the solidication of graphite can be explained by the relatively fast cooling and the under-cooling needed for graphite nucleation. In addition, dendritic interaction, which is a visual estimate of the percentage area of dendrites intersecting in a eld of view, varied in the specimens tested. The largest degree of dendritic interaction was observed in ductile irons chilled using high cooling rates. Figs. 4 and 5 are the microstructures of different specimens at the chill end. chilled using various type of chills specimens C and D., in which a high concentration of cementite can be seen in the bainitic matrix. 3.2. Dendrite arm spacing and eutectic cell count Solidication of ductile iron begins with the crystallization of primary graphite. The primary graphite develops as straight graphite nodules which are totally surrounded by the liquid. The composition of the remaining liquid shifts toward the eutectic where the liquid is believed to solidify in a manner similar to that of the eutectic although the primary graphite may inuence the size of the eutectic cell and the distribution of the eutectic graphite. Close observation of the photomicrographs Figs. 6 and 7. show the existence of cored dendrites dark areas. and inter dendritic eutectic light areas.. The DAS increases as the cooling rate decreases because there is less time available for diffusion of the solute. Hence, it is believed that diffusion controls the DAS, a deduction conrmed by the work of other researchers w11x. It is generally accepted that the eutectic cell count is an indication of the number of nuclei on which solidication has proceeded. Microphotographs of eutectic cells of water-cooled and sub-zero chilled ductile iron

Fig. 5. Microstructure of specimen D cast with sub-zero chill; austempering temperature: 300 C; austempering time: 3 h; magnication: 500 = ..

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Fig. 7. Dendrite arm spacing of specimen D cast with sub-zero chill; austempering temperature:300 C; austempering time: 3 h; magnication: 1000 = ..

Fig. 9. Photomicrograph of eutectic cells of specimen D cast with sub-zero chill; austempering temperature: 300 C; austempering time: 3 h; magnication: 5 = ..

are shown in Figs. 8 and 9, respectively. The number of nuclei available for solidication of sub-zero chilled ductile iron is higher than the number of nuclei available for water-cooled chilled ductile iron, but a smaller effect in the case of silicon carbide chilled ductile iron. In other words, the nucleation conditions in case the of sub-zero and water-cooled chilled ductile iron are completely different from those of silicon carbide and steel chilled ductile irons, the surprising fact for this variation is the under-cooling effect due to chilling. Perhaps the most important fact to recognize that the cell structure develops after the precipitation of austenite dendrite structure that solidies rst. The dendritic structure hosts the cells and therefore can have a major effect on cell nucleation and growth. Therefore, the general picture of solidication of chilled ductile iron with various eutectic cell counts can be summarized as follows.

The solidication of silicon carbide chilled ductile iron will start on a low number of nuclei as compared against the chilled water-cooled and sub-zero. ductile iron which reected with large number of nuclei resulting in high eutectic cell count. Since the growth conditions in the liquid are favorable, these nuclei will start growing as soon as the temperature drops below the equilibrium temperature in case of silicon carbide chilled ductile iron and with maximum under-cooling in case of water-cooled and sub-zero chilled ductile iron. 3.3. Ultimate tensile strength (UTS) Table 2 shows the UTS of the ductile iron specimens at the chill end. chilled using various types of chills. Figs. 2 and 3 are plots showing the relationship between the UTS with DAS and ECC for the water-cooled specimen C. and the liquid nitrogen cooled specimen D.. It can be seen from Fig. 2 that the UTS decreases monotonically as the DAS increases, i.e. moving away from the chill end towards the riser end. Tensile tests reveal that the higher strengths are associated with larger dendrite interaction of under-cooled irons. Higher dendritic interaction areas reect the inter weaving of dendrites through eutectic cells. Since dendrites are formed from primary austenite and do not contain carbon, they have higher fracture stress than eutectic liquid that decomposed to form austenite and eutectic graphite. Therefore, austenite dendrite interaction is also observed to be a major factor affecting the UTS of the material. It can be seen from Fig. 3 that UTS increases as eutectic cell count increases until the cells become compacted refer to Fig. 9.. A difference is observed between the eutectic cell count of chilled ductile iron

Fig. 8. Photomicrograph of eutectic cells of specimen C cast with water-cooled chill; austempering temperature: 300 C; austempering time: 3 h; magnication: 5 = ..

J. Hemanth r Materials and Design 21 (2000) 1 8

cast using silicon carbide and sub-zero chill, this difference is small as compared between water-cooled and sub-zero chilled ductile iron. It is generally acknowledged that most of the mechanical qualities of cast iron can be best represented by its tensile strength. Optimum tensile strength in the present investigation is obtained by increasing the amount of graphite-free area in most cases, primary austenitic dendrites., rening eutectic cell size and establishing the bainitic matrix. This is consistent with the deductions made by other researchers w25,26x. Treating the base metal with commercial inoculants and neutralizing certain elements will inhibit graphite nucleation and can result in the formation of more eutectic cells. In addition to the above, when the rate of cooling is slow, i.e. when there is no super-cooling effect, the UTS approaches that of fully annealed ductile iron.

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w1x Hemanth J, Seah KWH, Sharma SC. J Mater Sci 1996;30:4986. w2x Hemanth J, Seah KWH, Sharma SC. WEAR 1996;192:134. w3x Hemanth J, Seah KWH, Sharma SC. J Mater Design 1995;16:175. w4x Hemanth J, Seah KWH, Sharma SC. J Mater Sci 1998;33:23. w5x Bishop HK, Brandt FA, Pillini WS. Trans Am Foundryman Soc 1951;59:435. w6x Berry JT. Trans Am Foundryman Soc 1970;78:421. w7x Sun GX, Loper CR. Trans Am Foundryman Soc 1983;91:841. w8x Wallace JF. Trans Am Foundryman Soc 1975;88:363. w9x Church N, Wieser PF, Wallace JF. Trans Am Foundryman Soc 1966;74:113. w10x Alexander BH, Rhines MB. Trans AIME 1950;188:1267. w11x Michael AB, Bever MB. Trans AIME 1950;188:47. w12x Howard JA, Mondolfo LF. Acta Metall 1962;10:1037. w13x Pande KS, Pande SK, Premkumar P. Indian Foundry J 1979;25:4. w14x Baker TJ. Trans Am Foundryman Soc 1978;86:345. w15x Suzuki K, Kayama N. Trans Am Foundryman Soc 1982;90:423. w16x DeHoff RT, Rhines FN. Trans Am Foundryman Soc 1981; 89:335. w17x Ruff GF, Wallace JF. Trans Am Foundryman Soc 1977;85:179. w18x Dawson JV, Oldeld W. BCIRA J 1960;8:221. w19x Dumpy RD, Pillini WS. Trans Am Foundryman Soc 1952; 60:775. w20x Minkof I. Trans Am Foundryman Soc 1968;72:18. w21x Dorazil E. J Int Cast Metals 1982;7:52. w22x Muthukumaraswamy S. Indian Foundry J 1992;39:23. w23x Voigt RC, Loper CR. 1st Int Conference on ADI, Chicago 1984;84:23. w24x Dodd J, Gundlach RB. BCIRA Conference on Development for Future Foundry, University of Warwick, 1984. w25x Le Rolland P, Plenard E. Foundrie 1956;131:477. w26x Fuller AG. BCIRA J 1956;11:358.

4. Conclusions Analysis of data on austempered chilled ductile iron chilled using various types of chill shown that the cooling rate has a marked effect on DAS, ECC and UTS. It was found that UTS decreases as DAS increases and UTS increases as ECC increases. The UTS, however, increases as the rate of cooling increases, showing a direct relationship with ECC and inverse relationship with DAS. If the rate of cooling is reduced beyond a certain point, the UTS approaches an asymptotic value, which is the UTS of fully annealed ductile iron.