Morphological and Electrochemical Characterization of Ti/MxTiySnzO2 (M = Ir or Ru) Electrodes Prepared by the Polymeric Precursor Method

This paper describes the effect of the composition of the oxide films on the properties of electrodes Ti/MxTiySnzO2 (M = Ir or Ru) prepared by the polymeric precursor method. XRD studies showed that the anodes are formed by solid solutions. The electrodes containing IrO2 exhibit lower activity for the oxygen evolution reaction. The doping of the electrode surface with SnO2 improves the catalytic properties of the anodes. However, it should be held in appropriate compositions, because the change in the atomic ratio of this element shows a marked effect on the stability of the oxides. Electrode Ti/Ir0.2Ti0.3Sn0.5O2 has lower lifetime, i.e. 6 hours. The 20% decrease in the stoichiometric amount of SnO2 increases the time to a value above 70 hours, as observed for Ti/Ir0.3Ti0.4Sn0.3O2. Electrode Ti/Ru0.3Ti0.4Sn0.3O2 shows lifetime of 11 hours;therefore IrO2 is more stable than RuO2 under the conditions investigated. These results suggest that electrode Ti/Ir0.3Ti0.4Sn0.3O2 is promising for different applications, such as water electrolysis, capacitors and organic electrosynthesis.

Use of Perovskite-Type Lanthanum Nickelate Synthesized by the Polymeric Precursor Method in the Steam Reforming Reaction of Methane

In the current work, LaNiO3 perovskite was synthesized using the polymeric precursor method. The materials were thermally treated at 300°C for 2 hours, subsequently supported on alumina or zirconia and finally calcined at 800°C for 4 hours. The resulting samples were characterized by X-ray diffraction, thermogravimetry, BET surface area and thermo-programmed reduction. Steam reforming reactions were carried out at 750°C and 6 bar during 4 hours using a pilot reactor under a H2O:CH4 ratio of 2.5. The mass of catalysts was about 5.7 g. X-ray diffraction patterns confirmed the formation of the perovskite structure in all samples prepared. The results also showed that lanthanum nickelate was more efficient when supported on alumina than zirconia. Finally, it was observed that the methane conversion was approximately 94% and the selectivity to hydrogen was about 70%. In all cases low selectivity to CO and CO2 was verified.

TiO_(2)/CuO Films Obtained by Citrate Precursor Method for Photocatalytic Application

In the present work, the hybrid catalyst films of TiO2/CuO containing up to 10% in mol of copper were deposited onto glass surface. Precursor solutions were obtained by citrate precursor method. Films were porous and the average particle size was 20 nm determined by FEG-SEM analysis. The photocatalytic activities of these films were studied using Rhodamine B as a target compound in a fixed bed reactor developed in our laboratory and UV lamp. It was observed that the addition of copper to TiO2 increased significantly its photocatalytic activity during the oxidation of Rhodamine B. The degradation exceeded 90% within 48 hours of irradiation compared to 38% when pure TiO2 was used. Moreover, there was a reduction in the particles band gap energy when compared to that of pure TiO2. These results indicate that the TiO2/CuO films are promising catalysts for the development of fixed bed reactors to be used to treat effluents containing azo dyes.

Synthesis and Characterization of LaNixCo1-xO3 Perovskites via Complex Precursor Methods

This work presents a study on the synthesis of LaNixCo1-xO3 perovskites via complex precursor methods. Perovskite oxides with the composition LaNixCo1-xO3 were synthesized by chelating precursor and polymeric precursor methods using nickel and/or cobalt nitrates, lanthanum nitrate, ethylene glycol, citric acid, and EDTA as starting source. The obtained perovskite were characterized by thermogravimetric analysis, infrared spectroscopy, X-ray diffraction and the morphology of the samples were investigated by N2 adsorption experiments and average medium particle size. TG curves and FTIR spectra were particularly useful in establishing of the optimal calcination temperature of the precursor powders. X-ray diffraction patterns revealed the formation of the perovskite structure in all samples prepared by both synthesis method and after calcinations at 700℃. The results showed that the preparation method resulted in oxides with the intended structure. The specific surface area values were influenced by preparation method.

Preparation and characterization of nanometer-sized barium titanate powder by complex-precursor method

A new complex-precursor method was proposed to prepare nanometer-sized BaTiO3 powder. Firstly,Ti2O(O2)2(ta)24-complex ions were prepared by the reaction of H2O2,Ti4+ and ta3-(ta=C6H6O6N3-) with a desirable amount of surface active agent,and then the Ba2Ti2O(O2)2(ta)2·2H2O precursor was obtained by reaction between Ti2O(O2)2(ta)24-and Ba2+. Finally,the precursor was annealed at 800 ℃ for 2 h to obtain BaTiO3 powder. The morphology,the particle size distribution,the purity and the molar ratio of Ba to Ti of BaTiO3 powder were investigated systematically by TEM,XRD,IR,Raman and chemical analysis,respectively. The results show that the BaTiO3 powders with the grain size of about 40 nm have a tetragonal crystalline structure at room temperature and a spherical morphology.

Ultrathin layered double hydroxide nanosheets prepared by original precursor method for photoelectrochemical photodetectors

Layered double hydroxides(LDHs)are widely used owing to their unique alternating anionic and cationic layered twodimensional(2D)structures.However,studies on the preparation of 2D LDH nanosheets with uniform thickness and their photodetectors are limited.In this study,two novel ultrathin LDH(Ca-In and Ca-Al LDH)nanosheets are peeled off from precursor bimetallic phosphides through the original precursor method.Both Ca-In and Ca-Al LDH nanosheets demonstrate a uniform thickness distribution with an average thickness of 3–4 nm,micron-level lateral sizes,and moderate bandgap.Owing to its broad light absorption range,hydrophilicity,and stability,Ca-In and Ca-Al LDH nanosheets are applied for the first time in photoelectrochemical photodetectors,realizing a wide range of light detection from ultraviolet(365 nm)to visible light(635 nm).Moreover,the fabricated photodetectors exhibit excellent cycle stability,and the average photocurrent density shows no reduction after 70 days.Therefore,this study provides an effective method to prepare 2D Ca-In and Ca-Al LDH nanosheets with uniform thickness and photoelectric application prospects.

Effect of Sn precursor on the synthesis of SnO2 and Sb-doped SnO2 particles via polymeric precursor method

SnO2 and Sb-doped SnO2 particles were synthesized using the polymeric precursor method with different Sn salt precursors： SnCl2.2H2O, SnCl4.5H20, or Sn citrate. Sb2O3 was used as the precursor of Sb, and the molar ratio of nsn：nsb was held constant. FTIR and TGA/DTA were used to examine the influence of the Sn precursor on the formation and thermal decomposition of the Sn and Sn-Sb complexes. The calcination products obtained from heating the Sn and Sn-Sb complexes at 500℃ in air were analyzed using XRD and TEM analysis. The results revealed that the SnO2 and Sb-doped SnO2 formation temperatures depended on the nature of the Sn precursor. The calcination products were found to be SnO2 and Sb-doped SnO2 particles, which crystallized in a tetragonal cassiterite structure with a highly preferred （110） planar orientation. The Sn precursor and the presence of Sb in the SnO2 matrix strongly influenced the crystallinity and lattice parameters.

Systematic examination of ‘precursor waves’ of strong earthquakes by using the wavelet method

Based on the borehole strainmeter recordings immediately before the strong earthquakes （Ms〉7.5） during the period from 2001 to 2005 observed at the Taian observation station, Shandong Province, the authors make a systematic and objective examination of the precursor waves of the quakes. The effects of Earth tides with periods larger than 128 min are eliminated through high-pass filtering; and atmospheric-pressure inferences are removed by linear regression. The 2-128 min signals are then separated into six frequency bands by employing the wavelet method. Results indicate that the wavelet method is capable of picking out information of weak variations in the signals. According to the characteristics of the ＇precursor waves＇ obtained from wavelet transformation, the method of overrun ratio analysis is put forward for examination. All the detailed components of the wavelets have been analyzed. For the time series of the overrun rate in all these components, statisitical calculation has been made for the slopes of fit curves, and mean values and standard deviations were obtained and positive-negative slope ratios were analyzed. The three statistical data show that ＇precursor waves＇ are not widely recorded by borehole strainmeter within 15 days before remote strong earthquakes.

The Optimal Precursors for ENSO Events Depicted Using the Gradientdefinition-based Method in an Intermediate Coupled Model

The predictability of El Ni-o-Southern Oscillation (ENSO) has been an important area of study for years. Searching for the optimal precursor (OPR) of ENSO occurrence is an effective way to understand its predictability. The CNOP (conditional nonlinear optimal perturbation), one of the most effective ways to depict the predictability of ENSO, is adopted to study the optimal sea surface temperature (SST) precursors (SST-OPRs) of ENSO in the IOCAS ICM (intermediate coupled model developed at the Institute of Oceanology, Chinese Academy of Sciences). To seek the SST-OPRs of ENSO in the ICM, non-ENSO events simulated by the ICM are chosen as the basic state. Then, the gradient-definition-based method (GD method) is employed to solve the CNOP for different initial months of the basic years to obtain the SSTOPRs. The experimental results show that the obtained SST-OPRs present a positive anomaly signal in the western-central equatorial Pacific, and obvious differences exist in the patterns between the different seasonal SST-OPRs along the equatorial western-central Pacific, showing seasonal dependence to some extent. Furthermore, the non-El Ni-o events can eventually evolve into El Ni-o events when the SST-OPRs are superimposed on the corresponding seasons;the peaks of the Ni-o3.4 index occur at the ends of the years, which is consistent with the evolution of the real El Ni-o. These results show that the GD method is an effective way to obtain SST-OPRs for ENSO events in the ICM. Moreover, the OPRs for ENSO depicted using the GD method provide useful information for finding the early signal of ENSO in the ICM.

有机前驱体法制备氮化硼纤维的研究

氮化硼(BN)纤维是一种耐热和介电性能优异的陶瓷纤维,目前的主要合成方法为有机前驱体转化法。以聚三甲胺基环硼氮烷为前驱体,通过熔融纺丝、不熔化和力热耦合热解处理,制备出直径均匀的BN纤维。利用扫描电镜(SEM)、X射线衍射(XRD)、X光电子能谱(XPS)、BET比表面积等手段对BN纤维的微观结构、结晶性能、元素组成以及孔隙率进行详细表征。结果表明:1600℃热处理得到的BN纤维,表面光滑,织态结构完整,拉伸强度可达640.3MPa,而1000℃热处理得到的BN纤维,孔隙率高,比表面积最大,比表面积可达362.64m^(2)/g。

硅基聚合物耐高温衍生陶瓷涂层制备与应用研究进展

随着航空航天领域的不断发展,金属以及碳材料等高温结构部件的服役条件日益苛刻。通过恰当的工艺在高温结构部件表面制备硅基陶瓷涂层并赋予其特殊性能,可有效提高高温结构部件的使用寿命。近年来,聚合物前驱体转化陶瓷涂层逐渐成为一种无机涂层制备的新方法。该方法具有制备工艺简便、涂层功能拓展性强等特点,得到了研究者越来越多的关注。本文主要综述了硅基聚合物前驱体转化陶瓷涂层的研究进展。首先从聚合物陶瓷涂层的制备展开,简要介绍了硅基聚合物前驱体、填料种类以及涂覆工艺和裂解方式对涂层结构以及性能的影响。随后,重点讨论了聚合物前驱体转化陶瓷涂层在耐高温防护领域,包括抗氧化、环境障、热障涂层的应用进展。最后,指出了聚合物陶瓷涂层在涂层性能提升及缺陷控制等方面的问题,并对其发展方向进行了展望,例如通过在硅基前驱体中引入Hf,Zr,Ta等超高温元素,提高陶瓷涂层的耐温等级,以及发展高效的陶瓷化新技术,从而提高陶瓷转化效率及涂层适用性范围等。

先驱体转化法制备含异质元素碳化硅纤维的研究进展

连续SiC纤维及其复合材料以其优异的耐高温、抗氧化以及机械性能在航空航天以及核领域有着广泛的应用前景。先驱体转化法已成为制备连续SiC纤维最重要的方法。特定异质元素的引入可以有效改善SiC纤维的性能。本文结合我们团队近40年在先驱体转化法制备高性能SiC纤维领域的相关工作,首先综述了异质元素的引入方式,主要包括物理共混和化学改性;从提高先驱体的陶瓷产率、促进纤维烧结致密化,提高SiC纤维的耐高温性能以及拓展SiC纤维的功能化应用等方面阐述了异质元素的作用和机理;然后分别介绍了国内外含Ti、Al、Zr、Fe、B以及难熔金属(Hf、Ta、Nb)等含异质元素SiC纤维的组成、结构与性能以及发展现状,最后对陶瓷先驱体体系构建、异质元素种类含量与纤维性能构效关系研究、以及纤维工程化应用等研究方向进行了展望。

外加电场加速前驱体法制备SiOC陶瓷材料

采用闪速热解法通过聚合物前驱体制备了硅氧碳(SiOC)陶瓷材料。外加电场显著加速了SiOC微观相结构变化,与传统方法相比,SiOC前驱体在较低的热解温度下发生相分离,产生了碳和SiC相。在电场作用下,样品会形成更多的碳化硅和更有序的碳相。其基本原理可以用电场和焦耳加热共同作用下的显著改变相变驱动力来解释。这项工作提供了一个低温合成SiOC纳米复合材料新路线。

陶瓷纤维制备技术的研究进展

综述了石英纤维、碳化硅纤维、氮化硅纤维、氮化硼纤维、氧化铝纤维、莫来石纤维、硅酸铝纤维等不同种类陶瓷纤维的制备技术研究现状和技术难点。石英纤维主要采用溶胶-凝胶法制备,需要纤维表面引入氮化硼涂层改善其界面析晶行为;碳化硅纤维主要采用前驱体转化法和活性炭转化法制备,需进行表面涂层增强其性能;氮化硅纤维主要采用溶胶-凝胶法和碳热还原氮化法制备;氮化硼纤维主要采用无机转化法和有机前驱体法制备;溶胶-凝胶法是氧化铝、莫来石和硅酸铝纤维的主要制备方法。未来国内陶瓷纤维研究应进一步提高纤维性能、开发新品种、提高制备技术水平、加强应用研究和拓展应用领域。

溶胶-凝胶法合成SiZrNOC陶瓷前驱体的微观结构和相演化

陶瓷材料作为一种高强度、高硬度、耐磨性、耐高温的材料,在航空航天领域拥有着广阔的前景。通过溶胶凝胶法以硅酸四乙酯作为硅源,二苯基甲烷二异氰酸酯作为氮源,正丙醇锆作为锆源合成了SiZrNOC预陶瓷聚合物。通过失重率测试结果显示,当Zr/N比为3∶1时,陶瓷产率最高,达到53%。使用扫描电子显微镜对陶瓷微观结构进行分析,结果表明,随着热解温度的升高,材料的内部结构变得规整,致密化程度显著增强。设计的陶瓷材料将有能力改善或扩展其在未来航空航天相关领域的应用。为开发高温下具有热稳定性和抗氧化性的材料提供了一个新的选择。

镍钴锰三元前驱体的制备及性能研究

研究了采用共沉淀法制备镍钴锰三元前驱体,考察了氨水浓度、体系pH、反应时间、反应温度对所制备前驱体性能指标的影响。结果表明:在氨水浓度1 mol/L,体系pH=12、反应温度55℃、反应温度28 h最佳试验条件下,所制备前驱体产品粒度分布良好,呈均匀的类球形,结晶致密;混锂煅烧后的正极材料在2.8~4.4 V、0.2 C充放电制度下首次放电容量为169.14 mAh/g,首次效率为88.32%。

硅硼碳氮陶瓷前驱体聚硼硅氮烷的合成与表征

以三氯化硼(BCl3)、三氯硅烷(HSiCl3)和六甲基二硅氮烷(Me6Si2NH)为原料,通过聚合物前驱体转化陶瓷(polymer-derived ceramics,PDCs)法成功合成了硅硼碳氮(SiBNC)陶瓷前驱体--聚硼硅氮烷(PBSZ)。采用傅里叶变换红外光谱、核磁共振、X射线光电子能谱、热重分析和差示扫描量热对PBSZ的结构和热性能进行分析。结果表明,PBSZ结构中存在硅氮硼(Si—N—B)网络和六元硼氮(B—N)环。在氮气中,800℃时PBSZ的陶瓷产率为53.9%。

酶联免疫法测定甘精胰岛素中单链前体残留研究

目的 建立酶联免疫法检测甘精胰岛素中单链前体残留,为甘精胰岛素药物质量控制和安全性评价提供新方法。方法采用双抗夹心酶联免疫法,以甘精胰岛素原为标准品,建立单链前体残留检测方法,验证方法的重复性、准确度、范围和精密度,并应用该方法检测9批甘精胰岛素原料药。结果在0.156~10.00 ng·mL^(-1)浓度范围内,对甘精胰岛素原标准品进行四参数曲线拟合,曲线相关系数R~2大于0.99,方法准确度较高、重复性良好。重复检测3批甘精胰岛素原料药,平均加标回收率在104%~113%范围内,RSD%小于10%,方法精密度良好。9批样品中单链前体残留量均小于1 ng·mg^(-1)。结论建立的酶联免疫法可用于甘精胰岛素及其他重组人胰岛素类似物中单链前体残留量的质量控制和安全性评价。

Synthesis of LaPO_4:Ce,Terbium by Co-Precipitation Method

The synthesis of precursor of green phosphors, LaPO4: Ce, Tb, by means of co-precipitation with cocurrent flow feed was studied. The effects of the reaction temperature, the kind and concentration of the acid in the bottom water, and the charging rate on the physical properties, such as particle size, were investigated. It is found that the particle size of the powder is controllable by adjusting acidity in bottom water and charging rate. The powder with diameter size of 3 to 5μm was obtained. Its XRD and SEM were analyzed. XRD patterns of the as-prepared green phosphor powders display the typical peaks of CePO4. SEM shows that the morphology of powders is ball-shaped.

Study on Synthesis of Nanometer SiC Precursors with Sol-Gel of SiO_2-Lignin in the Pulp Black Liquor

In the process of synthesis of nanometer SiC precursors with sol-gel of SiO2 and lignin , the products of all sizes required can be controlled by the concentration of reac-t ants , pH, temperature, reaction and ageing time , and so on . The best conditions in this research are : the concentration of Na2SiO3 and organic matters are 4. 50% and 26.4% respectively, pH = 3.3 , T = 65℃ , ageing time is 30min , dried at 150 ℃ , the size of SiC precursors is about 2.0μm .