Thermal shock behavior of Ti2AlC from 200°C to 1400°C

The thermal shock behavior of Ti₂AlC synthesized by means of self‐propagating high‐temperature combustion synthesis with pseudo hot isostatic pressing is investigated, with a focus on the effect of the quenching temperature and quenching times. In general, Ti₂AlC exhibits a better thermal shock resistance than typical brittle ceramics like Al₂O₃. Although the flexural strength decreases quickly in the temperature range of 300°C‐500°C, no discontinuous decrease in the retained strength is observed in Ti₂AlC which, as with other MAX phases, differs from the behavior of typical brittle ceramics. Overall, the initial strength (grain size) plays a determining role in the thermal shock behavior of Ti₂AlC and other MAX phases. On increasing quench times to 5 cycles, the retained flexural strength decreases further, however with a lower rate of decrease compared with the first quench. Quenching at 300°C and above, voids after the pullout of grains and cracks are present, which however are absent in the un‐quenched samples, indicating the weakening of bonding among grains and the induced damage around the grain boundary during the thermal shock.     

Oxidation Behavior of SiC Whiskers at 600–1400°C in Air

The oxidation behavior of SiC whiskers (SiC_W) with a diameter size of 50–200 nm has been investigated at 600°C–1400°C in air. Experimental results reveal that SiC_W exhibit a low oxidation rate below 1100°C while a significant larger oxidation rate after that. This can be attributed to the small diameter size of SiC_W, which determines that it is hard to form a protective SiO₂ layer thick enough to hamper the diffusion of oxygen effectively. Both nonisothermal and isothermal oxidation kinetics were studied and the apparent oxidation energy was calculated to further understand the oxidation behavior of the SiC_W.     

High‐Temperature Oxidation of ZrB2–SiC–AlN Composites at 1600°C

The effect of AlN substitution on oxidation of ZrB₂–SiC was evaluated at 1600°C up to 5 h. Replacement of ZrB₂ by AlN, with 30 vol% SiC resulted in improved oxidation resistance with a thinner scale and reduced oxygen affected area. On the other hand, substitution of AlN for SiC resulted in a deterioration of the oxidation resistance with an abnormal scale and significant recession. The effect of SiC content was also studied, and was found to be consistent with the literature for the composites without AlN additions. A similar effect was observed when AlN was added, with the higher SiC content materials showing improved oxidation resistance. X‐ray photoelectron spectroscopy showed the presence of Al₂O₃ and SiO₂ on the surface, which could possibly lead to a modification in the viscosity of the glassy oxide scale. Possibly, the oxidation behavior of ZrB₂–SiC composites can be improved with controlled AlN additions by adjusting the Al:Si ratios.     

Wear of zirconia-dispersed alumina at ambient temperature, 140 °C and 250 °C

Commercial grade alumina along with 5, 10, 15 and 20 wt.% zirconia-dispersed aluminas were tested for their wear resistance at ambient temperature, 140 °C and 250 °C using a pin on disk tribotester fitted with a hot stage. The sample suite was investigated for physical characteristics including hardness, fracture toughness, bulk density, alumina grain size and zirconia grain size. The wear track and wear debris were investigated using profilometry, SEM as well as TEM.

The 5 wt.% zirconia-dispersed aluminas had the lowest wear volume loss over the temperature range. The alumina sample exhibited a wear dependence with relative humidity which is attributed to the formation of a tribochemical layer. Investigation of the tribochemical layer using SEM/EDS and TEM electron diffraction showed the tribochemical layer to be aluminium hydroxide. The major wear mechanism for all samples was brittle fracture.     

Oxidation behavior of C–SiC composites with a Si–W coating from room temperature to 1500°C

Oxidation tests of carbon fiber reinforced silicon carbide composites with a Si–W coating were conducted in dry air from room temperature to 1500°C for 5 h. A continuous series of empirical functions relating weight change to temperature after 5 h oxidation was found to fit the test results quite well over the whole temperature range. This approach was used to interpret the different oxidation mechanisms. There were two cracking temperatures of the matrix and the coating for the C–SiC composite. Oxidation behavior of the C–SiC composite was nearly the same as that of the coated C–C composite above the coating cracking temperature, but weight loss of the C–SiC composite was half an order lower than that of the coated C–C composite below the cracking temperature. As an inhibitor, the SiC matrix increased the oxidation resistance of C–SiC composites by decreasing active sites available for oxidation. As an interfacial layer, pyrolytic carbon decreased the activation energy below 700°C. From 800°C to 1030°C, uniform oxidation took place for the C–SiC composite, but non-uniform oxidation took place for the coated C–C composite in the same temperature range. The Knudsen diffusion coefficient could be used to explain the relationship between weight loss and temperature below the coating cracking temperature and the matrix cracking temperature.     

Resistivity and Thermal Reproducibility of High‐Density Polyethylene Heaters Filled With Carbon Black

Summary: Various output heaters were extruded with CB‐filled HDPE composites. The effects of crystallinity on the PTC and thermal reproducibility of the quenched, annealed, and E‐beam crosslinked heaters were examined during heating and cooling cycles at an applied voltage of 220 V. Conductor resisitivity and PTC effect of the heaters increased as crystallinity of composites increased. During the thermal cycling test, significant changes in heater‐output and resistivity for annealed and quenched heaters were observed. However, for quenched/E‐beam radiated and annealed/E‐beam radiated heaters no significant difference was found. These results indicate that the annealing process did not affect the thermal and electrical reproducibility of HDPE/CB heaters significantly.

Acetylene black aggregates in polyethylene matrix.     

Oxidation behavior of oxidation protective coatings for PIP-C/SiC composites at 1500 °C

Three-dimensional carbon fiber reinforced silicon carbide (C/SiC) composites were fabricated by precursor infiltration and pyrolysis (PIP) with polycarbosilane as the matrix precursor, SiC coating prepared by chemical vapor deposition (CVD) and ZrB₂-SiC/SiC coating prepared by CVD with slurry painting were applied on C/SiC composites, respectively. The oxidation of three samples at 1500 °C was compared and their microstructures and mechanical properties were investigated. The results show that the C/SiC without coating is distorted quickly. The mass loss of SiC coating coated sample is 4.6% after 2 h oxidation and the sample with ZrB₂-SiC/SiC multilayer coating only has 0.4% mass loss even after oxidation. ZrB₂-SiC/SiC multilayer coating can provide longtime protection for C/SiC composites. The mode of the fracture behavior of C/SiC composites was also changed. When with coating, the fracture mode of C/SiC composites became brittle. When after oxidation, the fracture mode of C/SiC composites without and with coating also became brittle.     

The start‐up of anaerobic sequencing batch reactors at 20 °C and 25 °C for the treatment of slaughterhouse wastewater

The objective of this research was to evaluate the feasibility, the stability and the efficiency of a start‐up at 20 °C and 25 °C of anaerobic sequencing batch reactors (ASBRs) treating slaughterhouse wastewater. Influent chemical oxygen demand (COD) and suspended solids concentrations averaged 7500 and 1700 mg dm^?3, respectively. Reactor start‐up was completed in 168 and 136 days at 20 °C, and 25 °C, respectively. The start‐up process was stable at both temperatures, except for a short period at 20 °C, when effluent volatile fatty acid (VFA) concentrations increased from an average of 40 to 400 mg dm^?3. Effluent quality varied throughout start‐up, but in the last 25 days of the experiment, as the ASBRs were operated under organic loading rates of 2.25 ± 0.21 and 2.86 ± 0.24 kg m^?3 d^?1 at 20 °C and 25 °C, respectively, total COD was reduced by 90.3% ± 1.3%. Methanogenesis was not a limiting factor during start‐up. At 20 °C, the limiting factor was the acidification of the soluble organics and, to a smaller extent, the reduction of propionic, isobutyric and isovaleric acids into lower VFAs. At 25 °C, the limiting factor was the hydrolysis of particulate organics. To minimize biomass loss during the start‐up period, the organic loading rate should be increased only when 75 –80% of the COD fed has been transformed into methane within the design hydraulic retention time. © 2001 Society of Chemical Industry     

Fatigue of three advanced SiC/SiC ceramic matrix composites at 1200°C in air and in steam

High‐temperature mechanical properties and tension‐tension fatigue behavior of three advanced SiC/SiC composites are discussed. The effects of steam on high‐temperature fatigue performance of the ceramic‐matrix composites are evaluated. The three composites consist of a SiC matrix reinforced with laminated, woven SiC (Hi‐Nicalon?) fibers. Composite 1 was processed by chemical vapor infiltration (CVI) of SiC into the Hi‐Nicalon? fiber preforms coated with boron nitride (BN) fiber coating. Composite 2 had an oxidation inhibited matrix consisting of alternating layers of silicon carbide and boron carbide and was also processed by CVI. Fiber preforms had pyrolytic carbon fiber coating with boron carbon overlay applied. Composite 3 had a melt‐infiltrated (MI) matrix consolidated by combining CVI‐SiC with SiC particulate slurry and molten silicon infiltration. Fiber preforms had a CVI BN fiber coating applied. Tensile stress‐strain behavior of the three composites was investigated and the tensile properties measured at 1200°C. Tension‐tension fatigue behavior was studied for fatigue stresses ranging from 80 to 160 MPa in air and from 60 to 140 MPa in steam. Fatigue run‐out was defined as 2 × 10⁵ cycles. Presence of steam significantly degraded the fatigue performance of the CVI SiC/SiC composite 1 and of the MI SiC/SiC composite 3, but had little influence on the fatigue performance of the SiC/SiC composite 2 with the oxidation inhibited matrix. The retained tensile properties of all specimens that achieved fatigue run‐out were characterized. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Oxidation of ZrB2–SiC‐Graphite Composites Under Low Oxygen Partial Pressures of 500 and 1500 Pa at 1800°C

The oxidation behavior of ZrB₂–SiC‐graphite composites under low oxygen partial pressures of 500 and 1500 Pa at 1800°C was investigated. The phase composition and microstructure of the oxidized scale were characterized using TEM, SEM, XRD, XPS, EDS. The analytical results indicated that a low oxygen partial pressure had a remarkable effect on the oxidation mechanism of ZrB₂–SiC‐graphite composites. When oxidized at 1500 Pa, the oxidation kinetics was controlled by the rate of oxygen diffusion into the composite. When the composite was oxidized at 500 Pa, control of the oxidation kinetics changed from the rate of oxygen diffusion to the rate of the oxidation reaction. The rate of oxidation decreased with decreasing oxygen partial pressure. Higher partial pressures of oxygen resulted in less oxidation resistance by the ZrB₂–SiC‐graphite composites.     

Investigation of emissions from heated essential‐oil‐rich fuels at 200 °C

Essential oil of fuels is closely linked with the behavior of forest fires, especially high intensity fires and eruptive fires. It is assumed that the potential reason is the large quantities of flammable gases released from essential oil‐rich fuels before pyrolysis in fire environment. However, few studies have been carried out on the hypothesis. The purpose of the present study is to investigate the emissions from essential oil‐rich fuels. The fuels were collected from three coniferous species. In the experiment, needles and twigs were heated in a vacuum oven at 200 °C, and the emissions within 15 min had been sampled using Tenax tubes. Gas chromatography–mass spectrometry served as an analytical instrument. The results showed that the emissions contained high proportion of monoterpenes, such as α‐pinene, camphene, β‐pinene, 3‐carene, and d ‐limonene. The monoterpene emissions from heated needles and twigs of Pinus pumila, Larix gmelinii, and Pinus sylvestris were 61.221, 49.606, and 37.853 µg g^?1 dry weight (needles), and 211.727, 139.957, and 121.505 µg g^?1 dry weight (twigs), respectively. Statistical analyses showed the significant differences not only among species but also between needles and twigs. Copyright © 2012 John Wiley & Sons, Ltd.     

Effect of AlN Substitutions on the Oxidation Behavior of ZrB2–SiC Composites at 1600°C

The oxidation behavior of ZrB₂–SiC composites, with varying amounts of AlN substituting for ZrB₂, was studied isothermally under static ambient air at 1600°C for up to 5 h. Small amounts of AlN substitutions (≤10 vol%) were found to result in marginal improvement in the oxidation resistance, whereas larger amounts resulted in a significant deterioration. The size of ZrO₂ clusters formed on the oxidized surface was found to be a function of the AlN content. This effect was more pronounced after longer oxidation times (~1 h) as opposed to shorter durations (~5 min). It was postulated that presence of AlN results in the formation of Al₂O₃ during the oxidation process, subsequently resulting in a lowering of viscosity of the glassy silica scale, which facilitates the coarsening of ZrO₂ clusters. This also increases oxygen permeation through the scale which adversely affects the oxidation resistance of the high AlN content composites.     

Two‐step synthesis of zirconolite‐rich ceramic waste matrice and its physicochemical properties

In this study, the synthesis of single‐phase zirconolite powder was explored using two‐step route of combustion synthesis (CS) plus acid treatment. Zirconolite/Cu composite was firstly produced from the combustion reaction using CuO and Ti as the oxidant and reductant. After pickling and desiccation, refined zirconolite‐rich ceramic powder was obtained with bimodal particle size distribution. The ceramic powder was finally preformed and calcined at 1050‐1300°C for 6‐48 hours, which resulted in bulk density and Vickers hardness of 4.02 g/cm³ and 11.54 GPa after sintering at 1100°C for 18 hours. Aqueous durability of the calcined waste matrice was evaluated according to MCC‐1 standard. The 42 days normalized leaching rates of Ca, Ti and Zr were measured to be 3.96 × 10^?3, 4.52 × 10^?6 and 1.54 × 10^?6 g·m^?2·d^?1.     

Creep in Interlaminar Shear of a Nextel™720/aluminosilicate Composite at 1100°C in Air and in Steam

Creep in interlaminar shear of an oxide–oxide ceramic composite was evaluated at 1100°C in air and in steam. Composite consists of a porous aluminosilicate matrix reinforced with mullite/alumina (Nextel^?720) fibers, has no interface between fibers and matrix, and relies on the porous matrix for flaw tolerance. The interlaminar shear strength was 7.6 MPa. Creep behavior was examined for shear stresses of 2–6 MPa. Creep run‐out of 100 h was not achieved. Larger creep strains and higher creep strain rates were produced in steam. However, steam had a beneficial effect on creep lifetimes. Composite microstructure, damage, and failure mechanisms were investigated.     

Separating Test Artifacts from Material Behavior in the Oxidation Studies of HfB2–SiC at 2000°C and Above

Oxidation characteristics of HfB₂‐15 vol% SiC prepared by field‐assisted sintering was examined at 2000°C by heating it in a zirconia‐resistance furnace and by direct electrical resistance heating of the sample. Limitations of the material and the direct electrical resistance heating apparatus were explored by heating samples multiple times and to temperatures in excess of 2300°C. Oxide scales that developed at 2000°C from both methods were similar in that they consisted of a SiO₂/HfO₂ outer layer, a porous HfO₂ layer, and a HfB₂ layer depleted of SiC. But they differed in scale thicknesses, impurities present, scale morphology/complexity. Possible test artifacts are discussed.     

Sintering of aluminum nitride by using alumina crucible and MoSi2 heating element at temperatures of 1650 °C and 1700 °C

Aluminum nitride (AlN) ceramics, prepared with Y₂O₃ and CaO sintering additives, have been densified in an Al₂O₃ crucible at temperatures of up to 1650 °C and 1700 °C using a conventional MoSi₂ heating element furnace. The results of this study show that relative densities in excess of 99% of theoretical and a relatively high-thermal conductivity of 147 W m⁻¹ K⁻¹ have been achieved for feedstock materials prepared with combined addition of 1 wt.% Y₂O₃ and 1 wt.% CaO. All of the phases in sintered samples have been shown to be crystalline AlN and minor amount of secondary phases, were detected such as enriched Y- and Ca-aluminates by the XRD patterns, back-scattered imagery and microprobe analysis. The advantage of using the particular experimental system and sintering condition is considered to be amenable to lower production cost and enhance the feasibility of mass production. Critical temperature for AlN densification to obtain the highest density is about 1650 °C.     

High‐temperature calorimetric study of oxide component dissolution in a CaO–MgO–Al2O3–SiO2 slag at 1450°C

Blast‐furnace slags are formed, as iron ore is reduced to metal, as a molten a mixture of refractory and not easily reducible oxides, largely silica, alumina, lime, and magnesia. Their relatively low silica content makes them basic and poor glass formers. Their thermodynamic properties, though important for modeling their formation and reactivity, as well as furnace heat balance, are poorly known. Solution calorimetry of small amounts of solid oxides in a molten oxide solvent at high temperature (up to about 1500°C) permits direct assessment of energetics of dissolution. The enthalpies of solution of slag forming oxides: CaO, SiO₂, Al₂O₃, MgO, and Fe₂O₃ in a simplified model slag of composition: CaO (45.9 mol%), SiO₂ (35.1 mol%), Al₂O₃ (8.3 mol%), MgO (10.7 mol%) were measured by high‐temperature drop solution calorimetry at 1450°C. For this slag composition, enthalpies of solution become more exothermic in the order: Fe₂O₃ (279.3 ± 20.8 kJ/mol), MgO (56.7 ± 9.1 kJ/mol), Al₂O, (41.6 ± 11.3 kJ/mol), CaO (?4.3 ± 2.3 kJ/mol), and SiO₂, (?20.4 ± 4.4 kJ/mol), reflecting the relatively basic character of this low‐silica melt. Within these fairly large experimental errors, characteristic of calorimetry at this high temperature, there is little or no discernible concentration dependence for these heats of solution. The trends seen for these five solutes parallel those seen for heats of solution of the same oxides in other melts at various temperatures, with changes in magnitude reflecting the differences in acid‐base character of the melts. The new data for quartz show systematic behavior which extends the range of basicity studied for the enthalpy of dissolution of silica. The results provide reliable data for future modeling of the thermal balance of steel‐making furnaces and geologic and ceramic systems.     

Performance of Ni‐based Anode‐Supported SOFCs with Doped Ceria Electrolyte at Low Temperatures Between 294 and 542°C

The performance of a conventional anode‐supported microtubular SOFC using doped ceria as an electrolyte and Ni‐based cermet as an anode is evaluated at low operating temperature between 294 and 542°C. An open‐circuit voltage (OCV) of >0.9 V is obtained at all measured operating temperatures, and power generation is observed at temperatures as low as 294°C. The power density of the cell is 0.6 W/cm² at 542°C operating temperature with 47% fuel utilization and is 5 mW/cm² at 294°C operating temperature with an open‐circuit voltage of 0.95 V. According to impedance spectroscopy, a greater influence of gas flow rate, on the cell performance, is observed at higher operating temperature.     

Hydrothermal synthesis (200 °C) of Co–kaolinite and Al–Co–serpentine

In the systems CoO–Al₂O₃–SiO₂–H₂O and CoO–Al₂O₃–SiO₂–HCl–H₂O, at initial pH between 5.5 and 8.1 and temperature of 200 °C, kaolinite is unstable and the following phases form through a dissolution-precipitation process: a) kaolinite and Co-bearing kaolinite; b) Al–Co–serpentine; and c) poorly crystalline phases. Identification of the several phases was carried out from a combination of X-ray diffraction and transmission/analytical electron microscopy.Co–kaolinite shows variable morphologies: a) Platy lath-shaped particles with very low Co content; b) Spherical particles, with relatively constant Co contents (in the order of 0.10 apfu); c) Kaolinite stacks with very variable Co contents (up to 0.25 apfu). Analytical data indicate that the presence of Co(OH)₂ in the system favors the dissolution process as well as serpentine formation but it leads to the parallel formation of abundant poorly crystalline phases. The Co-content in kaolinite increased as a function of the Co(OH)₂/CoCl₂ ratio in the initial systems, and it is reflected by a parallel increase of the b-cell parameter of kaolinite. The average composition of the coexisting Al–Co–serpentine is: (Al_1.20Fe_0.11Co_1.27)(Si_1.64Al_0.36)O₅(OH,Cl)₂, with Cl contents in the order of 0.14 apfu.The assemblage Co–kaolinite + Al–Co–serpentine, which appears to be stable at 200 °C, has not been described in natural environments, probably because it requires unusual Al- and Co-rich chemical systems.     

Conversion of calcium aluminate cement hydrates at 60°C with and without water

There have been different hypotheses about the transformation mechanisms of calcium aluminate cement hydrates and this work aims to clarify the long‐running debate about the conversion approaches. In this work, CAH₁₀ and C₂AH₈ were produced from the pastes of calcium aluminate cement (CAC) cured for 24 hours at 10 and 20°C separately. And the cured pastes were continually cured at 60°C for 3 days with water and without water, respectively. The hydration of the pastes was halted by freeze‐drying, and the phases and microstructure of hydrates were investigated by XRD and SEM, respectively. The results indicate that CAH₁₀ and C₂AH₈ converted into C₃AH₆ and AH₃ in water presence at 60°C, but did not transform into C₃AH₆ and AH₃ without water. It is confirmed that the conversion of CAH₁₀ and C₂AH₈ to C₃AH₆ and AH₃ happens through preceding solution of CAH₁₀ and C₂AH₈ and subsequent precipitation of C₃AH₆ and AH₃.