Characterisation of thermo-mechanical properties of MgO–Al2O3–SiO2 glass ceramic with different heat treatment temperatures

The effects of heat treatment temperature on crystallisation behaviour, precipitated phases and thermo-mechanical properties of some MgO–Al₂O₃–SiO₂ (MAS) glass-ceramics were investigated. Crystallisation behaviour of MgO–Al₂O₃–SiO₂ glasses in the presence of TiO₂ as a nucleation agent was studied. The crystalline phases present in the heat treated samples were identified by X-ray diffraction (XRD). It was observed from XRD studies that magnesium aluminium titanate initially precipitated and when the heat treatment temperature was increased to 1140 °C, depending on the thermal history, either magnesium silicate, aluminium titanate and quartz or magnesium aluminium titanate, magnesium aluminate and quartz were precipitated. SEM observation revealed that the heat treatment led to phase separation of droplet-shaped crystals before the needle-shaped crystals formed at 1140 °C. The effect of annealing temperature on the density and mechanical properties of these glass-ceramic were characterised by nanoindentation and the results revealed a significant increase in hardness of the fully crystallised system.     

Sol–gel derived CaO–B2O3–SiO2 glass/CaSiO3 ceramic composites: processing and electrical properties

The CaO–B₂O₃–SiO₂ glass/CaSiO₃ ceramic (CBS/CS) composites were fabricated via sol–gel processing routes. Their densification behavior, structures and dielectric properties were investigated. The precursors of CBS glass and CS ceramic filler were firstly obtained via individual soft chemical route and then mixed together in various proportions. The results indicated that the structures of CBS/CS composites are characteristic of CS and CaB₂O₄ (CB) ceramic phases distributed in the matrix of glass phase at 800–950 °C. The CS ceramic phase not only acts as fillers, but nuclei for the crystallization of CBS glass as well such that the CS content exhibits an effect on the densification and dielectric properties of the composites. The CBS/CS composites with 10% CS sintered at 850 °C own dielectric properties of ε_r < 5 and tanδ = 6.4 × 10⁻⁴ at 1 MHz.     

Thermo-mechanical properties of La2NiO4+δ

Elastic and fracture behavior of La₂NiO_4+δ have been assessed. Fracture stress and elastic modulus of porous La₂NiO_4+δ were evaluated from room temperature (RT) up to 900 °C on the basis of 4-point bending tests. Both parameters increase slightly from RT to 700 °C. However, at higher temperatures the elastic modulus decreases, whereas the fracture stress increases. In addition, elastic modulus and damping/internal friction of dense specimens were measured by a resonance method. A strong change of elastic modulus and internal friction between RT and 100 °C appears to be related to an orthorhombic-tetragonal phase transition. No indications of phase transition can be observed at higher temperatures. Although thermogravimetric measurements suggest that oxygen was continuously released from the lattice up to 1000 °C with increasing temperature, the thermal expansion coefficient showed a rather stable value from RT up to 1000 °C.     

Crystallization and magnetic properties of a 10Li2O–9MnO2–16Fe2O3–25CaO–5P2O5–35SiO2 glass

The crystallization behavior and magnetic properties of 10Li₂O–9MnO₂–16Fe₂O₃–25CaO–5P₂O₅–35SiO₂ (10LFS) glass have been studied using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) to observe the crystallization behavior and a superconducting quantum interference device (SQUID) for measurements of the magnetic properties. The DTA shows that the 10LFS glass has one broad exothermic peak at approximately 674 °C and one sharp (the highest) exothermic peak at 764 °C. When the 10LFS glass crystallized at 850 °C for 4 h, the crystalline phases identified by XRD were lithium silicate (Li₂SiO₃), β-wollastonite (β-CaSiO₃), lithium orthophosphate (Li₃PO₄), magnetite (FeFe₂O₄) and triphylite (Li(Mn_0.5Fe_0.5)PO₄). The SEM surface analysis revealed that the β-wollastonite and lithium silicate have a lath morphology. The TEM microstructure examination showed that the largest FeFe₂O₃ particles have a size of approximately 0.3 μm. When the 10LFS glass was heat treated at 850 °C for 16 h and a magnetic field of 1000 Oe was applied, a very small remnant magnetic induction of 0.01 emu g⁻¹ and a coercive force of 50 Oe were obtained, which revealed an inverse spinel structure.     

Atomistic study of vibrational properties of γ-Al2O3

A study of the vibrational density of states (DOS) of γ-Al₂O₃ is presented. Four structural models from the recent literature are considered: vacant spinel model and three nonspinel models. The vacant spinel and one of the nonspinel models have unit cells with 40 atoms, while the other two models have 160 atoms. The interatomic interactions are computed using classical force fields that include Coulomb and van der Waals attractive interactions, short range repulsive interactions, as well as three-body terms. The oxygen polarizability is included via a core-shell potential. The DOS is compared with ab initio calculations recently published for the vacant spinel model. The classical and ab initio DOS show some differences for frequencies higher than 200 cm⁻¹, the ab initio having more peaks and having a frequency cutoff 100 cm⁻¹ lower than the classical DOS. The DOS of all models present some small differences. While the 160-atoms nonspinel models present a rather structureless DOS, 40-atoms models present peaks and dips relative to the 160-atoms models. The elastic constants of polycrystalline γ-Al₂O₃ are also estimated using several force fields. In general, the classical force field predict higher elastic moduli than the ab initio method. The infrared spectra of the four models are calculated.     

ZnCl2活化茄子秸秆制备活性炭及表征

以茄子秸秆为原料、ZnCl2为活化剂制备活性炭。通过正交实验方法确定了制备活性炭的最佳工艺条件,采用低温氮气吸附、BET、Langmuir和BJH理论对其孔结构进行了表征,利用红外光谱分析样品的表面官能团,扫描电镜观察表面形貌。结果表明以茄杆活性炭的最佳工艺条件:浸渍比为2,浸渍时间为8h,活化温度为550℃,活化时间为60min,所得的活性炭的碘吸附值为1270.06mg/g,亚甲基蓝吸附值为17.4mL/g;BET和Langmuir比表面积分别为1649.615和1851.649m2/g,吸附总孔容为0.488cm3/g,吸附平均孔径为2.241nm。     

Microwave dielectric properties of BaO–TiO2–TeO2 ternary system

Besides the applications as optical functional materials, tellurium oxides also have attracted interest as microwave dielectric materials. Most TeO₂-based binary and ternary system have large negative temperature coefficient of resonant frequency (τ_f), which is not compatible for the low-temperature cofired ceramic. To compensate τ_f close to zero, two single-phase predecessors of BaTe₄O₉ and TiTe₃O₈ are synthesized in air at 530–560 and 620–680 °C, respectively. The two predecessors show exceptional dielectric properties and their τ_f are opposite. The BaO–TiO₂–TeO₂ ternary system compounds are investigated by adjusting the ratio of BaTe₄O₉ and TiTe₃O₈ and sintered at 520–580 °C to develop the microwave properties and compensate the τ_f. After sintered at 560 °C, the ceramic sample with the composition of 0.47BaTe₄O₉–0.53TiTe₃O₈ exhibits a dielectric permittivity of 28, a Q × f-value of 12,200 GHz, and a τ_f of 4.0 ppm/°C measured at 10 GHz.     

Synthesis and properties of magnetic solid superacid: SO4/ZrO2–B2O3–Fe3O4

A magnetic SO₄²⁻/ZrO₂–B₂O₃–Fe₃O₄ solid superacid catalyst is prepared via a simple chemical co-precipitation approach. The obtained materials were characterized in detailed by X-ray powder diffraction, thermogravimetric analysis–different scanning calorimetry, Fourier transform infrared spectroscopy (FTIR), electron microscopy (SEM and TEM), and Mossbauer spectra. Powder X-ray diffraction patterns show that in this composite oxide the transformation temperature of ZrO₂ from tetragonal to monoclinic phase is higher compared to the pristine SO₄²⁻/ZrO₂ material. The introduction of Fe₃O₄ endows the superacid with a super-paramagnetic property while in a ferromagnetic state after calcination. The superacid exhibits high catalytic activity in forming ethyl acetate by esterification.     

Synthesis and properties of β-Ga2O3 nanostructures

A novel method was utilized to synthesize one-dimensional β-Ga₂O₃ nanostructures. In this method, β-Ga₂O₃ nanostructures have been successfully synthesized on Si(111) substrates through annealing sputtered Ga₂O₃/Mo films under flowing ammonia in a quartz tube. The as-obtained samples were analyzed in detail using the methods of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDX) attached to the HRTEM instrument. The results show that the formed nanostructures are single-crystalline Ga₂O₃. The annealing temperature has an evident influence on the morphology of the β-Ga₂O₃ nanostructures. The growth mechanism of the β-Ga₂O₃ nanostructures is also discussed by conventional vapor-solid (VS) mechanism.     

YBa2Cu3O7-δ薄膜的BaCl2/BaF2-MOD法制备及超导特性研究

传统三氟乙酸金属有机化学溶液沉积法(TFA-MOD)制备YBa₂Cu₃O_7-δ (YBCO)超导层,Ba倾向于与F结合,从而避免BaCO₃的形成。本工作开展了新型基于BaCl₂/BaF₂途径的化学溶液法生长YBCO超导薄膜的研究。重点研究了添加Cl对YBCO薄膜晶粒取向、微观结构和超导性能的影响,并通过生长反应的热化学计算,分析了BaCl₂途径YBCO薄膜的物相转变机制。结果表明:添加Cl有利于抑制a轴晶粒取向,促进c轴晶粒成核。添加Cl的YBCO双层膜起始转变温度(Tc-onset)没有明显变化,约为89.6 K,其临界电流密度(Jc)显著提升, Jc达到2.07 MA/cm²(77K,自场)。此外,生长反应过程的物相转变分析表明Cl优先与Ba结合形成BaCl₂,有效避免BaCO₃的形成。本研究结果表明:添加Cl对制备YBCO超导厚膜有促进作用,这为MOD法制备YBC...     

Synthesis and properties of glasses in the K2O–SiO2–Bi2O3–TiO2 system and bismuth titanate (Bi4Ti3O12) nano glass–ceramics thereof

Glasses were prepared by the melt-quench technique in the K₂O–SiO₂–Bi₂O₃–TiO₂ (KSBT) system and crystallized bismuth titanate, BiT (Bi₄Ti₃O₁₂) phase in it by controlled heat-treatment at various temperature and duration. Different physical, thermal, optical, and third-order susceptibility (χ³) of the glasses were evaluated and correlated with their composition. Systematic increase in refractive index (n) and χ³ with increase in BiT content is attributed to the combined effects of high polarization and ionic refraction of bismuth and titanium ions. Microstructural evaluation by FESEM shows the formation of polycrystalline spherical particles of 70–90 nm along with nano-rods of average diameter of 85–90 nm after prolonged heat treatment. A minor increase in dielectric constants (ε_r) has been observed with increase in polarizable components of BiT in the glasses, whereas a sharp increase in ε_r in glass–ceramics is found to be caused by the formation of non-centrosymmetric and ferroelectric BiT nanocrystals in the glass matrix.     

Optical properties and structure of R2O–Ga2O3–SiO2 and RO–Ga2O3–SiO2 glasses

Refractive index and molar refraction of Li₂O–, Na₂O–, CaO–, and BaO–Ga₂O₃–SiO₂ glasses have been used to test the validity of a structural model of silicate glasses containing Ga₂O₃ glasses. Ga₂O₃ enters these types of glass in a similar manner as Al₂O₃. It is assumed that, for (SiO₂/Ga₂O₃) >1 and (Ga₂O₃/R₂O) ≤1, Ga₂O₃ associates primarily with modifier oxides to form GaO₄ units. The rest of modifier oxide forms silicate units with non-bridging oxygen ions. Silicate structural units have the same factors as found for binary alkali- and alkaline earth silicate glasses. Differences between experimental and model values suggest another structure for (Ga₂O₃/SiO₂) ≥1.     

Synthesis and photoluminescence properties of Eu-doped γ-Ca3(PO4)2

Eu³⁺-doped (1% and 3%) γ-Ca₃(PO₄)₂ was synthesized by high-pressure and high-temperature experimental method and the samples were characterized by X-ray diffraction. The luminescence properties of samples were investigated by emission and excitation spectra. The excitation spectra of Eu³⁺-doped γ-Ca₃(PO₄)₂ showed that samples were mainly attributed to Eu³⁺–O²⁻ charge-transfer band at 270 nm, and some sharp lines were also attributed to Eu³⁺ f–f transitions in near-UV regions with the strongest peaks at 395 nm. Under the 395 nm excitation, the intense red emission peak at 611 nm was observed. The strongest line (395 nm) in excitation spectra of those phosphors matched well with the output wavelength of UV InGaN-based light-emitting diodes (LEDs) chip. The luminescent properties suggested that Eu³⁺-doped γ-Ca₃(PO₄)₂ might be regarded as a potential red phosphor candidate for near-UV LEDs.     

Photoluminescence properties of β-Ga2O3:Tb nanofibers prepared by electrospinning

One-dimensional Tb³⁺-doped β-Ga₂O₃ nanofibers were prepared by a simple and cost-effective electrospinning process. Field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Raman technique, and photoluminescence (PL) were used to characterize the electrospun nanofibers. FE-SEM results indicated that the diameters all of the nanofibers ranged from 100 to 300 nm, and the lengths of nanofibers reached up to several millimeters. The XRD and Raman results showed that the Ga₂O₃ phase belongs to the monoclinic phase. Under ultraviolet excitation, the β-Ga₂O₃:Tb³⁺ samples showed green emission with the strongest peak at 550 nm, corresponding to ⁵D₄ → ⁷F₅ transition of Tb³⁺ ions. The luminescence intensity had been further studied as a function of the doping concentration of Tb³⁺ in the β-Ga₂O₃ samples.     

Preparation of Ca-α SiAlON hollow spheres by carbothermal reduction-nitridation of CaO-Al2O3-SiO2 glass

Ca-α SiAlON powders were prepared by carbothermal reduction-nitridation of CaO-Al₂O₃-SiO₂ glasses at 1450 °C for 2 h in nitrogen. The content of Ca-α SiAlON phase was 65-81% in the products, and the other phases were AlN and β-SiAlON. The products contained hollow spheres with the size of around 5 μm in diameter. The particle morphology was almost identical to that of Ca-α SiAlON prepared from CaCO₃-Al₂O₃-SiO₂ powder mixtures.     

响应面法优化ZnCl2/AlCl3改性生物炭吸附甲基紫工艺

利用高温热解法制备ZnCl₂/AlCl₃改性生物炭,将其用于吸附甲基紫染料。探究ZnCl₂/AlCl₃-AC投加量、溶液pH、甲基紫浓度、反应时间和吸附温度这5个因素对甲基紫吸附率的影响。利用Plackett-Burman设计联合响应面分析法,筛选优化出对甲基紫吸附率影响较为显著的因素,并探究各因素间的交互影响作用,确定ZnCl₂/AlCl₃-AC吸附甲基紫的最佳工艺条件。结果表明:在选取的五个因素中,对甲基紫吸附率影响显著的因素为ZnCl₂/AlCl₃-AC投加量>甲基紫浓度>吸附温度;其中ZnCl₂/AlCl₃-AC投加量和吸附温度对甲基紫吸附率影响最明显,甲基紫浓度和吸附温度影响最不显著;ZnCl₂/AlCl₃-AC吸附甲基紫最佳工艺条件为:活性炭投加量为47.00 mg、甲基紫溶液浓度为82.00 mg/L、吸附温度为22.90℃,pH为7、反应时间为120 min,其甲基紫吸附率可达到93.04%,与模型预测值的误差仅为3.51%。     

Preparation and electrical properties of (1 ? x)(Ba,Y)TiO3 · xPbTiO3 materials containing low-melting B2O3-PbO-SiO2 glass additions

We have studied the electrical properties of (1 − x)(Ba,Y)TiO₃ · xPbTiO₃-based solid solutions containing different percentages of low-melting glass. The materials were prepared by solid-state reactions, sintered in air at temperatures from 1100–1300°C, and characterized by complex impedance measurements in wide frequency and temperature ranges. The results demonstrate that the positive temperature coefficient of resistance effect in these materials, containing different percentages of low-melting glass, is contributed mainly by both the grain boundaries and surface layer. With increasing glass content, the ratio of the maximum resistivity to the minimum resistivity increases and the influence of the surface layer on the positive temperature coefficient of resistance effect becomes stronger. With increasing glass content, the grainboundary potential barrier height in the (1 − x)(Ba,Y)TiO₃ · xPbTiO₃ materials increases.     

Densification and dielectric properties of SrO–Al2O3–B2O3 ceramic bodies

The influence of SrO (0·0–5·0 wt%) on partial substitution of alpha alumina (corundum) in ceramic composition (95 Al₂O₃–5B₂O₃) have been studied by co-precipitated process and their phase composition, microstructure, microchemistry and microwave dielectric properties were studied. Phase composition was revealed by XRD, while microstructure and microchemistry were investigated by electron-probe microanalysis (EPMA). The dielectric properties by means of dielectric constant (ε _r ), quality factor (Q × f) and temperature coefficient of resonant frequency (τ _f ) were measured in the microwave frequency region using a network analyser by the resonance method. The addition of B₂O₃ and SrO significantly reduced the sintering temperature of alumina ceramic bodies to 1600 °C with optimum density (∼ 4g/cm³) as compared with pure alumina powders recycled from Al dross (3·55g/cm³ sintered at 1700 °C).     

Thermal properties and crystallization of PbO–MoO3–P2O5 glasses

Thermal properties and crystallization of glasses from PbO–MoO₃–P₂O₅ ternary system were studied in three compositional series (100 − x)[0.5PbO–0.5P₂O₅]–xMoO₃ (A), 50PbO–yMoO₃–(50 − y)P₂O₅ (B), and (50 − z)PbO–zMoO₃–50P₂O₅ (C). Glass transition temperature, crystallization temperature, coefficient of thermal expansion, and dilatation softening temperature of the studied glasses were determined by differential thermal analysis and dilatometry. Crystallization products of annealed glass samples were investigated by X-ray diffraction and Raman spectroscopy. X-ray diffraction analysis of crystallized glasses revealed the formation of PbP₂O₆, Pb₃P₄O₁₃, and PbMoO₄ in the samples of the B series. In the series A and C in the samples with a high MoO₃ content, crystalline compounds of Pb(MoO₂)₂(PO₄)₂ and (MoO₂)(PO₃)₂, respectively, were identified. Raman spectra of crystalline samples confirmed the results of X-ray diffraction measurements and provided also information on thermal stability of glasses and formation of glass-crystalline phases in the studied glass series.