Microwave-Assisted Heating Method for the Decoration of Carbon Nanotubes with Zinc Sulfide Nanoparticles

This study focuses on in situ synthesis of ZnS nanoparticles on the surface of multiwalled carbon nanotubes. By microwave-assisted chemical reaction of Zn(Ac)₂·2H₂O and NaS·9H₂O in glycol solution with carbon nanotubes, which were pretreated by oxidization in concentrated HNO₃. Zinc sulfide crystallite densely supported on carbon nanotubes with the diameter about 1 nm. The carbon nanotubes decorated by ZnS were characterized using transmission electron microscopy and x-ray diffraction. It is found that the multi-walled carbon nanotubes can not only act as a substrate but also change the crystal structures of ZnS in the reaction.     

紫外线辐照制备单分散ZnS纳米颗粒

以硫代硫酸钠和乙酸锌为反应物、柠檬酸为调控剂,在紫外光辐照下制备出单分散的ZnS纳米颗粒。采用XRD、TEM、低温氮吸附-脱附、HRTEM和EDS等方法研究了反应物浓度、辐照时间和柠檬酸用量等因素对产物颗粒尺寸和分布的影响。结果表明,随着反应时间延长,产物收率增高,平均晶粒度增大,比表面积变小。反应物浓度对产物组成和比表面积有较大影响,但对产物的平均晶粒度影响不大。适量添加柠檬酸,有利于制备单分散的ZnS纳米颗粒。     

片状Co9S8/ZnS/C复合材料的制备及电催化产氧性能

以六水合硝酸钴[Co(NO_3)_2·6H_2O]为钴源、六水合硝酸锌[Zn(NO_3)_2·6H_2O]为锌源、2,2′-硫代二乙酸(C4H6O4S)为硫源,采用溶剂热法制备出了片状的Co_9S_8/ZnS/C复合材料。采用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和N_2吸附/脱附测试等手段对于片状Co_9S_8/ZnS/C复合材料结构和形貌等进行表征,同时对片状Co_9S_8/ZnS/C复合材料进行了电催化产氧性能测试。结果表明:片状Co_9S_8/ZnS/C复合材料的起始过电位为390 mV,塔菲尔斜率为144 mV·dec~(-1),具有高的电催化产氧性能。     

室温一步固相反应合成纳米氧化锌的表征、光催化性能及动力学

以七水硫酸锌、氢氧化钠为原料,采用室温一步固相反应合成ZnO纳米粒子,并分别利用X射线衍射分析（XRD）、傅里叶变换红外光谱分析（FTIR）、热重分析（TG）、扫描电子显微分析（SEM）、透射电子显微分析（TEM）、N₂吸附-脱附、紫外可见漫反射光谱分析（UV-Vis DRS）等方法对ZnO纳米粒子进行表征。实验结果表明：不需任何添加剂,室温下可通过一步固相反应合成ZnO纳米粒子,其形成过程首先是ZnSO₄·7H₂O和NaOH充分接触,然后反应形成Zn₄SO₄（OH）₆·5H₂O,最后NaOH的溶解热可使Zn₄SO₄（OH）₆·5H₂O转变为ZnO并逐渐长大形成纳米粒子。同时以甲基橙为降解对象评价了ZnO纳米粒子的光催化活性,实验结果表明：紫外光照射下,该方法合成的ZnO纳米粒子对甲基橙具有较好的光催化活性,且光催化动力学方程符合准一级反应动力学。     

Selective Synthesis of a Hexagonal Co(Ⅱ)-Substituted Sodium Zincophosphate via a Simple and Novel Route

A simple and novel route was provided for the preparation of the hexagonal Co(II)‐substituted sodium zincophosphate (CoZnPO‐HEX), which was obtained with ZnSO₄·7H₂O, CoCl₂·6H₂O and Na₃PO₄·12H₂O as raw materials and polyethylene glycol‐400 (PEG‐400) as a surfactant via a one‐step solid‐state reaction at low heating temperature (60°C), and characterized with X‐ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), diffuse reflectance spectra, thermogravimetric analysis and the 1st derivative of thermogravimetric analysis (TG/DTG) and transmission electron microscopy (TEM). The experimental results showed that the CoZnPO‐HEX was selectively formed via this reaction at ambient temperature in the presence of PEG‐400.     

Oriented-aggregation of organic organization: Morphology-controllable synthesis,surface photovoltage spectroscopy and morphology-dependent optical property

Assembled ZnQ₂·2H₂O microstructures, such as microsheet, sandwich-like structure and hexangular microflake, have been successfully prepared in CTAB microemulsion system through the stacking of ZnQ₂·2H₂O molecules and oriented aggregation of ZnQ₂·2H₂O original building blocks. Controlled experiments demonstrated that the morphologies of building block and final product could be readily tuned by reaction parameters, and a formation mechanism, involving re-precipitation, growth and oriented aggregation process, has been proposed on the basis of time-dependent experimental results. The obtained products were carefully characterized by X-ray powder diffraction (XRD), thermal gravimetric analysis (TGA), transmission electron microscope (TEM), field-emission scanning electron microscope (FESEM), FT-IR spectrum, UV–vis spectrum and photoluminescence (PL) spectrum. The surface photovoltage (SPV) of the obtained ZnQ₂·2H₂O microstructures was investigated by means of surface photovoltage spectroscopy (SPS) and field-induced surface photovoltage spectroscopy (FISPS). The SPS and FISPS revealed that the photogenerated charges of ZnQ₂·2H₂O could be separated distinctly and ZnQ₂·2H₂O possessed p-type semiconductor characteristics, respectively. Furthermore, UV–vis and PL spectra evidenced the optical properties of ZnQ₂·2H₂O were sensitive to its microstructure or morphology.     

Preparation, characterization, and catalytic activity of rare earth metal oxide nanoparticles

In present study, a series of rare earth metal oxide (CeO₂, Pr₂O₃, and Nd₂O₃) nanoparticles have been prepared by sol–gel route using Ce(NO₃)₃·6H₂O, Pr(NO₃)₃·6H₂O and Nd(NO₃)₃·6H₂O, and citric acid as precursor materials. Powder X-ray diffraction, scanning electron microscopy, and transmission electron microscopy are employed to characterize the size and morphology of the nano oxide particles. The particles are spherical in shape and the average particle size is of the order of 11–30 nm. Their catalytic activity was measured on the thermal decomposition of ammonium perchlorate and composite solid propellants (CSPs) by thermogravimetry (TG), TG coupled with differential thermal analysis (TG–DTA), and ignition delay measurements. The ignition delays and activation energies are found to decrease when rare earth metal oxide nanoparticles were incorporated in the system. Addition of metal oxide nanoparticles to AP led to shifting of the high temperature decomposition peak toward lower temperature and the burning rate of CSPs was also found to enhance. However, E _a activation energy for decomposition was also found to decrease with each catalyst.     

Synthesis,structural characterization and reactivity of manganese tungstate nanoparticles in the oxidative degradation of methylene blue

Nanoparticles of manganese tungstate (MnWO₄) were prepared via an impregnation method using Mn(NO₃)₂·4H₂O and WO₃ as a source of Mn and W, respectively. The morphology of the manganese tungstate nanoparticles was studied in detail by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). MnWO₄ nanoparticles showed severe catalytic performances for the degradation of organic dye (methylene blue, MB) in the presence of tert-butyl hydrogen peroxide, TBHP, as the oxidant at room temperature in water.     

A tetragonal polymorph of caesium hydroxide monohydrate,CsOH·H2O,from X‐ray powder data

Tetragonal caesium hydro­xide monohydrate, CsOH·H₂O, a clathrate hydrate, is a polymorph of three known hexagonal or pseudo‐hexagonal modifications. It was obtained as a by‐product in a high‐pressure experiment. Whether it is a high‐pressure polymorph, however, remains to be verified. The Cs atoms are situated in cavities of the form of a bicapped pentagonal prism, within an infinite three‐dimensional hydrogen‐bonded oxy­gen framework that is locally identical to layers found in the hexagonal modifications. The Cs atom and one of the two H atoms are at sites with symmetry, the O atom has mm site symmetry and the second H atom has 2/m symmetry.     

In situ and one-step synthesis of hydrophobic zinc borate nanoplatelets

The polycrystalline and hydrophobic zinc borate (Zn₂B₆O₁₁·3H₂O) nanoplatelets were in situ successfully synthesized via one-step precipitation reaction in aqueous solution of Na₂B₄O₇·10H₂O and ZnSO₄·7H₂O with oleic acid as the modifying agent. The microstructures and morphology of the as-obtained samples were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) equipped with an energy-dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Measurements of the relative water contact angle and the active ratio indicated that Zn₂B₆O₁₁·3H₂O samples were hydrophobic. It had been found that the as-prepared materials displayed nanoplatelet morphology with average diameters 100–500 nm and thickness 30 ± 5 nm and the morphology and size of the samples were controlled effectively.     

Chlorination as a means for changing the composition of iron-containing nanoparticles in a polyethylene matrix

Mössbauer spectroscopy, X-ray powder diffraction, and transmission electron microscopy were used to study the reactions of Fe₃O₄ or FeCl₂ · 4H₂O nanoparticles stabilized in a polyethylene (HPPE) matrix with gaseous chlorine and hydrogen chloride. These reactions produce FeCl₂ · 2H₂O nanoparticles, which retain the particle size and distribution over the HPPE matrix intrinsic to precursor nanoparticles. We propose chemical modification of iron-containing nanomaterials as a means for manufacturing iron(II) chloride nanoparticles.     

S/Cd物质的量比对微波水热制备CdS微晶的形貌影响及光学性能研究

采用微波水热法,以CdCl2·H2O和Na2S2O3·5H2O为镉源和硫源,在不同的S/Cd物质的量比条件下合成了CdS微晶。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FE-SEM)、EDS、透射电子显微镜(TEM)等对样品的物相、形貌和元素组分进行了分析。结果表明:随着S/Cd物质的量比的增大,产物CdS的形貌发生规律性变化,由四面体结构逐渐转变为准球形结构;准球形结构具有分级结构,是由更小的纳米晶组装而成;光致发光性质研究结果表明,所得的CdS微晶具有较好的蓝光发射性能。     

微波诱导燃烧法合成类花状ZnO纳米材料及其晶体结构、荧光性质研究

以硝酸锌[Zn(NO3)2.6H2O]和尿素[CO(NH2)2]作前驱体,通过微波诱导燃烧技术可控合成具有不同形貌的ZnO纳米晶体,并用热重分析和差热分析进行了研究。对各种生长条件:微波功率,辐射时间和尿素/Zn2+物质的量的比对ZnO纳米晶体形貌的影响作了分析。结果表明:尿素/Zn2+物质的量的比对ZnO纳米材料的形貌具有显著影响。X衍射图表明合成的ZnO纳米结构呈六角形。傅里叶变换红外光谱图中400~500 cm-1处明显的峰为Zn-O的振动峰。ZnO纳米结构的发光光谱在366 nm的带边发射,因缺陷又由许多可见光发射峰组成。用扫描电子显微镜、透射电子显微镜、选区电子衍射研究了花状ZnO纳米结构的增长机理。本方法仅需几分钟就获得的了ZnO纳米结构。     

Novel Nonenzymatic Hydrogen Peroxide Sensor Based on Ag/Cu2O Nanocomposites

The nanocomposites of Ag nanoparticles supported on Cu₂O were prepared and used for fabricating a novel nonenzymatic H₂O₂ sensor. The morphology and composition of the nanocomposites were characterized using the scanning electron microscope (SEM), transmission electron microscope (TEM), energy‐dispersive X‐ray spectrum (EDX) and X‐ray diffraction spectrum (XRD). The electrochemical investigations indicate that the sensor possesses an excellent performance toward H₂O₂. The linear range is estimated to be from 2.0 μM to 13.0 mM with a sensitivity of 88.9 μA mM^?1 cm^?2, a response time of 3 s and a low detection limit of 0.7 μM at a signal‐to‐noise ratio of 3. Additionally, the sensor exhibits good anti‐interference.     

Synthesis and Characterization of H3PW12O40 and H3PMo12O40 Nanoparticles by a Simple Method

In this study H₃PW₁₂O₄₀·9H₂O and H₃PMo₁₂O₄₀·6H₂O (HPA) particles were changed into nano forms by heat-treatment in an autoclave as a simple, repaid, inexpensive and one step method. The particle size of these nanoparticles was around 25 nm. The as-synthesized nanostructures were characterized by dynamic light scattering, X-ray powder diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and inductively coupled plasma analyzer. Thermal stability of nanoparticles was surveyed by thermal gravimeter analyse. Acidity of prepared nanoparticles was investigated by pyridine adsorption method. Results showed rising acidity by declining particle size of HPA.     

Effect of CaO additive on sintering and crystallization behavior of cordierite glass–ceramic prepared by sol–gel method

In the present work, cordierite glass–ceramic was prepared via sol–gel method using TEOS, AlCl₃·6H₂O, MgCl₂·6H₂O as starting materials. Different steps of phase transformations to cordierite have been studied by DSC and XRD. Various phases have been formed at different heat-treatment temperatures. Addition of CaO led to an increase in both the formation rate and the intensity of α-cordierite. Sinterability of the samples was determined too. The results showed that high content of CaO improved sintering. Morphology of hexagonal prism for α-cordierite was displayed by SEM.     

Influence of Microwave Synthesis Parameters on the Size and Morphology of the Resulting MgAl2O4 Nanoparticles

In the present study, Nano-sized magnesium aluminate powders were successfully synthesized via microwave process based on the reaction between Mg (NO₃)₂·6H₂O and Al (NO₃)₃·9H₂O in distilled water, at various conditions. The products were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, photoluminescence (PL) spectroscopy, and EDAX analysis. The effects of different parameters such as reaction time and microwave power on the morphology, particle size, and PL properties of the product were studied by SEM images and the PL.     

Different morphologies of ZnO nanostructures via polymeric complex sol–gel method: synthesis and characterization

Various morphologies of ZnO nanostructures, such as nanoparticles, nanorods and nanoflowers have been achieved controllably by polymeric sol–gel method. In this approach, zinc nitrate Zn(NO₃)₂·6H₂O, citric acid and ethylene glycol were used as the source of Zn²⁺, the chelating agent and the solvent agent, respectively. The microstructure of the ZnO nanostructures was characterized by X-ray diffractometry, scanning electron microscopy with the energy dispersive X-ray spectroscopy, transmission electron microscopy, thermogravimetric analysis and Fourier transform infrared spectroscopy. The effect of ethylene glycol to citric acid mole ratio on the morphology and structure of the products was discussed. The ZnO nanoparticles with diameter between 24 ± 2 nm was obtained with EG:CA mole ratio equal to 2:1. The optical properties of as-obtained power were investigated by ultraviolet–visible spectroscopy.     

Immobilization of cerium (IV) and erbium (III) in mesoporous MCM‐41: Two novel and highly active heterogeneous catalysts for the synthesis of 5‐substituted tetrazoles,and chemo‐ and homoselective oxidation of sulfides

Two well‐ordered 2D ‐ hexagonal cerium (IV) and erbium (III) embedded functionalized mesoporous MCM ‐ 41(MCM‐41@Serine/Ce and MCM ‐ 41@Serine/Er) have been developed via functionalization of mesoporous MCM ‐ 41. The surface modification method has been used in the preparation of serine‐grafted MCM ‐ 41 and led to the development of MCM‐41@Serine. The reaction of MCM‐41@Serine with Ce (NH₄)₂(NO₃)₆·2H₂O or ErCl₃·6H₂O in ethanol under reflux led to the organization of MCM‐41@Serine/Ce and MCM‐41@Serine/Er catalysts. The structures of these catalysts were determined using scanning electron microscopy, mapping, energy‐dispersive X‐ray spectroscopy, Fourier transform‐infrared, thermogravimetric analysis, X‐ray diffraction, inductively coupled plasma, and Brunauer–Emmett–Teller analysis. These MCM‐41@Serine/Ce and MCM‐41@Serine/Er catalysts show outstanding catalytic performance in sulfides oxidation and synthesis of 5‐substituted tetrazoles. These catalysts can be recycled for seven repeated reaction runs without showing a considerable decrease in catalytic performance.     

Controlled modification of multi-walled carbon nanotubes with CuO,Cu2O and Cu nanoparticles

Multi-walled carbon nanotubes (MWNTs) have been successfully modified with CuO, Cu₂O and Cu nanoparticles via a simple method, and the calcination temperature, the amount of NH₃·H₂O and soaking time play critical roles in controlling the final products. The modified MWNTs have been characterized by X-ray diffraction, infrared spectrum, scanning electron and transmission electron microscopies. Optical absorption of the obtained products has also been investigated, and the quantum confinement effect was illustrated in the absorption spectra.