Densification of nanocrystalline ITO powders in fast firing: effect of specimen mass and sintering atmosphere

Nano-sized indium tin oxide (ITO) powders were prepared by a coprecipitation method, and the sintering characteristics in fast firing were examined. The mass of the specimen, sintering atmosphere and sintering temperature varied. Oxygen atmosphere promoted the densification in normal rate sintering, while oxygen inhibited the densification in fast firing. Fast firing severely retarded densification as the mass of the specimen and the sintering temperature increased. This was explained by differential densification, which could easily occur in conditions with a high densification rate and a high thermal gradient in the specimen, where the outer region of the specimen densifies much faster than the center. Once the highly densified outer skeleton is formed, the inside of the specimen is difficult to densify because the outer skeleton geometrically constrains densification.     

Preparation of nanocrystalline MgO by surfactant assisted precipitation method

Nanocrystalline magnesium oxide with high surface area was prepared by a simple precipitation method using pluronic P123 triblock copolymer (Poly (ethylene glycol)-block, Poly (propylene glycol)-block, Poly (ethylene glycol)) as surfactant and under refluxing conditions. The prepared samples were characterized by X-ray diffraction (XRD), N₂ adsorption (BET) and scanning and transmission electron microscopies (SEM and TEM). The obtained results revealed that the refluxing time and temperature and the molar ratio of surfactant to metal affect the structural properties of MgO, because of the changes in the rate and extent of P123 adsorption on the prepared samples. The results showed that the addition of surfactant is effective to prepare magnesium oxide with high surface area and affects the morphology of the prepared samples. With increasing the P123/MgO molar ratio to 0.05 the pore size distribution was shifted to larger size. The sample prepared with addition of surfactant showed a plate-like shape which was completely different with the morphology of the sample prepared without surfactant. The formation of nanoplate-like MgO was related to higher surface density of Mg ions on the (0 0 1) plane than that on the other planes of the Mg(OH)₂ crystal. The (0 0 1) plane would be blocked preferentially by the adsorbed P123 molecules during the growing process of Mg(OH)₂ nanoentities and the growth on the (0 0 1) plane would be markedly restricted, and the consequence is the generation of nanoplate-like MgO. In addition, increase in refluxing temperature and time increased the specific surface area of the prepared MgO samples.     

Barium hydroxyapatite nanoparticles synthesized by citric acid sol-gel combustion method

Barium hydroxyapatite (BaHAP) nanoparticles have been synthesized by citric acid sol-gel combustion method using citric acid as a reductant/fuel and nitrate as an oxidant at a relatively low temperature of 600 °C. The thermal decomposition of nitrate-citrate xerogel was investigated by thermogravimetric/differential thermal analysis (TG/DTA) technique. The yielding powders calcined at 600 °C have been characterized by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and transmission electron microscope (TEM). The possible combustion process was presented.     

The crystallinity of calcium phosphate powders influenced by the conditions of neutralized procedure with citric acid additions

Calcium phosphate powders with nano-sized crystallinity were synthesized by neutralization using calcium hydroxide and orthophosphoric acid with the assistance of citric acid. The influence of processing parameters, such as free or additive citric acid, synthetic temperature and ripening time, on the crystallinity of hydroxyapatite were investigated. The results of X-ray diffraction and microstructure observations showed that the crystallinity and morphology of nano-sized hydroxyapatite particles were influenced by the presence or absence of citric acid. It was found that the crystallinities and crystallite sizes of hydroxyapatite powders prepared with the additive citric acid increased with increasing synthetic temperature and ripening time. Especially, the crystallinities of (h k 0) planes were raised and more homogeneously grown particles were obtained with increasing synthetic temperature.     

Preparation of nanocrystalline bredigite powders with apatite-forming ability by a simple combustion method

Nanocrystalline bredigite (Ca₇MgSi₄O₁₆) powders were synthesized by a simple solution combustion method. Phase pure bredigite powders with particle sizes ranging from 234 to 463 nm could be obtained at a relatively low temperature of 650 °C. The apatite-forming ability of the bredigite powders was examined by soaking them in a stimulated body fluid. The compositional and morphological changes of the powders before and after soaking were analyzed by X-ray diffraction and scanning electron microscopy and the results showed that hydroxyapatite was formed after soaking for 4 days.     

Synthesis of alumina powders by the glycine-nitrate combustion process

The combustion synthesis technique using glycine as fuel and aluminum nitrate as an oxidizer is able to produce alumina powders. Thermodynamic modeling of the combustion reaction shows that as the fuel-to-oxidant ratio increases, the amount of gases produced and adiabatic flame temperatures also increases. X-ray diffractions showed the amorphous structure for as-synthesized powder and presence of well-crystallized α-Al₂O₃ after calcination at 1100 °C during soaking time of 1 h. Alumina's largest measured specific surface area was 15 m²/g with BET method and 0.51 glycine-to-nitrate ratio.     

Synthesis of nanocrystalline magnesium titanate by an auto-igniting combustion technique and its structural, spectroscopic and dielectric properties

Nanocrystalline magnesium titanate was synthesized through an auto-ignited combustion method. The phase purity of the powder was examined using X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy and Raman spectroscopy. The transmission electron microscopy study showed that the particle size of the as-prepared powder was in between 20 and 40 nm. The nanopowder could be sintered to 98% of the theoretical density at 1200 °C for 3 h. The microstructure of the sintered surface was examined using scanning electron microscopy. The dielectric constant (?_r) of 16.7 and loss factor (tan δ) of the order of 10⁻⁴ were obtained at 5 MHz when measured using LCR meter. The quality factor (Q_u × f) 73,700 and temperature coefficient of resonant frequency (τ_f) −44.3 ppm/°C, at 6.5 GHz are the best reported values for sintered pellets obtained from phase pure nanocrystalline MgTiO₃ powder.     

Synthesis of nanocrystalline rare earth oxides by glycothermal method

The reaction of yttrium acetate hydrate in 1,2-propanediol at 300 °C yielded a product containing acetate groups and glycol moieties. From this product, Y₂O₃ was directly crystallized at 400 °C without the formation of a carbonate oxide phase. The thus-obtained Y₂O₃ samples had a small crystallite size (2.2 nm) and significantly large surface area (280 m²/g). Other nanocrystalline rare earth (Gd-Yb) oxides were also obtained by this method.     

Formation and control of mechanism for the preparation of ultra-fine barium strontium titanate powders by the citrate precursor method

A modified citrate precursor method, combining the advantages of the nitrate autocombustion method by introducing the nitric acid, was successfully used to synthesize ultrafine Ba_0.70Sr_0.30TiO₃ powders. Slight agglomerated and homogenized BST powders, with an average particle size of 20 nm, were obtained at 800 °C. Combining the results of TG/DTA and XRD, it can be concluded that the formation of BST powders takes place via two reaction mechanisms: decomposition of an intermediate oxycarbonate mechanism (DIOm) at low temperature, and solid-state reaction mechanism (SSRm) between nanocrystalline carbonates and amorphous TiO₂ at high temperature. TEM shows higher amount of CA led to BST powders of better quality in morphology. Based on results of chemical analysis, it is suggested that higher amount of CA drives the mechanism to tend to DIOm. By simply adjusting the ratio of reagents, the reaction mechanism can be dominated and we can greatly control the final morphology of the powders.     

Fabrication and dissolution behavior of hollow hydroxyapatite microspheres intended for controlled drug release

Hollow hydroxyapatite (HA) microspheres were fabricated by a simple spray drying method in this study. Moreover, the dissolution behavior of these hollow HA microspheres after immersion in simulated body fluid (SBF) was also studied. The results indicated that the dissolution of the HA microspheres in SBF is not homogeneous in a layer-by-layer fashion but was preferential at different locations of the particle surface. Generically, dissolution preferentially occurs on the location with looser structure and high porosity of the microspheres. The degradable HA microspheres are expected to have potential applications in bone local drug delivery systems.     

Formation, sintering, and electrical conductivity of (Nd1−xCax)CrO3 (0≤x≤0.25) using citric acid as a gelling agent

In Ca²⁺-substituted NdCrO₃, single-phase perovskite compounds (Nd_1−xCa_x)CrO₃, where x=0-0.25, have been formed by a citric acid processing. (Nd_1−xCa_x)CrO₃ powders consisting of submicrometer-size particles are sinterable; dense materials can be fabricated by sintering for 2 h at 1700°C under atmospheric pressure. The relative densities, grain sizes, and electrical conductivities increase with increased Ca²⁺ content. (Nd_0.75Ca_0.25)CrO₃ materials show an excellent electrical conductivity of 1.9×10 S m⁻¹ at 1000°C.     

Synthesis and microwave dielectric properties of CaO-MgO-SiO2 submicron powders doped with Li2O-Bi2O3 by sol-gel method

Using Ca(NO₃)₂·4H₂O, Mg(NO₃)₂·6H₂O, Si(OC₂H₅)₄, LiNO₃ and Bi(NO₃)₃·5H₂O as raw materials, CaO-MgO-SiO₂ submicron powders were prepared at low temperature by sol-gel method. The crystallization temperature was decreased enormously by the introduction of Li-Bi liquid phase sintering aids into Ca-Mg-Si sol, and the powders with average particle sizes of 80-100 nm and 200-400 nm were obtained at the calcining temperature of 750 °C and 800 °C, respectively. The sintering characteristic and dielectric properties of powders calcined at 750 °C with different content of powders calcined at 800 °C were studied. When the content of powders calcined at 800 °C was 10 wt%, the dielectric ceramic sintered at 890 °C had compact structure, and possessed excellent microwave dielectric properties: ?_r = 7.16, Q × f = 25630 GHz, τ_f = −69.26 ppm/°C.     

Activated combustion features in the Mo-Si-C-promoter system and synthesis of MoSi2-SiC composite powders

Opportunities on combustion synthesizing the MoSi₂-SiC ceramic composites in a wide range of compositions under the chemical activated mode were studied. Molybdenum, silicon powders and carbon black were used as initial reagents, and Teflon was used as an activating additive. It was established that Teflon displays a dual (kinetic and thermal) impact on the interaction between reagents. The phasic character of the combustion process evolution, being characterized by low- and high-temperature regimes, was revealed. The end-products were subjected to SEM, XRD and chemical analyses.     

Effect of dispersant on preparation of barium-strontium titanate powders through oxalate co-precipitation method

The quantitative precipitation of barium-strontium titanyl oxalate: (Ba_0.6Sr_0.4TiO(C₂O₄)₂·4H₂O, BSTO) precursor powders were successfully prepared through oxalate co-precipitation method. The pyrolysis of BSTO at 800 °C/4 h produced the barium-strontium titanate (Ba_0.6Sr_0.4TiO₃, BST) powders. Two kinds of dispersants namely ammonium salt of poly mathacrylic acid (PMAA-NH₄) and polyethylene glycol (PEG) were added respectively during the co-precipitation procedure. The powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), etc. Experimental results show that the addition of the dispersants reduced the productive rate of BST powders. The BSTO and BST powders obtained by aforementioned technique without dispersants were homogeneous with quasi-orbicular morphology. The particles grew into spindle shape with the effect of PEG. The morphology homogeneity was broke with small grains as well as large agglomerated particles concurrent when PMAA-NH₄ was added. The mechanism of the effect of the two dispersants was investigated in detail.     

Synthesis of ultrafine YAG:Tb phosphor by nitrate-citrate sol-gel combustion process

Ultrafine terbium-doped yttrium aluminum garnet (YAG:Tb) phosphor powders are prepared by a nitrate-citrate sol-gel combustion process using 1:1 ratio of citrate/nitrate. Phase evolution of the synthesized powder is determined by X-ray diffraction (XRD) techniques. Single-phase cubic YAG:Tb crystalline powder is obtained by calcinating the amorphous materials at 900 °C and no intermediate phase is observed. Transmission electronic microscope (TEM) morphology shows that the resultant YAG:Tb powders have uniform size and good homogeneity. The particle size of the product is investigated as a function of the calcination temperature. The photoluminescence (PL) spectrum of Tb³⁺ substituted for Y³⁺ in YAG with 5.0% content has been measured on samples calcined at different temperatures.     

Synthesis of aluminum borate nanorods by a low-heating-temperature solid-state precursor method

Well-crystalline Al₄B₂O₉ nanorods were synthesized by a low-heating-temperature solid-state precursor method. This process does not involve the use of metal catalyst or protective gas. The products were characterized by thermogravimetry and differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results showed the products to possess a single phase, large surface area, narrow size distribution of 20-30 nm and lengths up to several micrometers. A self-catalytic growth mechanism of the aluminum borate nanorods is proposed.     

Preparation of hydroxyapatite rod-like crystals by protein precursor method

Hydroxyapatite (HAP) rod-like crystals were successfully prepared by thermolysis of bovine serum albumin (BSA)/calcium-phosphate (CaP) colloidal precursors. The precursors were obtained by precipitation method from Ca(H₂PO₄)₂ and Ca(OH)₂, in which BSA was added as regulation additive and ultrasound irradiation was utilized as assistant technology. The properties of the precursors, such as size distribution, morphology, thermodynamic changes, were determined by DLS, SPM and TGA-DTA. The characterization results from DLS, SPM, TG-DTA, XRD and SEM indicated that BSA interacted with CaP particles and formed about 7-130 nm BSA/CaP hybrid colloidal particles between 2 and 4 g/L of BSA concentration. With the increasing of sintering temperature, BSA disintegrated and burned out, and rod-like HAP crystals formed at about 600 °C. With the increasing of BSA concentration, the phase composition of products did not change and the HAP crystals became more uniform and smaller. The ratio of length to width ranged from 7.6 to 12 at 4 g/L BSA concentration. This method provides for a controllable bottom-up fabrication of HAP rod-like crystals.     

Combustion of TiO2-Mg and TiO2-Mg-C systems in the presence of NaCl to synthesize nanocrystalline Ti and TiC powders

The combustion process of TiO₂-Mg and TiO₂-Mg-C systems with sodium chloride as an inert diluent was investigated. The values of combustion parameters and temperature distribution on a high-temperature wave according to the amount of sodium chloride were obtained by the thermocoupling technique. The leading stages of combustion processes are found and the sizes of reactionary zones were estimated. It is shown that the introduction of NaCl in an initial mixture promotes the formation of a nanocrystalline structure of the final products. As a result, nanosized titanium, and titanium carbide powders have been successfully obtained.     

Lead magnesium niobate-lead titanate fibres by a modified sol-gel method

Lead magnesium niobate-lead titanate (PMN-PT) ceramic fibres with the nominal composition of 0.65Pb(Mg_1/3Nb_2/3)O₃-0.35PbTiO₃ have been fabricated by a modified sol-gel method. Due to the difficulty of dissolving the magnesium component, the mixed oxide method was used together with the traditional sol-gel method. To obtain crack-free fibres, pyrolysis was carried out at a very slow heating rate under specific atmosphere to control the organic burnout. The thermal and microstructural properties were investigated using thermogravimetric analysis, scanning electron microscopy and X-ray diffraction. The optimum sintering temperature is 1200 °C and yields a fibre with a final diameter of around 100 μm. A single PMN-PT fibre has been poled and its electrical properties were measured. The properties of the fibre are found to be better than that of a ceramic disc.     

Synthesis of nanocrystalline TiO2 with high photoactivity and large specific surface area by sol-gel method

Nano-TiO₂ powder was prepared by sol-gel method with modified precursor, tetrabutyl titanate (TBT), and photocatalytic oxidation was applied in removal of organics in the powder. The microstructure of as-prepared nano-TiO₂ was determined using UV-vis, TEM, XRD and BET. The results indicated that the nano-TiO₂, with grain size of 3.8 nm and specific surface area of 359.1 m²/g, was composed of anatase alone, and that it exhibited significant blue-shift in its UV-vis spectrum. The decomposition of organics in the sample was systematically investigated using FT-IR and TG-DTA. According to the testing results, we could conclude that organics in the samples were completely eliminated by means of photocatalytic oxidation. With photocatalytic decoloration of active brilliant red X-3B in aqueous solution as model reaction, the photocatalytic activity of as-prepared nano-TiO₂ was investigated and was compared with that of the samples experiencing heat treatment and Degussa P-25 as well. The experimental results indicated that the photoactivity of as-prepared nano-TiO₂ is much higher than that of the samples experiencing heat treatment.