Lead titanate nanotubes synthesized via ion-exchange method: Characteristics and formation mechanism

A two-step method is presented for the synthesis of one dimensional lead titanate (PbTi₃O₇) nanotubes. Firstly, titanate nanotubes were prepared by an alkaline hydrothermal process with TiO₂ nanopowder as precursor, and then lead titanate nanotubes were formed through an ion-exchange reaction. We found that sodium titanate nanotubes have ion exchangeability with lead ions, while protonated titanate nanotubes have not. For the first time, we distinguished the difference between sodium titanate nanotubes and protonated titanate nanotubes in the ion-exchange process, which reveals a layer space effect of nanotubes in the ion-exchange reaction. In comparison with sodium titanate, the synthesized lead titanate nanotubes show a narrowed bandgap.     

水热法制备纳米结构TiO2的生长机制及表征

将钛片放入NaOH溶液中,用水热法制备了TiO2纳米线阵列薄膜。系统地研究了水热参数对产物的影响以及纳米结构TiO2的生长机制。通过场发射扫描电子显微镜(FESEM)、X射线衍射仪(XRD)、透射电子显微镜(TEM)等对样品进行了表征。结果表明,水热过程中,钛溶解和钛酸盐结晶生长之间的动态平衡决定了产物的结构和形貌。在相同温度下,NaOH溶液浓度降低,水热产物的维度就增加。温度升高会促进钛溶解和钛酸盐扩散,使产物在一维尺度上生长。同时高温使晶体结构更加完整。制备的TiO2纳米线陈列显示了良好的光电性能。     

Preparation and performance of titanate nanotube by hydrothermal treatment

Titanate nanotubes were synthesized by hydrothermal treatment in concentrated NaOH solution followed by HCl washing. The as-prepared nanotubes were characterized by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, and N2 adsorption-desorption isotherm measurements （BET）. The results displayed that the hydrothermal treatment temperature within 110-160℃ not only affected the structure of the nanotube, but also the anatase-to-rutile transformation temperature. The nanotube could be obtained only in an appropriate concentration of NaOH solution. The diameter of the nanotube was 6-10 nm. The surface area of the product initially increased with increasing treatment temperature, to reach a maximum of about 630 m^2/g at 130℃, and then decreased with a further increase in temperature.     

ZnSe微球在不同水热条件下的制备与表征(英文)

以Zn(NO3)2·6H2O和Na2SeO3作为原料,通过水热法制备ZnSe纳米晶。探讨了水热反应温度、反应时间、NaOH浓度和N2H4·H2O的添加量对最终产物的相组成、显微形貌和颗粒尺寸的影响,并借助XRD、SEM、TEM、PL等测试手段对产物的相组成、显微形貌和颗粒尺寸进行表征。添加20 mL 1 mol/L NaOH溶液和10 mL N2H4·H2O溶液,在180°C的温度下水热反应4 h制备的产物主要是立方闪锌矿结构的ZnSe微球,所得的ZnSe微球从内到外是由平均尺寸约20 nm的ZnSe纳米晶组成。结果表明:较低的水热温度和较短的反应时间都不利于得到结晶好的纯相ZnSe,产物结晶性不好,而且还会产生杂相和有较多缺陷。添加适量浓度的NaOH和水合肼才能确保得到形貌均匀、发光性能好的ZnSe微球。     

二氧化钛纳米管的合成及其表征

采用水热合成法，以TiO2粉体和NaOH为原料，成功地制备出了TiO2纳米管。用XRD，SEM，HRTEM，紫外吸收光谱分析仪和光谱辐射分析仪等手段对纳米管进行微观形貌、光学性能的表征，并探讨了其生长机理。结果表明，所得产物为锐钛矿和金红石混晶型TiO2纳米管，管壁为多层，管的外径分布在10nm～50nm，长度可达几微米甚至十几微米，呈开口状；TiO2纳米管的生长机理符合3-2-1D的生长模型，其紫外吸收光谱和光致发光光谱相对于原料粉均呈现出蓝移现象，光致发光光谱显示TiO2纳米管在可见光区的发光强度明显增强。     

Synthesis of lanthanum carbonate nanoparticles via sonochemical method for preparation of lanthanum hydroxide and lanthanum oxide nanoparticles

Lanthanum carbonate nanoparticles were synthesized from the reaction of lanthanum acetate and Na₂CO₃ under sonication via sonochemical method. Lanthanum hydroxide nanoparticles were prepared by facial hydrothermal processing from the resulted product at 110 °C for 24 h. The role of surfactant, calcination temperature and sonication time were investigated on the morphology and particle size of the products. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS), and Fourier transform infrared (FT-IR) spectra. La₂O₃ nanoparticles were obtained by calcinations of the nanoparticles of lanthanum carbonate at 600 °C.     

水热法氧化钒纳米管生长过程的研究

以十二胺和五氧化二钒为原料通过水热反应合成了氧化钒纳米管，并用X射线衍射仪(XRD)和高分辨透射电子显微镜(HRTEM)进行表征。实验结果表明，用这种方法合成的氧化钒纳米管转化率很高，可以实现宏量制备；纳米管内管径分布很窄，约为20nm；纳米管结构独特，十二胺内嵌入管壁层间成为支撑管子的骨架，并影响管壁层间距；水热反应时间显著影响氧化钒纳米管的生长，理想的水热反应时间为6～8天，因此纳米管热稳定性差。     

Synthesis of titanate/anatase composites with highly photocatalytic decolorization of dye under visible light irradiation

Titanate/anatase nanocomposites consisting of titanate nanotubes and leaf-like anatase TiO₂ nanoparticles were successfully prepared via a novel combinational hydrothermal method. The samples were characterized by means of X-ray diffraction (XRD) and transmission electron microscopy (TEM). The activity of the nanocomposites was examined by photocatalytic decolorization of rhodamine B under visible light irradiation. It is found that the nanocomposites exhibited a much improved photocatalytic activity in comparison with titanate nanotube, anatase TiO₂ nanoparticle, and even the commercial Degussa P-25. The photocatalytic mechanism of the as-prepared nanocomposites was discussed.     

Hydrothermal express synthesis of CNT/MnO<Subscript>2</Subscript> composite for asymmetric supercapacitor

A hydrothermal technique for the express synthesis of a composite based on carbon nanotubes (CNTs) and manganese dioxide by means of the direct reduction of potassium permanganate from an aqueous isopropanol solution is proposed in this work. The synthesis conditions (time, temperature, ratios between reagents) are optimized; the primary and secondary processes taking place in the system are considered in detail. The synthesized CNT/MnO₂ composite is studied with the help of a wide range of physicochemical and electrochemical methods to assess the possibility of its use as a positively charged electrode of an asymmetric supercapacitor (SC). The assembled SC cell based on this composite and an activated carbon (AC) electrode has fairly high power typical of conventional electric double-layer capacitors (0.82 kW/kg) with a twofold increase in the energy density (12.14 W h/kg).     

基于统计方法的超声振动电火花油的空化场表征

通过铝箔腐蚀法测定不同条件下电火花工作液中的超声空化场分布,用Image-J软件提取腐蚀位置,借鉴金属盐雾腐蚀试验统计方法量化超声空化效应。结果表明:超声在电火花工作液作用区域内的空化场分布不均匀,且随着铝箔与超声振板距离的增加,铝箔的腐蚀面积减小,空化效应减弱;频率为28 k Hz的超声波在90 W功率条件下,80 mm范围内的空化作用的衰减率降至75%,且随着频率增加,衰减变快。     

High-temperature integrated and flexible ultrasonic transducers for nondestructive testing

Integrated ultrasonic transducers (IUTs) and flexible ultrasonic transducers (FUTs) are presented for nondestructive testing at high temperatures. These transducers are made of sol–gel-sprayed piezoelectric thick (>40 μm) ceramic films. The ceramic materials are lead-zirconate-titanate, bismuth titanate and lithium niobate which are for thickness measurements up to 150, 400 and 800 °C, respectively. The IUT can also be deposited onto one end of a long ultrasonic delay line to perform nondestructive testing at the other end at even higher temperatures. FUTs made of bismuth titanate films onto thin stainless steel foils are also used for thickness measurements at 300 °C with a high-temperature couplant sandwiched between the FUT and a steel substrate. All experiments at high temperatures were performed in pulse-echo mode and ultrasonic echoes with signal-to-noise ratios above 20 dB were obtained. The center operation frequencies of both IUTs and FUTs range from 4.4 to 10.7 MHz.     

A redox-assisted molecular assembly of molybdenum oxide amine composite nanobelts

In this paper, the nanobelts of molybdenum oxide amine composite were successfully synthesized via a redox-assisted molecular assembly route under the hydrothermal conditions. The synthesized nanobelts were characterized by XRD, SEM, TEM, TG and FT-IR measurements. The thickness of nanobelts is found to be ca. 20-30 nm and their lengths are up to several tens of micrometers. Based on a series of the experimental results, a possible model, redox-intercalation-exfoliation, was suggested for the formation of nanobelts of molybdenum oxide amine composite.     

外场作用下由工业TiOSO4液合成介孔二氧化钛

以工业硫酸氧钛为钛源,采用复合模板合成路线,分别于超声,微波和水热外场作用下合成了介孔二氧化钛前驱体.通过调节反应体系的pH值来控制TiOSO4液的水解和缩聚速率.煅烧脱除模板后得到锐钛型的介孔二氧化钛.产物采用XRD,氮等温吸附脱附,粒度分布,SEM,TEM,SAD和X射线能谱分析(XPS)等技术进行了表征.结果表明具有强极化作用和温和水热环境的外场利于制备结构更佳的介孔二氧化钛;超声振动利于介观结构的形成.在微波辐照下,所制得介孔二氧化钛的比表面积为146.6 m2/g,平均孔径2.57 nm,晶粒尺寸13.65 nm.超声、微波和水热较常规合成方法更利于形成和稳定介孔结构.     

不同基片/催化剂生长碳纳米管的研究

分别以Nb、Nb/(Au+Pd)、不锈钢箔和不锈钢箔/二茂铁作为基片/催化剂,高温裂解无水乙醇制备碳纳米管,并研究了纳米管形貌和产率的变化.发现在纯净Nb片上得不到碳纳米管,而以Nb/(Au+Pd)作为基片/催化剂时,碳纳米管产率高、直径较细且长度较长;在纯净不锈钢箔上生长碳纳米管的直径很细但长度非常短,而乙醇中加入二茂铁后纳米管变长且粗.     

Hydrothermal synthesis of vanadium oxide nanotubes by a facile route

Vanadium oxide nanotubes were synthesized by hydrothermal treatment from V2O5·nH2O sols as precursor and dodecylamine as structure-directing template. The morphology and structure of the nanotubes were characterized by SEM, TEM, XRD, TG-DTA and FTIR. The experimental results reveal that the duration of the hydrothermal treatment is of importance for obtaining Vox-NTs which have a layered structure. TG-DTA study indicates that V5+ cations in nanotubes are partially reduced to V4+ cations. The results from FTIR spectra indicate the difference in V-O vibrations between before and after hydrothermal treatment. From the results, it suggests that during hydrothermal treatment, the rearrangement of the vanadium oxide structure leads to the formation of VOx nanotubes from lamellar structure because of the presence of V4+ species.     

Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd²⁺ with Pb²⁺ ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.     

Hydrothermal synthesis of CeO2 nano-particles

Nano-crystalline particles of CeO₂ have been synthesized via a low temperature hydrothermal synthesis process. Two types of precursors were studied—cerium hydroxide and ceria acetate. The precursors were adjusted to a basic (pH 10) and acidic (pH 4) medium before hydrothermal treatment at various durations of 6, 12, 18, and 24 h at 250 °C using a Teflon-lined hydrothermal bomb. The synthesized samples were characterized using DTA/TGA, XRD and TEM. Based on the characterization results, both precursor systems produced crystalline ceria nano-particles after 6 h of hydrothermal synthesis at 250 °C. The average crystallite sizes were 6 and 15 nm for the hydroxide and acetate system, respectively. The acetate precursor system appeared to produce better particles in terms of crystallinity and morphology. Based on the DTA/TGA analysis, hydrothermal synthesis had been effective in reducing the amount of intermediate products. With increasing hydrothermal treatment duration of up to 24 h, the samples did not exhibit a remarkable improvement in properties. The synthesized nano-particles were subsequently heat treated at 500 and 1000 °C for 2 h. After the heat treatment, enhanced crystallinity and growth in crystallite size was observed, but particles appeared more agglomerated.     

预处理气氛对铁离子掺杂的氧化钛纳米管微结构和光催化活性的影响

本文通过在空气和还原性气氛中煅烧铁离子掺杂的锐铁矿纳米粉体,并且采用水热合成法制备了具有锐铁矿结构的纳米管,研究了它们的微结构和物理化学行为。研究发现,与在空气中煅烧相比,还原性气氛下煅烧引入了低价态Fe₂₊和Ti₃₊离子以及更多的表面吸附氧,纳米管的比表面积、亚甲基蓝吸附能力以及光吸收阈值得到显著提高。1 mol% Fe 掺杂以及还原处理产生了最高的吸附和光催化活性及其降解持久性,过多掺杂反而降低了光催化性能。此外,水热合成引起纳米管的含铁量下降。     

Photoluminescence properties and synthesis of a PZT mesostructure obtained by the microwave-assisted hydrothermal method

Micro-cube-shaped lead zirconate titanate was synthesized using the microwave-assisted hydrothermal method. Photoluminescence and field emission scanning electron microscopy were used for monitoring the formation of mesocrystals. Based on these results, a growth mechanism was then proposed which involved nanoparticle aggregation, nanoplate self-assembly on specific architecture and the final formation of mesoscopic micro-cube-shaped lead zirconate titanate.     

Formation of ZnO Nanotubes from Zn/ZnO cables by thermal evaporation

Various types of nanostructures were synthesized by the simple thermal evaporation of ZnO powders at 1300 °C. Three types of nanostructure were formed as the substrate temperature increased from 100 °C to 300 °C: Zn-core/ZnO-shell nanocables (120 °C to 150 °C), Zn-ZnO core-shell nanocables connected to mesoporous ZnO (200 °C to 260 °C), and ZnO nanotubes (260 °C to 300 °C). The formation process of the ZnO nanotubes, which were formed at the highest temperature (260 °C to 300 °C), involved the solidification of liquid Zn droplets, surface oxidation, and the sublimation of the Zn. This result was demonstrated experimentally as well as via microstructural analysis using XRD, field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM) equipped with an energy dispersive X-ray spectrometer (EDS).