Chemical synthesis and characterization of magnesium substituted amorphous calcium phosphate (MG-ACP)

Amorphous calcium phosphate (ACP) was synthesized by a simple aqueous precipitation using CaCl₂ and Na₃PO₄ in the presence of MgCl₂ to ensure the formation of the ACP phase at room temperature. Magnesium substituted ACP phases corresponding to two different compositions representing the two most prominent calcium phosphate phases (hydroxyapatite: Ca + Mg/P = 1.67 and tricalcium phosphate: Ca + Mg/P = 1.5) were synthesized by this simple approach. Both compositions of ACP phases resulted in their transformation into β-tricalcium phosphate upon heat treatment in air at 600 °C. X-ray diffraction (XRD), heat treatment, scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) and Brunauer-Emmett-Teller (BET) analyses were used to characterize the phase, thermal stability, surface area, and morphology of the synthesized ACP powders corresponding to the two different nominal Ca/P compositions. Although it is known that α-TCP is the phase that appears upon heat treatment at 600 °C unsubstituted ACP, substitution of magnesium ion in ACP (both TCP and HA composition) stabilized the structure of β-TCMP phase at 600 °C. Moreover, FT-IR analysis revealed that the ACP phase regardless of the composition, exhibited characteristic bands corresponding to that of HA, with the exception of the ACP corresponding to HA composition which exhibited a prominent OH vibrational mode.     

Preparation and characterization of hydroxyapatite synthesized from oyster shell powders

The ready availability and the low cost of oyster shells, which is composed predominantly of calcium carbonate with rare impurities, along with natural wastes are attractive features for converting the biological material into hydroxyapatite (HA) powders for biomedical applications. The HA powder was synthesized using oyster shell powders and dicalcium phosphate dihydrate (CaHPO₄·2H₂O, DCPD) through ball milling and subsequently heat treatment. The HA was initiated through sintering the 1-h milled sample at 1000 °C for 1 h, while pure HA phase is formed after sintering the 10-h milled sample. The as-prepared samples, obtained after 5 or 10 h of milling and then heat-treating at 1000 °C for 1 h, contain the phase of β-tricalcium phosphate (β-TCP). Moreover, the result of FTIR analysis showed that the as-prepared HA sample is A- and B-type carbonate-containing calcium phosphates. The as-synthesize HA powder containing trace elements Mg and Sr exhibited good crystallinity (96.3%) and high phase-purity.     

Synthesis and phases evolution of Si–C–Ti from polycarbosilane (PCS) and metal Ti

Si–C–Ti ceramics were synthesized by reactive pyrolysis of polycarbosilane (PCS) precursor filled with metal Ti powder. Pyrolysis of mixture with atomic ratio of Ti:Si through 3:1–3:2 was carried out in argon atmosphere at given temperature up to 1500 °C. The metal–precursor reactions, and phase evolution were studied using X-ray diffraction and scanning electron microscopy with EDX. The Ti₃SiC₂ phase was obtained firstly from reaction of PCS and Ti. Ti₃SiC₂ formation starts at 1300 °C and its amount increases significantly in a narrow temperature range between 1400 °C and 1500 °C. In addition, addition of CaF₂ can promote the formation of Ti₃SiC₂ phase.     

Room temperature synthesis of high temperature stable lanthanum phosphate–yttria nano composite

A facile aqueous sol–gel route involving precipitation–peptization mechanism followed by electrostatic stabilization is used for synthesizing nanocrystalline composite containing lanthanum phosphate and yttria. Lanthanum phosphate (80 wt%)–yttria (20 wt%) nano composite (LaPO₄–20%Y₂O₃), has an average particle size of ～70 nm after heat treatment of precursor at 600 °C. TG–DTA analysis reveals that stable phase of the composite is formed on heating the precursor at 600 °C. The TEM images of the composite show rod shape morphology of LaPO₄ in which yttria is acquiring near spherical shape. Phase identification of the composite as well as the phase stability up to 1300 °C was carried out using X-ray diffraction technique. With the phases being stable at higher temperatures, the composite synthesized should be a potential material for high temperature applications like thermal barrier coatings and metal melting applications.     

Green light-emitting Lu3Al5O12:Ce phosphor powders prepared by spray pyrolysis

Green light-emitting Lu_2.985Al₅O₁₂:Ce_0.015 (LuAG:Ce) phosphor powders are prepared by spray pyrolysis. The only crystallized phase in the precursor powders and post-treated powders at temperatures below 800 °C is Lu₂O₃ and the other components are amorphous. Phase pure cubic garnet LuAG:Ce phosphor powders are obtained by post-treatment at 1000 °C. Phosphor powders post-treated at temperatures below 1400 °C retain the spherical shape of the precursor powders. The mean crystallite sizes of phosphor powders post-treated at 1200, 1400, and 1500 °C are 30, 46, and 54 nm, respectively. The excitation spectra contain two bands: a weak band with the maximum peak at 345 nm and a strong broad band in the spectral range from 400 to 490 nm with the maximum peak at 455 nm. The LuAG:Ce phosphor powders have broad emission spectra between 480 and 600 nm, with the maximum peak intensity located at 507 nm. The photoluminescence intensity of the phosphor powders post-treated at 1400 °C is 84.2% of that of the powders post-treated at 1500 °C.     

Microstructure control of TCP/TCP-(t-ZrO2)/t-ZrO2 composites for artificial cortical bone

In this study, bone like continuously porous TCP/TCP-(t-ZrO₂)/t-ZrO₂ composites with a central channel were fabricated using a multi-pass extrusion process and their mechanical properties and microstructure at different sintering temperatures were investigated. Hydroxyapatite (HAp) powder was used as the raw powder which undergoes a phase transformation into the α-tricalcium phosphate phase (α-TCP) at a sintering temperature of 1500 °C. The external diameter and inside cylindrical hollow core were approximately 10.3 mm and 4.8 mm, respectively. The frame region contained numerous microchannels that extended from one side of the fabricated body to the other. The channeled frame region had a multi-layer microstructure with a TCP/TCP-(t-ZrO₂)/t-ZrO₂ layer configuration. The inner layer consisted of TCP, which make the wall of the microchannel. The material properties were characterized and microstructural analysis was carried out. The maximum pore size, compressive strength, and relative density of the fabricated system were approximately 86 μm, 53 MPa, and 77% when sintered at 1500 °C. The composites exhibited excellent biocompatibility and cell proliferation behavior resulted in the MTT assay and cell adhesion test using osteoblast-like MG-63 cells.     

Al2TiO5–Al2O3–TiO2 nanocomposite: Structure,mechanical property and bioactivity studies

Novel biomaterials are of prime importance in tissue engineering. Here, we developed novel nanostructured Al₂TiO₅–Al₂O₃–TiO₂ composite as a biomaterial for bone repair. Initially, nanocrystalline Al₂O₃–TiO₂ composite powder was synthesized by a sol–gel process. The powder was cold compacted and sintered at 1300–1500 °C to develop nanostructured Al₂TiO₅–Al₂O₃–TiO₂ composite. Nano features were retained in the sintered structures while the grains showed irregular morphology. The grain-growth and microcracking were prominent at higher sintering temperatures. X-ray diffraction peak intensity of β-Al₂TiO₅ increased with increasing temperature. β-Al₂TiO₅ content increased from 91.67% at 1300 °C to 98.83% at 1500 °C, according to Rietveld refinement. The density of β-Al₂TiO₅ sintered at 1300 °C, 1400 °C and 1500 °C were computed to be 3.668 g cm^?3, 3.685 g cm^?3 and 3.664 g cm^?3, respectively.Nanocrystalline grains enhanced the flexural strength. The highest flexural strength of 43.2 MPa was achieved. Bioactivity and biomechanical properties were assessed in simulated body fluid. Electron microscopy confirmed the formation of apatite crystals on the surface of the nanocomposite. Spectroscopic analysis established the presence of Ca and P ions in the crystals. Results throw light on biocompatibility and bioactivity of β-Al₂TiO₅ phase, which has not been reported previously.     

Effect of low temperature on formation mechanism of calcium phosphate nano powder via precipitation method

Calcium phosphate powders were synthesized with Ca/P molar ratios of initial reagents ranging from 1.660 to 1.667 using wet precipitation method. This work deals with allocating a specific temperature level to each H₃PO₄ solution and Ca(OH)₂ suspension prior to the mixing process, and studying their influences on powder composition. A high pH value of the synthesis medium and the incorporation of numerous carbonate ions into the structure were attained by dropping the temperature of the Ca(OH)₂ suspension down to 5 °C. X-ray diffractometry and FTIR spectroscopy showed that heating samples that had a medium temperature exceeding 25 °C resulted in the dominant HAp phase, regardless of the initial acid solution temperature. By maintaining the medium temperature at 5 °C, a sudden formation of the β-TCP phase occurred after thermal treatment at 1300 °C, and this trend continued with the concurrent decrease in the temperature of the initial acid solution. An interpretation of the formation mechanism under these low-temperature conditions is proposed in terms of the temperature and pH value of the medium and the state of the phosphate and carbonate ions.     

Soft chemistry synthesis,structure and electrochemical characterization of iron phosphates Fe(H2PO4)3 and Fe(PO3)3

The iron phosphate, Fe(H₂PO₄)₃, was synthesized through a precipitation route by means of acidic media. As the compound is highly hygroscopic, the structure was solved ab initio by powder X-ray diffraction under nitrogen flow at room temperature and 200 °C. This phase is antiferromagnetic below 30 K. It converts into Fe(PO₃)₃ at 550 °C, after dehydration. Electrochemical characterizations, performed on the last compound, show irreversible decomposition into metallic iron.     

Transformations of neat and heated struvite (MgNH4PO4⋅6H2O)

Struvite (MgNH₄PO₄?6H₂O) is the mineral phase of one of the urinary tract stones of humans and animals, besides being an important phase seen in waste water treatment and purification plants. Single-phase and highly crystalline struvite powders were synthesized in this study at room temperature in aqueous solutions containing dissolved salts of MgCl₂?6H₂O and (NH₄)₂HPO₄ at the Mg/P molar ratio of 1.00. As-synthesized, crystalline struvite powders (neat powders) completely transformed into cryptocrystalline apatitic calcium phosphate (Ap-CaP), in less than 72 h, when soaked in Ca-containing saline solutions at 37 °C. Moreover, crystalline struvite powders heated at temperatures from 90° to 200 °C became x-ray amorphous. Amorphous powders stirred for 4 h at room temperature in water containing dissolved diammonium hydrogen phosphate recrystallized back into struvite.     

Sodium niobate particles with controlled morphology synthesized by hydrothermal method and their use as templates in KNN fibers

Sodium niobate – NN (NaNbO₃) powders were synthesized by hydrothermal process to be used as template particles in the fabrication of textured lead free piezoelectric ceramics. Sodium hexaniobate–Na₈Nb₆O₁₉⋅13H₂O particles with rod-like morphology were synthesized at 120 °C. Particles with needle-like morphology and Na₂(Nb₂O₆)(H₂O) phase started to form at temperatures of 130 °C and above. Synthesis at 150 °C yields particles with totally needle-like morphology and consisting entirely of the Na₂(Nb₂O₆)(H₂O) phase. Sodium niobate–NaNbO₃ particles with cubic morphology were synthesized at temperatures of 160 °C and above. Rod-like and needle-like morphology was retained even after annealing at 400 °C for 1 h. A preliminary study was also done to integrate these anisometric template particles in the preparation of textured potassium sodium niobate (KNN) fibers.     

Microwave-assisted synthesis and characterization of Ti1 − xVxO2 (x = 0.0–0.10) nanopowders

Ti_1 ? xV_xO₂ (x = 0.0–0.10) nanopowders were successfully synthesized by a microwave-assisted sol–gel technique and their crystal structure and electronic structure were investigated. The products were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman and UV–Vis spectroscopy. The results revealed that TiO₂ powders maintained the anatase phase for calcination temperature below 600 °C, but gradually changed to the rutile phase above 800 °C. The formation of the rutile phase was completed at 1000 °C. For Ti_1 ? xV_xO₂ (x = 0.05) powders, the phase transformation appeared at 600 °C. The absorption edge of Ti_1 ? xV_xO₂ (x > 0) powders broadened to the visible region with increasing V concentration and a strong visible light absorption was obtained with 10% V doping. V doping and subsequent coexistence of both anatase and rutile phases in our Ti_1 ? xV_xO₂ nanoparticles are considered to be responsible for the enhanced absorption of visible light up to 800 nm.     

Powder synthesis and properties of LiTaO3 ceramics

The LiTaO₃ powders with sub micrometer grade grain size have been synthesized successfully using a molten salt method. Lithium tantalate began to form at 400 °C reaction temperature and transformed to pure phase without residual reactants when it was processed at 500 °C for 4 h in static air. The undoped LiTaO₃ ceramics with a Curie temperature about 663 °C were obtained by pressureless sintering at 1300 °C for 3 h. The relative dielectric constant (ɛ_r) increases from 50 to 375 at temperature ranging from 30 to 663 °C and then decreases quickly as the temperature increases above 663 °C. The ceramics shows a relative dielectric constant of 49.4, a dielectric loss factor (tan δ) of 0.007, a coercive field (Ec) of 28.66 kV/cm and a remnant polarization (Pr) of 32.48 μC/cm² at room temperature.     

Coating and spark plasma sintering of nano-sized TiN on Y-α-sialon

TiN coating on Y-α-sialon was accomplished by depositing TiO₂ on their particle surfaces through controlled hydrolysis of TiCl₄ and Ti(O-i-C₃H₇)₄ and subsequent nitridation with NH₃ gas at 1000 °C. TiN particles covering Y-α-sialon were about 20 nm in size. Spark plasma sintering (SPS) of TiN/Y-α-sialon particles produced composite ceramics with continuous TiN networks at 1400 °C, but with TiN grains isolated in elongated β-sialon grains at 1600 °C. The relative density and Vickers hardness of TiN/sialon ceramics SPSed at 1400–1600 °C containing 25 vol.% TiN were measured. The electrical resistivity was in a wide range of 10⁻⁴ to 10⁰ Ω cm for the ceramics sintered at 1400 °C, but lowered to the order of magnitude of 10⁻¹ and 10⁵ Ω cm at higher temperatures ≥1500 °C. It was found that the complete transition to β-sialon increased the resistivity to 10³ to 10⁵ Ω cm, due to breaking up continuous TiN layers by elongated β-sialon grains.     

Synthesis of La0.85Sr0.15Ga0.85Mg0.15O2.85 materials for SOFC applications by acrylamide polymerization

The La_0.85Sr_0.15Ga_0.85Mg_0.15O_2.85 (LSGM) powders are synthesized using a novel method based on acrylamide polymerization technique. The phase evolution was determined by using XRD analysis. The sintering property was studied by using dilatability analysis. The electrical conductivity was also measured. XRD pattern indicates that the perovskite phase is formed at 1000 °C, and the impurity phase, LaSrGa₃O₇ still exists in the sintered sample. The shrinkage curve shows that the fast sintering temperature is 1432 °C. The sinterability was investigated as a function of sintering time and temperature. The results show that the densification rate of the sample was fast at first 5 h. The electrical conductivity was 0.093 S/cm at 800 °C. And a transitional temperature in the Arrhenius plot is 700 °C.     

Effect of hydrothermal temperature on structure and photochromic properties of WO3 powder

Tungsten trioxide (WO₃) powders were prepared via a simple hydrothermal method. The morphology, structure and photochromic activity of the synthesized WO₃ powders were studied by X-ray diffraction, scanning electron microscopy and UV–vis spectrophotometer combined with color difference meter. The results showed the synthesized WO₃ powders with hexagonal phase got much better photochromic properties than the WO₃ powders with cubic phase, the ones not appear until about 160 °C. Besides, the WO₃ powder synthesized at 120 °C exhibited the best photochromic properties of the samples prepared below 160 °C, the particles of which formed a shape of clusters of cactus with uniform size and good dispersion.     

Phase transformation in Ti–48Al–6Nb porous alloys and its influence on pore properties

Ti–48Al–6Nb porous alloys were synthesized by the powder metallurgy (PM) method, and the associated phase transformation and pore parameter were investigated in order to reveal the pore-formation mechanism. The present results indicate that the Nb–Al and Ti–Al phase transformations contribute to the pore-formation. It was found that the five-step phase transformations for the Ti–48Al–6Nb porous alloys occur as follows: (1) Ti + Al → TiAl₃ at 600–700 °C; (2) Nb + Al → NbAl₃ at 700–900 °C; (3) TiAl₃ + Ti → TiAl at 900–1100 °C; (4) TiAl + Ti → Ti₃Al/TiAl at 1100–1350 °C; (5) NbAl₃ + Nb → Nb₂Al and the Ti₃Al turns to the major phase at 1350 °C. These phase transformations made the pore-diameter increasing continuously from 1.71 μm to 12.10 μm and also made the pore volume distributing widely. At the second step of 700–900 °C, the Nb–Al phase transformation leads to 5% more volume expansion compared to the Ti–Al based porous alloys. Meanwhile, the porosity and total pore area initially increase and then decrease at this step, but they increase intensely at the final step, which is needed as a catalytic carrier.     

Sintering temperature-induced electrical properties of (Ba0.90Ca0.10)(Ti0.85Zr0.15)O3 lead-free ceramics

Effects of the sintering temperature on the microstructure and electrical properties of (Ba_0.90Ca_0.10)(Ti_0.85Zr_0.15)O₃ (BCTZ) lead-free piezoelectric ceramics have been studied, where these ceramics were prepared by the conventional oxide-mixed method at varied sintering temperatures from 1300 °C to 1500 °C. These BCTZ ceramics exhibits a phase transition from a rhombohedral phase to the coexistence of rhombohedral and tetragonal phases with an increase of sintering temperature. With an increase of sintering temperature, their relative density and average grain size gradually increase, and electrical properties are improved greatly. These BCTZ ceramics sintered at ～1440 °C have optimum electrical properties: d₃₃ ～ 442 pC/N and k_p ～ 48.9%, making it a promising material for lead-free piezoelectric ceramics.     

Magnetic and catalytic properties of cubic copper ferrite nanopowders synthesized from secondary resources

Cubic copper ferrite CuFe₂O₄ nanopowders have been synthesized via a hydrothermal route using industrial wastes. The synthesis conditions were systematically studied using statistical design (Box–Behnken Program) and the optimum conditions were determined. The results revealed that single phase of cubic copper ferrite powders can be obtained at different temperatures from 100 to 200 °C for times from 12 to 36 h with pH values 8–12. The crystallite size of the produced powders was in the range between 24.6 and 51.5 nm. The produced copper ferrite powders were appeared as a homogeneous pseudo-cubic-like structure. A high saturation magnetization (M_s 83.7 emu/g) was achieved at hydrothermal temperature 200 °C for 24 h and pH 8. Photocatalytic degradation of the methylene blue dye using copper ferrite powders produced at different conditions was investigated. A good catalytic efficiency was 95.9% at hydrothermal temperature 200 °C for hydrothermal time 24 h at pH 12 due to high surface area (118.4 m²/g).     

Preparation and characterization of selenite substituted hydroxyapatite

Selenite-substituted hydroxyapatite (Se-HA) with different Se/P ratios was synthesized by a co-precipitation method, using sodium selenite (Na₂SeO₃) as a Se source. Selenium has been incorporated into the hydroxyapatite lattice by partially replacing phosphate (PO₄^3 ?) groups with selenite (SeO₃^2 ?) groups. X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM) techniques reveal that substitutions of phosphate groups by selenite groups cause lower carbonate groups occupying at phosphate sites and change the lattice parameters of hydroxyapatite. The powders obtained are nano-crystalline hydroxyapatite when the Se/P ratios are not more than 0.1. The particle shape of Se-HA has not been altered compared with selenite-free hydroxyapatite but Se-incorporation reduces the crystallite size. The crystallinity was reduced as the Se/P ratios increased until amorphous phase (Se/P = 0.3) appeared in the Se-HA powder obtained, and then another crystal phase presented as calcium selenite hydrate (Se/P = 10). In addition, the sintering tests show that the Se-HA powders with the Se/P ratio of 0.1 have thermal stability at 900 °C for 2 h; hence they have great potential in the fabrication of bone repair scaffolds.