Transactions on Engineering Sciences vol 17, 1997 WIT Press, ISSN

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1 Heat treatment and properties of high performance hot working tool steel M. Rosso", A. Bennani^ * Department of Engineering Materials, Politecnico di Torino, C.so *Duca degli Abruzzi, Torino. Italy COGNE Acciai Speciali, ViaParavera 16, Aosta. Italy Abstract The properties, in the as hardened condition or after nitriding treatment, of a new Cr hot working tool steel, having a composition similar to A1SI H10 but with reduced Mo and V contents, have been studied on KCU test bars, taking into account the effects of the metallurgical directions and of the position at the surface or at the core of the steel block, trom which the test specimens have been machined. In the as hardened condition, the steel guarantees good isotropic properties, whilst nitriding induces brittle behaviour in the KCU samples taken from the core of the steel block, caused by small microstructural differences between the surface and the core of the material. The morphology of the surface of the fracture confirms the presence of brittle zones in the material at the center of the block, whilst the fracture always exhibits toughness at the block surface. However, the presence of brittle and tough mixed structures in the zones at the core of the steel block enables the die to absorb and redistribute the tension which has been applied. Introduction In service tools are subjected to extremely high loads and they must withstand these loads a great number of times without breaking and without undergoing excessive wear or deformation, eventually under conditions that develop high temperatures in the tool. Consequently, selection of the proper tool material needs to achieve the optimum combination of properties like wear resistance, toughness and resistance to softening at elevated temperatures. In order to attain these aims, steels used to make tools require high-quality, close compositional and physical tolerances and must be heat treated. Most tool steels are firstly formed or machined to produce the required shape and then heat treated as required. However simple shapes may be obtained directly from tool steel producers in correctly heat treated condition, with economical and technical advantages. Hot working tool steels with new composition have been recently developed, they are characterised by lower content of alloying elements, Mo and V especially, but they can be easily

2 126 Surface Treatment, Computer Methods and Experimental Measurements through hardened and subsequently, the tool can be shaped by standard machining or spark erosion operations. These steels, in the hardened condition, exhibit very good isotropic properties III. The life of hot work tools can be succesfully increased by successive surface treatments, nitriding being one of the most common. These treatments increase surface hardness and reduce friction, giving as a result, better wear resistance properties and a higher number of working cycles before failure. Nit-riding treatments allow nitrogen enrichment of the surface of treated steels and cause the formation of surface nitrided layers constituted by y'-fe4n nitride and eventually by 8 solid solution of the Fe-N system, their amount being controlled by the nitrogen potential of the process. Nitrogen diffuses under the surface layer and the depth of the diffusion depends upon the nitrogen potential of the process (the higher the potential, the thicker is the diffusion zone), and upon the treatment duration, while the nitrogen diffusion is reduced by increasing amounts of elements which form nitnde precipitates 121. The rate of the diffusion layer growth is not constant. Generally two stages can be observed. In fact it has been demonstrated /3/ that this rate depends upon the nitrogen potential until a continuous surface layer has been completely formed. From that moment the rate is controlled and reduced by the nitrogen concentration at the interface between the surface layer and the ferritic matrix. The presence of 8 phase allows higher rates with respect to y' compound. The characteristics of the nitrided phases, y' and s, however, are quite different, that is y' nitride is very hard, while s phase has very low hardness values, which can be increased introducing C together with nitrogen /4/, moreover then 8 phase containing only N atoms is very brittle, while, with the introduction of carbon atoms, it becomes tough. Carbon can be introduced by adopting nitrocarburizing processes. With simple nitriding treatments the only possibility is the C counter diffusion from the interior to the surface of the steel, but the effects are insignificant. The diffusion zone, owing to the precipitation of nitrides favoured by the presence of nitride stabilizing elements, experiences strengthening and the subsurface hardness increases, favouring better wear resistance properties of the tools. Moreover, it is noteworthly that the interstitial diffusion of nitrogen atoms and eventually C, causes the establishement of a residual compressive stress pattern in the directions parallel to the surface; this state of residual stress is very beneficial for enhancing the fatigue resistance properties, with improvement of the endurance limit /5, 6/. The aim of this research is the study of the influence of nitriding treatment on the properties of a new Cr hot working tool steel, having a composition similar to AISI H10 but with reduced Mo and V contents, which is able to guarantee in the massive hardened state, good isotropic properties. Experimental The subject steel is produced in electric arc furnace, with subsequent remelting by ESR process and then forged to produce bars with section 360x230 mm. The bars are annealed to 220 HB hardness and then hardened to hardness

3 Surface Treatment. Computer Methods and Experimental Measurements 127 values of about HRC. After the surfaces of the bars are milled to dimensions 340x210 mm, the blocks are cut for the die production. The chemical composition (wt %) of the studied steel being: C 0.34, Si 0.30, Mn 0.50, Cr 3.0, Mo 1.0 and V From a block 150 mm long Charpy U impact tests bars have been machined. The tests bars have been taken at the surface and at the center of the block, in the longitudinal direction, that is the direction of the metallurgical axis of the original bar, and in the two transversal directions, short and long. For each of these, 6 test bars have been produced and marked with the following: MAS & MAC: metallurgical axis direction, surface and core respectively. STS & STC: short transverse direction, surface and core respectively. LTS & LTC: long transverse direction, surface and core respectively. Three of each series of test specimens have been gas nitrided in cracked ammonia atmosphere, adopting the following parameters: Washing of the furnace with nitrogen. Heating at 520 C in ammonia, flux /h. 520 C in 25 % cracked ammonia for 31.5 hrs. 570 C in 55 % cracked ammonia for 19.3 hrs. Cooling in the furnace with nitrogen until 80 C The Charpy impact test has been performed on nitrided samples and on the untreated ones, on the fracture specimens HRC hardness has been checked and on their transverse section optical metallography and Vickers microhardness tests (load 0.1 kg) have been performed, while the fracture morphology has been analysed by means of SEM. Results and discussions The average values of the hardnesses HRC and of the impact energy checked on the as hardened or nitrided samples are showed in table I. There are some differences between the core and the surface, that is the hardness of the as hardened samples is higher at surface. Moreover, a little influence of the sample orientation is noticeable, being the highest values checked on the metallurgical axis oriented samples, but the successive nitriding treatment increases the hardness values at about 55 HRC and all the differences related to surface, center or orientation are eliminated. However, the impact energy values are more sensitive to the previous parameters and, while in the as hardened state the KCU values show acceptable differences, certifying a good degree of isotropic properties, the differences between core and surface of the nitrided samples became dramatic. This apparently negative behaviour of the core nitrided samples can be substantiated comparing the micrestructures of the as hardened samples, figure 1 (A & B). In fact, while the surface samples show a dispersion of very fine and globular carbides in a tempered martensite matrix (Fig. 1 A), the micros true ture of the samples at the core of the blocks comprises of both larger grain dimensions tempered martensite and retained austenite or, more probably, by

4 128 Surface Treatment, Computer Methods and Experimental Measurements austenite not transformed in martensite, but preferably in some bainitic structures (Fig. IB). Table I. Hardness HRC and impact energy of nitrided and untreated samples. Samples MAS STS LTS MAC STC LTC HRC As hardened KCU [J/cm^l HRC nitrided KCU [J/crn^l A 20 j B Figure 1: Microstructure of as hardened samples, at surface zones (A) and at the core (B). It is well known that the iron products are affected by composition inhomogeneity caused during the alloy solidification and sligtly reduced by the forging deformation and there are different kind of micro-segregations at the surface and at the core. In particular the micro-segregation at the center has negative effects on the hardcnability, because the TTT curves tend to displace toward left, decreasing the hardcnability of the core material in relation to the surface. These phenomenons, together with the reduced cooling rate at the

5 Surface Treatment, Computer Methods and Experimental Measurements 129 center, can explain the presence of structures originated from austenite not transformed in martensite at the core of the hardened bar. The microhardness profiles of nitrides samples are practically independent of the position and orientation of the specimens: in Fig. 2 the profiles of the surface and core metallurgical axis oriented samples are shown. There are none substantial differences between surface and core materials, that is the profiles in the diffusion layers are practically coincident and show equal depth of diffusion. Under the diffusion zone the hardness falls to the core values. The morphology of the nitrided layers show that the performed nitriding cycle has not caused the formation of the withe layer, however a surface layer. about 15 jam thick has been formed, figure 3 (A & B), in which the presence of very fine precipitates can be observed (Fig. 3A). X-Ray diffraction analysis demonstrates the presence in this layer of nitrides and carbides of the alloying elements. Under a few white and elongated precipitates, extending in direction parallel to the surface and following the grain boundaries, are clearly visible in Fig. 3B. The reduced presence of these precipitates is beneficial, because they can nucleate cracks, which may extend by fatigue to the surface, thus causing premature die failure. LO ^ 00 rl- COO} CDOO O T-C\J T LO OO T- T- T- C\J CM LO LO T- O) C\J OO surface distance LO LO O LO O O CD co r>- co oo i- TJ- LO LO co CD r*- Figure 2: Microhardness profiles of nitrided samples, surface distance in [jam]. The microstructure at the core of the nitrided samples does not show differences with respect to the only as hardened ones, figure 1 (A & B), in fact the structures related to the austenite not transformed in martensite, on the MAC, STC and LTC samples are still appearing. The fracture morphology of the as hardened samples is evidence of the different toughness of the specimens taken at the center or at the surface of the block. In fact, the surface fracture of the last ones shows only the presence of dimples, figure 4A. This means ductility, while in figure 4B (core samples) cleavage zones coexist with dimpled ones. At higher magnification the dimples showed in Fig. 4B appear very fine, because the failure process affected the material only to a small depth. Details of these dimpled zones can be observed in Fig 5A, while in Fig. 5B a surface of cleavage can be observed at higher magnification.

6 130 Surface Treatment, Computer Methods and Experimental Measurements In figure 6 (A & B) it is possible to observe that the appearance of the fracture of the nitrided samples is still of the dimpled type for the material at the surface of block (Fig. 6A), while samples have been taken at the core essentially cleavage fracture can be observed (Fig. 6B). However in Fig. 6A some zones with fine dimples appear. This effect can be attributable to the nitnding effect, which tends to decrease the toughness of the treated materials. The presence of brittle and tough zones at the center of the bars, however, has not negative effects when the dies are installed and working, because these mixed structures, owing to the presence of ductile phases, are able to absorb and redistribute the applied state of tension, in such a way, that the tool life is not hindered. Otherwise when considering the massive treatment of a die instead of the very small Charpy U test bars, the negative effects are surely mitigated. A 300 iim B 40 jam Figure 3: Morphology of the nitrided layers.

7 Surface Treatment. Computer Methods and Experimental Measurements 131 B Figure 4: Fracture morphology of the as hardened samples. A type MAS lype MAC. and B

8 132 Surface Treatment, Computer Methods and Experimental Measurements B Figure 5: Higher magnification view of fracture details of as hardened samples type MAC.

9 Surface Treatment, Computer Methods and Experimental Measurements 133 B Figure 6: Fracture morphology of the nitrided samples. A type MAS MAC. and B type

10 134 Surface Treatment, Computer Methods and Experimental Measurements Conclusions The properties, in the as hardened state or after nitriding treatment, of a new Cr hot working tool steel, having a composition similar to AISI H10 but with reduced Mo and V contents, have been studied on KCU test bars. The test samples have been taken at the surface and at the center of a steel block, in the longitudinal direction, that is the direction of the metallurgical axis of the original steel bar, and in the two transversal directions, short and long. In the as hardened state the steel is able to guarantee good isotropic properties, even if the micros true ture analysis shows that the samples taken at the core of the steel block the austenite has not been completely transformed in martensite during quenching. The execution of nitriding treatment suffers from the microstructural differences between the surface and the core of the steel block and the toughness of the KCU samples taken at the core experience a dramatic fall with respect to that of the only as hardened samples. The morphology of the surfaces of fracture confirmes the presence of brittle zones in the material at the core of the steel block, while at the surface of the block the type of fracture shows always toughness. The brittleness caused on the KCU test specimens at the core of the steel block, should not detract from the effective qualities of this steel, because in performing the nitriding treatments on more massive parts, Like a die, the differences between core and surface will be surely mitigated or cancelled out. Moreover, the presence of brittle and tough mixed structures in the zones at the core of the steel block make the die capable of absorbing and redistributing the applied state of tension. Acknowledgements: The authors kindly thank Mr Graham Benn of the COGNE Stainless Steel UK for checking the paper. References. 1 - M. Rosso, A. Bennani, Notiziario Tecnico AMMA, 51, 4 (1996), p B. Mortimer, P. Grieveson, K.H. Jack, Scand. J. Metall., I, (1972), p D.H. Jack, I.M. Stoney, Scand. J. Metall., 1, (1972), p D. Firrao, M. Rosso, Atti Ace. Sc. Torino, 114, (1980), P J.M. Lessels, Strength of resistance of metals, John Wiley, New York, (1954). 6 - T. Bell, N.L. Loh, J. Heat Treating, 2, (1982), p. 232.

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