Surfactant directed synthesis of mesoporous alumina and α‐alumina single crystal

Mesoporous Al₂O₃ were positively synthesized via treatment of the freshly precipitated amorphous alumina gel using aluminium sulphate as aluminium source, and sodium dodecyl sulphate (SDS) as structure‐directing agent (SDAs). The microstructures, morphologies and textural properties of the as‐prepared materials were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM) and thermo gravimetric analysis (TG‐DTA). The calcined product at 600 °C was highly porous in nature having a BET surface area of 42 m²/g. These porous Al₂O₃ exhibits excellent adsorption performance for Congo red and the corresponding decolourisation efficiencies reached 99% in just 15 min at 27 °C. The subsequent calcined product at 1200 °C is the alpha alumina single crystal hexagonal platelets with rhombohedral crystallization.     

Effect of heat treatment on phase transformation of aluminum nitride ultrafine powder prepared by chemical vapor deposition

Ultrafine aluminum nitride (AlN) powders were obtained by chemical vapor deposition via AlCl₃–NH₃–N₂ system operated at various temperatures and at a same 200 cm³/min flow rate of NH₃ and N₂, respectively. It has been shown that when the reaction temperature of AlCl₃ and NH₃ was above 600°C, then crystalline AlN powder can be formed; whereas, amorphous AlN was obtained with NH₄Cl if reacted in a lower-temperature zone of the reaction chamber. The amorphous AlN powder was heat treated at 1400°C under NH₃ and N₂ atmosphere for 2 h, then the crystalline phases of the obtained powder belong to a single phase of AlN; a mixture of AlN and Al₂O₃ and only AlON, respectively. On the other hand, if crystalline AlN powder is heat treated at 1400°C under N₂ atmosphere for 2 h, the crystalline phases were composed of the major phase of AlN and a minor phase of Al₂O₃. The morphology, particle size and agglomerate size of the AlN powder were strongly dependent on the heat-treatment temperature. The particle size of AlN powder increases from 28.1 to 45.0 nm, as the heat treatment temperature increases from 800 to 1400°C.     

Vapor phase growth of alumina whiskers by hydrolysis of aluminum fluoride

The vapor phase growth of alumina whiskers by the hydrolysis of aluminium flouride has been studied at an elevated temperature. The product was obtained in various forms: wool-like whiskers, needle-like whiskers, jointed needle-like crystals which consisted of linked small single crystals, tightly coagulated powder or as thin film covering the substrate. Aluminium oxi-fluoride was suggested as the intermediate gaseous species in the formation of alumina. The relation between the growth mechanism and crystal morphologies was studied.     

Acidity-dependent mesostructure transformation of highly ordered mesoporous silica materials during a two-step synthesis

Highly ordered mesoporous silica materials have been synthesized under mildly acidic conditions by templating with a nonionic triblock copolymer (Pluronic P104) in a two-step process. It was found that a transformation from the SBA-15 type 2-dimensional (2D) hexagonal channel mesostructure (p6mm symmetry) to the MSU-X type 3-dimensional (3D) worm-like mesostructure could be induced by varying the pH whilst keeping all other conditions constant. The transformation between two types of mesoporous silica materials can be attributed to the effect of varying proton concentration on the interaction between organic micelles and inorganic species. Both types of mesoporous materials have high surface areas, large pore volumes, thick pore walls, large mean pore sizes, and narrow pore size distribution.     

Effect of alumina on enthalpy of mixing of mixed alkali silicate glasses

The enthalpy of mixing of mixed alkali (Na₂O and K₂O) silicate glasses containing various concentrations of alumina was determined using an ion-exchange equilibrium method. For glasses with a constant alkali concentration, the enthalpy of mixing was found to become less negative with alumina addition. Consistent with our previous results on the enthalpy of mixing of alumina-free mixed alkali silicate glasses, the magnitude of enthalpy of mixing exhibited a good correlation with the molar volume mismatch of the corresponding two single alkali glasses as well as with the extent of conductivity mixed alkali effect, e.g. excess activation energy of conductivity, ΔE. The reduction of the magnitude of the enthalpy of mixing with alumina addition can be attributed to the reduction of non-bridging oxygen and ionic field strength. Combining the present results with results obtained earlier, the magnitude of the enthalpy of mixing for all mixed alkali (Na₂O and K₂O) silicate glasses with and without alumina was expressed by a simple function of a modified Tobolsky parameter, which takes into account the alkali concentration and the difference in cation-to-effective anion distances. The enthalpy of mixing data of the mixed alkali glasses was then compared with reported experimental data on the conductivity of mixed alkali aluminosilicate glasses. What appears to be conflicting experimental data can be understood in terms of the magnitude of the enthalpy of mixing and we can conclude that the mixed alkali effect is closely correlated with the negative enthalpy of mixing.     

The influence of the boundary conditions on the character of the phase transition nematic-smectic C

The possibility is investigated for inducing the intermediate smectic A structure in substances with nematic and smectic C phases by the boundary forces. Different geometries are used: homeotropic, homogeneous and tilted under a different angle toward the supporting substrates of the liquid crystal cell. At homeotropic and at tilted orientation where the molecules tilt toward the supporting substrates is different from the molecule tilt in the smectic layer, an intermediate smectic A structure is observed at the transition nematicsmectic C in a narrow temperature interval. In this case the phase transition nematicsmectic C extends and transforms into phase transition of second order. At homogeneous orientation and at tilted orientation of an angle equal to the molecule tilt in the smectic layer, the transition nematic-smetic C carried out in two stages, as partially it begins on the surface still in the nematic phase and terminates at the temperature of the phase transition N-Sc. The influence of the boundary forces depends essentially on the energy of the phase transition N-S_C of the substances.     

Effect of fluorspar and alumina on the viscous flow of calcium silicate melts containing MgO

For the investigation of the effect of fluorspar and alumina on the viscous flow and the crystallization behavior of the silicate melts, the viscosity of the CaO-SiO₂-10 wt%MgO-CaF₂ (or -Al₂O₃) system was measured. The addition of CaF₂ decreased the crystallization temperature (T_CR) of the CaO-SiO₂-MgO-CaF₂ system, while the T_CR of the CaO-SiO₂-MgO-Al₂O₃ (wt%CaO/wt%SiO₂=1.0) system exhibited a minimum value at 10 wt% Al₂O₃. The activation energy was decreased in the CSMF system and vice versa in the CSMA system by addition of CaF₂ or Al₂O₃ in each system. From the relationship between the activation energy and the composition of the glasses, the following equation could be obtained. , where the B^total is the ratio of (wt%CaO + wt%CaF₂ + wt%MgO)/(wt%SiO₂ + wt%Al₂O₃). This means that CaO, CaF₂, and MgO would behave as a network modifier, while SiO₂ and Al₂O₃ behave as a network former in the glasses investigated.     

Dependence of RF power on the phase transformation for boron nitride films deposited on graphite at room temperature

Cubic boron nitride (cBN) thick films deposited on mainly c-axis-oriented graphite substrate at room temperature and zero bias by radio frequency (RF) magnetron sputtering were studied. In the growth process, RF power plays a key role in determining the content of cubic phase in films, while the conventional substrate heating and biasing have been neglected. With increase in RF power, the dominated content of films converts from explosion boron nitride (eBN) to cBN. The transformation mechanism has been discussed. The unique structural properties of the “soft” graphite are favorable to propose simple conditions for growing “hard” cBN films. Furthermore, the optical band gap of BN films having ∼90% cubic phase is of ∼5.8 eV obtained from ultraviolet–visible optical transmission measurement. The electron field emission examination shows that cBN film on graphite has a high emission current density of 2.8×10⁻⁵ A/cm² at an applied field of ∼30 V/μm.     

The phase transformation behaviors of Sn2+-doped Titania gels

The transformation behaviors of Sn²⁺-doped titania gels, such as transformation temperature, conversion rate and the crystal granularity, were studied by using thermo-gravimetric/differential thermal analysis and X-ray diffraction methods. Experimental results show that, anatase, rutile and SnO₂ phases can exist in the sintering products by varying Sn²⁺ content and sintering temperature. Sn²⁺-doping greatly depresses the growth of anatase and rutile crystals and so obtaining nanosized crystals The transformation temperatures of gel to anatase and anatase to rutile first decrease and then increase with an increase of Sn²⁺ content, while both of the transformation rates are associated with Sn²⁺ content, change in its valence and the sintering temperature. It is suggested that by adjusting Ti⁴⁺/Sn⁴⁺ ratio and sintering temperature, the crystal granularity and the ratio of anatase to rutile can be tailored to optimize properties of TiO₂–SnO₂ humidity sensing ceramics.     

The influence of water steam on the direct phase transformation of zeolite NaA to nepheline by thermal treatment

Heating of zeolite NaA leads to the consecutive formation of amorphous phase, carnegieite and nepheline in the high temperature region. These phase transformations are influenced not only by temperature but also by the presence of water (inside of the crystals). Water causes destruction of zeolite framework by hydrolytic splitting of Si-O-Al-bonds in addition to thermal effects. Thus, the amorphous phase as the first product of phase transformation occurs in the presence of water steam at a lower temperature. The formation of the crystalline phases carnegieite and nepheline was observed in a temperature range, 300 K lower than usually, and without occurrence of the amorphous phase.     

Effect of synthesis conditions on the fractal structure of yttrium-stabilized zirconium dioxide

The effect of synthesis conditions (sequential precipitation, coprecipitation, and sol–gel method) on the fractal structure of yttrium-stabilized zirconium dioxide has been investigated. It has been shown that the difference between methods manifests itself clearly in xerogel nanostructures, viz. by the number of fractal aggregation levels (three levels in hydroxide precipitates and two in sol–gel) and the absence of mass-fractal aggregation in sol–gel. It is been determined that the mass-fractal aggregation of precursors contributes to good filtration of hydroxide precipitates and allows preparation of oxides with soft, readily destructible aggregates, and that surface-fractal aggregation makes for good pressability of oxides.     

Effect of phase separation on weathering of soda-lime-silica glasses

Accelerated weathering tests on phase-separated and non-separated soda-lime-silica glasses have been made under static conditions of 75% relative humidity at 70°C. Detailed studies of the change of weatherability show that the rate of weathering is reduced if phase separation results in a connected structure of a silica-rich phase, whereas droplets of a silica-rich phase are more liable to weathering. The weathering products were examined by an X-ray wavelength dispersive spectrometer.     

The effect of dynamic recrystallization on the growth velocity of new phase crystals at polymorphic transformation of tin and thallium

The analysis of dynamic recrystallization influencing the crystal growth of the new phase in high purity tin and thallium (99.9995%) is carried out. It is shown that in tin, in which the β → α transition proceeds on the dislocation or the normal mechanisms (depending upon a supercooling degree, ΔT) a superposition of dynamic recrystallization results in an increase of the growth velocity of α-Sn crystals. The most distinct of acceleration is observed at −21 ÷ − 23 °C, when the growth velocity of recrystallization centers and the maximal growth velocity, V_max, of the crystals are comparable values. The dynamic recrystallization superposition in thallium offers to transform the transformation mechanism. Thereby an erase of the features of the martensite α ⇄ β transition mechanism and an appearance of the features of the normal crystal growth mechanism of the new phase are observed.     

Effect of some manufacturing conditions on the optical loss of compound glass fibers

The effect of the use of platinum crucibles and gas flow at glass melting and fiber drawing on the optical loss of compound silicate glass fibers have been investigated for the purpose of obtaining low-loss optical fibers. In concentrations of more than 50 ppm, platinum impurity dissolved into the glass from a platinum crucible increases the optical loss. The flow of oxidizing gas decreases the optical loss due to the Fe²⁺ ions. The flow of dry gas also decreases the absorption loss at 0.96 μm by water. The improvement based on these results lowers the total loss of clad fibers to 9.5 dB/km at 0.84 μm and 15 dB/km at 1.06 μm.     

Effect of the preparation method on the structural and magnetic properties of the Fe2Nb alloy

In this paper we carried out the structural and magnetic study of the Fe₂Nb stoichiometric alloy by means of x‐rays diffraction and Mössbauer spectrometry. The samples were obtained by two different techniques, arc‐melting and mechanical alloying, and then they were thermally treated. The structural properties of the alloy depend on the method of preparation: by the melting method it was possible to obtain the hcp‐Fe₂Nb ordered structure; while by mechanical alloying besides of the hcp structure also were formed the fcc‐NbO and bcc‐FeNb structures. After heat treatment of the melted alloy, this was submitted to mechanical alloying during 16 and 32 hours. Mechanical alloying allows the formation of bcc‐FeNb grains which behave as superparamagnetic due to their small size and they are surrounded by hcp grains. Before heat treatment of the alloy obtained by mechanical alloying it was also found the existence of superparamagnetic bcc grains and the heat treatment increases the size of these bcc grains and the superparamagnetic‐ferromagnetic transition is induced.     

Polyhedral to nearly spherical morphology transformation of silver microcrystals grown from vapor phase

Silver microcrystals of various shapes were grown from co-evaporation of Ag₂O and SiO powders in the nominal evaporating temperature range (heat source temperature) from 800 to 1200 °C under a reductive atmosphere. Pathways for the polyhedral to nearly spherical morphology transformation were established. At evaporating temperatures below 900 °C, the polyhedral crystals are generally bounded by {1 1 1}-facets and {1 0 0}-facets. With increase in evaporation temperature facets of the {1 1 0}-, {2 1 0}- and {3 1 0}-families come forth successively, that make the Ag polyhedron microcrystals transform into nearly spherical microcrystals. A mechanism based on the recession of {1 0 0} or {1 1 0} steps induced by the solvent SiO_x (x～2.0), which modifies the growth kinetics, is proposed to explain the emergence of {2 1 0}- and {3 1 0}-facets at high temperatures. By evaporating at 1200 °C, smooth-looking spherical Ag crystals with 6 nm multi-layered steps on the {1 1 1} facets were obtained. These results are also of significant industry relevance when preparation of noble metal particles with high-index facets is of concern.     

Influence of synthesis temperature on the structural characteristics of mesoporous silica

The characteristics of mesoporous silica prepared at different temperatures and the behavior of this system relating to the microencapsulation of a model drug were investigated. The preparation of mesoporous materials was initiated with the dissolution of a surfactant in distilled water and strong acid medium. After this, tetraethyl orthosilicate was added under agitation. The mixture was heated for 24 h at the synthesis temperature (60 °C, 80 °C, 100 °C and 130 °C) under static conditions. The surfactant was removed by calcination, which was carried out by increasing the temperature to 550 °C for 5 h. Atenolol was used as a model drug to study the kinetics of drug delivery. It could be observed that aging materials at higher temperatures presents no microporosity, and this influences the control of the release of the model drug.     

Effect of method of preparation on photophysical properties of Rh-B impregnated sol-gel hosts

Rhodamine-B (Rh-B) impregnated sol-gel samples have been prepared using two different methods - mentioned as the dope and dip methods. Two types of dye impregnated samples were prepared using the dope method and one type using the dip method. A comparative study of photophysical properties of the three types of samples were carried out with the lapse of time of preparation up to about an year. The two types of samples prepared by dope method showed degradation in absorption/fluorescence properties with the lapse of time whereas no such degradation was observed with those samples prepared by dip method. The change in the absorption/fluorescence properties of Rh-B in dope samples has been associated with the increasing acid environment during sol-gel-xerogel transitions resulting in conversion of molecular form from cation to weakly fluorescent higher protonated form of Rh-B. On the other hand, Rh-B in dip samples have very stable absorption/fluorescence properties with high fluorescence quantum yield value equal to 0.98(±0.1). On the basis of a comparative study of the three types of Rh-B impregnated samples, Rh-B dipped samples were found to have the best performance and may be useful as laser active materials in solid state dye lasers.     

Effect of preparation procedure on redox states of iron in soda-lime silicate glass

The redox state of iron in soda-lime silicate glass was determined by analysis of the optical absorption bands due to Fe²⁺ and Fe³⁺ states. When raw materials containing Fe₂O₃ were heated gradually to 1400 °C, the total-Fe content of the glass was 9.4% Fe²⁺, but rapid heating at 1400 °C increased the Fe²⁺ content to 11.7%. The oxygen activity (aO₂) in the corresponding melts was measured using zirconia and Pt electrodes. The value increased with increasing temperature in the gradually heated sample and reached log(aO₂) = 0.03 at 1400 °C, but was about 2.5 times lower in the rapidly heated sample at log(aO₂) = ?0.37. After SnO addition to the raw material, oxygen activity depended strongly on heating speed: log(aO₂) at 1400 °C fell as low as ?1.8 with rapid temperature increase but was about ?0.2 or higher with gradual heating. The Fe²⁺ content of the cooled glass was consistent with the oxygen activity of the melts. The effect of heating speed was attributed to the formation of a melt layer on the surface of the raw material.