Phase Transformation and Microstructure of Zn2Ti3O8 Nanocrystallite Powders Prepared Using the Hydrothermal Process

This paper examines the phase transformation and microstructure of Zn₂Ti₃O₈ nanocrystallite powders prepared using the hydrothermal process that includes TiCl₄ and Zn(NO₃)₂·6H₂O as the initial materials. Differential thermal analysis, X-ray diffraction, transmission electron microscopy (TEM), selected area electron diffraction, nanobeam electron diffraction, and high resolution TEM were utilized to characterize the transition behavior of zinc titanate precursor powders after calcination. Nanocrystalline Zn₂Ti₃O₈ powders with a size range of about 5.0 to 8.0 nm were obtained when the precursor powders were calcined at 773 K (500 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour, the cubic crystal of Zn₂Ti₃O₈ with a _o = 0.8399 ± 0.0003 nm still remained the predominant crystalline phase and the crystallite size increased to 20.0 nm. In addition, ZnTiO₃ phase first appeared because of the 13.8 pct of Zn₂Ti₃O₈ decomposition when the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 9 hours, the Zn₂Ti₃O₈ crystallites grew continuously to 80.0 nm and enhanced the crystallinity. When the precursor powders were calcined at 1273 K (1000 °C) for 1 hour, Zn₂TiO₄ crystallites with a _o = 0.8461 ± 0.0002 nm were the predominant crystalline phase.     

Phase Formation of Zinc Titanate Precursor Powders Prepared by a Hydrothermal Process in Various pH Environments

For the precursor, powders were calcined at 773 K (500 °C) for 1 hour. The anatase TiO₂ and ZnO appear as the predominant and minor phases, respectively, when the precursor powders are obtained at pH 5. The phases of Zn₂Ti₃O₈, anatase TiO₂, and ZnO coexist for the precursor powders obtained at pH 7. In addition, the Zn₂Ti₃O₈ and ZnO are the predominant and minor phases, respectively, for the precursor powders obtained at pH 9.     

Synthesis of Nanostructured and Nanoporous TiO<Subscript>2</Subscript>-AgO Mixed Oxide Derived from a Particulate Sol-Gel Route: Physical and Sensing Characteristics

Nanocrystalline TiO₂-AgO thin films and powders were prepared by an aqueous particulate sol-gel route at the low temperature of 573 K (300 °C). Titanium tetraisopropoxide and silver nitrate were used as precursors, and hydroxypropyl cellulose was used as a polymeric fugitive agent in order to increase the specific surface area. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed that the phase composition of the mixed oxide depends upon the annealing temperature, being a mixture of TiO₂ and AgO in the range 573 K to 773 K (300 °C to 500 °C) and a mixture of TiO₂, AgO, and Ag₂O at 973 K (700 °C). Furthermore, one of the smallest crystallite sizes was obtained for TiO₂-AgO mixed oxide, being 4 nm at 773 K (500 °C). Field emission–scanning electron microscopic (FE-SEM) and atomic force microscopic (AFM) images revealed that the deposited thin films had nanostructured and nanoporous morphology with columnar topography. Thin films produced under optimized conditions showed excellent microstructural properties for gas sensing applications. They exhibited a remarkable response toward low concentrations of CO gas (i.e., 25 ppm) at low operating temperature of 473 K (200 °C), resulting in an increase of the thermal stability of sensing films as well as a decrease in their power consumption. Furthermore, TiO₂-AgO sensors follow the power law for the detection of CO gas.     

Dry Sliding Wear Behavior of Ti-6.5Al-3.5Mo-1.5Zr-0.3Si Alloy

Dry sliding wear tests were performed for Ti-6.5Al-3.5Mo-1.5Zr-0.3Si alloy against AISI 52100 steel under the loads of 50 to 250 N at 298 K to 873 K (25 °C to 600 °C). The wear behavior of the alloy varied with the change of test conditions. More or less tribo-oxides TiO₂ and Fe₂O₃ formed on worn surfaces under various conditions. At lower temperature [298 K to 473 K (25 °C to 200 °C)], less and scattered tribo-oxide layers did not show wear-reduced effect. As more number of and continuous tribo-oxide layers appeared at higher temperatures [773 K to 873 K (500 °C to 600 °C)], the wear rate would be substantially reduced. It can be suggested that Ti-6.5Al-3.5Mo-1.5Zr-0.3Si alloy possessed excellent wear resistance at 773 K to 873 K (500 °C to 600 °C). The wear-reduced effect of tribo-oxides seemed to depend on the appearance of Fe₂O₃ and the amount of tribo-oxides.     

Analysis of Particle and Crystallite Size in Tungsten Nanopowder Synthesis

Tungsten nanopowders were synthesized by a low-temperature technique and then heat treated in a gaseous reductive atmosphere in order to study the phase evolution, crystallite size, and particle size of the powders as the heat treatment temperature was modified. Synthesis of the powders was carried out in aqueous media using NaBH₄ as a reducing agent using careful control of the pH of the solutions. The XRD patterns of the as-synthesized powders showed an amorphous phase. After washing, energy dispersive spectroscopy showed that the powders had peaks for oxygen and tungsten. In order to promote crystallization and eliminate the oxygen, the powders were heat treated at 773 K, 923 K, and 1073 K (500 °C, 650 °C, and 800 °C) in a H₂/CH₄ reducing atmosphere for 2 hours. XRD after heat treatment showed α-W peaks for the powders treated at 1073 K and 923 K (800 °C and 650 °C) and a mixture of β-W and α-W for the powders treated at 773 K (500 °C). The crystallite sizes determined from X-ray peak broadening were 12, 16, and 20 nm, whereas the average particle sizes from dynamic light scattering were 260, 450, and 750 nm, for heat treatment temperatures of 773 K, 923 K, and 1073 K (500 °C, 650 °C, and 800 °C), respectively. The average crystallite size and particle sizes increased proportionally with the treatment temperature, in contrast to what has been found for some ceramics, in which as the heat treatment temperature is increased, the crystallite size increases, but the particle size stays constant.     

Oxidation of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Scale-Forming MAX Phases in Turbine Environments

High temperature oxidation of alumina-forming MAX phases, Ti₂AlC and Cr₂AlC, were examined under turbine engine environments and coating configurations. Thermogravimetric furnace tests of Ti₂AlC showed a rapid initial transient due to non-protective TiO₂ growth. Subsequent well-behaved cubic kinetics for alumina scale growth were shown from 1273 K to 1673 K (1000 °C to 1400 °C). These possessed an activation energy of 335 kJ/mol, consistent with estimates of grain boundary diffusivity of oxygen (~375 kJ/mol). The durability of Ti₂AlC under combustion conditions was demonstrated by high pressure burner rig testing at 1373 K to 1573 K (1100 °C to 1300 °C). Here good stability and cubic kinetics also applied, but produced lower weight gains due to volatile TiO(OH)₂ formation in water vapor combustion gas. Excellent thermal stability was also shown for yttria-stabilized zirconia thermal barrier coatings deposited on Ti₂AlC substrates in 2500-hour furnace tests at 1373 K to 1573 K (1100 °C to 1300 °C). These sustained a record 35 µm of scale as compared to 7 μm observed at failure for typical superalloy systems. In contrast, scale and TBC spallation became prevalent on Cr₂AlC substrates above 1423 K (1150 °C). Cr₂AlC diffusion couples with superalloys exhibited good long-term mechanical/oxidative stability at 1073 K (800 °C), as would be needed for corrosion-resistant coatings. However, diffusion zones containing a NiAl-Cr₇C₃ matrix with MC and M₃B₂ particulates were commonly formed and became extensive at 1423 K (1150 °C).     

Er and Gd Co-Doped Ceria-Based Electrolyte Materials for IT-SOFCs Prepared by the Cellulose-Templating Method

Ce_0.9?x Gd_0.1Er _x O_1.9?x/2 (0 ≤ x ≤ 0.1) (EGDC) powders were successfully synthesized with a fast and facile cellulose-templating method for the first time and characterized by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The samples were calcined at a relatively low calcination temperature of 773 K (500 °C). The sintering behavior of the calcined EGDC powders was also investigated at 1673 K (1400 °C) for 6 hours. Calcined Ce_0.9?x Gd_0.1Er _x O_1.9?x/2 (0 ≤ x ≤ 0.1) powders and sintered Ce_0.9?x Gd_0.1Er _x O_1.9?x/2 (0 ≤ x ≤ 0.1) pellets crystallized in the cubic fluorite structure. It was found that the relative densities of the sintered EGDC pellets were over 95 pct for all the Er contents studied. Moreover, the effect of Er content on the ionic conductivity of the gadolinium-doped ceria (GDC, Ce_0.9Gd_0.1O_1.90) was investigated. The highest ionic conductivity value was found to be 3.57 × 10^?2 S cm^?1 at 1073 K (800 °C) for the sintered Ce_0.82Gd_0.1Er_0.08O_1.91 at 1673 K (1400 °C) for 6 hours.     

Chromium Extraction <Emphasis Type="Italic">via</Emphasis> Chemical Processing of Fe-Cr Alloys Fine Powder with High Carbon Content

Ferrous alloys are important raw materials for special steel production. In this context, alloys from the Fe-Cr system, with typical Cr weight fraction ranging from 0.45 to 0.95, are prominent, particularly for the stainless steel industry. During the process in which these alloys are obtained, there is considerable production of fine powder, which could be reused after suitable chemical treatment, for example, through coupling pyrometallurgical and hydrometallurgical processes. In the present study, the extraction of chromium from fine powder generated during the production of a Fe-Cr alloy with high C content was investigated. Roasting reactions were performed at 1073 K, 1173 K, and 1273 K (800 °C, 900 °C, and 1000 °C) with 300 pct (w/w) excess NaOH in an oxidizing atmosphere (air), followed by solubilization in deionized water, selective precipitation, and subsequent calcination at 1173 K (900 °C) in order to convert the obtained chromium hydroxide to Cr₂O₃. The maximum achieved Cr recovery was around 86 pct, suggesting that the proposed chemical route was satisfactory regarding the extraction of the chromium initially present. Moreover, after X-ray diffraction analysis, the final produced oxide has proven to be pure Cr₂O₃ with a mean crystallite size of 200 nm.     

Mechanical Property Enhancement of Ti-6Al-4V by Multilayer Thin Solid Film Ti/TiO2 Nanotubular Array Coating for Biomedical Application

With the intention of improving the mechanical properties of Ti-6Al-4V, samples were first coated with pure titanium using the physical vapor deposition (PVD) magnetron sputtering technique. The Taguchi optimization method was used to attain a higher coating on substrate adhesion. Second, pure titanium-coated samples with higher adhesion were anodized to generate TiO₂ nanotubes. Next, the TiO₂-coated specimens were heat treated at annealing temperatures of 753.15 K and 923.15 K (480 °C and 650 °C). The XRD results indicate that the varying heat treatment temperatures produced different phases, namely, anatase [753.15 K (480 °C)] and rutile [923.15 K (650 °C)]. Finally, the coated samples’ mechanical properties (surface hardness, adhesion, and fretting fatigue life) were investigated. The fretting fatigue lives of TiO₂-coated specimens at 753.15 K and 923.15 K (480 °C and 650 °C) annealing temperatures were significantly enhanced compared to uncoated samples at low and high cyclic fatigue. The results also indicate that TiO₂-coated samples heat treated at an annealing temperature of 753.15 K (480 °C) (anatase phase) are more suitable for increasing fretting fatigue life at high cyclic fatigue (HCF), while at low cyclic fatigue, the annealing temperature of 923.15 K (650 °C) seemed to be more appropriate. The fretting fatigue life enhancement of thin-film TiO₂ nanotubular array-coated Ti-6Al-4V is due to the ceramic nature of TiO₂ which produces a hard surface as well as a lower coefficient of friction of the TiO₂ nanotube surface that decreases the fretting between contacting components, namely, the sample and friction pad surfaces.     

Effects of Solute and Surfactant Addition on the Crystallization and Morphology of Hydroxyapatite Powders Synthesized by Hydrolysis of Calcium Hydrogen Phosphate Dehydrate (DCPD)

The effects of the addition of alcohol and cetyltrimethylammonium bromide (CTAB) on the crystallization and the morphology of hydroxyapatite (HA) powders synthesized by hydrolysis of calcium hydrogen phosphate dehydrate (DCPD) in the 2.5 M NaOH solutions at 348 K (75 °C) for 1 hour have been studied. The values of zeta potential have large differences between the sums of DCPD with CTAB (Z _DCPD+CTAB) minus the sum of DCPD and CTAB (Z _DCPD + Z _CTAB), and of HA with CTAB (Z _HA+CTAB) minus the sum of HA and CTAB (Z _HA + Z _CTAB), respectively. When the hydrolysis of DCPD occurred in the 2.5 M NaOH solutions at 348 K (75 °C) for 1 hour both with and without alcohol and CTAB, XRD results show the only one phase of HA in the as-dried powders. When the NaOH solution does not contain CTAB, the crystallite size of HA powders decreased from 23 ± 1 to 16 ± 1 nm as the alcohol content was more than 50 pct. The crystallite size of HA powders obtained from DCPD synthesized in the 2.5 M NaOH solution with 1.0 × 10^?3 M CTAB decreased when the alcohol content was increased to 70 pct, whereas the crystallite size increased when the alcohol concentration was greater than that of 70 pct. SEM images show that the HA powders have a rod-like shape when DCPD was synthesized in the 2.5 M NaOH solution without CTAB or alcohol. When the NaOH solution had 1.0 × 10^?3 M CTAB and various alcohol concentrations, the morphology of HA powder still maintained a rod-like or needle-like shape. The HA powder had a maximum specific surface area of 180.25 m²/g when the hydrolysis of DCPD occurred in a 2.5 M NaOH solution containing 1.0 × 10^?3 M CTAB and 70 pct alcohol at 348 K (75 °C) for 1 hour.     

Phase Evolution and Mechanical Properties of Nano-TiO2 Dispersed Zr-Based Alloys by Mechanical Alloying and Conventional Sintering

The present study deals with the synthesis of 1.0 to 2.0 wt pct nano-TiO₂ dispersed Zr-based alloy with nominal compositions 45.0Zr-30.0Fe-20.0Ni-5.0Mo (alloy A), 44.0Zr-30.0 Fe-20.0Ni-5.0Mo-1.0TiO₂ (alloy B), 44.0Zr-30.0Fe-20.0Ni-4.5Mo-1.5TiO₂ (alloy C), and 44.0Zr-30.0Fe-20.0Ni-4.0Mo-2.0TiO₂ (alloy D) by mechanical alloying and consolidation of the milled powders using 1 GPa uniaxial pressure for 5 minutes and conventional sintering at 1673 K (1400 °C). The microstructural and phase evolution during each stage of milling and the consolidated products were studied by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM), and energy-dispersive spectroscopy. The particle size of the milled powder was also analyzed at systemic intervals during milling, and it showed a rapid decrease in particle size in the initial hours of milling. XRD analysis showed a fine crystallite size of 10 to 20 nm after 20 hours of milling and was confirmed by TEM. The recrystallization behavior of the milled powder was studied by differential scanning calorimetry. The hardness of the sintered Zr-based alloys was recorded in the range of 5.1 to 7.0 GPa, which is much higher than that of similar alloys, developed via the melting casting route.     

Carbide Precipitation During Tempering of a Tool Steel Subjected to Deep Cryogenic Treatment

Using transmission electron microscopy, Mössbauer spectroscopy, and measurements of hardness, the carbide precipitation during tempering of steel X153CrMoV12 containing (mass pct) 1.55C, 11.90Cr, 0.70V, and 0.86Mo is studied after three treatments: quenching at RT and deep cryogenic treatment, DCT, at 77 K or 123 K (?196 °C or ?150 °C). In contrast to some previous studies, no fine carbide precipitation after long-time holding at cryogenic temperatures is detected. After quenching at room temperature, RT, the transient ε(ε′) carbide is precipitated between 373 K and 473 K (100 °C and 200 °C) and transformed to cementite starting from 573 K (300 °C). In case of DCT at 123 K (?150 °C), only fine cementite particles are detected after tempering at 373 K (200 °C) with their delayed coarsening at higher temperatures. Dissolution of cementite and precipitation of alloying element carbides proceed at 773 K (500 °C) after quenching at RT, although some undissolved cementite plates can also be observed. After DCT at 123 K (?150 °C), the transient ε(ε′) carbide is not precipitated during tempering, which is attributed to the intensive isothermal martensitic transformation accompanied by plastic deformation. In this case, cementite is the only carbide phase precipitated in the temperature range of 573 K to 773 K (300 °C to 500 °C). If DCT is carried out at 77 K (?196 °C), the ε(ε′) carbide is found after tempering at 373 K to 473 K (100 °C to 200 °C). Coarse cementite particles and the absence of alloying element carbides constitute a feature of steel subjected to DCT and tempering at 773 K (500 °C). As a result, a decreased secondary hardness is obtained in comparison with the steel quenched at RT. According to Mössbauer studies, the structure after DCT and tempering at 773 K (500 °C) is characterized by the decreased fraction of the retained austenite and clustering of alloying elements in the α solid solution. It is suggested that a competition between the strain-induced transformation of the retained austenite and carbide precipitation during the wear can control the life of steel tools.     

Effect of Er,Gd, and Nd Co-Dopants on the Properties of Sm-Doped Ceria Electrolyte for IT-SOFC

Doped ceria electrolytes of Ce_0.8Sm_0.20O_1.90 (SDC), Ce_0.8Er_0.08Sm_0.12O_1.90 (ESDC), Ce_0.8Gd_0.08Sm_0.12O_1.90 (GSDC), and Ce_0.8Nd_0.08Sm_0.12O_1.90 (NSDC) were prepared by a citric–nitrate combustion process. The thermal decomposition of the precursor was investigated by simultaneous thermogravimetric analysis and differential thermal analysis experiments. The phase structure of the calcined and sintered powders was characterized by X-ray diffraction analysis. All of the samples were fluorite-type ceria-based solid solutions. The calcined and sintered powders were also characterized by Fourier transform infrared spectroscopy. Scanning electron microscopy was used to characterize the samples after calcination and sintering. A relative density over 95 percent of the theoretical density was achieved after the sintering process. Electrical conductivities of the sintered samples were measured using the impedance spectra method. The highest ionic conductivity value was found to be 5.28 × 10^?2 S cm^?1 at 1023 K (750 °C) for GSDC sintered at 1673 K (1400 °C) for 6 hours.     

Effect of Annealing Temperature on the Thermoelectric Properties of the Bi0.5Sb1.5Te3 Thin Films Prepared by Radio-Frequency Sputtering

The effect of annealing temperature on the crystallinity, thermoelectric properties, and surface morphology of the Bi_0.5Sb_1.5Te₃ thin films prepared on SiO₂/Si substrate by radio-frequency (RF) magnetron sputtering was investigated using X-ray diffraction (XRD), the four-point probe method, and scanning electron microscopy (SEM). XRD results show that the crystallite structure of the Bi _x Sb_2–x Te₃ thin films belong to Bi_0.5Sb_1.5Te₃. When the Bi _x Sb_2–x Te₃ thin films were annealed between 423 K and 523 K (150 °C and 250 °C) for 10  minutes, the crystallinity of the thin films continuously increases with the temperature increase. In addition, the (015) reflection plane as the preferred orientation and the oxidation compound of Bi_3.73Sb_1.5O₃ first appeared when the Bi_0.5Sb_1.5Te₃ thin films were annealed at 523 K (250 °C) for 10 minutes. An activation energy of 51.66 kJ/mol for crystallite growth of Bi_0.5Sb_1.5Te₃ thin films annealed between 423 K and 523 K (150 °C and 250 °C) for 10 minutes was obtained. The resistivity was 2.69 × 10² and 5.93 × 10  μΩ·m, respectively, for the as-deposited Bi_0.5Sb_1.5Te₃ thin films and annealed at 523 K (250 °C) for 10 minutes. The maximum values of the Seebeck coefficient and power factor were 256.5 μV/K and 1.12 × 10³ μW/m·K², respectively, for the Bi_0.5Sb_1.5Te₃ thin films annealing treatment at 523 K (250 °C) for 10 minutes.     

Stability of Ni3(Al,Ti) Gamma Prime Precipitates in a Nickel-Based Superalloy Inconel X-750 Under Heavy Ion Irradiation

Phase stability of Ni₃(Al, Ti) precipitates in Inconel X-750 under cascade damage was studied using heavy ion irradiation with transmission electron microscope (TEM) in situ observations. From 333 K to 673 K (60 °C to 400 °C), ordered Ni₃(Al, Ti) precipitates became completely disordered at low irradiation dose of 0.06 displacement per atom (dpa). At higher dose, a trend of precipitate dissolution occurring under disordered state was observed, which is due to the ballistic mixing effect by irradiation. However, at temperatures greater than 773 K (500 °C), the precipitates stayed ordered up to 5.4 dpa, supporting the view that irradiation-induced disordering/dissolution and thermal recovery reach a balance between 673 K and 773 K (400 °C and 500 °C). Effects of Ti/Al ratio and irradiation dose rate are also discussed.     

The Influence of Precipitation of Alpha2 on Properties and Microstructure in TIMETAL 6-4

Samples of Hot Isostatically Pressed (HIPped) powder of TIMETAL 6-4 (Ti-6Al-4V, compositions in wt pct unless indicated), which was HIPped at 1203 K (930 °C), and of forged bar stock, which was slowly cooled from above the beta transus, were both subsequently held at 773 K (500 °C) for times up to 5 weeks and analyzed using scanning and transmission electron microscopy and atom probe analysis. It has been shown that in the samples aged for 5 weeks at 773 K (500 °C), there is a high density of alpha2 (α₂, an ordered phase based on the composition Ti₃Al) precipitates, which are typically 5 nm in size, and a significantly smaller density was present in the slowly cooled samples. The fatigue and tensile properties of samples aged for 5 weeks at 773 K (500 °C) have been compared with those of the HIPped powder and of the forged samples which were slowly cooled from just above the transus, and although no significant difference was found between the fatigue properties, the tensile strength of the aged samples was 5 pct higher than that of the as-HIPped and slowly cooled forged samples. The ductility of the forged samples did not decrease after aging at 773 K (500 °C) despite the strength increase. Transmission electron microscopy has been used to assess the nature of dislocations generated during tensile and fatigue deformation and it has been found that not just is planar slip observed, but dislocation pairs are not uncommon in samples aged at 773 K (500 °C) and some are seen in slowly cooled Ti6Al4V.     

Experimental Investigation and Thermodynamic Calculations of the Bi-Ge-Sb Phase Diagram

A phase diagram of the Bi-Ge-Sb ternary system was investigated experimentally by differential thermal analysis (DTA), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS), and X-ray powder diffraction (XRD) methods and theoretically by the CALPHAD method. The liquidus projection; invariant equilibria; and three vertical sections, Sb-Bi_0.5Ge_0.5, Ge-Bi_0.5Sb_0.5, and Bi-Ge_0.5Sb_0.5, as well as isothermal sections at 773 K and 373 K (500 °C and 100 °C), were predicted using optimized thermodynamic parameters for constitutive binary systems from the literature. In addition, phase transition temperatures of the selected samples with compositions along calculated isopleths were experimentally determined using DTA. Predicted isothermal sections at 773 K and 373 K (500 °C and 100 °C) were compared with the results of the SEM-EDS and XRD analysis from this work. In both cases, good agreement between the extrapolated phase diagram and experimental results was obtained. Alloys from the three studied vertical sections were additionally analyzed using the Brinell hardness test.     

Process Parameters on the Crystallization and Morphology of Hydroxyapatite Powders Prepared by a Hydrolysis Method

The effects of process parameters on the crystallization and morphology of hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂, HA) powders synthesized from dicalcium phosphate dihydrate (CaHPO₄·2H₂O, DCPD) using a hydrolysis method have been investigated. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were used to characterize the synthesized powders. When DCPD underwent hydrolysis in 2.5 NaOH solution (Na_(aq)) at 303 K to 348 K (30 °C to 75 °C) for 1 hour, the XRD results revealed that HA was obtained for all the as-dried samples. The SEM morphology of the HA powders for DCPD hydrolysis produced at 348 K (75 °C) shows regular alignment and a short rod shape with a size of 200 nm in length and 50 nm in width. With DCPD hydrolysis in 2.5 M NaOH_(aq) holding at 348 K (75 °C) for 1 to 24 hours, XRD results demonstrated that all samples were HA and no other phases could be detected. Moreover, the XRD results also show that all the as-dried powders still maintained the HA structure when DCPD underwent hydrolysis in 0.1 to 5 M NaOH_(aq) at 348 K (75 °C) for 1 hour. Otherwise, the full transformation from HA to octa-calcium phosphate (OCP, Ca₈H₂(PO₄)₆·5H₂O) occurred when hydrolysis happened in 10 M NaOH_(aq). FT-IR spectra analysis revealed that some carbonated HA (Ca₁₀(PO₄)₆(CO₃), CHA) had formed. The SEM morphology results show that the 60 to 65 nm width of the uniformly long rods with regular alignment formed in the HA powder aggregates when DCPD underwent hydrolysis in 2.5 M NaOH_(aq) at 348 K (75 °C) for 1 hour.     

Sintering characteristics and microwave dielectric properties of 0.5Ca0.6La0.267TiO3-0.5Ca(Mg1/3Nb2/3)O3 ceramics prepared by reaction-sintering process

0.5 Ca_(0.6)La_(0.267)TiO_3-0.5 Ca(Mg_(1/3)Nb_(2/3))O_3(5 CLT-5 CMN) ceramics were prepared by a reaction-sintering process and their sintering characteristics, microwave dielectric properties were investigated in detail.Without any calcination stage involved,a mixture of CaCO_3, La_2 O_3, TiO_2, MgO and Nb_2 O_5 was pressed and sintered directly. Pure phase 5 CLT-5 CMN ceramics with high density and dense microstructure can be obtained after sintered at 1400 ℃ for 4 h. Compared with those prepared by the conventional ceramic route, 5 CLT-5 CMN ceramics produced by the reaction-sintering process exhibit slightly higher dielectric constant and Q×f value. Fine microwave dielectric properties of ε_r= 56.4, Q×f= 48,550 GHz and T_f = +8.7 ppm/℃ for 5 CLT-5 CMN ceramics sintered at 1400 ℃ for 4 h are obtained, suggesting reactionsintering process is a simple and efficient method to produce pure phase 5 CLT-5 CMN ceramics as a potential candidate for the fabrication of microwave devices.     

Dissolution Behavior of Rhodium in the Na2O-SiO2 and CaO-SiO2 Slags

To understand the behavior of rhodium during its recovery process, the dissolution behaviors of rhodium in Na₂O-SiO₂ and in CaO-SiO₂ slags at temperatures ranging from 1423 K to 1623 K (from 1150 °C to 1350 °C) and from 1773 K to 1873 K (from 1500 °C to 1600 °C), respectively, in an oxidizing atmosphere were investigated. The solubility of rhodium in the slags was found to increase with increasing oxygen partial pressure, temperature, and the basic oxide content. The correlation between the solubility of rhodium and the oxygen partial pressure suggested that rhodium dissolved into the slags as RhO_1.5. The dissolution of rhodium was slightly endothermic: the enthalpy change of the dissolution of solid rhodium was determined to be 50 ± 10 kJ/mol for the 50(mass pct)Na₂O-50SiO₂; and 188 ± 94 kJ/mol for the 56(mass pct)CaO-44SiO₂ slag systems. The increase in the solubility of rhodium with the basic oxide content indicated that rhodium exhibits acidic behavior in slags. The correlation between the solubility of rhodium and the sulfide capacity of the slags suggested that the ionic species of rhodium in slags is the rhodate ion, RhO ₂ ^? . The rhodate capacity of the slags was defined, and its application to estimate the possible rhodium content in various slag systems was proposed.