Cold model on bubble growth and detachment in bottom blowing process

The bubble growth and detachment behavior in the bottom blowing process were investigated. Four multi-hole nozzle configurations with different opening ratios were assessed experimentally using high-speed photography and digital image processing. For these configurations, the experiments reveal that the bubble growth consists of a petal-like stage, an expansion stage and a detachment stage. The petal-like shape is qualitatively described through the captured images, while the non-spherical bubbles are analyzed by the aspect ratio. The bubble size at the detachment is quantified by the maximum caliper distance and the bubble equivalent diameter. Considering the dependence on the opening ratio, different prediction models for the ratio of maximum caliper distance to hydraulic diameter of the nozzle outlet and the dimensionless bubble diameter are established. The comparative analysis results show that the proposed prediction model can accurately predict the bubble detachment size under the condition of multi-hole nozzles.     

High-resolution FIB-TEM-STEM structural characterization of grain boundaries in the high dielectric constant perovskite CaCu3Ti4O12

In this work, the grain boundaries composition of the polycrystalline CaCu₃Ti₄O₁₂ (CCTO) was investigated. A Focused Ion Beam (FIB)/lift-out technique was used to prepare site-specific thin samples of the grain boundaries interface of CCTO ceramics. Scanning transmission electron microscopy (STEM) coupled with energy dispersive X-ray spectrometry (EDXS) and Electron Energy Loss Spectroscopy (EELS) systems were used to characterize the composition and nanostructure of the grain and grain boundaries region. It is known that during conventional sintering, discontinuous grain growth occurs and a Cu-rich phase appears at grain boundaries. This Cu-rich phase may affect the final dielectric properties of CCTO but its structure and chemical composition remained unknown. For the first time, this high-resolution FIB-TEM-STEM study of CCTO interfacial region highlights the composition of the phases segregated at grain boundaries namely CuO, Cu₂O and the metastable phase Cu₃TiO_4.     

全透明高压反应釜甲烷水合物动力学实验

水合物的生长和分解规律对开发海洋天然气水合物资源，实现深水天然气水合物气液固多相管道输送都具有重要意义。为了进一步揭示水合物的生长和分解特性，本文采用高压全透明反应釜装置，进行了温度0～30℃、压力3.35～8.16MPa和搅拌速率200～1000r/min范围内的16组甲烷水合物生长和分解动力学实验研究。结果表明：实验过程可分为水合物诱导期、快速生长期、缓慢生长期以及分解期这4个阶段。在水合物快速生长阶段，获得了温度、压力、搅拌电机扭矩和水合物生长速率随时间的变化规律，观察到了水合物颗粒的均相和非均相分布状态。通过加热促使水合物分解，揭示了分解阶段温度、压力和分解速率等关键参数的变化规律以及水合物块的分解形态。分析表明，水合物颗粒的分布状态与水合物浆液的流动性直接相关；水合物块的静态分解过程受到分解气传质控制。     

Modification of glass network and crystallization of CaO–Al2O3–MgO–SiO2 based glass ceramics with addition of iron oxide

Modification of glass network and crystallization process of a CaO–Al₂O₃–MgO–SiO₂ (CAMS) based glass ceramic to form diopside through addition of iron oxide were investigated using differential thermal analysis (DTA), Raman spectrum, X-ray diffraction, SEM and EBSD techniques. The experimental results showed that addition of Fe₂O₃ led to remarkable reductions in both the glass transition temperature (Tg) and crystallization temperature (Tp) of the CAMS glass ceramic. At addition level below 5 wt%, the Tg and Tp temperatures were 651°C and 903°C, respectively, and the crystallization only occurred on the surface of the glass ceramic samples. Increasing the addition level to 10 wt% and 15 wt%, not only led to reduction in the Tg and Tp temperatures to 643-641°C and 892-876°C, respectively, but also promoted the formation of crystalline diopside throughout the CAMS samples. Based on the results of Raman spectrums, it was confirmed that Fe₂O₃ addition reduced the strength of glass connection as a result of chemical reactions between the isolated Si–O tetrahedron and Fe³⁺ ion, forming Fe³⁺O₄–SiO₄, which can be regarded as Q₂ unit. And this is the first experimental evidence that proving the approach of Fe³⁺ mending glass network. Microstructural examination also identified the formation of large numbers of spherical Fe-enriched regions within the CAMS glass matrix as a result of the amorphous phase separation due to the Fe₂O₃ addition. The interfaces between the Fe-enriched regions and the glass matrix acted as preferred nucleation sites for the diopside, facilitating the crystallization. Crystallographic analysis using EBSD technique determined the <001> as the most favorite growth direction for the diopside crystals in the CAMS based glass ceramic.     

合成工艺对氮化硼纳米管显微结构和性能的影响

采用无定型B粉为原料,在催化剂Fe2O3和CaO辅助作用下,控制反应气氛氨气的流量(150~200 mL/min),在1200℃下于真空管式炉中保温4 h,制备氮化硼纳米管(BNNTs)。采用透射电子显微镜(TEM)、X射线衍射(XRD)和傅里叶转换红外光谱分析(FTIR)等手段对产物的结构和形貌进行了表征,结果表明:所得产物为竹节状氮化硼纳米管(BNNTs),其晶体结构为六方氮化硼,外径约为35~100 nm,长度为数微米至数十微米。     

A compromise between piezoelectricity and transparency in KNN-based ceramics: The dual functions of Li2O addition

Transparent ceramics with good electrical performance have recently drawn broad interest as promising multifunctional materials. Here, we report that a superior transmittance (T = 75 % at 2000 nm) and good piezoelectricity (d₃₃ ∼ 150 pC/N) can be simultaneously realized in 0.93K_0.5Na_0.5NbO₃-0.07SrZrO₃ (KNN-SZ) ceramics by Li₂O regulation. The effect of Li₂O regulation has two parts: first, the presence of Li₂O facilitates the grain growth of KNN-SZ, considering that it melts at a relatively low temperature as a proper sintering aid; second, the introduced Li⁺ causes local lattice distortion, resulting in the coexistence of orthogonal and tetragonal (O–T) phases. The enlarged grains reduce the light scattering by grain boundaries for a higher optical transmittance; meanwhile, large grains stand as a prerequisite for the macroscopic domain structure favoured for decent piezoelectricity, which could also be partly caused by the coexistence of O–T phases. We believe that these findings might make KNN-based ceramics a preferable candidate for optoelectronic devices.     

Grain size effect on microwave dielectric properties of Na2WO4 ceramics prepared by cold sintering process

In this work, cold sintering was adopted to prepare Na₂WO₄ ceramics with different grain sizes ranging from 0.632 μm to 17.825 μm. Their microstructures, complex impedance, and microwave dielectric properties were studied in-depth. It was found that samples with relative densities higher than 92% can be successfully synthesized by cold sintering process at a low temperature of 240 °C. However, their electrical properties have strong dependence on the grain size. Specifically, the resistance of grain boundaries decreases dramatically with the increase of grain sizes, while the quality factor has a positive correlation with the grain sizes of Na₂WO₄ ceramics. Excellent microwave dielectric properties, including permittivity = 5.80, Q × f = 22,000 GHz, and TCF = −70 ppm/°C, are obtained for Na₂WO₄ ceramics with a grain size of 4.477 μm prepared by cold sintering process.     

Structure analysis,tuning photoluminescence and enhancing thermal stability on Mn4+-doped La2-xYxMgTiO6 red phosphor for agricultural lighting

Currently, phosphor-converted LEDs (pc-LEDs) are revolutionizing the industry of plant growth lighting. To meet the requirements of this technology, phosphors with tunable photoluminescence, high thermal stability and luminous intensity are required. Herein, we found that the simple substitution of yttrium for lanthanum in La₂MgTiO₆:Mn⁴⁺ (LMT:Mn⁴⁺) system could satisfy above three criteria simultaneously. The photoluminescence properties can be regulated by continuously controlling the chemical composition of La_2-xY_xMgTiO₆:Mn⁴⁺ solid solution. The La sites are occupied by Y ions, causing a significant blue shift in the emission spectra which owing to the change of local crystal field strengthen. Meanwhile, the thermal stability and decay lifetimes are also varied due to the variation of local structure and band gap energy. The thermal stability of the material reaches 83.5% at 150 °C, which is better than the reported La₂MgTiO₆:Mn⁴⁺ and Y₂MgTiO₆:Mn⁴⁺ phosphors. The electronic luminescence (EL) of pc-LED devices using La_2-xY_xMgTiO₆:Mn⁴⁺ red phosphor is evaluated, which matching the absorption regions of plant pigments well, reflecting the superiority of the studied phosphors in plant growth lighting areas.     

稀土石膏常压酸化法制备硫酸钙晶须的研究

以含稀土的石膏为原料运用常压酸化法合成硫酸钙晶须,探讨了不同工艺条件对生成的硫酸钙晶须形貌的影响,同时还考察了晶型助长剂的种类和晶型助长剂的含量对硫酸钙晶须生长的影响,利用SEM和XRD分别对硫酸钙晶须的表面形貌、物相特征做了表征分析。实验得到制备硫酸钙晶须的最佳的反应条件：稀土石膏质量浓度为0.22 g/mL、反应时间为25 min、盐酸浓度为2.8 mol/L、反应温度为70 ℃、陈化时间为4 h,在此条件下合成的硫酸钙晶须平均长度为61 μm,平均长径比为30.5;通过对比实验选出了CuCl₂作为促进硫酸钙晶须生长的助长剂,在添加5%（质量分数）的CuCl₂的情况下可使硫酸钙晶须长径比从30.5增至41,长度从61 μm增至81 μm。     

Novel process for recrystallized silicon carbide through β-α phase transformation

A novel process was investigated to produce recrystallized silicon carbide through β-α phase transformation. The specimen was prepared from carbon and β-SiC powder mixture, first by infiltration with liquid silicon at 1500 °C to form β-SiC preform with a high density, and then by heating it further up to 2200 °C. When the β-SiC particles were transformed into α-SiC at 2200 °C, the rapid grain growth occurred of the α-SiC by consuming β-SiC particles, resulting in an interconnected network structure with huge and elongated α-SiC grains. The specimen recrystallized at 2200 °C had a measured density of 2.7 g/cm³ and strength of 134 MPa. The infiltration behavior, microstructure evolution and mechanical properties of the recrystallized silicon carbide were examined and discussed.