Effect of Grain Shape on Abnormal Grain Growth in Liquid-Phase-Sintered Nb1−xTixC–Co Alloys

The effect of titanium substitution for niobium on the grain shape change, grain growth inhibition, and abnormal grain growth during liquid-phase sintering of Nb_{1− x} Ti_xC–Co alloy was studied. With increased titanium substitution, the shape of the Nb_{1− x} Ti _x C grains in the liquid cobalt matrix was changed from a cube with round corners to a cube with angular corners, which implied increased edge energy. As the grain corners became more angular, the grain growth became markedly inhibited, and abnormal grain growth occurred. The results could be best explained by the increased edge energy of the interface of the Nb_{1− x} Ti _x C grains, which increased the barrier for the growth by two-dimensional nucleation.     

Enhanced Densification of Liquid-Phase-Sintered WC–Co by Use of Coarse WC Powder: Experimental Support for the Pore-Filling Theory

Densification during liquid-phase sintering of WC–Co with various WC powder sizes has been measured in order to identify the densification mechanism. During heating of powder compacts in the solid state, densification was enhanced with a reduction of WC powder size. However, the behavior was reversed when the densification occurred in the presence of a liquid: enhanced densification with increasing WC powder size. This result is in contradiction to a prediction of the conventional theory of liquid-phase sintering, the contact flattening theory, but in good agreement with a prediction of the pore-filling theory. Microstructural analysis further confirmed that the densification at the liquid-phase sintering temperature occurred by pore filling. The calculated densification kinetics based on the pore-filling theory also fitted well with the measured data. The observed densification behavior thus demonstrates experimentally the prediction of the pore-filling theory that the densification is enhanced with increasing average grain size for the same pore size distribution.     

Interface Character Distributions in WC–Co Composites

The geometric and crystallographic characteristics of interfaces in WC–Co composites with a range of grain sizes and carbide volume fractions have been comprehensively characterized. The carbide crystals are most frequently terminated by (0001) and     surfaces. The average number of carbide vertices per grain and the basal-to-prismatic face area ratio of the WC–Co interfaces increase with the carbide volume fraction. The three most frequently occurring WC/WC grain boundaries are 90° twist boundaries about     , 30° twist boundaries about [0001], and asymmetric 90° boundaries about     . The boundary populations do not vary with grain size or carbide volume fraction, suggesting that they are determined by the grain boundary energy anisotropy.     

Role of Vanadium Carbide Additive during Sintering of WC–Co: Mechanism of Grain Growth Inhibition

In a WC–Co specimen, the shape of WC crystals was a triangular prism with truncated corners. When VC was added to inhibit grain growth, the crystal shape changed to a triangular prism without truncation. This shape change was related to the variation of edge energy, which has a significant influence on the coarsening process of WC grains.     

Tribological Characterization of WC–Co Plasma Sprayed Coatings

Atmospheric plasma spraying of WC coatings is typically characterized by increased decarburization, with a consequent reduction of their wear resistance. Indeed, high temperature and oxidizing atmosphere promote the appearance of brittle crystalline and amorphous phases. However, by using a high helium flow rate in a process gas mixture, plasma spraying may easily be optimized by increasing the velocity of sprayed particles and by reducing the degree of WC dissolution. To this purpose, a comparative study was performed at different spray conditions. Both WC–Co powder and coating phases were characterized by X-ray difraction. Their microstructure was investigated by scanning electron microscopy. Mechanical, dry sliding friction, and wear tests were also performed. The wear resistance was highly related to both microstructural and mechanical properties. The experimental data confirmed that high-quality cermet coatings could be manufactured by using optimized Ar–He mixtures. Their enhanced hardness, toughness, and wear resistance resulted in coatings comparable to those sprayed by high velocity oxygen-fuel.     

Grain Growth Kinetics in Liquid-Phase-Sintered Zinc Oxide–Barium Oxide Ceramics

Grain growth of ZnO in the presence of a liquid phase of the ZnO–BaO system has been studied for temperatures from 1300° to 1400°C. The specimens were treated in boiling water and the grains were separated by dissolving the matrix phase in an ultrasonic bath. As a consequence three-dimensional grain size measurements were possible. Microstructural examination shows some grain coalescence with a wide range of neck size ratios and corresponding dihedral angles, however, most grains are isolated. Lognormal grain size distributions show similar shapes, indicating that the growth mechanism is invariant over this time and temperature. All regressions between G ⁿ and time for n = 2 and 3 proved statistically significant. The rate constants calculated with the growth exponent set to n = 3 are on the same order of magnitude as in metallic systems. The apparent activation energy for growth is estimated between 355 and 458 kJ/mol.     

Texture Development by Templated Grain Growth in Liquid-Phase-Sintered α-Alumina

The distribution and orientation of platelet-shaped particles of α-alumina in a fine-grained alumina matrix is shown to template texture development via anisotropic grain growth. The textured microstructure ranges from 4 wt% oriented platelet particles in calcined samples to nearly 100% oriented α-Al₂O₃ grains after sintering at 1400°C. A CaO + SiO₂ liquid phase creates favorable thermodynamic and kinetic conditions for anisotropic grain growth and grain reorientation during sintering. Important criteria for templated grain growth include (1) anisotropic crystal structure and growth, (2) high thermodynamic driving force for template grain growth, and (3) modification of diffusion in the system to continuously provide material to the anisotropically growing template grains.     

Impurity-Dependent Morphology and Grain Growth in Liquid-Phase-Sintered Alumina

The alumina grains in liquid-phase-sintered (LPS) materials prepared from different commercial sources have a predominantly platelet morphology. Generally, the MgO:(CaO + BaO + Na₂O + K₂O) ratio in the chemical composition controls the morphology in LPS alumina that is 91–94 wt% pure. Within a given range of SiO₂ content (i.e., 4.3–5.2 wt% in the chemical composition), a low MgO:(CaO + BaO + Na₂O + K₂O) ratio (i.e., <1.0) in the LPS compositions favors the formation of elongated grains, whereas ratios of >1.0 result in equiaxed grains. SiO₂ contents outside the 4.3–5.2 wt% range favor the formation of elongated grains. A tendency to form platelike grains is observed for LPS alumina with a purity of 91–94 wt% when both the MgO:(CaO + BaO + Na₂O + K₂O) ratio and the SiO₂ content are relatively low. The sintered density generally increases as the SiO₂ content in the chemical composition decreases.     

Structural Analysis on Planar Defects Formed in WC Platelets in Ti-Doped WC–Co

Platelet-reinforced WC–Co alloys are processed by liquid-phase sintering from very fine-grained WC powders in the presence of small amounts of TiC. Large and flat WC grains develop in the material. The microstructure of these platelets is investigated by high-resolution electron microscopy in order to obtain information on their formation mechanism. Inside the grains, an extended defect parallel to the basal plane is observed. It can be described by a pair of stacking faults with a shear vector equal to 1/3 〈0-110〉 occurring in two successive (0001) planes. At the level of the faults, the plane spacing is slightly reduced. The defect area is similar to a thin cubic layer about 0.5 nm thick at the interior of the platelet. The enhanced grain growth of the platelets is likely related to the presence of the defect area.     

Effect of Sintering Atmosphere on Grain Shape and Grain Growth in Liquid-Phase-Sintered Silicon Carbide

We investigated the effects of the sintering atmosphere on the interface structure and grain-growth behavior in 10-vol%-YAG-added SiC. When α-SiC was liquid-phase-sintered in an Ar atmosphere, the grain/matrix interface was faceted, and abnormal grain growth occurred, regardless of the presence of α-seed grains. In contrast, when the same sample was sintered in N₂, the grain interface was defaceted (rough), and no abnormal grain growth occurred, even with an addition of α-seed grains. X-ray diffraction analysis of this sample showed the formation of a 3C (β-SiC) phase, together with a 6H (α-SiC) phase. These results suggest that the nitrogen dissolved in the liquid matrix made the grain interface rough and induced normal grain growth by an α→β reverse phase transformation. Apparently, the growth behavior of SiC grains in a liquid matrix depends on the structure of the grain interface: abnormal growth for a faceted interface and normal growth for a rough interface.     

Facet–Defacet Transition of Grain Boundaries in Alumina

Grain boundaries in pure alumina powder compacts sintered at 1400°C are smoothly curved, indicating that they have atomically rough structures. When these specimens are heat-treated at temperatures between 900° and 1100°C, a small fraction of the grain boundaries develop either hill-and-valley or kinked shapes with flat segments. Some of these flat boundary segments lie on the {011[Twomacr]} plane of one of the grain pairs. These grain boundaries thus appear to become singular at these temperatures. When a corundum crystal with a basal surface is sintered in alumina powder at 1400°C, all grain boundaries formed between the corundum basal surface and small grains, as well as those between the small grains, are smoothly curved, indicating their rough structure. When heat-treated at 900°C for 3 days, about 30% of the grain boundaries between the corundum basal surface and the small grains develop kinks with flat boundary segments, and some of these flat segments lie on the basal plane of the corundum. When heat-treated again at 1400°C, all grain boundaries are curved, indicating that they become reversibly rough. These observations show that at least some of the grain boundaries in alumina undergo roughening-singular transitions at temperatures between 900° and 1100°C.     

Modeling the Influence of Orientation Texture on the Strength of WC–Co Composites

Two-dimensional finite element simulations were used to study the effects of orientation texture on the transverse rupture strengths of WC–Co composites. The model incorporates observed microstructural geometries, anisotropic thermal and elastic properties, and a fracture criterion that reproduces the strengths of known specimens. The results show that the greatest potential for increasing the strength occurs when the [001] axes of the carbide grains are orientated perpendicular to the sample loading direction. Furthermore, the strength increases in proportion to the degree of texture, and the texture-derived strength enhancement is greater in microstructures with a larger contiguity.     

Surface Integrity Effects on the Fracture Resistance of Electrical-Discharge-Machined WC–Co Cemented Carbides

The flexural strength evolution for two WC–16 vol% Co cemented carbides, with different mean carbide size, subjected to sequential and upgrading electrical-discharge machining (EDM) is studied. It is compared with the fracture behavior exhibited by a reference surface finish condition, attained through conventional mechanical grinding and polishing using diamond as abrasive. Considering that rupture is related to existing defects, either introduced during sample elaboration or induced by machining, a detailed fractographic examination by scanning electron microscopy is conducted to discern fracture origins. The experimental findings indicate that the flexural strength of WC–Co hardmetals may be strongly affected by EDM, depending on the correlation existing between natural defects, as given by particular microstructural parameters, and EDM-induced flaws. An analysis of the results using a linear–elastic fracture mechanics approach permits one to establish a clear connection between surface integrity and fracture resistance. Quantitative discrepancies between the estimated and the experimentally measured critical flaw sizes for all the EDM-related grades are rationalized through the existence of local residual tensile stresses of considerable magnitude at the shaped surface. Release of these stresses through final mechanical and annealing treatments is pointed out as a quite effective alternative for improving the fracture behavior of WC–Co cemented carbides shaped by EDM.     

Compaction as a Critical Factor for Success in the Sintering of Ultra-Fine WC–Co Powders

Heat treatment of ultra-fine WC–13Co powders was carried out prior to cold compaction, in an attempt to improve the sintered density. The findings indicate that a preheat treatment of ultra-fine or nano-sized powders significantly improves the densification process. This study showed that a low compacting pressure, <200 MPa, can be effectively used through this technique to retain ultra-fine structure. The densification behavior of preheated powder was compared with the samples prepared by a conventional technique and explained with size distribution, standard deviation, and surface effect.     

Energy of Grain Boundaries in Halite

Relative grain boundary energy measurements were made by the tracrystal method for [100] tilt boundaries in NaCl. The dependence of boundary energy on grain misorientation was similar to that in metals; however, the presence of significant torque term effects, i.e. dependence of the boundary energy on boundary orientation, is indicated. A method of measuring the relative magnitudes of the torque terms by applying a driving force to boundaries in bi-crystals is described.     

Wear-Resistant Titanium Carbonitride Coatings onto WC–Co Cutting Tools by Pulsed High-Energy Density Plasma

Nanometer grain superhard ternary Ti(C,N) coatings with Vicker's nanohardness more than 50 GPa were deposited onto WC–Co cutting tools at ambient temperature using pulsed high-energy density plasma coaxial gun. Young's modulus of the coated tools was about 550 GPa. Because of the continuously graded interfaces between the coatings and substrates, the coatings are well adherent to the tool substrates with very high critical load up to more than 100 mN measured by nanoscratch tester. The coefficients of friction were lower than 0.1. In contrast with the uncoated tools, the coated tools could be applied in turning hardened CrWMn steel at high speed under industrial conditions without lubricants, and the cutting performances were greatly improved with rather low flank wear and long tool life.     

Grain Boundaries in Fine-Grained Magnesium-Doped Aluminas

The distribution and some characteristics of grain boundaries have been determined in three samples of fine-grained Mg-doped alumina which had undergone different thermo-mechanical treatments: as-pressed at 1500°C, stress-free annealed, and deformed at the same temperature. The analyses of some particular features point out the role of the grain-boundary type "special' or "general' on the creep deformation mechanisms.     

Texture Development and Microstructure Evolution in Liquid-Phase-Sintered α-Alumina Ceramics Prepared by Templated Grain Growth

Texture development in alumina that contains calcia and silica and has been templated with platelet-shaped α-Al₂O₃ particles has been evaluated. The texture fraction is shown to be related directly to template growth. Texture quality is controlled by the template concentration, decreasing at template concentrations of >10%, as a result of template–template interactions during tape casting. Almost fully textured alumina has been obtained at template concentrations of ≥20%. The growth of template grains is much more rapid in the radial direction and is shown to be inversely related to the thickness of the grain-boundary liquid. The activation energy for growth (376 kJ/mol) and the inverse relation with the grain-boundary thickness indicate that template growth in the radial direction is controlled by Al³⁺ diffusion.     

Microwave Heating of Grain Boundaries in Ceramics

It has been suggested that enhanced sintering of ceramics by microwave heating may be the result of accelerated grainboundary diffusion caused by the grain boundaries being heated to temperatures significantly greater than the bulkspecimen temperature. Heat flow calculations show that the temperature difference between the grain boundary and grain interior will be a small fraction of a degree, even under extreme conditions.