Low-temperature synthesis of leucite crystals using kaolin

Synthesis of leucite crystals below 1000 °C using natural kaolin as the primary raw material was investigated. Spherical leucite crystals having a diameter of approximately 50 μm were prepared by heating a powder mixture of Al₂(SO₄)₃, kaolin and K₂SO₄ (in mass ratios of 3:3:15) at 900 °C for 3 h. Quartz, the main accessory phase in kaolin, and the amorphous metakaolin formed upon heating kaolin were found to be responsible for the decreased synthesis temperature.     

Grain growth and microstructural evolution of yttrium aluminum garnet nanocrystallites during calcination process

An yttrium aluminum garnet (YAG) precursor precipitate was synthesized by urea method using yttria (Y₂O₃) and aluminum nitrate (Al(NO₃)₃·9H₂O) as raw materials. The fresh wet precipitate was dried by supercritical carbon dioxide (CO₂) fluid and the resulting powder was calcined at temperatures from 600 to 1600 °C. Crystallization of YAG was detected at 800 °C, and completed at 900 °C. HRTEM images of the YAG product obtained above 900 °C revealed crystallographically specific oriented attachment along the [1 1 2] direction. Based on the observation of the particle morphology a possible growth mechanism of YAG nanoparticles was presented. The fast increase on the average crystallite size of YAG at temperatures from 900 to 1300 °C is attributed to the crystallographically specific oriented attachment growth process. As the growth process proceeds at higher temperatures, oriented attachment based growth becomes less important because of the increase on particle size, and the self-integration assisted by the Ostwald ripening becomes dominant.     

Sintering mechanism of blast furnace slag–kaolin ceramics

A general ceramics processing scheme by cold uniaxial pressing and conventional sintering process have been used to prepare ceramics from mixtures of blast furnace slag (BFS) and kaolin (10%, 30% and 50% kaolin). The properties of the ceramics were studied by measuring linear shrinkage, bulk density, apparent porosity and mechanical properties of samples heated at temperatures from 800 °C to 1100 °C. The formed crystalline phases were characterized using X-ray diffraction (XRD) and scanning electron microscope (SEM). Slag melt formed at relatively low temperatures (800–900 °C) modified the sintering process to liquid phase sintering mechanism. Combination of BFS with 10% kaolin gave the highest mechanical properties, densification and shrinkage at relatively low firing temperatures. The crystalline phases were identified as gehlenite (Ca₂Al₂SiO₇) in both BFS and BFS with 10% kaolin samples. Anorthite (CaAl₂Si₂O₈) phase increased with increasing kaolin contents. In the case of kaolin-rich mixtures (30% and 50% kaolin), increased expansion took place during firing at temperatures in the range 800–1000 °C. This effect could be attributed to the entrapment of released gases.     

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.     

Factors affecting the performance of metakaolin geopolymers exposed to elevated temperatures

The effects of geopolymer binder systems exposed to elevated temperatures are examined. Geopolymers investigated were synthesized from metakaolin, activated by combinations of sodium/potassium silicate and sodium/potassium hydroxide. The specimens were then exposed to temperatures of 800 °C. The factors studied were: (1) calcining temperatures of kaolin; (2) Si/Al ratio of the geopolymer; (3) activator/metakaolin ratio; (4) curing temperature; and (5) alkali cation type. Altogether 30 geopolymer formulations were studied. The samples were subjected to compressive strength, thermogravimetry, and scanning electron microscopy tests. Results showed that Si/Al ratio has a significant influence on elevated temperature exposure deterioration. Lesser strength loss due to elevated temperature exposures were observed in geopolymer with high Si/Al ratios (>1.5). The geopolymer binders activated by potassium-based activators showed an enhanced post-elevated temperature exposure performance compared to sodium-based systems. The optimum calcining temperature of kaolin and curing temperatures for improved temperature performance are also reported.     

CTAB-assisted sol-gel synthesis of Li4Ti5O12 and its performance as anode material for Li-ion batteries

A simple CTAB-assisted sol-gel technique for synthesizing nano-sized Li₄Ti₅O₁₂ with promising electrochemical performance as anode material for lithium ion battery is reported. The structural and morphological properties are investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The electrochemical performance of both samples (with and without CTAB) calcined at 800 °C is evaluated using Swagelok™ cells by galvanostatic charge/discharge cycling at room temperature. The XRD pattern for sample prepared in presence of CTAB and calcined at 800 °C shows high-purity cubic-spinel Li₄Ti₅O₁₂ phase (JCPDS # 26-1198). Nanosized-Li₄Ti₅O₁₂ calcined at 800 °C in presence of CTAB exhibits promising cycling performance with initial discharge capacity of 174 mAh g⁻¹ (∼100% of theoretical capacity) and sustains a capacity value of 164 mAh g⁻¹ beyond 30 cycles. By contrast, the sample prepared in absence of CTAB under identical reaction conditions exhibits initial discharge capacity of 140 mAh g⁻¹ (80% of theoretical capacity) that fades to 110 mAh g⁻¹ after 30 cycles.     

Stability of 8-hydroxyquinoline aluminum films encapsulated by a single Al2O3 barrier deposited by low temperature atomic layer deposition

100 nm thick 8‐AlQ₃ films deposited onto silicon wafers have been encapsulated by mean of low temperature atomic layer deposition of Al₂O₃ (20 nm). Investigation of the film evolution under storage test as harsh as 65 °C/85% RH has been investigated up to ~ 1000 h and no severe degradation could be noticed. The results have been compared to raw AlQ₃ films which deteriorate far faster in the same conditions. For that purpose, fluorescence measurements and atomic force microscopy have been used to monitor the film evolution while transmission electron microscopy has been used to image the interface between AlQ₃ and Al₂O₃. This concept of bilayer AlQ₃/Al₂O₃ barrier films has finally been tested as an encapsulation barrier onto an organic light-emitting diode.     

The phase evolution of phosphoric acid-based geopolymers at elevated temperatures

The Al₂O₃-2SiO₂ powders for sol-gel synthesis have good phosphoric acid activation properties. The phase evolution of phosphoric acid-based geopolymers at elevated temperatures is similar to that of alkali-based metakaolin geopolymers. The chemosynthetic phosphoric acid-based geopolymers have been found to possess extremely good thermal stability, with no sign of melting up to 1550 °C. The onset temperature of crystallization of the specimens occurred at 900 °C. The amount of quartz and berlinite crystal reached a maximum at approximately 1000 °C. Further exposure to 1150 °C showed that quartz and berlinite phases were converted to cristobalite and aluminum phosphate.     

Thermal behaviour of inorganic geopolymers and composites derived from sodium polysialate

Inorganic polymers based on alumina and silica polysialate units were synthesised at room temperature from metakaolinite and sodium silicate in a highly alkaline medium, followed by curing and drying at 65 °C. When properly cured, these polymers exhibit remarkable thermal stability; after losing their hydration water at about 200 °C, they retain their X-ray-amorphous tetrahedral Al and Si network up to the onset of melting at 1300 °C. A small amount of mullite and corundum formed at 1200-1300 °C may result from the presence of a trace of unreacted metakaolinite. Similar experiments with poorly-curing formulations containing higher Na and Si contents show that their unpolymerised components form crystalline nepheline (NaAlSiO₄) at 800 °C, prior to melting at about 1100 °C.A series of geopolymer composites were prepared containing 10-20 vol.% of various granular inorganic fillers ranging from waste demolition materials through mineral tailings to engineering ceramics. The physical and thermal properties (bulk density, compressive strength and thermal expansion) of these composites were measured. The thermal expansion is influenced by the properties of the filler, but all the samples showed only slight expansion up to ∼800 °C on the first heating cycle. Microcracking of the composite bodies during drying can be minimised by the addition of a small amount of glycerol.     

Microstructure evolution and oxidation behaviour of Tif/TiAl3 composites

In this paper, Ti_f/TiAl₃ composites were fabricated by infiltration–in situ reaction method and its oxidation behaviours were investigated by cyclic oxidation testing at 700 °C, 800 °C and 900 °C. The microstructure evolution and oxidation of Ti_f/TiAl₃ composites were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive X-ray diffraction (EDX). The reaction between Ti₃Al particles and Al was more violent than that of Ti fibres and Al. Ti₃Al/Al reaction consumed a large amount of Al and inhibited the reaction of Ti fibres indirectly. Reactant of Ti fibres was TiAl₃ at 700 °C, and four reaction layers surrounding Ti fibre (Ti₃Al, TiAl, TiAl₂ and TiAl₃ from inner to outside) were observed above 800 °C. The thickness of the total reaction layers increased little with temperature and time, while the thickness of inner reaction layers increased remarkably. A model corresponding to the microstructure evolution process was drawn schematically. Oxidation resistance of Ti_f/TiAl₃ composites decreased with increasing of temperature, and changed from cubic law at 700 °C to parabolic law at 900 °C. The oxidation weight gain of Ti_f/TiAl₃ composite was dominated by the exposed Ti fibres. Due to outward diffusion of Ti and Al element, the oxide of Ti fibre at 900 °C changed to mushroom-shape. Fortunately, when TiAl₃ was oxidized, a thin and continuous Al₂O₃ layer was formed, protecting matrix from further oxidation.     

Effect of lanthanum replacement by strontium in lanthanum nickelate crystals synthetized using gelatin as organic precursor

La_1-xSr_xNiO₃ (0 ≤ x ≤ 0.8) nanopowders were successfully synthesized using gelatin as a polymerization agent. Powders were calcined for 4 h at 700 and 900 °C and characterized using thermal analysis, X-Ray diffraction and scanning electron microscopy. Perovskite phase formation was achieved at 700 °C, with an increase in crystallinity and secundary phases forming in powders calcined at 900 °C. The structure of the lanthanum nickelate was confirmed as rhombohedral and transition to tetragonal structure occurred by partially substituting lanthanum with strontium.     

Combination formation in the reinforcement of metakaolin geopolymers with quartz sand

Although quartz sand is widely used as filler material in construction, a few studies investigated the incorporation of quartz sand in geopolymers. To study the incorporation of quartz sand in the reinforcement of metakaolin geopolymer not only fills this gap, but also gives a clue on using non-calcinated aluminosilicates (e.g., mine tailings) in the synthesis of geopolymers. In the presence of sodium silicate, metakaolin geopolymers were synthesized with quartz sand of various size ranges as filler material. XRD, FTIR, SEM and NMR characterizations on the geopolymers indicate the dissolution, precipitation, and the formation of combination on quartz particles that associates them into the geopolymeric gel, so as to reinforce the mechanical strength of geopolymers. The compressive strength of metakaolin geopolymers with only silicate, silicate plus quartz sand and silicate plus rutile sand is 31.2, 52.2 and 41.5 MPa, respectively. In geopolymer with silicate and quartz sand, a decreasing Si/Al ratio as increasing distance from the quartz particle is observed through an energy dispersive X-ray (EDX) mapping. The SEM images and NMR spectra suggest that the formed combination is of several micrometers with main species of polysialates (-Si-O-) such as Q⁴(2Al), Q⁴(1Al).     

Comparison for the crystal structure,synthesis and microwave dielectric properties of alkaline earth orthophosphates

A₃(PO₄)₂ compounds have different crystal structures when A sites are occupied by Ca or heavy alkaline earth metal atoms (Sr or Ba). The compounds with isomorphous crystal structure were synthesized by solid-state reaction method when the A-site atoms were Sr or Ba, and their crystal structure and microstructure of the sintered ceramics were investigated by X-ray powder diffraction (XRD) and scanning electron microscope (SEM), respectively. The microwave dielectric properties were measured using a network analyzer. It was found that Ba₃(PO₄)₂ could be sintered at 1060 °C, while the α-Sr₃(PO₄)₂ ceramics that has a smaller Sr²⁺ ionic radius, could be sintered at 1200 °C, and higher relative densities were obtained. The dielectric constant (?) of the α-Sr₃(PO₄)₂ is higher than that of Ba₃(PO₄)₂, but Ba₃(PO₄)₂ has a higher Q × f value than that of β-Ca₃(PO₄)₂ and α-Sr₃(PO₄)₂, which could be interpreted by the differences in ionic polarizability and bond strength. The temperature coefficients of resonant frequency (τ_f) for all samples with isomorphous crystal structure have positive values, ranging between +11 and +66 ppm °C⁻¹.     

Microwave hydrothermal synthesis of nanoporous cobalt oxides and their gas sensing properties

In this paper, the precursors were synthesized by microwave hydrothermal method using Co(NO₃)₂·6H₂O as raw material, CO(NH₂)₂ and KOH as precipitants, respectively. The precursors and calcined products were characterized by XRD, FESEM, and BET-BJH. The results show that both constituent and synthetic condition can determine the products morphology. When using KOH as precipitant, hollow Co₃O₄ nanorings were obtained whose precursor was synthesized at 140 °C for 3 h and calcined at 500 °C in air for 2 h. While using CO(NH)₂, Co₃O₄ like-nanochains were obtained whose precursor was synthesized at 110 °C for 1 h and calcined at 420 °C in air for 2 h, and Co₃O₄ nanosheets were obtained while their precursor was synthesized at 140 °C for 3 h and calcined at 500 °C in air for 2 h. The sensitivity test of Co₃O₄ to alcohol reveals that the hollow Co₃O₄ nanorings show the best sensitivity, porous Co₃O₄ like-nanochains are superior to that of the porous nanosheets.     

Preparation and characterization of Y3Al5O12 (YAG) nano-powder by co-precipitation method

YAG precursor was synthesized by a co-precipitation method from a mixed solution of aluminum and yttrium nitrates with aqueous ammonia as the precipitator. The structure, phase evolution and morphology of YAG precursor and the sintered powders were studied by means of IR, TG/DTA, XRD, TEM methods. It was found the precursor with approximate composition of Al(OH)₃·0.3[Y₂(OH)₅·(NO₃)₂·2H₂O] directly transformed to pure-YAG phase at 800 °C and no intermediate phases were detected. YAG nanocrystalline powders from sintering the precursor at different temperatures were less-aggregated and the diameters of the grains were about 40-100 nm. BET surface area of the particles decreased with increase of calcination temperature and the powder sintered at 800 °C can be used for fabrication of transparent YAG ceramics.     

La1−xSrxCuO2.5−δ as new cathode materials for intermediate temperature solid oxide fuel cells

La_1−xSr_xCuO_2.5−δ (LSCu), which exhibit excellent electrical conductivity and oxygen vacancies were investigated as potential cathode materials for solid oxide fuel cell (SOFC) applications. The structure stability, electrical conductivity, cathodic overpotential, and the reactivity with yttria-stabilized zirconia (YSZ) were examined in this study. It was found that the LSCu perovskite was obtained only when the addition of strontium fell in the range between 15 and 30%. With more than 20% of strontium addition, this material showed excellent electrical property and immunity to the reaction with YSZ at 800 °C. The conductivities of LSCu were as high as 900 S/cm at 600 °C, and 800 S/cm at 800 °C. The cathodic overpotential of this material was approximately 3.8 and 10.6 mV at a current density of 100 mA/cm² at 850 and 750 °C, respectively. These properties are superior to Sr-doped lanthanum manganite (LSM), which is the state-of-the-art cathode material of SOFCs.     

In situ fabrication of (α-Al2O3 + Al3Zr)/Al composites in an Al–ZrO2 system

Synthesis of a (α-Al₂O₃ + Al₃Zr)/Al in situ composite via exothermic dispersion synthesis (XD) process in an Al–ZrO₂ system has been investigated. Thermodynamic analysis indicates that the reaction between Al and ZrO₂ can spontaneously occur due to its negative Gibbs free energy of the Al–ZrO₂ system. When the reinforcement volume fraction is 30 vol.%, there is only one exothermic peak observed in the DSC curve. The final combustion products are α-Al₂O₃ particles and Al₃Zr blocks, which distribute uniformly in the aluminum matrix. The tensile strength, elongation rate and micro-hardness are 215.2 MPa, 3.0% and 304 MPa, respectively. However, if the reinforcement volume fraction increases to 100 vol.%, two exothermic peaks are observed in its corresponding DSC curve and the peak intensities are significantly increased. When the heating rates are 10 °C/min, 20 °C/min and 30 °C/min, the initiation temperatures are 744 °C, 776 °C and 782 °C, respectively. The reactions occurred in the Al–ZrO₂ system have two steps: the first is that the Al atom reacts with ZrO₂ to produce the α-Al₂O₃ and active Zr atoms, and the second is that the active Zr atoms disperse into the matrix and react with Al to form Al₃Zr. The values of activation energy of the two reactions are around 315.8 kJ/mol and 191.1 kJ/mol, respectively.     

TG/DSC analysis of Fe8(OOH)16Cl1.3 nanospindles

The thermal analysis of Fe₈(OOH)₁₆Cl_1.3 (Akaganeite-M) nanospindles prepared by the hydrolysis of FeCl₃ solutions are determined by thermogravimetric analyses and differential scanning calorimetry (TG/DSC), in conjunction with field-emission scanning electron microscopy (FE-SEM), and X-ray diffraction (XRD). Different products are formed after Fe₈(OOH)₁₆Cl_1.3 nanospindles are calcined at different temperatures for 30 min in N₂ atmosphere: Fe_1.833(OH)_0.5O_2.5 and magnetite obtained at 250 °C; pure magnetite (Fe₃O₄) obtained at 630 °C; and magnetite containing some iron nitrides (Fe₂N and Fe₄N) obtained at 800 °C. The calcination of Fe₈(OOH)₁₆Cl_1.3 provides a new method to prepare pure magnetite.     

Al and Ti/Al contacts on n-GaN

Al(60 nm) and Ti(40 nm)/Al(160 nm) metal layers have been deposited by thermal evaporation onto n-GaN epitaxial layers grown by metal organic chemical vapour deposition (MOCVD) on a c-plane sapphire substrate. The samples have been annealed at 300, 400, 700 or 900 °C for 10 min in vacuum. The microstructural and electrical properties of the contacts have been investigated by electron microscopy, X-ray diffraction and by current-voltage measurements. As-deposited Al and Ti/Al contacts were rectifying with Schottky barrier heights below 0.35 eV and 0.38 eV, respectively. After heat treatment at 300 °C and 400 °C both contacts exhibited linear current-voltage characteristics. After annealing at 700 °C Al contacts became rectifying with a barrier height of 0.42 eV, while Ti/Al contacts remained nearly linear at the same temperature. The electrical characteristics and XRD analysis indicated that the upper metal in Ti/Al contact diffused in the Ti layer already during deposition. Cross-sectional transmission electron microscopy revealed that in the case of Ti/Al contacts, the continuity of the Ti layers ceased when annealing above 700 °C. X-ray diffractions showed, that a Ti₂N interface phase formed in Ti/Al contacts at 700 and 900 °C, and an AlN interface phase developed in the same contact at 900 °C.     

Photocatalysis and characterization of the gel-derived TiO2 and P-TiO2 transparent thin films

The gel-derived TiO₂ and P-TiO₂ transparent films coated on fused-SiO₂ substrates were prepared using a spin-coating technique. Effects of phosphorus dopants and calcination temperature on crystal structure, crystallite size, microstructure, light transmittance and photocatalytic activity of the films were investigated. By introducing P atoms to Ti-O framework, the growth of anatase crystallites was hindered and the crystal structure of anatase-TiO₂ could withstand temperature up to 900 °C. The photocatalytic activities of the prepared films were characterized using the characteristic time constant (τ) for the photocatalytic reaction. The titania film with a smaller τ value possesses a higher photocatalytic ability. After exposing to 365-nm UV light for 12 h, the P-TiO₂ films calcined between 600 °C and 900 °C can photocatalytically decomposed ≥ 84 mol% of the methylene blue in water with corresponding τ ≤ 7.1 h, which were better than the pure TiO₂ films prepared at the same calcination temperature.