Microstructures and Properties of W-Ti Alloys Prepared Under Different Cooling Conditions

W-(10 to 15) wt.% Ti alloys were sintered at 1400 or 1500 °C and cooled under different cooling conditions. The microstructures and properties of W-Ti alloys were affected by the cooling conditions. XRD, SEM, EBSD, and TEM were carried out to investigate the effects of cooling conditions and sintering temperature on the microstructures of W-Ti alloys. The nanohardness and elastic modulus of the alloys were also investigated. The results showed that when the temperature was 1500 °C, the content of Ti-rich phase in W-(10 to 15) wt.% Ti alloys decreased obviously with the increase of cooling rate (the average cooling rate of furnace cooling, air cooling and water cooling was 0.2, 10, and 280 °C/s, respectively). For the W-10 wt.% Ti alloy, the content decreased from 20.5 to 9.7%, and the grain size decreased from 2.33 to 0.67 μm. When the temperature decreased to 1400 °C, the grain size was also decreased sharply with the increase of cooling rate, but there was a little change in the microstructure. Meanwhile, the grain sizes were smaller than those of the alloys sintered at 1500 °C. The nanohardness and elastic modulus increased with the increase of cooling rate, and the alloys sintered at different temperatures had different nanohardness and elastic modulus which depended on the cooling conditions. Sintering at a proper temperature and then cooling at a certain cooling condition was a useful method to fabricate alloy with less Ti-rich phase and high properties.     

Tribological and Thermal Properties of Mullite Coating Prepared by Atmospheric Plasma Spraying

The primary mullitized andalusite powders were spray-dried and heat-treated to improve sprayable capability. Then, mullite coating was deposited by atmospheric plasma spraying and heat treatment was contributed to recrystallization of the amorphous phase present in the as-sprayed mullite coating. Scanning electron microscopy and x-ray diffraction were used to characterize the microstructure and phase composition of mullite coating. Meanwhile, the phase transition temperature, enthalpy, and specific heat capacity of as-sprayed coatings as well as recrystallized mullite coatings were determined by means of differential scanning calorimetry (DSC). Moreover, tribological properties of as-sprayed coating were investigated by SRV-IV friction and wear tester from 200 to 800 °C. It has been found that the as-sprayed coating possesses good thermal stability. DSC analysis reveals that recrystallization of the glassy phase present in the mullite coating occurs at about 980 °C. The friction coefficient of mullite coating was gradually increased from 0.82 at 200 °C to the highest value of 1.12 at 800 °C, while wear rates of the coating were at the order of 10^?5 mm³/Nm. The as-sprayed coating suffered the most severe wear at 800 °C. The observed wear mechanisms were mainly abrasive wear, brittle fracture, and pulling-out of splats.     

Plasma Sprayed Coating Using Mullite and Mixed Alumina/Silica Powders

Plasma sprayed ceramic coatings are widely used for thermal barrier coating applications. Commercially available mullite powder particles and a mixture of mechanically alloyed alumina and silica powder particles were used to deposit mullite ceramic coatings by plasma spraying. The coatings were deposited at three different substrate temperatures (room temperature, 300?°C, and 600?°C) on stainless steel substrates. Microstructure and morphology of both powder particles as well as coatings were investigated by using scanning electron microscopy. Phase formation and degree of crystallization of coatings were analyzed by x-ray diffraction. Differential thermal analysis (DTA) was used to study phase transformations in the coatings. Results indicated that the porosity level in the coatings deposited using mullite initial powder particles were lower than those deposited using the mixed initial powder particles. The degree of crystallization of the coatings deposited using the mixed powder particles was higher than that deposited using mullite powder particles at substrate temperatures of 25 and 300?°C. DTA curves of the coatings deposited using the mixed powders showed some transformation of the retained amorphous phase into mullite and alumina. The degree of crystallization of the as sprayed coatings using the mixed powder particles was significantly increased after post deposition heat treatments. The results indicated that the mechanically alloyed mixed powder can be used as initial powder particles for deposition of mullite coatings instead of using mullite powders.     

Mullite shell mould for casting of advanced CG and SX components in nickel based superalloys

Abstract

Mullite base shell mould system is used for casting of superalloys in columnar and single crystal grains in temperature range of 1480–1550°C. The colloidal silica gel+mullite filler with and without fine alumina slurries was prepared followed by two shell moulds: one without alumina (shell system I) and the other with alumina (shell system II). Shell made with slurry system II resulted in increase in green strength by 10% and fired (950°C) strength by 125% respectively. Sag resistance capability was observed more for shell system II for tested temperatures from 1500 to 1650°C. Dimensional stability of low pressure turbine blade cast at 1550°C was also studied. No shell bulging effect was observed for both shell moulds. The importance of mullite filler material for shell mould to be used for investment casting and its capability to withstand high temperature without metal mould reaction have been highlighted.     

Erosion Performance of Gadolinium Zirconate-Based Thermal Barrier Coatings Processed by Suspension Plasma Spray

7-8 wt.% Yttria-stabilized zirconia (YSZ) is the standard thermal barrier coating (TBC) material used by the gas turbines industry due to its excellent thermal and thermo-mechanical properties up to 1200 °C. The need for improvement in gas turbine efficiency has led to an increase in the turbine inlet gas temperature. However, above 1200 °C, YSZ has issues such as poor sintering resistance, poor phase stability and susceptibility to calcium magnesium alumino silicates (CMAS) degradation. Gadolinium zirconate (GZ) is considered as one of the promising top coat candidates for TBC applications at high temperatures (>1200 °C) due to its low thermal conductivity, good sintering resistance and CMAS attack resistance. Single-layer 8YSZ, double-layer GZ/YSZ and triple-layer GZdense/GZ/YSZ TBCs were deposited by suspension plasma spray (SPS) process. Microstructural analysis was carried out by scanning electron microscopy (SEM). A columnar microstructure was observed in the single-, double- and triple-layer TBCs. Phase analysis of the as-sprayed TBCs was carried out using XRD (x-ray diffraction) where a tetragonal prime phase of zirconia in the single-layer YSZ TBC and a cubic defect fluorite phase of GZ in the double and triple-layer TBCs was observed. Porosity measurements of the as-sprayed TBCs were made by water intrusion method and image analysis method. The as-sprayed GZ-based multi-layered TBCs were subjected to erosion test at room temperature, and their erosion resistance was compared with single-layer 8YSZ. It was shown that the erosion resistance of 8YSZ single-layer TBC was higher than GZ-based multi-layered TBCs. Among the multi-layered TBCs, triple-layer TBC was slightly better than double layer in terms of erosion resistance. The eroded TBCs were cold-mounted and analyzed by SEM.     

High Temperature Mechanical Behavior of UHTC Coatings for Thermal Protection of Re-Entry Vehicles

In this work, the high temperature mechanical properties of ultra high temperature ceramics (UHTC) coatings deposited by plasma spraying have been investigated; particularly the stress-strain relationship of ZrB₂-based thick films has been evaluated by means of 4-point bending tests up to 1500 °C in air. Results show that at each investigated temperature (500, 1000, and 1500 °C) modulus of rupture (MOR) values are higher than the ones obtained at room temperature (RT); moreover at 1500 °C the UHTC coatings exhibit a marked plastic behavior, maintaining a flexural strength 25% higher compared to RT tested samples. The coefficient of linear thermal expansion (CTE) has been evaluated up to 1500 °C: obtained data are of primary importance for substrate selection, interface design and to analyze the thermo-mechanical behavior of coating-substrate coupled system. Finally, SEM-EDS analyses have been carried out on as-sprayed and tested materials in order to understand the mechanisms of reinforcement activated by high temperature exposure and to identify the microstructural modifications induced by the combination of mechanical loads and temperature in an oxidizing environment.     

Matrix Transformation in Boron Containing High-Temperature Co–Re–Cr Alloys

An addition of boron largely increases the ductility in polycrystalline high-temperature Co–Re alloys. Therefore, the effect of boron on the alloy structural characteristics is of high importance for the stability of the matrix at operational temperatures. Volume fractions of ε (hexagonal close-packed—hcp), γ (face-centered cubic—fcc) and σ (Cr₂Re₃ type) phases were measured at ambient and high temperatures (up to 1500 °C) for a boron-containing Co–17Re–23Cr alloy using neutron diffraction. The matrix phase undergoes an allotropic transformation from ε to γ structure at high temperatures, similar to pure cobalt and to the previously investigated, more complex Co–17Re–23Cr–1.2Ta–2.6C alloy. It was determined in this study that the transformation temperature depends on the boron content (0–1000 wt. ppm). Nevertheless, the transformation temperature did not change monotonically with the increase in the boron content but reached a minimum at approximately 200 ppm of boron. A probable reason is the interplay between the amount of boron in the matrix and the amount of σ phase, which binds hcp-stabilizing elements (Cr and Re). Moreover, borides were identified in alloys with high boron content.     

Effect of MgO and CaO on Transformation of Andalusite to Mullite

Andalusite as a refractory material can be transformed to mullite and a silica-rich liquid phase in a temperature range of 1100-1600?°C. In this paper, the influences of MgO and CaO mineralizers on transformation of andalusite to mullite were investigated. Different amounts of MgO and CaO were introduced to andalusite by solution (precipitation) method. Then the precipitated particles were pressed, dried, and fired at 1300, 1400, 1500, and 1600?°C for 2?h. The microstructures of these samples were studied by XRD and SEM. The results showed that the addition of MgO and CaO affected mullitization of andalusite, so that the addition of these oxides increased the amount of mullite formation in andalusite.     

Room Temperature Adsorptive Removal of Thiophene over Zinc Oxide-Based Adsorbents

This study investigated the room temperature adsorptive removal of thiophene over zinc oxide adsorbents in the presence of hydrogen. The bulk zinc oxide was prepared by precipitation method and calcined at different temperatures in the range of 300-550 °C. Supported zinc oxide was prepared by co-precipitation of 30 wt.% ZnO with alumina and calcined at 550 °C. Properties of the adsorbents were determined by various characterization techniques such as surface area and pore volume analysis, XRD, FESEM, EDX and TPR. The desulfurization process was carried out in a down-flow packed bed reactor at room temperature (30 °C). The BET surface area of bulk zinc oxide adsorbents decreased with the increase in calcination temperature from 300 to 550 °C. The surface area of bulk zinc oxide adsorbents was 30.5 and 14.6 m²/g when calcined at 300 and 550 °C, respectively. The surface are of supported zinc oxide adsorbents was 177 m²/g. The highest average pore size was obtained for bulk ZnO calcined at 550 °C (45 nm) compared to that calcined at 300 °C (42 nm) and supported ZnO (27 nm). The XRD peaks corresponded to the hexagonal structure of zinc oxide. The removal of thiophene was most significant for bulk ZnO calcined at 550 °C. The higher removal efficiency for this adsorbent in spite of lower surface area may be attributed to its higher percentage of larger pores and higher average pore size.     

Microstructure and Thermal Properties of Atmospheric Plasma-Sprayed Yb<Subscript>2</Subscript>Si<Subscript>2</Subscript>O<Subscript>7</Subscript> Coating

In the present work, Yb₂Si₂O₇ powder was synthesized by solid-state reaction using Yb₂O₃ and SiO₂ powders as starting materials. Atmospheric plasma spray technique was applied to fabricate Yb₂Si₂O₇ coating. The phase composition and microstructure of the coating were characterized. The density, open porosity and Vickers hardness of the coating were investigated. Its thermal stability was evaluated by thermogravimetry and differential thermal analysis (TG-DTA). The thermal diffusivity and thermal conductivity of the coating were measured. The results showed that the as-sprayed coating was mainly composed of crystalline Yb₂Si₂O₇ with amorphous phase. The coating had a dense structure containing defects, such as pores, interfaces and microcracks. The TG-DTA results showed that there was almost no mass change from room temperature to 1200 °C, while a sharp exothermic peak appeared at around 1038 °C in DTA curve, which indicated that the amorphous phase crystallized. The thermal conductivity of the coating decreased with rise in temperature up to 600 °C and then followed by an increase at higher temperatures. The minimum value of the thermal conductivity of the Yb₂Si₂O₇ coating was about 0.68 W/(m K).     

Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

Al₂O₃-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss ~ 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss ~ 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness (R_a = 6.53 µm) compared to the sample sintered at 1500 °C (R_a = 0.66 µm) corroborating the abrasion wear test results.     

Sintering of commercial mulite powder: Effect of MgO dopant

MgO is one of the sintering aids most commonly used in the processing of mullite bodies. However, few studies have investigated the influence of MgO on the densification and microstructural development of mullite bodies, and the amount of MgO to be used as dopant is still a matter of controversy. Thus, this work investigated the efficiency of small amounts of MgO in the sintering of industrial mullite. MgO was added to obtain dopant concentrations of 0.1 and 0.5 wt.% in the mullite samples. Doped and nondoped samples were produced by cold isostatic pressing (CIP) at 200 MPa and pressureless sintering at 1500, 1550, 1600 and 1650 °C for 2 h. The use of 0.1 and 0.5 wt.% of MgO increased the final density of the sintered samples, with the doped samples reaching densities of 99% and the nondoped samples reaching densities of 95%. Elongated mullite grains were observed in the nondoped samples when their density fell below 95%, while the microstructures of bodies containing 0.1 wt.% of MgO were controlled up to densities of 98%. The 0.5% doped samples required lower sintering temperatures, however elongated mullite grains were observed when densities of 99% were reached.     

The Effect of TaC Reinforcement on the Oxidation Resistance of CNTs/SiC CMCs

This study focuses on a two-stage spark plasma sintering (SPS) of TaC and/or carbon nanotubes (CNTs)-reinforced SiC ceramic matrix composites (CMCs). The oxidation mechanism of SiC-based CMCs with CNTs reinforcement as well as the TaC additives effect on the thermal oxidation resistance of the SiC-CNTs-TaC systems are investigated. The oxidation behavior up to 1500 °C is characterized in terms of mass changes, oxide layer formation, and thickness. The results showed that more disorder occurred in the CNT network with increased oxidation temperature. TaC additives exhibited an enhanced protective effect in increasing the oxidation temperature of CNTs from 460 to 550 °C, and this protective effect was effective at 1200 °C achieved by the crystalized Ta₂O₅ which grew with a preferred orientation giving rise to the phase separation in the glassy protective layer. Degraded oxidation resistance was found at 1500 °C.     

连续氮化硅纤维的氧化行为与高温影响研究

连续氮化硅陶瓷纤维是透波／承载一体化陶瓷基复合材料的关键原材料,也是制约复合材料耐高温性能与力学性能的关键因素。本文系统研究了国防科技大学研制的连续氮化硅纤维的抗氧化性能,分析了高温处理后纤维的组成结构与力学性能变化规律。结果表明：1000°C氧化1h后纤维强度高于原始纤维强度,主要是形成的玻璃相能减少和弥补纤维的表面缺陷。随着空气中处理温度提高,氧含量增加,纤维表面形成的SiO₂层逐渐变厚,纤维强度明显降低。纤维在1200°C氧化1h后强度保留率为63%,表明在此温度以下纤维有较好的服役性能。另一方面,氮化硅纤维在1450°C N₂中处理1h的强度保留率为57%,表现出良好的耐高温性能。纤维表面氧化对其在N₂下的耐高温性能具有不利影响,1000°C氧化的纤维在1450°C处理后丧失强度,1500℃处理后形成氮化硅结晶,失重明显增长,纤维内部也开始产生缺陷。     

Wetting Behavior and Reactivity of Molten Silicon with h-BN Substrate at Ultrahigh Temperatures up to 1750 °C

For a successful implementation of newly proposed silicon-based latent heat thermal energy storage systems, proper ceramic materials that could withstand a contact heating with molten silicon at temperatures much higher than its melting point need to be developed. In this regard, a non-wetting behavior and low reactivity are the main criteria determining the applicability of ceramic as a potential crucible material for long-term ultrahigh temperature contact with molten silicon. In this work, the wetting of hexagonal boron nitride (h-BN) by molten silicon was examined for the first time at temperatures up to 1750 °C. For this purpose, the sessile drop technique combined with contact heating procedure under static argon was used. The reactivity in Si/h-BN system under proposed conditions was evaluated by SEM/EDS examinations of the solidified couple. It was demonstrated that increase in temperature improves wetting, and consequently, non-wetting-to-wetting transition takes place at around 1650 °C. The contact angle of 90° ± 5° is maintained at temperatures up to 1750 °C. The results of structural characterization supported by a thermodynamic modeling indicate that the wetting behavior of the Si/h-BN couple during heating to and cooling from ultrahigh temperature of 1750 °C is mainly controlled by the substrate dissolution/reprecipitation mechanism.     

Effect of Homogenization Temperature on Microstructure and Conductivity of Al-Mg-Si-Ce Alloy

Microstructure evolution of Al-0.2wt.%Mg-0.36wt.%Si-0.3wt.%Ce alloy at three different homogenization temperatures for 6 h was observed by optical microscopy, scanning electron microscopy, and x-ray diffraction. Conductivity and tensile properties of the alloy were tested. Results indicate that homogenization temperature has little effect on the macro-segregation and grain size of the as-cast Al-Mg-Si-Ce alloy; however, it has a significant effect on the conductivity. The conductivity is first improved to a maximum value of about 57.3% IACS with homogenization temperature increasing to 560 °C (2.7% higher than that of the as-cast sample), and then decreased when the temperature continuously increasing. The main contributor is considered to be vacancy concentration, which is directly related to the lattice distortion, thus affects the conductivity. The studied homogenization temperatures almost make no difference among the tensile properties of the alloy. The best homogenization temperature for Al-0.2wt.%Mg-0.36wt.%Si-0.3wt.%Ce alloy is 560 °C with the highest conductivity and no decrement of strength.     

Thermal behaviors and growth of reduced ferronickel particles in carbon-laterite composites

The thermal behaviors of single laterite ore and graphite-laterite mixtures were investigated by thermogravimetry (TG), derivative thermo-gravimetry (DTG), and differential thermal analysis (DTA). Four mass loss steps maximized at about 78, 272, 583, and 826°C are observed for the laterite ore, representing the vaporization of free water, the dehydroxylation of goethite, the decomposition of serpentines, and the second dehydroxylation of serpentines, respectively. The reduction reactions of the graphite-laterite mixtures start at around 700°C and can be divided into three major temperature regions. Coal-laterite composites with an addition of 10 wt.% CaO were roasted at 1100-1350°C for 30 min, and the reduced samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results indi-cate that the reduction reactions proceed more completely at higher temperatures. The growth of the reduced ferronickel particles is greatly influenced by the roasting temperature. Obvious growth of the reduced ferronickel particles appears with the formation of worm-like crystals for the sample reduced at 1250°C, and spheric particles are observed for the sample reduced at 1300°C. When the reduction temperature in-creases to 1350°C, the reduced ferronickel particles agglomerate to ferronickel granules of 3-8 mm in diameter. The main elements in the granules include iron, nickel, chromium, carbon, and sulfur, with the content of nickel and that of iron of 9.08 wt.% and 85.21 wt.%, respec-tively.     

The superior thermal stability and tensile properties of hot rolled W-HfC alloys

Herein, a W-0.5wt%HfC (WHC05) alloy is fabricated by conventional sintering and multi-step hot-rolling. The high-temperature stability and tensile properties at different temperatures, ranging from room temperature to 600 °C, are studied to demonstrate the influence of HfC addition. The results reveal that the WHC05 alloy has a higher recrystallization temperature (1400 °C–1500 °C) than the previously reported as-rolled pure W (1200 °C) and as-rolled W-0.5wt%ZrC (WZC05 ~ 1300 °C) alloy. Moreover, after recovery and recrystallization (annealing at 1600 °C), the WHC05 alloy maintained a high ultimate tensile strength of ~300 MPa and exhibited a desirable increase in total elongation (>35%), which is ~1.6 times higher than the recrystallized WZC05 at 500 °C. The superior thermal stability and excellent high-temperature mechanical properties can be ascribed to the unique microstructure and uniform dispersion of nano-sized HfC particles in W matrix. The influence of annealing temperature on grain structure, grain orientation and distribution of nano-sized HfC particles has been studied to unveil the possible mechanism of enhanced thermal stability and superior mechanical properties.     

Synthesis,Fabrication and Characterization of ZnO-Based Thin Films Prepared by Sol–Gel Process and H<Subscript>2</Subscript> Gas Sensing Performance

In this paper, an attempt is made to deposit ZnO thin films using sol–gel process followed by dip-coating method on p-silicon (100) substrates for intended application as a hydrogen gas sensor owing to the low toxic nature and thermal stability of ZnO. The thin films are annealed under annealing temperatures of 350, 450 and 550 °C for 25 min. The crystalline quality of the fabricated thin films is then analyzed by field-emission scanning electron microscopy and transmission electron microscope. The gas sensing performance analysis of ZnO thin films is demonstrated at different annealing temperatures and hydrogen gas concentrations ranging from 100 to 3000 ppm. Results obtained show that the sensitivity is significantly improved as annealing temperature increases with maximum sensitivity being achieved at 550 °C annealing temperature and operating temperature of 150 °C. Hence, the modified ZnO thin films can be applicable as H₂ gas sensing device showing to the improved performance in comparison with unmodified thin-film sensor.     

Effect of 0.1 wt.% Co on the Hot Deformation and Toughness of Fine-Grained Low-Carbon Steel at Sub-zero Temperatures

The effect of 0.1 wt.% Co on the hot deformation behavior of fine-grained low-carbon microalloyed steel was investigated at temperatures of 850-1200 °C and a strain rate of 5 s^?1. Furthermore, the toughness of the steel with and without Co at sub-zero temperatures was evaluated. The results suggest that the addition of 0.1 wt.% Co increases the flow stress and delays the occurrence of dynamic recrystallization (DRX) at the same deformation temperature and strain. The DRX fraction of steel specimens without and with 0.1 wt.% Co was about 67.4 and 43.9% at 850 °C, respectively. Then, it increased to 100% at 1100 °C. Compared with steel without Co, cementite particles in the tempered sorbite of steel with 0.1 wt.% Co decreased in size but increased in quantity, yield strength increased from 756 to 787 MPa, and Charpy V-notch energy at ? 20 and ? 50 °C improved from 69 and 41 to 102 and 65 J, respectively. The fracture morphology and crack propagation characteristics were consistent with the variation in impact energy.