等离子体氧化热分解法制备超细氧化锆

利用空气等离子体氧化热分解碱式碳酸锆和喷雾法等离子体热分解氯氧化锆水溶液制备超细氧化锆粉体,固相氧化热分解所制氧化锆平均粒径可达0.1 μm左右,晶型为亚稳立方、四方和单斜混晶结构,喷雾法等离子体热分解氯氧化锆水溶液所得氧化锆粉体平均粒径为5～60 nm,亚稳混晶结构.在反应过程中对等离子体温度进行控制,可得到形貌为球形的微粉产品.

五羰基铁雾化-热分解-氧化合成氧化铁纳米粒子

建立了将五羰基铁超声雾化、分段加热分解-氧化及产物收集-修饰一体化的纳米氧化铁合成装置,研究了不同修饰剂对纳米粒子的相组成和形貌的影响。采用XRD、TEM和FTIR对合成的纳米粒子进行了表征。通过在雾化液或收集液中添加不同修饰剂,得到平均粒径11.4～36.5 nm的球形水溶性γ-Fe2O3纳米粒子。

二氧化硅/氧化钌超级电容器电极材料的制备

以水合三氯化钌和正硅酸乙酯为原料,以钛片为基底,采用热分解氧化法制备了二氧化硅/氧化钌复合膜电极,利用扫描电子显微镜观察电极表面形貌,利用循环伏安曲线法研究电极的电容性能·考察了原料配比,烧结温度,烧结时间等制备条件对电极电容性能的影响·结果发现,二氧化硅/氧化钌复合膜电极具有优良的电容性能,当水合三氯化钌与正硅酸乙酯的物质的量的比为5∶2,烧结温度为350℃,烧结时间为1h时单电极的比容量最高可达137mF·cm-2,比文献值提高了近3个数量级·

Ni-Ru-Ir氧化物阴极涂层的析氢活性

应用热分解氧化法制备Ni-Ru-Ir氧化物活性阴极.循环伏安、Tafel曲线及计时电流测试表明,在90℃、30%(bymass)的NaOH溶液中,电流密度0.3A·cm-2条件下,Ru∶Ir质量比为1∶1的Ni-Ru-Ir氧化物电极的析氢过电位比Ni电极低300mV;表面粗糙度是Ni网电极的32倍;交换电流密度是Ni网电极的4倍;其析氢性能显然远优于Ni网电极,有望应用于氯碱工业以期降低能耗.

雾化-热分解法合成氧化铁纳米粒子及其磁性能

建立了将五羰基铁超声雾化、分段加热分解-氧化及产物收集-修饰一体化的氧化铁纳米粒子合成装置,研究了不同温度参数对纳米粒子的相组成和形貌的影响,并通过在雾化液及收集液中添加修饰剂以控制合成纳米粒子的粒径和分散性。采用XRD、TEM和SQUID对合成的纳米粒子进行了表征。成功合成了不同结晶性和分散性的球形γ-Fe2O3纳米粒子。随着粒径减小,合成纳米粒子由顺磁性过渡到超顺磁性。

Fabrication of a monoclinic/hexagonal junction in WO_3 and its enhanced photocatalytic degradation of rhodamine B

A series of WO3 samples with different crystalline phases were prepared by the thermal decomposition method from ammonium tungstate hydrate.X-ray diffraction（XRD）,scanning electron microscopy（SEM）,high-resolution transmission electron microscopy（HRTEM）,X-ray photoelectron spectroscopy,and N2 adsorption-desorption were used to characterize the crystalline phase,morphology,particle size,chemical composition,and surface area of the WO3 samples.The formation of hexagonal（h-WO3） and monoclinic（m-WO3） crystal structures of WO3 at different temperatures or different times was confirmed by XRD.m-WO3 is formed at 600 ℃,while m-WO3 starts to transform into h-WO3 at 800℃.However,h-WO3,which forms at 800℃,may transform into m-WO3 by increasing the calcination temperature to 1000℃.SEM results indicate that m-WO3 particles exhibit a bulky shape with heavy aggregates,while h-WO3 particles exhibit a rod-like shape.Moreover,m-WO3 crystals are sporadically patched on the surface of the h-WO3 rod-like particles,resulting in the exposure of both m-WO3 and h-WO3 on the surface.It is observed that the monoclinic phase（m-WO3）/hexagonal phase（h-WO3） junction was fabricated by tuning the calcination temperature and calcination time.The relative ratios between m-WO3 and h-WO3 in the phase junction can readily be tailored by control of the calcination time.The photocatalytic activities of WO3 with different crystalline phases were evaluated by the photocatalytic degradation of rhodamine B as a model pollutant.A higher photocatalytic activity was observed in the WO3 sample with the m-WO3/h-WO3junction as compared with the sample with only m-WO3.The improvement of photocatalytic activity can be attributed to the reduction of the electron-hole recombination rate owing to the formation of the phase junction,whose presence has been confirmed by HRTEM and photoluminescence spectra.

Thermal oxidation of two aviation synthetic lubricant base oils

The thermal degradation of two synthetic lubricants base oils, poly-a-olefins （PAO） and di-esters （DE）, was investigated under oxidative pyrolysis condition and their properties were characterized in simulated ＂areo-engine＂ by comparing the thermal stability and identifying the products of thermal decomposition as a function of exposure temperature. The characterization of the products were performed by means of Fourier transform infrared spectrometry （FTIR）, gas chromatography/mass spectrometry （GC/MS） and viscosity experiments. The results show that PAO has the lower thermal stability, being degraded at 200℃ different from 300 ℃ for DE. Several by-products are identified during the thermal degradation of two lubricant base oils. The majority of PAO products consist of alkenes and olefins, while more oxygen-contained organic compounds are detected in DE samples based on GC/MS analysis. The related reaction mechanisms are discussed based on the experimental results.

气相合成亚微米级超细、功能性粉体材料

(合作方式:技术转让、合作开发均可)一、项目概况该项目利用等离子态时物质所处的高激发、高活性、高能密度的特点,采用不同气氛和反应物在高温下氧化热分解、气化以及"骤冷"等条件,使产品"冻结"在一特殊状态,制备出超细氧化锆、钠米级氧化锌、氧化钴及氧化镁等产品,高频等离子体装置可连续稳定运行。

Ni/PdO/RuO_2复合型活性阴极的制备与表征

采用热分解氧化法,在Ni基体上制备以PdO为中间层、RuO2为活性层的Ni/PdO/RuO2复合型活性阴极,并通过XPS、XRD、能量色散X荧光(EDXRF)、SEM、极化曲线、循环伏安法和交流阻抗谱等表征其组成、结构与电化学性能。结果表明,Pd和Ru分别以PdO和RuO2的形式存在于Ni/PdO/RuO2复合型活性阴极中,其含量分别为1.25wt%和1.71wt%;在363K、11mol·L-1NaOH溶液、3kA·m-2电流密度下,Ni/PdO/RuO2复合型活性阴极的析氢过电位比Ni电极和Ni/RuO2电极分别低371和125mV;循环伏安法循环72h后,该复合型活性阴极双电层电容值减小30.6%,比Ni/RuO2电极表层结构更稳定;Ni/PdO/RuO2复合型活性阴极的表面粗糙度大且无明显的裂纹存在,与纯镍电极相比,该复合型活性阴极比表面积增加了31.12倍。

Efficient destruction of sodium cyanide by thermal decomposition with addition of ferric oxide

Efficient destruction of cyanide by thermal decomposition with ferric oxide addition was proposed. The mechanism of destruction of sodium cyanide with or without ferric oxide addition under various conditions was examined by XRD, DSC-TG, and chemical analysis technologies. In the absence of ferric oxide, sodium cyanide decomposes at 587.4 ℃ in air and 879.2 ℃ in argon atmosphere. In the presence of ferric oxide, about 60% of sodium cyanide decomposes at 350 ℃ for 30 min in argon, while almost all sodium cyanide decomposes within 30 min in air or O2 with mass ratio of ferric oxide to sodium cyanide of 1:1. The increase of ferric oxide addition, temperature, and heating time facilitates the destruction of sodium cyanide. It is believed that with ferric oxide addition, NaCN reacts with Fe2O3 to form Na4Fe(CN)6, Na2CO3, NaNO2 and Fe3O4 in argon. NaCN decomposes into NaCNO, Na4Fe(CN)6, minor NaNO2, and the formed NaCNO and Na4Fe(CN)6 further decompose into Na2CO3, CO2, N2, FeOx, and minor NOx in air or O2.

Simulation of alumina dissolution and temperature response under different feeding quantities in aluminum reduction cell

In the feeding process of aluminum electrolytic, feeding quantity of alumina affects eventually dissolved quantity at the end of a feeding cycle. Based on the OpenFOAM platform, dissolution model coupled with heat and mass transfer was established. Applying the Rosin-Rammler function, alumina particle size distribution under different feeding quantities was obtained. The temperature response of electrolyte after feeding was included and calculated, and the dissolution processes of alumina with different feeding quantities (0.6, 0.8, 1.0, 1.2, 1.4, 1.6 kg) after feeding were simulated in 300 kA aluminum reduction cell. The results show that with the increase of feeding quantity, accumulated mass fraction of dissolved alumina decreases, and the time required for the rapid dissolution stage extends. When the feeding quantity is 0.6 kg and 1.2 kg, it takes the shortest time for the electrolyte temperature dropping before rebounding back. With the increase of feeding quantity, the dissolution rate in the rapid dissolution stage increases at first and then decreases gradually. The most suitable feeding quantity is 1.2 kg. The fitting equation of alumina dissolution curve under different feeding quantities is obtained, which can be used to evaluate the alumina dissolution and guide the feeding quantity and feeding cycle.

Estimation of thermal decomposition temperatures of organic peroxides by means of novel local and global descriptors

The thermal decomposition temperature is one of the most important parameters to evaluate fire hazard of organic peroxide. A quantitative structure-property relationship model was proposed for estimating the thermal decomposition temperatures of organic peroxides. The entire set of 38 organic peroxides was at random divided into a training set for model development and a prediction set for external model validation. The novel local molecular descriptors of AT1, AT2, AT3, AT4, AT5, AT6 and global molecular descriptor of ATC have been proposed in order to character organic peroxides’ molecular structures. An accurate quantitative structure-property relationship （QSPR） equation is developed for the thermal decomposition temperatures of organic peroxides. The statistical results showed that the QSPR model was obtained using the multiple linear regression （MLR） method with correlation coefficient （R）, standard deviation （S）, leave-one-out validation correlation coefficient （RCV） values of 0.9795, 6.5676 ℃ and 0.9328, respectively. The average absolute relative deviation （AARD） is only 3.86% for the experimental values. Model test by internal leave-one-out cross validation and external validation and molecular descriptor interpretation were discussed. Comparison with literature results demonstrated that novel local and global descriptors were useful molecular descriptors for predicting the thermal decomposition temperatures of organic peroxides.

Synthesis of ZnO whiskers via hydrothermal decomposition route

ZnO whiskers with a length of 30-40μm and a diameter of about 1μm were synthesized by co-precipitation of ZnSO 4 and Na2CO3 solution at room temperature followed by hydrothermal treatment of the as-prepared Zn5(CO3)2(OH)6 precursor at 160 ℃for 6 h.The increase of the initial solution pH promotes the hydrothermal conversion of the particulate Zn5(CO3)2(OH)6 to ZnO whiskers.The presence of minor amount of EDTA in the hydrothermal solution promotes the one dimensional growth of ZnO whiskers,leading to the formation of ZnO whiskers with a length of 50-60μm and a diameter of 1-2μm.

Obtaining Thin Film of SnO2/Cu2O and Characterization by X-Ray Diffraction

Thin films of tin and copper oxide forming heterojunction are being studied for applications in photovoltaic systems. The procedure for obtaining such a film was based on the technique of spray pyrolysis with working temperature of 600 ℃. The XRD （X-ray diffraction） showed the formation of tin oxides （SnO2） and copper （Cu2O） and its structural parameters are a, b and c, 4.7534 A^°, 4.7534 A^°, 3.1998 A^° （tetragonal form） and 4.2580 A^°, 4.2580 A^°, 4.2580 A^° （cubic form）, respectively. Highseore Plus program was used for phase identification and DBWSTool2.4 program used for refinement. The grain size was estimated by Williamson-Hall.

Synthesis and Characterization of Modified Epoxy Resins by Silicic Acid Tetraethyl Ester and Nano-SiO_2

A kind of modified epoxy resins was obtained by condensation of epoxy resin with silicic acid tetraethyl ester（TEOS） and nano-SiO2. The reactions were performed with hydrochloric acid as a catalyst at 63 ℃. The structure, thermal stability and morphological characteristics of the modified epoxy resins were studied through infrared spectra（FT-IR） analysis, thermogravimetric（TG） analysis and scanning electron microscopy respectively. It has been found from the IR and TG study that modified epoxy resins have greater thermal stability than epoxy resins, and its thermal stability has been improved by the formation of inter-crosslinked network structure. The modified epoxy resins exhibit heterogeneous morphology and heterogeneity increases with more TEOS feeding, which in turn confirms the formation of inter-crosslinked network structure in modified epoxy resins.

Synthesis, characterization of monodispersed MgO microspheres and thermal decomposition kinetics of its precusor

Monodispersed MgO microspheres were successfully synthesized by a simple solvothermal method using PEG-400 as solvent. The samples were characterized by X-ray diffraction(XRD) and scanning electron microscopy(SEM). The results reveal that the precusor was monoclinic Mg5(CO3)4(OH)2·4H2O and composed of nanosheets with the thickness of about 250 nm. By calcining the precusor at 500 °C for 5 min, cubic MgO with similar morphology was obtained. According to the SEM images, it is found that the volume ratio of PEG-400 to deionized water is considered as a crucial factor in the evolution of the morphology. Based on the SEM images obtained under different experimental conditions, a possible growth mechanism which involves self-assembly process was proposed. The thermal decomposition process of MgO precusor was studied by thermogravimetry-differential thermogravimetry(TG-DTG) at different heating rates in air. Thermal analysis kinetics results show that the most probale mechanism models of MgO precusor are An and D3, respectively. In addition, isothermal prediction was studied to quantitatively characterize the thermal decomposition process.

Direct spray pyrolysis of aluminum chloride solution for alumina preparation

The effects of pyrolysis mode and pyrolysis parameters on Cl content in alumina were investigated, and the alumina products were characterized by XRD, SEM and ASAP. The experimental results indicate that the spray pyrolysis efficiency is higher than that of static pyrolysis process, and the reaction and evaporation process lead to a multi-plot state of the alumina products by spray pyrolysis. Aluminum phase starts to transform into γ-Al2O3 at spray pyrolysis temperature of 600 °C, which is about 200 °C lower than that of static pyrolysis process. The primary particle size of γ-Al2O3 product is 27.62 nm, and Cl content in alumina products is 0.38% at 800 °C for 20 min.

Double layered,one-pot hydrothermal synthesis of M-TiO_2(M=Fe^(3+),Ni^(2+),Cu^(2+)and Co^(2+)) and their application in photocatalysis

A double layered, one-pot hydrothermal method was adopted in this work to prepare transition metal ions （Fe3＋, Ni2＋, Cu2＋ and Co2＋） doped TiO〉 The morphology and chemical properties of TiO2 and the status of metal ions were characterized with XRD, TEM, BET, UV-Vis and XPS analysis. TEM images show that the obtained TiO2 was very uniform with an average particle size of 10.4 nm. XPS, TEM and XRD results show that transitional metals were doped onto TiO2 in the form of ions. Photocatalytic decomposition of oxalic acid under UV illumination and methylene blue degradation under visible light on these materials were conducted, respectively. The results reveal that Cu2＋-TiO2 and C02＋-TiO2 showed a highest activity under UV and visible light illumination, respectively, and they were both more active than commercial P25 TiO2. With this special design of double layers, the hydrolysis of titanium precursor in the system with water can be easily controlled and metal ions are simply doped. This strategy can be further applied to synthesize metal ion doped TiO2 using various metal precursors with controllable amounts, and thus lead to better optimization of highly active photocatalyst.