On-machine dry electric discharge truing of diamond wheels for micro-structured surfaces grinding

Precision grinding with diamond wheels gives a promising alternative to achieve high quality micro-structured surfaces on optical molds. However, it is difficult to true these diamond wheels efficiently, because of the remarkable resistance property and the geometrical limitation of small wheel profile. In this paper, an on-machine dry-EDT method to precision shape and prepare diamond wheels with various profiles was proposed for micro-structured surface grinding. Firstly, the fundamental truing errors were analyzed based on the dry-EDT kinematics. And then the capabilities of dry-EDT truing for high abrasive concentration metal bonded diamond wheels were presented. Next, the effects of kinematic parameters variables on trued wheel profile accuracy were investigated. Finally, the micro-structured surfaces on SiC ceramic and tungsten carbide WC were ground by these trued diamond wheels. The experiments results showed that the arc-shaped diamond wheel (diameter of 200 mm) with 4 μm profile error (PV) and 1.0023 mm profile radius, and the V-shaped diamond wheel with 22.5 μm V-tip radius and 120.03° profile angle could be obtained by on-machine dry EDT. The kinematic parameters of dry-EDT have an important influence on truing profile accuracy of diamond wheels, especially for the tip of V-shaped wheel. The subsequent grinding show that the edge radius of V groove array on SiC is less than 2 μm, while the radius of included corner is around 55 μm. The PV error of ground arc groove array on WC is less than 5 μm. The surface roughness of ground micro-structured surface R_a is 142 nm and 97 nm for SiC and WC, respectively.     

Sintering of Al2O3–TiB2 nano-composite derived from milling assisted sol–gel method

Synthesis and sintering of an alumina /titanium diboride nano-composite have been studied as an alternative for pure titanium diboride for ceramic armor applications. Addition of TiB₂ particles to an Al₂O₃ matrix can improve its fracture toughness, hardness and flexural strength and offer advantages with respect to wear and fracture behavior. This contribution, for the first time, reports the sintering, microstructure, and properties of Al₂O₃–TiB₂ nano-composite densified with no sintering aids. Nano-composite powder was produced by combination of sol–gel and mechano-chemical methods. The densification experiments were carried out using both hot pressing and pressureless sintering routes. In the pressureless sintering route, a maximum of 92.3% of the theoretical density was achieved after sintering at 1850 °C for 2 h under vacuum. However, hot pressing at 1500 °C for 2 h under the same condition led to achieving a 99% of the theoretical density. The hot pressed Al₂O₃–TiB₂ nano-composites exhibit high Vickers hardness (16.1 GPa) and a modest indentation toughness (~ 4.2 MPa.m^1/2).     

Effect of initial particulate and sintering temperature on mechanical properties and microstructure of WC–ZrO2–VC ceramic composites

Owing to improving the mechanical properties of cemented carbides in high speed machining fields, a new composite tool material WC–ZrO₂–VC (WZV) is prepared from a mixture of yttria stabilized zirconia (YSZ) and micrometer VC particles by hot-press-sintering in nitrogenous atmosphere. Commercial WC, of which the initial particle sizes are 0.2 μm, 0.4 μm, 0.6 μm and 0.8 μm, is mixed with zirconia and VC powder in aqueous medium by following a ball mill process. The sintering behavior is investigated by isostatic pressing under different sintering temperature. The relative density and bending strength are measured by Archimedes methods and three-point bending mode, respectively. Hardness and fracture toughness are performed by Vickers indentation method. Microstructure of the composite is characterized by scanning electron microscopy (SEM). The correlations between initial particles, densification mechanism, sintering temperature, microstructure and mechanical properties are studied. Experimental results show that maximum densification 99.5% is achieved at 1650 °C and the initial particle size is 0.8 μm. When temperature is 1550 °C and particle size is 0.4 μm, the optimized bending strength (943 MPa) is obtained. The best hardness record is 19.2 GPa when sintering temperature is 1650 and particle size is 0.8 μm. The indention cracks propagate around the grain boundaries and the WC particles fracture, which is associated with particle and microcrack toughening mechanism.     

Effect of Ni content on the compression properties and abrasive wear behavior of the (TiB2–TiCxNy)/Ni composites

The (TiB₂–TiC_xN_y)/Ni composites were fabricated by the method of combustion synthesis and hot press consolidation in a Ni–Ti–B₄C–BN system. The effect of Ni content on the microstructure, hardness, compression properties and abrasive wear behavior of the composites has been investigated. The results indicate that with the increase in Ni content from 30 wt.% to 60 wt.%, the average size of the ceramic particles TiB₂ and TiC_xN_y decreases from 5 μm to ≤ 1 μm, while the hardness and the abrasive wear resistance of the composites decrease. The composite with the Ni content of 30 wt.% Ni possesses the highest hardness (1560.8 Hv) and the best abrasive wear resistance. On another hand, with the increase in the Ni content, the compression strength increases firstly, and then decreases. The composite with 50 wt.% Ni possesses the highest compression strength (3.3 GPa). The hardness and fracture strain of the composite with 50 wt.% Ni are 1251.2 Hv and 3.9%, respectively.     

Hardness and toughness enhancement of CeO2 addition to ZTA ceramics through HIPping technique

The aim of this research is to investigate the combined effects of CeO₂ additions and hot-isostatic pressing sintering (HIPping) technique on the hardness and toughness of ZTA ceramics. Addition of CeO₂ to ZTA ceramics leads to formation of a secondary phase (CeAl₁₁O₁₈) which played a vital role in affecting the Vickers hardness and toughness. Microstructure investigations showed that HIPping had a significant role in the removal of pores, and consequently affected both hardness and toughness of the samples. The highest Vickers hardness (1838.3 HV) and toughness (8.92 MPa·√m) were obtained with the 5 wt.% CeO₂ additions that also had the highest bulk density (4.48 g/cm³) and the lowest percentage of porosity (0.37%).     

Precision grinding of optical glass with laser micro-structured coarse-grained diamond wheels

This paper presents a series of micro-structured coarse-grained diamond wheels for optical glass surface grinding aiming to improve the grinding performance, especially subsurface damage. The 150 μm grit size, single layer electroplated diamond grinding wheels with different interval micro-groove arrays were manufactured by nanosecond pulsed laser, successfully. The influence of micro-structures on surface roughness and subsurface damage was investigated. Compared with conventional coarse-grained diamond wheel, the subsurface damage depth was reduced effectually from 5 to 1.5 μm, although the better surface roughness was not obtained by the micro-structured coarse-grained diamond wheel. In addition, the surface roughness and subsurface damage depth were both reduced with the decreasing interval of micro-groove arrays.     

Effect of reinforcement NbC phase on the mechanical properties of Al2O3-NbC nanocomposites obtained by spark plasma sintering

The sintering behavior of Al₂O₃-NbC nanocomposites fabricated via conventional and spark plasma sintering (SPS) was investigated. The nanometric powders of NbC were prepared by reactive high-energy milling, deagglomerated, leached with acid, added to the Al₂O₃ matrix in the proportion of 5 vol% and dried under airflow. Then, the nanocomposite powders were densified at different temperatures, 1450–1600 °C. Effect of sintering temperature on the microstructure and mechanical properties such as hardness, toughness and bending strength were analyzed. The Al₂O₃-NbC nanocomposites obtained by SPS show full density and maximum hardness value > 25 GPa and bending strength of 532 MPa at 1500 °C. Microstructure observations indicate that NbC nanoparticles are dispersed homogeneously within Al₂O₃ matrix and limit their grain growth. Scanning electron microscopy examination of the fracture surfaces of dense samples obtained at 1600 °C by SPS revealed partial melting of the particle surfaces due to the discharge effect.     

Investigation of microstructure and microhardness of pure W and W-2Y2O3 materials before and after ion-irradiation

Pure W and W-2Y₂O₃ materials were fabricated using powder metallurgy method. The microstructures of the materials were investigated by electron back-scattered diffraction and transmission electron microscopy techniques. Both materials contain 1–2 μm size W grains. In the case of W-2Y₂O₃, the material contains yttria particles having sizes between 300 and 900 nm. The W matrix in W-2Y₂O₃ shows stronger texture than that of pure W. Berkovich hardness values are 4.5 GPa in pure W and 4.9 GPa in W-2Y₂O₃ for a 10 N load. Ion irradiation experiments were performed on both materials at the JANNuS facility (Saclay, France) using Fe and He ions with energies of 24 MeV and 2 MeV, respectively. Radiation loops are present on the W grains whereas on yttria particles, radiation-induced damages appear as voids. Berkovich hardness values of irradiated materials are slightly higher than the non-irradiated materials. Results of the microstructure and microhardness of irradiated as well as non-irradiated materials are presented in detail.     

The aqueous electrophoretic deposition (EPD) of diamond–diamond laminates

The aqueous electrophoretic deposition (EPD) of a diamond/diamond laminate with two alternating grades of diamond was investigated. Diamond particles of average particle size 0.5 μm and 2 μm were deposited in an alternating manner onto tungsten carbide substrate. The layered diamond deposit was sintered with the carbide substrate in a high-pressure, high-temperature press. The sintered deposit was examined for evidence of alternating residual stresses. Differences of cobalt content in the 0.5 and 2 μm layers were observed by image analysis. The sintered diamond laminate demonstrated only minimal crack deflection during three-point bending.     

Electrically conductive ZTA–TiC ceramics: Influence of TiC particle size on material properties and electrical discharge machining

Processing of highly abrasive materials via powder injection molding or extrusion requires mold materials with high wear resistance to increase the durability of the tools and to sustain a high quality of the manufactured products. High performance ceramics which exhibit high hardness, bending strength and toughness show the perfect combination of properties for these applications. However they also have the usual drawback that they cannot be economically customized in complex shapes and low quantities, as they are required for tool and mold design. Recent material development enabled EDM of electrically conductive oxide ceramics, the most widespread machining process for machining of hard materials, as an alternative to conventional ceramic manufacturing and hard machining technologies.This study focuses on the influence of TiC particle sizes on material properties and EDM machinability of ZTA–TiC ceramics with 24 vol.% TiC, 17 vol.% ZrO₂ and 59 vol.% Al₂O₃. Fracture toughness, bending strength and electrical conductivity were analyzed for samples produced from TiC powders with particle sizes varying from 0.43 μm to 2.54 μm. Surface integrity of wire cut samples and feed rate during machining were investigated. It was shown that reducing the size of electrical conductive grains strongly increases the electrical conductivity and slightly decreases mechanical properties. Therefore also the machining characteristics are influenced by TiC grain size. The feed rate increases with decreasing particle size to a maximum at d₅₀ = 1–1.3 μm. Reduction of TiC particle size also leads to significantly decreasing surface roughness after the main cut. Additionally the necessary number of trimming steps to achieve a distinct surface roughness is also minimized for low particle sizes.     

Mechanical behavior of diamond matrix composites with ceramic Ti3(Si,Ge)C2 bonding phase

Polycrystalline diamond, PCD, compacts are usually produced by high pressure–high temperature (HP–HT) sintering. This technique always introduces strong internal stresses into the compacts, which may result in self-fragmentation or graphitization of diamond. This may be prevented by a bonding phase and Ti₃(Si,Ge)C₂ was so investigated. This layered ceramic was produced by Self Propagating High Temperature Synthesis and the product milled. The Ti₃(Si,Ge)C₂ milled powder was mechanically mixed, in the range 10 to 30 wt.%, with 3–6 μm diamond powder (MDA, De Beers) and compacted into disks 15 mm in diameter and 5 mm high. These were sintered at a pressure of 8.0 GPa and temperature of 2235 K in a Bridgman-type high pressure apparatus. The amount of the bonding phase affected the mechanical properties: Vickers hardness from 20.0 to 60.0 GPa and Young's modulus from 200 to 500 GPa, with their highest values recorded for 10 wt.% Ti₃(Si,Ge)C₂. For this composite fracture toughness was 7.0 MPa m^1/2, tensile strength 402 MPa and friction coefficient 0.08. Scanning and transmission electron microscopy, X-ray and electron diffraction phase analysis were used to examine the composites.     

Study on the microstructures,electrical resistance and mechanical properties of sputtering chromium target by HP,HIP and canning–HIP processes

In recent years, pure chromium (Cr) targets have been commonly used in metal surface coating treatment and flat-panel displays. In the traditional production of a pure Cr-target, there is a greater use of casting methods; however, the metal ingot frequently suffers from ingredient segregation, porosity and non-uniform microstructure defects. Powder metallurgy (PM) is a good method for fabricating high melting materials with better microstructure and properties. This study produced Cr targets using hot pressing (HP), hot isostatic pressing (HIP) and canning–HIP of PM technology. The experimental results showed that the Cr targets made by HP–HIP can further improve the density and mechanical properties. The relative density increases from 98.8% to 99.3%. Canning–HIP of the Cr target, in particular, can provide smaller grain size (50 μm), lower porosity about 0.3%, and increased relative density to 99.7%, with a TRS of up to 58 MPa. The canning–HIP process also shows the optimal electrical resistivity (8.003 × 10^− 5 Ω-cm), which suits for applications in the sputtering process.     

Reduced-temperature processing and consolidation of ultra-refractory Ta4HfC5

TaC, HfC, and WC powders were subjected to high-energy milling and hot pressing to produce Ta₄HfC₅, a composite of Ta₄HfC₅ + 30 vol.% WC, and a composite of Ta₄HfC₅ + 50 vol.% WC. Sub-micron powders were examined after four different milling intervals prior to hot pressing. XRD was used to verify proper phase formation. SEM, relative density, and hardness measurements were used to examine the resulting phases. Hot pressed compacts of Ta₄HfC₅ showed densification as high as 98.6% along with Vickers hardness values of 21.4 GPa. Similarly, Ta₄HfC₅ + 30 vol.% WC exhibited 99% densification with a Vickers hardness of 22.5 GPa. These levels of densification were achieved at 1500 °C, which is lower than any previously reported sintering temperature for Ta₄HfC₅. Microhardness values measured in this study were higher than those previously reported for Ta₄HfC₅. The WC additions to Ta₄HfC₅ were found to improve densification and increase microhardness.     

VC and Cr3C2 doped WCoB-TiC ceramic composites prepared by hot-pressing

The grain growth inhibitors (GGIs) VC and Cr₃C₂ doped WCoB-TiC ceramic composites were fabricated by hot-pressing. The microstructure, hardness, transverse rupture strength (TRS), fracture toughness (K_IC) and wear-resistance of WCoB-TiC ceramic composites were investigated. The results reveal that the grains can obviously become refined and the densification temperature of WCoB-TiC ceramic composites will be increased due to the VC and Cr₃C₂. The typical microstructure of WCoB-TiC ceramic composites mainly consist of bright W₂CoB₂ grains, gray TiC particles, dark TiB₂ and pores. WCoB-TiC ceramic composites doped with 0.3 wt% VC and 0.3 wt% Cr₃C₂ hot-pressing at 1420 °C show the optimum mechanical properties (hardness, TRS and K_IC are 92.6 HRA, 1976 MPa and 14.8 MPa m^1/2, respectively) and the best dry sliding wear-resistance.     

Grinding performance and workpiece integrity when superabrasive edge routing carbon fibre reinforced plastic (CFRP) composites

Data is presented for wheel wear, cutting forces and workpiece integrity when high speed routing 10 mm thick CFRP laminates using single layer electroplated diamond and CBN grinding points as opposed to standard end milling tools. A 60,000 rpm retrofit spindle was utilised to accommodate the 10 mm diameter wheels having grit sizes of 76, 151 and 252 μm employed under either roughing or finishing parameters. Wear of CBN points exhibited a near two-fold increase over diamond with a similar ratio for cutting forces. Despite use of flood cooling, point geometry when roughing compromised life and integrity due to excessive clogging.     

Densification and oxidation behavior of a novel TiB2–MoSi2–CrB2 composite

Titanium diboride (TiB₂) composite with MoSi₂ and CrB₂ has been prepared and tested to possess excellent oxidation resistance. Dense composite pellets were fabricated by hot pressing of powder mixtures. Microstructural characterization was carried out by XRD and SEM. Hardness and fracture toughness values were measured. Extensive oxidation studies of the composites were also carried out. Density of ≥ 96% ρ_th was obtained by hot pressing at 1800 °C under a pressure of 35 MPa for 1 h. Hardness and fracture toughness were in the range of 18–24 GPa and 3.5–4 MPa·m^1/2 respectively. Crack branching, deflection and bridging mechanisms were observed in the crack propagation paths. Isothermal and continuous oxidation studies of these composites up to 1000 °C showed improved oxidation resistance with the formation of protective glassy layer. TiO₂, Cr₂O₃ and SiO₂ phases were identified on the oxidized surface. Diffusion controlled mechanism of oxidation was observed in the composites.     

Fabrication of LiMn2O4 thin film cathode from chitosan-containing solution

Thin film of spinel LiMn₂O₄ was obtained by spin coating the chitosan-containing precursor solution on a platinumized Si substrate, followed by a two-step annealing procedure at 300 and 700 °C, respectively. It was demonstrated that the addition of the appropriate amount of chitosan to the precursor solution enhanced the deposition of LiMn₂O₄ films. The thickness of the deposited film from chitosan-containing precursor solution is about 5.2 μm after five-time spin coating under a spinning speed of 2500 rpm. Without the addition of chitosan in precursor solution, the deposited film was as thin as 0.16 μm under the same processing parameters. Furthermore, the electrochemical behavior for the deposited LiMn₂O₄ film calcined at 700 °C for 1 h was characterized by the charge–discharge test. The result shows that the 1st discharge capacity is 56.31 μAh cm⁻² μm⁻¹ at a discharge rate of C/2 and the fading rate of the discharge capacity is only 0.19% cycle⁻¹ after 50 cycles.     

Oxidation properties of self-propagating high temperature synthesized niobium disilicide

NbSi₂ monoliths were prepared by self-propagating high temperature synthesis (SHS) and hot pressing (HP) and their oxidation behavior was investigated at various temperatures (823–1123 K) in air. The combustion mode of SHS reaction was steady state combustion, and the combustion product was single-phase NbSi₂. Oxidation studies show that the highest mass gain was 0.95675 kg m⁻² at 1023 K. In cyclic oxidation, the oxidation rate was reduced and the mass gain was only 0.15507 kg m⁻². A dense protective amorphous SiO₂ scale formed at 823 K and 923 K whereas a porous multilayer SiO₂ and α/β-Nb₂O₅ oxide scales formed at and above 1023 K and spalled off. Pest oxidation of NbSi₂ monoliths was not observed in hot pressed NbSi₂ monoliths.     

Tungsten–vanadium–yttria alloys for fusion power reactors (I): Microstructural characterization

This study and a second part dedicated to the mechanical characterization provide a better knowledge of tungsten (W)–vanadium (V) alloys reinforced with yttrium oxide (Y₂O₃) particles, which have been scarcely investigated. Two W alloys (W-2 or 4 wt.% V-0.5 wt.% Y₂O₃) and a pure W material processed by powder metallurgy and consolidated by hot isostatic pressing were analysed. Along this part, the microstructure of the materials at room temperature is mainly analysed with a field emission scanning electron microscope.The densification in the compacts shows an increase with the V and Y₂O₃ additions. Porosity is reduced because of the formation of a W–V solid solution and V pools that fill the pores between the grains, although such effect is mainly observed in the W2V0.5Y alloy. The microstructure of pure W is composed of coarse polyhedral grains whereas a few coarse W grains, V pools and a nanostructured area, composed of fine W grains with dispersed Y, form the alloys. In contrast to previously studied W-4 wt.% V alloys, the V pools exhibit a reduction in the oxygen content, which prevents the formation of acicular oxide structures. Finally, the refinement of the microstructure induced by the addition of V and Y₂O₃ was analysed by electron backscattered diffraction measurements. Pure W presents high amount of grains over 1 μm (around 60% of the volume fraction) and only 2% below 100 nm. In the new alloys meanwhile, the population of micron size grains is highly reduced to less than 10% and grains smaller than 100 nm represent the 20%.     

SANS evidence for the dispersion of nanoparticles in W–1Y2O3 and W–1La2O3 processed by hot isostatic pressing

The development of a dispersion of nanoparticles in the W–1%Y₂O₃ and W–1%La₂O₃ (wt%) alloys processed by hot isostatic pressing have been investigated using small-angle neutron scattering. The analyses of the scattering data using the Beaucage unified approach reveal the presence of a bi-modal distribution of spherical scattering centers with sizes of less of 180 nm in these alloys. The mode values of these centers are found at ~ 10 and 40 nm in W–1%Y₂O₃, and at ~ 15 and 80 nm in W–1%La₂O₃. The scanning electron microscopy analyses showed the presence of small second phase particles. The contribution of the pore space to the scattering curves has been analyzed using the results obtained for pure W processed following the same procedure used for the alloys, and the porosity measurements of the samples.