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The main goal of the present work is to study the influence of the microstructure on the corrosion behavior of cemented carbides WC-Co in two corrosive media. Corrosion kinetics were determined by immersion tests while the electrochemical evolution of the Surface was analyzed using impedance testing. Damage tolerance to corrosion was evaluated by assessing fracture strength on specimens previously subjected to corrosion. Results pointed out that for both grades the corrosion rate was higher in seawater, being more significant for the grade with a medium grain size. The corrosion phenomenon that took place in both media was caused by the oxidation reaction of cobalt. In seawater, the polarization resistance decreased for both grades whereas in mine water increased, due to the formation of a layer of corrosion products, which slowed down the cobalt dissolution process in Surface. In both media, a greater strength loss of the ultrafine grades was evidenced.

WC–Co cemented carbides are geometrically complex composites constituted for two interpenetrating networks of the constitutive ceramic and metal phases. Accordingly, assessment of microstructural effects on the local mechanical properties of each phase is a challenging task, especially for the metallic binder. In this work, it is attempted by combining massive nanoindentation, statistical analysis, and implementation of a thin film model for deconvolution of the intrinsic hardness and flow stress of the metallic phase. Plotting of yield stress values as a function of the binder mean free path results in a Hall-Petch strengthening relationship with a slope (ky) of 0.98 MPa m1/2. This value points out the effectiveness of WC–Co phase boundaries as strong obstacles to slip propagation; and thus, for toughening of the brittle phase (WC) by means of crack-bridging ductile (Co) reinforcement.

The influence of microstructure on the R-curve behavior of hardmetals and its implication on their strength and reliability are studied. In doing so, an already validated model for R-curve description is implemented for rationalizing the fracture behavior of five microstructurally different WC-Co cemented carbides. Results indicate that hardmetals with R-curves developing smoothly over relatively long multiligament zones (i.e. lower slopes) exhibit reduced strength variability than those with steeper and shorter (i.e. higher slopes) ones. The reduced strength scatter associated with a low-slope R-curve behavior is discussed on the basis of the effectively developed toughness and the subcritical crack extension reached before unstable growth is triggered, both being dependent on microstructural length scale and initial flaw size. The results of this investigation highlight the relevance of an in-depth knowledge of R-curve characteristics of hardmetals in order to optimize the performance of engineering parts by means of microstructural design. Keywords: Cemented carbides, Fracture, Strength, R-curve, Reliability

Results are reported on cemented tungsten carbide (cWC) and boride-containing composite materials for the task of shielding the centre column of a superconducting tokamak power plant. The shield is based on five concentric annular shells consisting of cWC and water layers of which the innermost cWC shield can be replaced with boride composites. Sample materials have been fabricated changing the parameters of porosity P, binder alloy fraction f binder and boron weight fraction f boron. For the fabricated materials, and other hypothetical samples with chosen parameters, Monte Carlo studies are made of: (i) the power deposition into the superconducting core, (ii) the fast neutron and gamma fluxes and (iii) the attenuation coefficients through the shield for the deposited power and neutron and gamma fluxes. It is shown that conventional Co-based cWC binder alloy can be replaced with a Fe–Cr alloy (92 wt.% Fe, 8 wt.% Cr), which has lower activation than cobalt with minor changes in shield performance. Boride-based composite materials have been prepared and shown to give a significant reduction in power deposition and flux, when placed close to the superconducting core. A typical shield of cemented tungsten carbide with 10 wt.% of Fe–8Cr binder and 0.1% porosity has a power reduction half-length of 0.06 m. It is shown that the power deposition increases by 4.3% for every 1% additional porosity, and 1.7% for every 1 wt.% additional binder. Power deposition decreased by 26% for an initial 1 wt.% boron addition, but further increases in f boron showed only a marginal decrease. The dependences of power deposited in the core, the maximum neutron and gamma fluxes on the core surface, and the half attenuation distances through the shield have been fitted to within a fractional percentage error by analytic functions of the porosity, metallic binder alloy and boron weight fractions.

© 2017 Elsevier LtdThe study of mechanical response of materials at small length scales has gained importance due to the recent advances in micro- and nano-fabrication as well as testing systems. However, most of the reported work has been dedicated to investigate single-crystals or boundary-containing metallic systems, while much less attention has been paid to composite materials, and in particular those combining soft and hard phases. In this work, a systematic procedure is followed for machining micropillars of diameters ranging from 1 to 4 µm in a WC-Co composite with a WC mean grain size around 1 µm, by means of focused ion beam milling. In-situ uniaxial compression of the micropillars and subsequent field emission scanning electron microscopy inspection were conducted. Clear size effects are evidenced. Smaller test specimens (probe size approaching the mean WC size) exhibit deformation/failure mechanisms observed for WC crystals; while for bigger sample sizes, the mechanical response involves several mechanisms directly linked with the microstructural characteristics of the bulk-like cemented carbide material. On the other hand, independent of micropillar size, carbide-carbide or carbide-binder interfaces are found to be preferential sites for nucleation of critical damage events.

Strength and reliability of WC-Co cemented carbides (hardmetals) are dependent on effective fracture toughness as well as on nature, size and distribution of processing flaws. Regarding toughness, they exhibit a crack growth resistance (R-curve) behavior, derived from the development of a multiligament bridging zone at the crack wake. Accordingly, successful implementation of fracture mechanics requires consideration of tangency criterion, between applied stress intensity factor and R-curve, in addition to fractographic inspection. It is the aim of this study to evaluate the strength behavior of a series of experimental WC-Co grades on the basis of R-curve failure criteria. Results indicate that microstructural effects on the strength of hardmetals may be satisfactorily rationalized following the referred criterion. The analysis includes consideration of nature and distribution of fracture origins, found to be more diverse and wider, respectively, for the harder fine-grained grades. This experimental evidence, together with the fact that these hardmetals exhibit steeper rising R-curves than tougher coarse-grained ones, leads to lower reliability for the former. This investigation documents and validates the great relevance of R-curve behavior for optimizing the mechanical performance of WC-Co cemented carbides on the basis of microstructural design. Spanish Ministerio de Economía y Competitividad through Grant MAT2015-70780-C4-3-P (MINECO/FEDER) Andalusian government (Spain) under the excellence project P12-TEP-2622 Universitat Politècnica de Catalunya Agencia Española de Cooperación Internacional (MAEC-AECID)

There is a major interest in replacing cobalt binder in hardmetals (cemented carbides) aiming for materials with similar or even improved properties at a lower price. Nickel is one of the materials most commonly used as a binder alternative to cobalt in these metal-ceramic composites. However, knowledge on mechanical properties and particularly on fatigue behavior of Ni-base cemented carbides is relatively scarce. In this study, the fatigue mechanics and mechanisms of a fine grained WC-Ni grade is assessed. In doing so, fatigue crack growth (FCG) behavior and fatigue limit are determined, and the attained results are compared to corresponding fracture toughness and flexural strength. An analysis of the results within a fatigue mechanics framework permits to validate FCG threshold as the effective fracture toughness under cyclic loading. Experimentally determined data are then used to analyze the fatigue susceptibility of the studied material. It is found that the fatigue sensitivity of the WC-Ni hardmetal investigated is close to that previously reported for Co-base cemented carbides with alike binder mean free path. Additionally, fracture modes under stable and unstable crack growth conditions are inspected. It is evidenced that stable crack growth under cyclic loading within the nickel binder exhibit faceted, crystallographic features. This microscopic failure mode is rationalized on the basis of the comparable sizes of the cyclic plastic zone ahead of the crack tip and the characteristic microstructure length scale where fatigue degradation phenomena take place in hardmetals, i.e. the binder mean free path. (C) 2014 Elsevier Ltd. All rights reserved.

In an attempt to improve the material selection, design and reliability of rock bit WC-Co cemented carbides (hardmetals), an extensive and detailed study is conducted with the main goal of characterizing the fracture and fatigue crack growth (FCG) behavior of four hardmetal grades. Work includes basic microstructural and mechanical characterization of the materials, assessment of fracture toughness and FCG kinetics. It is found that rock bit cemented carbides exhibit relatively high fracture toughness values (between 17 and 20 MPa root m) in direct association with their specific microstructural characteristics, i.e. medium/coarse carbide grain size and medium cobalt content. The influence of microstructure on the measured crack growth mechanics under monotonic loading may be accounted by considering the effective operation of ductile ligament bridging and crack deflection as the prominent toughening mechanisms. Regarding FCG behavior, it is observed to exhibit a significant Km influence. Furthermore, relative increments in toughness are maintained, in terms of crack growth threshold, under cyclic loading. As a consequence, fatigue sensitivity for rock bit cemented carbides is found to be lower than that extrapolated from data reported for fine-grained grades. Crack growth resistance under cyclic loading for the hardmetals studied may be understood on the basis that prevalent toughening mechanisms (ductile ligament bridging and crack deflection) show distinct susceptibility to fatigue degradation and are thus critical in determining fatigue sensitivity. (C) 2014 Elsevier Ltd. All rights reserved.

The influence of the microstructure on the tolerance of WC-Co cemented carbides to corrosion damage was studied by using residual strength as the critical design parameter. In doing so, samples were immersed in synthetic mine water solution for different times, and changes induced by corrosion exposure were assessed. A detailed 3D FIB/FESEM tomography characterization of corrosion damage-microstructure interactions is included. Results reveal that corrosion damage may result in relevant strength degradation on the basis of stress rising effects associated with the formation of surface corrosion pits. Thus, as immersion time increases strength gradually decreases. Fractographic examination reveals the formation of semi-elliptical and sharp corrosion pits for studied medium- and ultrafine-sized cemented carbides, respectively. The latter has a much more pronounced stress rising effect, and consequently higher strength losses were determined for ultrafine grades. Corrosion process consists of a selective attack of the binder that is dissolved in the corrosive media. Initially, it is located at centres of binder pools and as exposure time in the media increases, corrosion evolves consuming the rest of the pools which finally leaves an unsupported WC grain skeleton at the surface. Keywords: Cemented carbides, Cobalt, Corrosion, Fracture, 3D FIB/FESEM tomography

Exceptional fracture toughness levels exhibited by WC-Co cemented carbides (hardmetals) are due mainly to toughening derived from plastic stretching of crack-bridging ductile enclaves. This takes place due to the development of a multiligament zone at the wake of cracks growing in a stable manner. As a result, hardmetals exhibit crack growth resistance (R-curve) behavior. In this work, the toughening mechanics and mechanisms of these materials are investigated by combining experimental and analytical approaches. Focused Ion Beam technique (FIB) and Field-Emission Scanning Electron Microscopy ( FESEM) are implemented to obtain serial sectioning and imaging of crack-microstructure interaction in cracks arrested after stable extension under monotonic loading. The micrographs obtained provide experimental proof of the developing multiligament zone, including failure micromechanisms within individual bridging ligaments. Analytical assessment of the multiligament zone is then conducted on the basis of experimental information attained from FIB/FESEM images, and a model for the description of R-curve behavior of hardmetals is proposed. It was found that, due to the large stresses supported by the highly constrained and strongly bonded bridging ligaments, WC-Co cemented carbides exhibit quite steep but short R-curve behavior. Relevant strength and reliability attributes exhibited by hardmetals may then be rationalized on the basis of such toughening scenario. Ministerio de España de Economía y Competitividad (Grant MAT2012-34602) Industry-University program between Sandvik Hyperion and Universitat Politècnica de Catalunya

The effect of corrosion damage on cemented carbides was investigated. The study included residual strength assessment and detailed fractographic inspection of corroded specimens as well as detailed 3D FIB-FESEM tomography characterisation. Experimental results point out a strong strength decrease associated with localised corrosion damage, i.e. corrosion pits acting as stress raisers, concentrated in the binder phase. These pits exhibit a variable and partial interconnectivity, as a function of depth from the surface, and are the result of heterogeneous dissolution of the metallic phase, specifically at the corrosion front. However, as corrosion advances the ratio between pit depth and thickness of damaged layer decreases. Thus, stress concentration effect ascribed to corrosion pits gets geometrically lessened, damage becomes effectively homogenised and relatively changes in residual strength as exposure time gets longer are found to be less pronounced.

Linear intercept on scanning electron microscopy micrographs is the most commonly used measurement method to determine carbide grain size and contiguity in WC–Co cemented carbides (hardmetals). However, it involves manual time-consuming measurements and is critically dependent on the quality of the micrographs as well as on the identification and definition of grain boundaries. In this study a two-stage methodology for microstructural characterization of hardmetals is presented. First, a digital semi-automatic image analysis procedure for grain size determination of the carbide phase is presented. It involves an experimental assessment of grain size on processed images corresponding to a series of WC–Co and WC–Ni cemented carbide grades with different microstructural characteristics. Obtained results are then compared to the values obtained by means of the linear intercept technique. A good correlation between the mean grain sizes determined following both measurement techniques was attained. Based on experimental findings, a series of empirical relations were found to correlate grain size distributions obtained following both methods. Second, an empirical relation for estimating carbide contiguity in WC–Co cemented carbides is proposed. This relation considers simultaneously the influence of the binder content and the experimentally determined mean grain size on contiguity. The proposed equation for contiguity estimation is based on extensive data collection from open literature. An excellent agreement was attained between contiguity values estimated from such equation and those obtained using the linear intercept technique. This validates the two-stage procedure as an effective time-saving methodology for microstructural characterization of WC–Co cemented carbides.

In this study, systematic nanomechanical andmicromechanical studies have been conducted in threemultilayer TiN/CrN systems with different bilayer periods (8, 19 and 25 nm). Additionally, experimental work has been performed on corresponding TiN and CrN single layers, for comparison purposes. The investigation includes the use of different indenter tip geometries aswell as contact loading conditions (i.e. indentation/scratch) such to induce different stress field and damage scenarioswithin the films. The surface and subsurface damage under the different indentation imprints and scratch tracks have been observed by atomic forcemicroscopy, field emission scanning electron microscopy and focused ion beam. Multilayer TiN/CrN coated systems are found to exhibit higher adhesion strength (under sliding contact load) and cracking resistance (under spherical indentation) than those coated with reference TiN and CrN monolayers. The main reason behind these findings is the effective development of microstructurally-driven deformation and cracking resistant micromechanisms: rotation of columnar grains (and associated distortion of bilayer period) and crack deflection of interlayer thickness length scale, respectively.

The fracture and fatigue characteristics of several cemented carbide grades are investigated as a function of their microstructure. In doing so, the influence of binder chemical nature and content (Co and 76 wt.% Co-24 wt.% Ni), as well as carbide grain size on hardness, flexural strength, fracture toughness and fatigue crack growth (FCG) behavior is evaluated. Mechanical testing is combined with a detailed inspection of crack-microstructure interaction, by means of scanning electron microscopy, in order to evaluate crack-path tortuosity and to discern fracture and fatigue micromechanisms within the metallic binder. Results show that CoNi-base hardmetals exhibit slightly lower hardness but higher toughness values than Co-base grades. Meanwhile, flexural strength is found to be rather independent of the binder chemical nature. Regarding FCG behavior, experimental results indicate that: (1) FCG threshold (K-th) values for coarse-grained grades are higher than those measured for the medium-grained ones; and (2) fatigue sensitivity levels exhibited by CoNi- and Co-base cemented carbides, for a given binder mean free path, are similar. These findings are rationalized on the basis of the increasing relevance of crack deflection mechanisms as microstructure gets coarser and the evidence of similar fatigue degradation phenomena within the binder independent of its chemical nature, respectively. (C) 2014 Elsevier Ltd. All rights reserved.

The intrinsic hardness of the constitutive phases in WC-Co composites is investigated by combining experimental and statistical analysis nanoindentation techniques. It is done on the basis of considering the cemented carbide material as effectively heterogeneous at the microstructure scale, i.e. consisting of three phases defined by either different chemical nature (carbides and binder) or distinct carbide crystal orientation (i.e. with surface normal perpendicular to either basal or prismatic planes). As main outcome, experimentally measured and statistically significant intrinsic hardness values for the defined phases (WC and constrained metallic binder) are analyzed and determined. Besides the evidence of crystal anisotropy for the WC phase, they permit to identify and account the expected strengthening of the plastic-constrained metallic binder, a critical input parameter for hardness and toughness modelling as well as for microstructural design optimization of ceramic composites reinforced by ductile metallic ligaments. (C) 2015 Elsevier Ltd. All rights reserved.

In thiswork,WC–Co micropillars machined by focused ion beamhave been tested under uniaxial compression to investigate the stress–strain behavior and associated deformation mechanisms. The results indicate that yielding phenomena is evidenced by multiple strain bursts. Experimental data is found to fall within the bounds defined by the mechanical responses expected for an unconstrained Co-binder like model alloy and a bulk-like constrained binder region in WC–Co composites; capturing then local phase assemblage and crystal orientation effects.