Abstract

Ultrafine grained (~ 1μm) steels have been the subject of extensive research work during the past years. These steels generally offer interesting perspectives looking for improved mechanical properties. UFG Powder Metallurgy hot work tool steels (HWTS) can be fabricated by high energy mechanical milling (MM) followed by spark plasma sintering (SPS). However, similarly to most UFG and Nano-Crystalline (NC) metals, reduced ductility and toughness result from the early plastic instabilities in these steels. Industrialization of UFG PM Tool Steels requires the application of specific metallurgical tailoring to produce tools with sound mechanical properties or in a more optimistic way, to break the Strength-Toughness “trade-off” in these materials. Among the possible ways proposed to restore ductility and toughness without losing the high strength, “Harmonic microstructure” design seems to be a very promising endeavor in this regard. Harmonic microstructure materials consist of a tunable volume fraction of evenly spaced “isolated” coarse-grained particles (CG) surrounded by a 3D interconnected network of UFG particles. CGs provide ductility and toughness, while high strength is guaranteed by the interconnected network of UFGs. This peculiar design offers an extra work hardening due to the generation of geometrically necessary dislocations at the interfaces of UFGs and confined CGs that are essentially present to accommodate the strain gradient imposed by the inhomogeneous (bimodal grained) microstructure. The first part of this work is devoted to the development of PM tool steels with harmonic microstructure. Due to the difficulties of processing hard tool steel particles according to the methods reported in the literature, an economical, simple alternative approach is also proposed. Near full density “Harmonic structure“ AISI H13 samples were produced using different volume fractions of UFG/NC mechanically milled (MM) and CG as-atomized particles followed by short time (30 min) low-temperature (1100°C) SPS. A combination of high hardness and significantly improved fracture toughness was achieved for the blends containing more that 50% UFG particles. The optimized mechanical properties was achieved by the mixture of 60% UFG particles where the sample showed a hardness near to the value predicted by the rule of mixtures (i.e. 405 HV10 vs. 406 HV10) while apparent fracture toughness (Kapp) was about 10% higher than that of predicted by the same rule (i.e. 52.0 MPa*m1/2 vs. ~47.0 MPa*m1/2). A toughening effect was evidenced for the samples essentially showing harmonic microstructure. Toughening was interpreted to be the result of the deviatory effect of coarse-grained round atomized particles together with energy dissipation by decohesion at the CG/UFG or UFG/UFG interfaces leading to a local drop of the driving force for the crack propagation. The design allowed to easily adjust the strength and toughness to meet the specific application-oriented requirements. The harmonic steel was also subjected to Thermal Fatigue (TF) testing. The preliminary results confirmed that this microstructure combined the beneficial effects of both of its constituents, i.e., the low crack nucleation rate of CG H13 and the low crack propagation rate of UFG H13, thus showing the lowest pyrocracking factor. Moreover, TF crack deflection as an extrinsic toughening mechanism was evidenced in Harmonic Microstructure. The second part of this work deals with the production and characterization of a PM HWTS reinforced with partially stabilized zirconia (PSZ). HWTS composites show improved hardness and remarkable wear resistance but generally also a systematic lower fracture toughness than the base material. Deteriorated toughness in metal matrix composites (MMCs) with a high strength matrix is mainly interpreted as a result of early damage initiation at the hard particles (HPs) or Matrix-HP interface. This damage can be even anticipated in the presence of readily damaged HPs (i.e. processing related flaws). Selection of PSZ as reinforcement was aimed at improving the strength and fracture toughness of the composite by taking advantage of the transformation toughening effect of PSZ. Two different types of PSZ, different volume fractions (10 and 20 vol. %) and sizes of reinforcement were used. Mechanical Alloying (MA) was used to process the composite powders to refine the matrix microstructure and both the matrix and PSZ particle size hence increasing the strength of the PSZ particles according to the Griffith strength formalism, and also to overcome the aggregation problems. Powders were consolidated by (SPS). The influence of processing parameters on density and microstructure was investigated. Short time (30 min) low-temperature (1100°C) consolidation by SPS allowed preserving the refined microstructure while achieving a maximum relative density of 98.6%. Moreover, short time sintering did not allow the extensive formation of thermodynamically plausible reaction products at the PSZ-H13 interface. As a result of dispersion hardening, the hardness of the as-sintered composites (i.e. maximum hardness of ~ 920 HV10) was increased compared to the mechanically milled UFG H13 (i.e. ~ 755 HV10), while in comparison to the as-atomized H13 (i.e. ~ 640 HV10) the improved hardness was ascribed to the synergic effect of dispersion hardening, microstructural refinement and strain hardening induced by MA. In these composites, tempering resistance at 550°C and 650°C was significantly improved due to the dispersion hardening effect. The hot compressive yield strength of the composites at 650°C and 450°C was increased up to 1.8 times the unreinforced UFG H13. t to m transformation during hot compression was evidenced and contributed to the strengthening. The hardness of the composites in heat treated condition (i.e. ~ 600 HV10) was significantly improved compared to that of the unreinforced matrix (i.e. ~ 420 HV10) while the apparent fracture toughness was drastically decreased to half the Kapp of the base material (19 MPa*m1/2 vs. 36 MPa*m1/2). However, the fracture toughness was slightly higher than that of a TiC reinforced H13 (i.e. 17 MPa*m1/2) with the same hardness (i.e. ~ 600 HV10).