Effect of particle size on the mechanical properties of reaction bonded boron carbide ceramics

In the present communication, effect of boron carbide particle size on the mechanical properties such as hardness, fracture toughness and flexural strength of reaction bonded boron carbide (RBBC) ceramics were investigated. RBBC composites were produced by the reactive infiltration of molten silicon into porous preform containing boron carbide and free carbon. Boron carbide powders with mean particle size of 18.65 μm, 33.70 μm and 63.35 μm were chosen for the RBBC composites. The experimental results show that hardness increases from 1261.70±64.74 kg/mm² to 1674.90±100.00 kg/mm² and fracture toughness drops from 5.76±0.26 MPa m^1/2 to 3.4±0.37 MPa m^1/2. However, flexural strength decreases from 403.41±5.70 MPa to 256.15±25.05 MPa with the increase in particle size. Indentation induced cracks in RBBC are mainly median type and number of cracks increase with the increase of starting particle size.     

CO2 laser peeling of Al2O3 ceramic and an application for the polishing of laser cut surfaces

A laser controlled fracture peeling technique is demonstrated to smooth the Al₂O₃ ceramic surface without thermal damages. It was found that a chip can be separated and curled from the ceramic surface during a focused CO₂ continuous wave (CW) laser dual-scanning. The thickness of the curled chip is ～50 μm and the formed subsurface roughness (R_a ≈ 2 μm) is close to the surface machined by mechanical breaking (R_a = 1.84 μm). The chip formation is attributed to the controlled fracture by the residual tensile stress in the recast layer, whereas the chip curling only occurs when the melting depth is shallower than the position of lateral cracks. The peeling technique can be applied to polish the cut surface of laser fusion cutting in ceramics. The polished cut surface (R_a = 2.18 μm) is free from recast, crack and heat effects. The microstructure is similar to the base material. The material removal rate during polishing is up to 0.125 mm³/s.     

Effect of dopants and sintering temperature on microstructure and low temperature degradation of dental Y-TZP-zirconia

Accelerated ageing of dental TZP were investigated at 134 °C for 2 h under 2.3 bar water vapor pressure. The TZP blanks were sintered in the range from 1350 to 1580 °C. The average grain size of 1350 and 1400 °C sintered materials were <0.3 μm whereas higher sintering temperatures led to larger grain sizes. The grain size and dopants influence the stability of tetragonal phase of zirconia under LTD conditions. The Y-TZP with average grain sizes <0.3 μm did not reveal the martensitic tetragonal-monoclinic phase transformation after ageing, whereas zirconia with grain sizes larger 0.3 μm showed fractions of monoclinic phase. Alumina and Ceria stabilized grain size and Y-TZP against LTD. Y-TZP with low amounts of Fe₂O₃ (<0.15%) used for coloring did not show any detrimental effects under LTD conditions. As the Y-TZP ceramics with grain size larger than 0.3 μm are not stable under LTD conditions they are not recommended for long term use in moist environment.     

Preparation of flat porous carbon films from paper-thin wood shavings and control of their mechanical,electrical and magnetic properties

A method for preparing flat porous carbonized films (FPCFs) by carbonizing paper-thin wood shavings was developed, and their structures and properties were investigated. The FPCFs were binder-free and had horizontal honeycomb structures consisting of macropores of 2–50 μm arising from tracheids and pittings. The FPCFs with approximate dimensions of 120 mm × 104 mm × 113 μm showed some flexibility. They were effectively reinforced and became twistable by introducing styrene–butadiene rubber (SBR) into the macropores via impregnation. The SBR-modified FPCFs carbonized at 1023 K retained electrical conductivity on the order of 10⁻³ S/m with the inclusion of SBR concentrations up to 15 mg/cm². The electrical conductivity of FPCFs carbonized at 773 K changed from nonconductive to 10⁻² S/m by impregnating the macropores with electrically conductive carbon paste or to 10⁵ S/m with Cu chemical plating. The FPCFs became responsive to a magnetic field by impregnating the macropores with a magnetic fluid or by creating ferrites through chemical reactions within the macropores.     

Enhanced oxidation resistance of ZrB2/SiC composite through in situ reaction of gadolinium oxide in patterned surface cavities

Micro-cavities on the surface of dense ZrB₂/20 vol.% SiC composites, machined by ultra-fast laser ablation, were filled with Gd₂O₃ nanopowder and oxidized in static air at 1600 °C. Optimized rectangular pattern of cavities, 10 μm diameter and deep, 20 μm apart conferred improved oxidation resistance compared to the untreated ZrB₂/20 vol.% SiC due to the formation of glasses of higher viscosity with lower oxygen diffusivities. Reduction of the oxidized depth was revealed by a significant decrease of 10 μm (60%) in the extent of the protective layer. The filled-cavity strategy leads to better protection against oxygen diffusivity into the composite without altering the bulk properties.     

Transesterified milkweed (Asclepias) seed oil as a biodiesel fuel

The methyl and ethyl esters of milkweed (Asclepias) seed oil were prepared and compared to soybean esters in laboratory tests to determine biodiesel fuel performance properties. The pour points of the methyl and ethyl milkweed esters measured −6 °C and −10 °C, respectively, which is consistent with the high levels of unsaturation characteristic of milkweed seed oil. The oxidative stabilities measured by OSI at 100 °C were between 0.8 and 4.1 h for all samples tested. The kinematic viscosities determined at 40 °C by ASTM D 445 averaged 4.9 mm²/s for milkweed methyl esters and 4.2 mm²/s for soybean methyl esters. Lubricity values determined by ASTM D 6079 at 60 °C were comparable to the corresponding soybean esters with average ball wear scar values of 118 μm for milkweed methyl esters and 200 μm for milkweed ethyl esters.     

Determination of fracture toughness of Y-TZP ceramics

The goal of this study is to determine the fracture toughness of 2Y-TZP and 2.5Y-TZP ceramics by single-edge V-notched beam (SEVNB) method and single-edge notched beam (SENB) method. The errors of fracture toughness values tested by SENB are also evaluated. The actual fracture toughness values obtained by SEVNB method are 6.4 ± 0.1 and 5.3 ± 0.1 MPa m^1/2 for 2Y-TZP and 2.5Y-TZP, respectively. After SENB method testing, the phase transformability (t-ZrO₂ → m-ZrO₂) on fractured surface is higher than that of SEVNB method testing. The relationship of fracture toughness values between by SEVNB and by SENB method is established.     

High power density in a piezoelectric energy harvesting ceramic by optimizing the sintering temperature of nanocrystalline powders

Piezoelectric energy harvesting is the research hotspot in the field of new energy, and its core is to prepare piezoelectric ceramics with high transduction coefficient (d₃₃ × g₃₃) and large mechanical quality factor (Q_m) as well. In addition, the miniaturization of the piezoelectric energy harvester also requires the material to have a submicron fine grain structure. In this work, submicron-structured ternary system, MnO₂-doped Pb(Zn_1/3Nb_2/3)O₃-Pb(Zr_0.5Ti_0.5)O₃ was constructed by pressureless sintering of nanocrystalline powders, which has been synthesized for the first time by high-energy ball milling route thereby evading the calcination stage. The microstructure and the energy harvesting characteristics were tailored through changing the sintering temperature. It was found that 1000 °C sintered fine-grained specimen (mean grain size ∼0.95 μm) showed the maximum d₃₃ × g₃₃ value of 9627 × 10⁻¹⁵ m²/N, meanwhile Q_m was as large as 774, which was almost seven times larger than pure counterpart. In the mode of the cantilever-type energy harvester, a high power density of 1.5 μW/mm³ were obtained for 1000 °C sintered specimen at a low resonance frequency of 90 Hz and acceleration of 10 m/s², which were further increased to 29.2 μW/mm³ when the acceleration increased to 50 m/s², showing the potential applications as a next generation high power multilayer energy harvester.     

Physicochemical properties of talc ore from three deposits of Lamal Pougue area (Yaounde Pan-African Belt,Cameroon), in relation to industrial uses

Three talc deposits were discovered at Ngoung, Lamal Pougue and Bibodi Lamal (Cameroon). They derived from ultramafic rocks and are enclosed in a Pan-African garnet and muscovite-bearing mica schist of the Yaoundé series. The physico-chemical properties of these talc deposits have been investigated by different techniques including Scanning Electron and Transmission Microscopy (SEM and TEM), chemical analyses, X-ray diffraction (XRD), infrared spectroscopy, particle size analysis by laser diffraction and low temperature gas absorption–desorption. The mineralogical composition deduced from XRD is wide (talc + chlorite + tremolite ± anthophyllite ± chromite ±serpentine ± brucite ± magnesite ± dolomite), but due to the high talc contents (≈ 90%) the samples are close to monomineralic. SEM studies reveal that all talc deposits comprise bundles of platy talc and a few prismatic crystals of amphiboles and other contaminating minerals. Laser diffraction confirms the coarse particle size of the talc crystals. Mode values are as high as 105–170 μm (except two samples displaying 76 and 42 μm) and d50 ranges from 107 to 25 μm. The values of specific surface area measured by BET and t-plot methods range from 1 to 6 m²/g and are correlated with external specific surface area measured by laser diffraction. Discrepancies from the trend are due to the semi-crystalline texture of the samples and mostly to intra-crystalline structural defects revealed by TEM observations. In infrared spectra, specific absorption bands are distinguished for talc, chlorite, tremolite, carbonates, serpentine, brucite and water. Occasional substitutions in minerals led to a shift in some absorption bands. The chemical composition criteria important for most of the industrial applications such as ceramics and pharmaceutics are closely complied with in untreated samples from these deposits. In summary, high talc proportions, chemical compositions, platy morphology and coarse grain size of its crystals lead to the conclusion that the studied deposits are economically attractive. The data set of the present work is an important tool for choosing the beneficiation methods for specific applications.     

Micronization of fenofibrate by rapid expansion of supercritical solution

Micronization of fenofibrate was investigated using rapid expansion of supercritical solution (RESS) process. Effects of pressure, temperature and nozzle on particle size were optimized using Taguchi's orthogonal array and analyzed using XRD, DSC, FT-IR, SEM, laser diffractometer and dissolution testing. Processed fenofibrate retained crystalline structure and has a similar chemical structure with unprocessed fenofibrate. The average particle size of fenofibrate was reduced from its original 68.779 ± 0.146 μm to 3.044 ± 0.056 μm under the optimum condition (T at 35 °C, P at 200 bar and nozzle diameter at 200 μm). The processed fenofibrate showed an enhanced dissolution rate by 8.13 times.     

Processing of Foturan® glass ceramic substrates for micro-solid oxide fuel cells

The microfabrication of Foturan^® glass ceramic as a potential substrate material for micro-solid oxide fuel cells (micro-SOFC) was investigated. Foturan^® was etched in 10% aqueous hydrofluoric (HF) acid solution at 25 °C with a linear rate of 22 ± 1.7 μm/min to create structures with an aspect ratio of 1:1 in 500 μm-thick Foturan^® substrates for micro-SOFCs. The concentration of the HF etchant was found to influence the etching rate, whereas the UV-exposure time creating nuclei in the glass for subsequent crystallization of the amorphous Foturan^® material had no significant influence on the etching rates. The surface roughness of the crystallized Foturan^® was determined by the crystallite size in the order of 10–15 μm. Free-standing micro-SOFC membranes consisting of a thin film Pt cathode, an yttria-stabilized-zirconia electrolyte and a Pt anode were released by HF etching of the Foturan^® substrate. An open-circuit voltage of 0.57 V and a maximum power density of 209 mW/cm² at 550 °C were achieved.     

Effect of laser scanning speed on geometrical features of Nd:YAG laser machined holes in thin silicon nitride substrate

0.5 mm thick Silicon nitride (Si₃N₄) substrates with MgO-Y₂O₃ additives were employed for hole machining study with a Nd:YAG two-dimensional laser machining (cutting) system. The effects of laser scanning speed on features of the machined holes such as hole diameter, hole circularity, taper angle, heat affected zone (HAZ), recast layer, and micro-cracks were studied. The results show that the diameters at the front side are larger than the back side for all holes machined at different spot scanning speed. The taper angle of the machined holes decreases, while the hole circularity increases with the increase of the spot scanning speed. In addition, the heat-affected-zone (HAZ) was observed clearly around the back side of drilled holes, whose area decreases with the increase of the laser spot scanning speed. The result shows that the HAZ is the largest when the laser scanning speed is 20 mm/min. Nevertheless, the machined hole did not completely cross through the thickness of the substrate when the laser scanning speed was 60 mm/min. To obtain holes with relatively good quality, laser scanning speed should be controlled between 30 mm/min and 50 mm/min.     

Particulate carbon in precipitation at European background sites

The particulate carbon content of precipitation was investigated in samples collected at five background sites located over a west-east European transect, from the Azores, in the mid-Atlantic Ocean, to the Hungarian plain, in central Europe. Sampling was performed on an event basis and the particulate carbon (elemental carbon, EC, and water insoluble organic carbon, WIOC) content was concentrated on quartz filters for the subsequent analysis by a thermal optical method in order to separate the EC and WIOC fractions. The average EC concentrations range from low values at the Azores (2.8±4.3 μg C L^?1) and at the high mountain site of Sonnblick (5.2±3.7 μg C L^?1) to high values at the more inland sites of Schauinsland (28±38 μg C L^?1) and K-Puszta (24±24 μg C L^?1). The average WIOC concentrations range from 98±56 μg C L^?1 at the coastal site of Aveiro and 113±78 μg C L^?1 at the Azores to 358±194 μg C L^?1 at the continental site of K-Puszta. These results are discussed in terms of factors affecting the spatial distribution of particulate carbon, such as emissions from surrounding areas and prevalent meteorological conditions. EC is found to be a minor contributor to total particulate carbon present in rain and snow samples (from 2.5% to 15%). This is particularly true at the remotes sites, where the EC contribution to total particulate carbon is <6.5%, consistent with a negligible impact of anthropogenic combustions locally. The EC and WIOC scavenging ratios were estimated and compared with those of sulfate, also evaluated at the same sampling sites. The results indicated that EC is removed from the atmosphere by wet deposition less efficiently than WIOC, and in turn this species is removed less efficiently than sulfate.     

Crack healing behaviour of Cr2AlC MAX phase studied by X-ray tomography

The autonomous crack-healing capability of Cr₂AlC MAX phase ceramic by surface oxidation at elevated temperatures has a huge potential for high temperature structural and protective coating applications. In this work we use time-lapse X-ray computed tomography (CT) to track the fine details of local crack filling phenomena in 3 dimensions (3D) with time. The maximum crack width that could be fully healed upon exposure to 1200 °C in air is 4.8 μm in 4 h and 10 μm after 12 h. Furthermore, during healing Cr₇C₃ phase is observed beneath the dense Al₂O₃ layer (average thickness of 1 μm on each crack surface) when the crack width exceeds 2 μm. The 3D image sequences indicated that the rate of healing is essentially independent of position along, or across, the crack faces. The crack healing kinetics of Cr₂AlC at 1200 °C broadly follows a parabolic rate law with a rate constant of 4.6 × 10⁻⁴ μm² s⁻¹. The microstructure, composition and thickness of the oxide scale in the healed crack area are characterized via post mortem SEM-EDS measurements and confirm the formation of an initial dense alumina layer on top of which a more porous layer forms. Impurity Cr particles appear to accelerate the oxidation process locally and correlative SEM imaging of the same region suggests this is by providing Cr₂O₃ nucleation sites.     

New laser machining technology of Al2O3 ceramic with complex shape

A new method was developed for the fabrication of complex-shaped Al₂O₃ ceramic parts by combining laser machining and gelcasting technique. The unwanted ceramic powders parts were selectively removed by laser machining specified by a computer program, and the gelcast Al₂O₃ green bodies were machined to a designed shape by a CO₂ laser at a wavelength of 10.6 μm. The influences of solid loading, laser output power, scanning speed and nitrogen purge on the machining of green Al₂O₃ ceramic bodies were studied. The experimental parameters were optimized, the green Al₂O₃ bodies with solid loading of 40 vol% or below were easier to be machined, while the green bodies with solid loading of 45 vol% or above were hard to be further machined due to the surface sintering. Better machining quality and deeper machining depth could be obtained when the laser power is 30 W. The green Al₂O₃ bodies with complex shape were obtained by the laser machining.     

Micromoulding of PZT film structures using electrohydrodynamic atomization mould filling

In this work, electrohydrodynamic atomization combined with a photolithography polymeric micromoulding technique was used to form PZT ceramic structures. PZT thick film structures consisting of squares and rectangles of various sizes and separations were produced and used to evaluate the process. An expansion effect of approximately 10 μm on the ceramic structure width relative to the 200 μm wide mould design was observed. The minimum continuous gap between features achieved using this process was 13.5 μm, and the smallest regular PZT square structure obtainable was 106 μm in width. A sloping side wall of the PZT structures caused by the shielding of the photoresist mould was also observed in the process. The resulting PZT structures had a homogenous microstructure and exhibited a relative permittivity of 250, d_33, f of 67 pCN^?1 and remnant polarisation of 8.8 μC/cm².     

Ceramic micro parts. Part 1: How thermal debinding can be utilized to enhance surface finish and mechanical properties

Thermal debinding represents the most critical processing step of powder injection moulding (PIM) of ceramics. Defects such as cracks and pores might be caused, when the process cannot be controlled properly. Considering low-pressure injection moulding (LPIM), however, thermal debinding opens up the possibility to enhance the mechanical properties of ceramic micro parts. In this study, the unique effect of surface defect healing is presented, which takes place during debinding. It enables improved surface finish and results in increased mechanical strength and reliability. As a model, 3Y-TZP micro bending bars with dimensions of 200 μm × 200 μm × 1200 μm were selected. It could be revealed that thermal debinding can be utilized to increase the characteristic 3-point-bending strength up to 3235 MPa with Weibull modulus of 21.4. This result corresponds to macroscopic bending strength of 1727 MPa, which can be achieved only by exhausting fabrication methods and surface post-processing.     

Tribological behaviour of RF-magnetron sputter deposited hydroxyapatite coatings in physiological solution

The aim of the paper is to explore the tribological performance of hydroxyapatite (HA) coatings deposited by radio frequency (RF) magnetron sputtering on AZ31 magnesium alloy (96% Mg, 3% Al, 0.7% Zn, 0.3% Mn) for biomedical applications. In this study, the position of the samples on a substrate holder, relative to a target erosion zone was taken into consideration in order to elucidate its impact on the coating characteristics, such as composition, morphology, surface topography and tribology. Substrate rotation and arc-movement were foreseen in the experimental set-up to increase the uniformity of thin film properties. The deposited HA thin films were revealed to exhibit an increase of the Ca/P ratio from 1.83 to 1.97, a decrease of (002) texture and thickness, as the samples were shifted towards the target erosion zone. By coatings, the roughness of Mg alloy was decreased (R_{a Mg alloy}=31.3 nm; R_{a coating}=29 nm and 21 nm). The coating placed in the centre of the substrate holder showed high hardness and Young's modulus (H =8.3±0.9 GPa; E=89±10 GPa) than the coating prepared under the target erosion zone (H =6.9±1.1 GPa; E=75±6 GPa). The coating deposited under target erosion zone exhibits superior friction behaviour in simulated body fluid environment, with the friction coefficient (μ) of 0.184, while the sample located in the centre of the substrate holder possesses the friction coefficient (0.306) comparable to the AZ31 substrate (0.307). The low wear rate was determined in the case of coating deposited under target erosion zone (4.83×10⁻⁵ mm³ N⁻¹ m⁻¹) than uncoated AZ31 substrate (0.00518 mm³ N⁻¹ m⁻¹) or than coating placed in the centre of the substrate holder (0.00294 mm³ N⁻¹ m⁻¹).     

Fabrication of micro-scale textured grooves on green ZrO2 ceramics by pulsed laser ablation

The green ZrO₂ ceramics were fabricated by cold isostatic pressing. Pulsed laser ablation with a wavelength of 1064 nm was performed to fabricate micro-scale textured grooves on the surface of green ZrO₂ ceramics. The influence of laser parameters on surface quality was studied. The heat-affected zone around the machined grooves and micromorphology of laser-irradiated surface were investigated. Results showed that micro-scale textured grooves with a width of 30–50 µm and a depth of 15–50 µm on the green ZrO₂ ceramic surfaces were successfully fabricated by pulsed laser ablation. The laser parameters had a profound influence on the surface quality of micro-scale textured grooves. Better surface quality could be obtained with frequency below 40 Hz, power below 6 W, and scanning velocity above 200 mm/s. A sintering layer was found on the laser-irradiated surfaces when frequency was above 60 Hz, power was above 10 W, and scanning velocity was below 150 mm/s. Analysis of this sintering layer revealed clear melting and resolidification of ZrO₂ particles.     

Effect of graphene addition on the mechanical and electrical properties of Al2O3-SiCw ceramics

This paper presents a study on graphene-reinforced Al₂O₃-SiCw ceramic composites and the relationship between graphene oxide (GO) loading and the resulting mechanical and electrical properties. Well-dispersed ceramic-GO powders were fabricated using a colloidal processing route. Dense composites were obtained via spark plasma sintering, a technique that has the ability to reduce GO to graphene in situ during the sintering process. The mechanical properties of the sintered composites were investigated. The composite with only a small amount of graphene (0.5 vol.%) showed the highest flexural strength (904 ± 56 MPa), fracture toughness (10.6 ± 0.3 MPa·m^1/2) and hardness (22 ± 0.8 GPa) with an extremely good dispersion of graphene within the ceramic matrix. In addition to these exceptional mechanical properties, the sintered composites also showed high electrical conductivity, which allows the compacts to be machined using electrical discharge machining and thus facilitates the fabrication of ceramic components with sophisticated shapes while reducing machining costs.