B2O3含量对SiO2–B2O3–Al2O3–Na2O系陶瓷结合剂结构与性能的影响

制备不同B₂O₃含量的SiO₂–B₂O₃–Al₂O₃–Na₂O系玻璃试样和陶瓷结合剂试样,利用电子多功能实验机、扫描电镜、显微硬度仪、平面流淌法、热膨胀系数测试仪等分别测试不同玻璃试样的密度和显微硬度,陶瓷结合剂试样的抗折强度、微观形貌和热膨胀系数等,并用X射线衍射仪、傅里叶变换红外光谱仪对陶瓷结合剂的结构和成分变化进行分析。结果表明:将B₂O₃引入陶瓷结合剂中可有效降低其烧结温度,提高其热稳定性并调节其热膨胀系数等。在陶瓷结合剂中加入摩尔分数为15%的B₂O₃时,其样条抗折强度最高为78.11 MPa,密度和硬度最高分别为2.45 g/cm3和856 MPa,且该陶瓷结合剂的热膨胀系数与金刚石最匹配。X射线衍射分析结果表明陶瓷结合剂是典型的玻璃相结构,且对磨料有良好的包覆效果。      

Dissolving behavior of ammonium paratungstate in (NH4)2CO3–NH3·H2O–H2O system

The effects of temperature, ammonia concentration and ammonium carbonate concentration on the dissolving behavior of ammonium paratungstate were studied in (NH₄)₂CO₃–NH₃·H₂O–H₂O system. The results show that rising temperature, prolonging duration, increasing ammonia concentration and decreasing ammonium carbonate concentration favor dissolving of ammonium paratungstate at temperature below 90 °C, while the WO₃ concentration decreases after a certain time at temperature above 100 °C. Furthermore, the undissolved tungsten exists in the form of either APT·4H₂O below 90 °C or pyrochlore-type tungsten trioxide above 100 °C. In dissolving process, the ammonium paratungstate dissolves into paratungstate ions followed by partially converting to tungstate ion, resulting in the coexistence of the both ions. This study may provide a new idea to exploit a novel technique for manufacturing ammonium paratungstate and pyrochlore-type tungsten trioxide.     

Electrodeposition of Co–Sb thermoelectric film from ethylene glycol–CoCl2–SbCl3 solution

The electrodeposition of cobalt–antimony thermoelectric semiconductor films was investigated in a non-aqueous solution of ethylene glycol (EG)–CoCl₂–SbCl₃ at 393 K. By controlling the bath composition and cathodic current density, Co–Sb alloys containing 0–94 mol% of Co were obtained at 50–300 Am^− 2. The resistance polarization caused by the formation of semiconductor film was observed in the polarization curve measured in the EG–CoCl₂–SbCl₃ (90.0–9.3–0.7 mol%) bath. In this bath, the Co–Sb (23.6–76.4 mol%) alloy was obtained by maintaining the constant potential electrolysis at 0.1 V. This alloy included CoSb₃ and exhibited a p-type thermoelectric conversion by the given temperature difference.     

Plasma spraying of Al2O3–WO3 composite coatings

Al₂O₃–WO₃ oxide composites are of considerable interest as solid acid catalysts in the petrochemical industry. Typically they consist of a monolayer of WO₃ dispersed over a high surface area alumina support. The aim of this work was to form a single layer Al₂O₃–WO₃ composite coating by plasma spraying. Ammonium metatungstate was dispersed through porous alumina particles and transformed to WO₃ by heat treatment. WO₃ doped powders were plasma sprayed using “low” and “high” enthalpy plasma systems. Plasma spraying led to dramatic changes in the WO₃ oxide to form metallic tungsten, a metastable Al₂O₃–W solid solution and the mixed oxide Al₂(WO₄)₃. The mechanisms accounting for these transformations are discussed.     

CeO2在CeF3–LiF–BaF2熔盐中的溶解过程及电化学行为研究

本文研究了CeO₂在CeF₃–LiF–BaF₂熔盐中的溶解机理,并采用钼金属电极研究了生成的Ce(III)在CeF₃–LiF–BaF₂熔盐中的电化学行为。通过循环伏安曲线、计时电流法、恒电位电解法研究了Ce(III)的电解还原机理,并采用XRD、SEM、EDS对溶解反应产物和电解产物进行了物相、成分和微观组织分析。结果表明：CeO₂通过可与CeF₃反应生成CeOF进而溶解于CeF₃–LiF–BaF₂熔盐中,CeOF可被直接电解还原生成金属Ce,Ce(III)在Mo电极上的电化学反应是一个单步的三电子可逆过程,反应受扩散控制。     

Enhanced cycling stability of Mg–F co-modified LiNi0.6Co0.2Mn0.2–yMgyO2–zFz for lithium-ion batteries

The layered LiNi_0.6Co_0.2Mn_0.2–yMg_yO_2–zF_z (0≤y≤0.12, 0≤z≤0.08) cathode materials were synthesized by combining co-precipitation method and high temperature solid-state reaction, with the help of the ball milling, to investigate the effects of F–Mg doping on LiNi_0.6Co_0.2Mn_0.2O₂. Compared with previous studies, this doping treatment provides substantially improved electrochemical performance in terms of initial coulombic efficiency and cycle performance. The LiNi_0.6Co_0.2Mn_0.11Mg_0.09O_1.96F_0.04 electrode delivers an high capacity retention of 98.6% during the first cycle and a discharge capacity of 189.7 mA·h/g (2.8–4.4 V at 0.2C), with the capacity retention of 96.3% after 100 cycles. And electrochemical impedance spectroscopy(EIS) results show that Mg–F co-doping decreases the charge-transfer resistance and enhances the reaction kinetics, which is considered to be the major factor for higher rate performance. It is demonstrated that LiNi_0.6Co_0.2Mn_0.11Mg_0.09O_1.96F_0.04 is a promising cathode material for lithium-ion batteries for excellent electrochemical properties.     

Thermal and electrical properties of TiB2–MoSi2

The present communication reports the effect of MoSi₂ addition on high temperature thermal conductivity and room temperature (RT) electrical properties of TiB₂. The thermal diffusivity and the thermal conductivity of the hot pressed TiB₂–MoSi₂ samples were measured over a range from room temperature to 1000 °C using the laser-flash technique, while electrical resistivity was measured at RT using a four linear probe method. The reciprocal of thermal diffusivity of TiB₂ samples exhibit linear dependence on temperature and the measured thermal conductivity of TiB₂-2.5% MoSi₂ composites correlate well with the theoretical predictions from Hashin’s model and Hasselman and Johnson’s model. A common observation is that the thermal conductivity of all the samples slightly increases with temperature (up to 200 °C) and then decreases with further increasing temperature. It is interesting to note that both the thermal conductivity and electrical conductivity of TiB₂ samples enhanced with the addition of 2.5 wt.% MoSi₂ sinter additive. Among all the samples, TiB₂-2.5 wt.% MoSi₂ ceramics measured with high thermal conductivity (77 W/mK) and low electrical resistivity (12 μΩ-cm) at room temperature. Such an improvement in properties can be attributed to its high density and low volume fraction of porosity. On the other hand, both the thermal and electrical properties of TiB₂ were adversely affected with further increasing the amount of MoSi₂ (10 wt.%).     

Cr23C6–NiCr涂层制备及其高温氧化行为

针对传统高温防护涂层在长期服役环境中可靠性不足等问题,设计了新型Cr23C6-NiCr金属陶瓷体系,并采用超音速火焰喷涂(High Velocity Oxy-fuel Spraying,HVOF)技术制备了相应复合结构涂层。利用XRD、SEM和高温电阻炉等设备,对比研究了其与传统Cr3C2-NiCr金属陶瓷涂层的微观组织结构特征及高温氧化行为。结果表明,复合涂层具有HVOF喷涂涂层典型的致密层状结构,喷涂过程中无明显相分解或氧化物生成。两种涂层在经过800℃循环氧化后具有相似的氧化动力学曲线,表面生成均匀致密的Cr2O3钝化膜阻止了氧原子向涂层内部的扩散,起到了较好的隔离防护作用,呈现出较为优异的抗高温氧化性能。     

Optical and structural properties of Nb2O5–SiO2 mixtures in thin films

Mixed material thin films are used in gradient index optical systems as their refractive index can be tailored to meet requirements. For the system to meet the optical performance requirements, it is necessary to relate the refractive index profile of the design to the volume fraction of the components of the mixture. Here we report that for electron-beam co-deposited Nb₂O₅–SiO₂ mixtures, the most appropriate effective medium theory is Lorentz–Lorenz theory. The optical properties of a mixture are related to the structure of the composite. The structural properties of the mixtures studied justify the appropriateness of Lorentz–Lorenz theory for this kind of effective medium.     

Heterostructured Co3O4–SnO2 composites containing oxygen vacancy with high activity and recyclability toward NH3BH3 dehydrogenation

Ammonia borane (NH₃BH₃,AB) has been regarded as a promising chemical hydrogen storage material owing to its high hydrogen density and superior stability.Thus,the development of low-cost and high-efficient heterogeneous catalysts for the dehydrogenation of AB has attracted considerable scholarly attention.In this study,heterostructured Co₃O₄–SnO₂ catalysts containing oxygen vacancy (V_o) with different Co/Sn atomic ratios (designate...     

Al2O3–TiB2复合陶瓷涂层制备及耐液锌腐蚀性能

针对连续热镀锌生产线中浸锌零部件表面的腐蚀磨损问题,应用高能高速等离子喷涂设备制备了Al2O3-TiB2复合陶瓷涂层。测试了涂层的显微组织、显微硬度、结合强度及耐熔融锌液腐蚀性能。结果表明涂层显微组织中不存在相互贯通的孔隙、微裂纹和未熔化颗粒,孔隙分布均匀且孔径较小,孔隙率<3%。涂层与基体结合状态良好,结合强度达到56 MPa。经过30天的熔融锌液浸泡,涂层表面未见有点蚀、裂纹或剥落现象。Al2O3-TiB2复合陶瓷涂层高的致密性和较好的抗热震性能对涂层力学性能和耐熔融锌液腐蚀性能提高起到了重要作用。     

Synthesis,characterization, electrical transport and magnetic properties of PEDOT–DBSA–Fe3O4 conducting nanocomposite

Electrical transport and magnetic properties of newly synthesized conducting polymer nanocomposites involving poly(3,4-ethylenedioxythiophene) (PEDOT) and Fe₃O₄ nanoparticles are studied. Nanocomposite samples of varying proportions of inorganic to organic components were synthesized by adding EDOT monomer stabilized in miceller solution of DBSA (dodecylbenzene sulphonic acid) to aqueous colloidal dispersion of Fe₃O₄ nanoparticles, followed by oxidative polymerization using ammonium peroxodisulphate (APS). Transmission electron microscopic (TEM) photographs show presence of distinct spherical Fe₃O₄ naonparticles having diameter range of 20–40 nm and they are incorporated within the polymer chain in the nanocomposite samples. Temperature-dependent DC conductivity analysis indicates a smooth cross-over of the charge conduction from the high temperature 3D Mott's variable range hopping (VRH) mechanism to the 2D ES (Efros and Shklovoskii)-VRH behaviour at low temperature. Temperature-dependent DC magnetization studies reveal enhancement of blocking temperature (T_B) in the nanocomposite samples compared to that of bare Fe₃O₄ nanoparticles. Core shell morphology of the nanoparticles seems to be the cause for lowering the value of saturation magnetization of the Fe₃O₄ nanoparticles. Estimated magnetic domain sizes are comparable to those of grain sizes for the nanocomposite samples having lower content of nanoparticles (P₅₀ and P₁₀₀). Temperature-dependent AC-susceptibility data also supports the superparamagnetic behaviour.     

Effect of WC content on the microstructure and mechanical properties of Ti(C0.5N0.5)–WC–Mo–Ni cermets

Ti(C_0.5N_0.5)–xWC–Mo–Ni system cermets were studied to investigate the effect of WC content on the microstructure and mechanical properties. The results showed that the lattice constant of Ti(C,N) hard phase in the Ti(C_0.5N_0.5)–WC–Mo–Ni system increases with the increase of WC content, but it is smaller than that in Ti(C_0.7N_0.3)–WC–Ni system. The microstructures of the cermets exhibit three kinds of grains: one has black core-grey rim structure, the second has white core-grey rim structure and the third has black core-white rim structure. The thickness of inner rim increases with the increasing of WC content. Additionally, the particle size of black core decreases with the increase of WC content in the range of 0–10 wt.%, and then increases slightly with further increase of WC. The TRS increases with the increase of WC content, but hardness decreases with the increase of WC content.     

NH4HF2 氟化Al2O3 制备无水AlF3 研究

采用热重-差热分析（TG-DTA）方法对不同NH₄HF₂/Al₂O₃质量比的Al₂O₃+NH₄HF₂混合物的热行为进行了分析,确定了DTA曲线的临界温度。进一步分析了各临界温度前后直接热处理所得产物的形貌和物相。结果表明,质量比对临界反应温度和反应过程没有影响。氟化反应在室温下以(NH₄)₃AlF₆的形成开始,在162.3~162.8 ℃时占主导地位,在180 ℃左右完成。进一步热处理后,(NH₄)₃AlF₆在249.8~250.1 ℃分解为NH₄AlF₄,在356.8~357.7 ℃分解为β-AlF₃;随后β-AlF₃在400~650 ℃向α-AlF₃转变。     

球形烧结态Cr3C2–25%NiCr复合粉末制备研究

试验通过添加高分子分散剂配制Cr₃C₂–25%NiCr料浆，采用喷雾干燥技术制备球形粉末，在保护气氛下进行液相烧结，气流粉碎分级后形成合适粒度粉末。实验研究了不同分散剂含量对喷雾干燥制备Cr₃C₂–25%NiCr复合粉末性能的影响，液相烧结工艺对Cr₃C₂与NiCr合金相之间冶金化结合状态的影响。研究结果表明：高分子分散剂能够很好的调解料浆性能，使喷雾干燥粉末具有良好的物性。采用SEM、XRD及化学成分分析表明粉末物理性能与国外粉末相当，超音速火焰喷涂涂层性能较好。     

La0.4Sr0.6Co0.7Fe0.2Nb0.1O3- δ -Gd0.2Ce0.8O2- δ 应用于可逆固体氧化物电池对称电极

为制备一种高催化性的对称型固体氧化物电池电极,采用一步法合成了La_0.4Sr_0.6Co_0.7Fe_0.2Nb_0.1O_3-δ-Gd_0.2Ce_0.8O_2-δ（LSCFN-GDC）。以LSCFN-GDC为电池阳极和阴极,La_0.8Sr_0.2Ga_0.83Mg_0.17O_3-δ（LSGM）为电解质,采用流延和丝网印刷工艺制备了结构为LSCFN-GDC||LSGM||LSCFN-GDC的电解质支撑型固体氧化物电池。分别采用固体氧化物燃料电池（SOFC）及固体氧化物电解池（SOEC）2种模式对对称电池性能进行了测试。在850 ℃测试温度下,分别采用湿H₂（3% H₂O）、H₂（0.01% H₂S）、CH₄和C₃H₈为燃料气,电池最大功率密度分别为1.036、0.996、0.479和0.952 W/cm²,电解H₂（50% H₂O）时,1.3 V电解电压下电池电流密度为0.943 A/cm²。LSCFN-GDC具有良好的耐积碳、抗硫和氧化还原稳定性能,能够在湿H₂（0.01% H₂S）、CH₄、H₂（3% H₂O）及H₂（50% H₂O）环境中稳定运行700 h。实验结果表明,一步合成法是一种简便而优化的电极制备方法,LSCFN-GDC||LSGM||LSCFN-GDC固体氧化物电池（SOC）具有广阔的应用前景。     

Fe2+-Ni2+-NH3-NH4+-C2O42-H2O体系的沉淀配合平衡热力学

针对草酸盐配位共沉淀热分解还原法制备超细铁镍合金粉过程中Fe2+-Ni2+-NH3-NH4+-C2O42--H2O体系的溶液平衡建立热力学分析模型,并根据模型进行相关计算,揭示反应体系中各物质随pH值、氨及草酸浓度的变化关系。结果表明:溶液中的Fe主要以[Fe(C2O4)n]2 2n络合物形式存在,而铁氨络合物含量很低。当氨含量较低时,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在;氨含量较高时,在酸性条件下,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在,在碱性条件下,则主要以[Ni(NH3)n]2+存在。低pH值下,Ni的沉淀率较Fe的高,而高pH值下,Ni的沉淀率则较Fe的低。     

电弧喷涂制备Fe65Cr20Mo7B3.5SiMn1.5W3涂层

在Q235低碳钢板上利用电弧喷涂工艺进行喷涂,以制得Fe65Cr20Mo7B3.5SiMn1.5W3涂层。喷涂材料为自行配制的丝材,按照35%的填充率将配好的粉填充到U型不锈钢外皮中,经过多道拉拔、挤压工艺制成Φ2mm的粉芯丝材。采用X射线衍射仪、扫描电镜、能谱分析仪、透射电镜对涂层的物相和组织形貌及成分进行了表征;采用差示扫描量热仪、显微硬度仪等设备对涂层的热稳定性及显微硬度进行了检测和分析。试验结果表明:涂层组织形貌呈典型的层状组织结构,由变形良好的带状粒子相互搭接堆积而成。涂层含有50.63%的非晶相,同时含有纳米级的晶相。涂层组织均匀、结构致密、孔隙率低,并且涂层硬度高达1040.5HV0.3,属硬质涂层,具有良好的热稳定性。     

Ti48Zr20Nb12Cu5Be15 非晶复合材料的内耗行为

对Ti₄₈Zr₂₀Nb₁₂Cu₅Be₁₅非晶复合材料的室温力学性能以及随温度变化的动态力学性能进行了研究。结果表明,该非晶复合材料的室温拉伸强度约为1350 MPa,断裂应变约为0.13。随着温度的升高,该非晶复合材料的整体状态由弹性转变为粘弹性。在准点缺陷模型框架下,引入了诸如损耗因子、相关系数等相关物理参数,全面分析了该非晶复合材料动态力学行为,并且模型的理论曲线与实验数据拟合程度较好。因此,准点缺陷模型可以很好地描述不同温度下的Ti₄₈Zr₂₀Nb₁₂Cu₅Be₁₅非晶复合材料的动态力学行为。     

Fe66Ni1Al5Ga2P9.65B7.6Si3C5.75非晶合金循环预处理的热力学分析

采用XRD、DSC方法研究了循环预处理对Fe₆₆Ni₁Al₅Ga₂P_9.65B_7.6Si₃C_5.75非晶合金热力学参数的影响和晶化过程中析出相自由能的变化。结果表明:与淬火态相比,经循环预处理后晶化样品的Tg、Tx、Tp均有所降低,过冷液相区扩大,整个非晶的晶化阶段均有所提前;晶化析出相种类增加,晶化体积大幅增加,其中经冷热循环处理样品的晶化体积最大为60.197%;晶化相Fe₃P、AlNi₃C_0.5、Fe₂P的ΔGT与温度的变化成正比例函数。