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1 This article appeared in a journal published by Elsevier. The attached copy is furnished to the author for internal non-commercial research and education use, including for instruction at the authors institution and sharing with colleagues. Other uses, including reproduction and distribution, or selling or licensing copies, or posting to personal, institutional or third party websites are prohibited. In most cases authors are permitted to post their version of the article (e.g. in Word or Tex form) to their personal website or institutional repository. Authors requiring further information regarding Elsevier s archiving and manuscript policies are encouraged to visit:

2 MATERIALS CHARACTERIZATION 59 (2008) Wear and oxidation behaviour of high-chromium white cast irons I. Fernández, F.J. Belzunce Higher Polytechnic School of Engineering, University of Oviedo, University Campus, Gijón, Spain ARTICLE DATA Article history: Received 20 February 2006 Received in revised form 20 March 2007 Accepted 25 May 2007 Keywords: White cast irons High-chromium Wear performance Oxidation ABSTRACT High-chromium white cast irons can attain very hard microstructures composed of intergranular chromium carbides dispersed in a tempered martensitic matrix. Two heattreated high-chromium white cast irons with different carbon contents were studied in this research work using compression at 500 C, and wear and oxidation tests at 500 and 600 C. The hot compression behaviour of these products is excellent, with high strengths and significant ductility. They also exhibited good wear and oxidation properties. Fracture micromechanisms are discussed in relation to the chemical composition and microstructure of the two alloys Elsevier Inc. All rights reserved. 1. Introduction High-chromium white cast irons are in demand for the mining, mineral processing, metallurgical and cement industries. Very high abrasive wear resistance combined with relatively low production costs make these alloys particularly attractive for applications where grinding, milling and pumping equipment is used to process materials such as ore, coal, and gravel [1 3]. Another important application of these iron alloys is the manufacture of working rolls for hot strip mills [4,5]. The typical microstructure of high-chromium white cast irons consist of chromium carbides of high hardness dispersed in a matrix which still contains a sufficient concentration of carbon to allow hardening as a result of transformation of austenite to martensite. This occurs after a quenching treatment [6]. These materials, after tempering, are used in ambient temperature services and also at moderate temperatures (below 500 C). The shaping of all these products is carried out by means of casting techniques, applied from the liquid state. These hypoeutectic cast irons start their solidification with the nucleation of austenite dendrites and then continue with the formation of the eutectic constituent γ+m 7 C 3. During cooling, significant quantities of the same carbides precipitate as a result of reduction in carbon solubility [7,8]. Heat treatment of these products consists of austenitization at a high enough temperature to dissolve most of the carbides that have precipitated in the previous cooling. A high-alloyed austenite with high carbon content is thus obtained. This is partially transformed into martensite by an appropriate quench. However, a significant fraction of retained austenite remains after the hardening treatment and must be completely eliminated by applying two or more tempering heat treatments. In the course of these tempering treatments, substantial structural hardening takes place (secondary hardening), resulting from a uniform precipitation of very fine carbides, along with the transformation of retained austenite to martensite. The tempering temperature limits the maximum service temperature allowed for the Corresponding author. address: inesfp@uniovi.es (I. Fernández) /$ see front matter 2007 Elsevier Inc. All rights reserved. doi: /j.matchar

3 670 MATERIALS CHARACTERIZATION 59 (2008) Table 1 Chemical composition of the product (wt.%) C (wt.%) Mn (wt.%) Si (wt.%) Cr (wt.%) Ni (wt.%) Mo (wt.%) V (wt.%) P (wt.%) S (wt.%) Fe (wt.%) HC b0.04 b0.02 Bal. LC b0.04 b0.02 Bal. product. After two or even three tempering treatments, final room temperature hardness of between 600 and 800 HV can be obtained [9,10]. 2. Experimental Procedure The chemical compositions of the two materials used in this study, a high-carbon high-chromium white cast iron (HC) and a low-carbon high-chromium white cast iron (LC), are shown in Table 1. These white cast irons are used in the manufacture of working rolls employed in hot strip mills. The alloys were austenized (HC at 1050 C and LC 1000 C), quenched and finally double tempered. Tempering temperatures higher than the maximum temperature that might be attained in service may always be chosen in order to assure the stability of the final microstructure. The heat-treated microstructures were observed under the scanning electron microscope and their eutectic carbide volume fraction was measured in the light optical microscope by manual point counting. The hardness of these products was determined using a Vickers indenter under a load of 30 kg. Hot compression, wear and oxidation tests were carried out on samples of both products. Hot compression tests were carried out at 500 C, in accordance with ASTM E9 and E209 standards, on specimens with a diameter and length of 5 mm and 6 mm respectively, under a strain rate of 1 mm/min. These tests were carried out with the aid of a furnace equipped with a temperature controller. The specimens were heated at a rate of 5 C/min until they reached 500 C. This temperature was then maintained for 30 min before commencement of the compression test. Subsequently, a similar test without a specimen was carried out under the same conditions to determine the deformation behaviour of the unit blocks and bars used to apply the load and thus obtain the real deformation of the specimen by difference. Wear tests were also performed under sliding conditions. These wear tests were carried out according to ASTM G77 standards on parallelepipedic mm 3 specimens. The tribometer employs a counterspecimen disk of 50 mm in diameter (AISI 1043) that rotates at a constant speed against a stationary test block (specimen). The test block is loaded against the rotating disk for a specified number of revolutions. The testing parameters selected are given in Table 2, where the lineal velocity was calculated using the mean rotation radius All these tests were carried out under dry conditions at room temperature. After every 1000 m of sliding distance, the specimens were weighed by means of a precision balance, subsequently cleaned with acetone and finally installed once more in the tribometer to proceed with the test until its conclusion, after completing 7000 m. Finally, oxidation tests were carried out at 500 and 600 C (in air) in a laboratory furnace on specimens measuring mm 3, which were first metallographically polished (on all their sides) and washed in acetone. The oxidation kinetics Fig. 1 Microstructure of the high-carbon high-chromium cast iron. Table 2 Wear tests parameters at room temperature Angular velocity [rpm] 382 Linear velocity [m/s] 1 Sliding distance between two weight [m] 1000 measurements Number of cycles between two weight [revolutions] 6350 measurements weight Total number of cycles of each test [revolutions] 44,450 Total sliding distance of each test [m] 7000 Applied load [N] 158 Fig. 2 Microstructure of the low-carbon high-chromium cast iron.

4 MATERIALS CHARACTERIZATION 59 (2008) Fig. 3 Hardness as a function of tempering temperature. was followed by weight gain measurements at different time intervals up to a maximum oxidation time of 80 h. At the end of the oxidation tests, the specimens were examined using X-ray diffraction. Three different specimens have been used in the case of compression and wear tests, and six specimens for the evaluation of the oxidation behaviour. All the specimens used in the experimental tests were observed under a scanning electron microscope in order to determine the degradation processes and the different failure micromechanisms. Fig. 4 Failure surfaces in 500 C compression tests for the high-carbon high-chromium cast iron (200 ). 3. Results 3.1. Microstructure Different tempering temperatures (between 500 and 600 C) were used with the aim of modifying the final hardness of the products within a practical range. Figs. 1 and 2 show the microstructure of the high-carbon and low-carbon highchromium cast irons, respectively. These are characterized by a martensitic phase with small carbides that have precipitated in the dendrites produced during original alloy solidification. These dendrites are surrounded by intergranular eutectic carbides of the M 7 C 3 type. The eutectic carbide volume fraction measured under the light optical microscope by manual point counting was found to be 14% for the lowcarbon iron and 25% for the high-carbon iron. Fig. 3 shows the variation in hardness in the two heattreated cast irons with the tempering temperature (two temperings, 5+5 h). From these data, the tempering heat treatment that gives the highest hardness in each product was selected: a double tempering at 525 C for the low-carbon cast iron and a double tempering at 500 C for the high-carbon cast iron, which produce hardness values of 703 and 788 HV, respectively. No significant microstructural differences were observed with the tempering temperature. Fig. 5 Failure surfaces in 500 C compression tests for the low-carbon high-chromium cast iron (200 ) Hot Compression Results Table 3 shows the results obtained in the compression tests for both materials. These results have been corrected as described in the experimental procedure section in order to obtain true stress deformation curves. Table 3 Results of the compression tests Material HV σ R (MPa) e R (%) HC LC Fig. 6 Failure surfaces in 500 C compression tests for the high-carbon high-chromium cast iron (1000 ).

5 672 MATERIALS CHARACTERIZATION 59 (2008) Fig. 7 Failure surfaces in 500 C compression tests for the low-carbon high-chromium cast iron (1000 ). Fig. 10 Worn surface after the wear test (high-carbon white cast iron). appearance of fracture on the high-carbon and low-carbon high-chromium white cast irons is shown in Figs. 4, 5, 6 and 7. In both cases, some plastic deformation is observed along with signs of heavy surface sliding. Both the dendritic and carbide regions appear flattened, presenting a quite uniform fracture surface pattern. The high stiffness and extreme hardness of the carbides present in these microstructures limit their deformation and promote failure along the weakest phase (tempered martensite). Small microcavities are also clearly seen in Fig. 8 in the dendritic phase as a consequence of the extraction of the very small carbides in the course of the fracture process. Fig. 8 Detail of the failure surface in 500 C compression tests (HC cast iron). The excellent behaviour displayed by these high-chromium white cast irons in the compression tests carried out at 500 C is worth highlighting. This was characterized by very high values of compressive strength, along with a relatively ductile behaviour. HC cast iron has higher compressive strength but lower ductility as a result of its higher carbon and carbide contents. Failure of hot compression specimens always took place by smooth fracture on a plane at 45 to the axis of load application, i.e., the maximum shear stress plane. The general 3.3. Wear Performance Fig. 9 presents the results of the wear tests carried out on the two materials under a normal load of 158 N. Both materials presented a very stable behaviour, as the data obtained are linear, corresponding to constant wear rates along the entire sliding distance. It was also observed that high-carbon white iron has a better wear behaviour than low-carbon white iron as a result of its higher hardness and greater volume fraction of chromium carbides. After the complete test sliding distance Fig. 9 Wear (cumulative weigh loss) against sliding distance. Fig. 11 Worn surface after the wear test (low-carbon white cast iron).

6 MATERIALS CHARACTERIZATION 59 (2008) Fig. 12 Oxidation curve (still air) of the HC white cast iron. Fig. 15 Oxidized surface (HC white cast iron, 600 C). Fig. 13 Oxidation curve (still air) of the LC white cast iron. of m, the wear weight loss of the former is approximately half that of the latter. The dimensionless wear coefficient, K [11], of the two materials may be obtained using their known densities (ρ HC = 7.4 g/cm 3, ρ LC = 7.7 g/cm 3 ), their hardness values, H (788 HV HC and 703 HV LC ), and the applied load (F=158 N): V=d ¼ðW=qÞ=d ¼ KF=H where W and V are the weight and volume loss, respectively, and d is the sliding distance. The obtained K value is lower for the high-carbon highchromium white cast iron (K HC = versus K LC = ). This means that under the same applied load (F) and the same product hardness (H), high-carbon high-chromium white cast irons exhibit significantly lower wear losses. In the course of these sliding wear tests, damage always started in both materials as a strong plastic deformation under compression, occurring in the contact zone between the specimen and the counterspecimen disk. Location of crack initiation is illustrated in Figs. 9 and 10, The deformation flow lines and crack growth are clearly seen. The significant deformability on the alloys shown in Figs. 10 and 11 may be rationalized by the quite high ductility measured in the 500 C compression tests (6 8%). Room temperature compression behaviour of these materials is not expected to be very different from the results obtained at 500 C Oxidation Results Figs. 12 and 13 show the weight gain per unit area of the specimens of both materials oxidized in still air at 500 C and 600 C during exposure times of up to 80 h. All the specimens follow parabolic oxidation kinetics. After 80 h at 500 C, oxidation is minimal. However, after 80 h at 600 C, small clusters of oxide begin to form, even though oxidation continues to be very low. In the case of lowcarbon white iron, oxides begin to appear in the interdendritic regions associated with the carbide network (Fig. 14), whereas in the high-carbon white iron, the oxide formation is clearly lower, due to the higher chromium content of this iron (Fig. 15) and can only be resolved at higher magnification in the form of 1- to 5-μm-long needles (Fig. 16). Fig. 14 Oxidized surface (LC white cast iron, 600 C). Fig. 16 Detail of the oxidized surface (HC white cast iron, 600 C).

7 674 MATERIALS CHARACTERIZATION 59 (2008) Conclusions The present work, aimed at studying the influence of carbon on the simulated in-service properties of heat-treated highchromium white cast irons, led to the following conclusions: The 500 C hot compression behaviour of heat-treated lowand high-carbon white cast irons is excellent: their strengths are very high and a significant ductility was also observed. The wear resistance of high-chromium white cast irons is inversely proportional to the hardness of the product. The wear micromechanism on both materials takes place by virtue of a strong plastic deformation under compression, which ultimately leads to necking and final cracking into small particles. High-carbon white cast iron, with a higher volume fraction of chromium carbides has a higher strength and a lower ductility and is also more wear-resistant than low-carbon white cast iron. Low-carbon white cast iron and specially high-carbon white iron (higher chromium content) hardly oxidize at 500 and 600 C in still air. The good oxidation resistance of these alloys is justified on account of their high-chromium content. [3] Dogan ON, Hawk JA, Laird G. Solidification structure and abrasion resistance of high chromium white irons. Metall Mater Trans A Phys Metall Mater Sci June 1997;28A. [4] Hwang KC, Lee S, Lee HC. Effects of tempering temperature on wear resistance and surface roughness of a high speed steel roll: Part I. Microstructural analysis. Mater Sci Eng A Struct Mater Prop Microstruct Process 1998;254:282. [5] Hwang KC, Lee S, Lee HC. Effects of tempering temperature on wear resistance and surface roughness of a high speed steel roll: Part II. Fracture behaviour analysis. Mater Sci Eng A Struct Mater Prop Microstruct Process 1998;254:296. [6] Davis JR, editor. Cast irons, ASM Specialty Handbook. Materials Park: ASM International; 1996, pp [7] Powell GLF, Bee YJV. Secondary carbide precipitation in an 18% Cr 1% Mo white iron. J Mater Sci 1996;31: [8] Bedolla-Jacuide A, Arias L, Hernández B. Kinetics of secondary carbides precipitation in a high-chromium white iron. J Mater Eng Perform 2003;12(4): [9] Dogan ON, Hawk JA, Laird II G. Solidification structure and abrasion resistance of high chromium white irons. Metall Mater Trans 1997;28A: [10] Zhang MX, Kelly PM, Gates JD. The effect of heat treatment on the toughness, hardness and microstructure of low carbon white cast irons. J Mater Sci 2001;36: [11] Chattopadhyay R. Surface wear. Analysis, treatment, and prevention. United States: ASM International; pp. REFERENCES [1] Tabrett CP, Sare IR. Fracture toughness of high-chromium white irons: influence of cast structure. J Mater Sci 2000;3: [2] Zhang MX, Kelly PM, Gates JD. The effect of heat treatment on the toughness, hardness and microstructure of low carbon white cast irons. J Mater Sci 2001;36:

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