室温氧化还原反应制备AgCuSe三元纳米棒

在室温下通过氧化还原反应制备了AgCuSe三元纳米棒.用X射线粉末衍射、透射电镜和X射线光电子能谱对产物进行了表征.X射线粉末衍射结果表明,产物是四方相AgCuSe;透射电镜结果表明,产物是纳米棒,其直径为5～20nm,长度为200～600nm;X射线光电子能谱结果表明,产物的纯度是很高的,没有单质Ag、Cu等杂质.应用化学热力学原理讨论了产物AgCuSe的生成机理.热力学计算表明,在这个反应体系中最终产物是纯AgCuSe.溶剂乙二胺不仅作为双齿配体与Ag+和Cu+形成稳定的配合物,而且还能溶解金属硒、增强硒的反应性,乙二胺在控制AgCuSe的成核和纳米棒的生长过程中起着重要的作用.     

微波辅助法制备纤维状NaFeS2纳米粒子及其XPS研究

常温下用微波辅助法制得了直径小于10nm的纤维状NaFeS2 三元化合物纳米粒子,并用X射线粉末衍射、透射电子显微镜、选区电子衍射和X射线光电子能谱对纳米微粒进行了表征。XPS能谱分析表明:产物中含有Na ,Fe,S三种元素,其比值为Na∶Fe∶S =1∶1 1∶1 9。探讨了纤维状NaFeS2 纳米粒子的形成机理。     

CdS纳米微粒有序组装体系的制备与结构研究

采用 LB膜技术制备了表面活性剂包埋的硫化镉纳米粒子多层膜 ,并利用傅里叶红外光谱、X射线光电子能谱、原子力显微镜和小角 X射线衍射对其结构进行了表征。结果表明制成的 Cd S纳米粒子 LB膜为准一维超晶格     

CdSe/ZnSe核-壳结构纳米粒子合成新方法

报道用“一步”合成新方法制备了CdSe/ZnSe核-壳结构的发光纳米粒子.该方法是将锌的前驱体注入表面Se富集的CdSe发光纳米粒子溶液中,通过Zn²⁺与Se共价键结合,从而在CdSe发光纳米粒子的表面形成ZnSe壳.分别通过X射线粉末衍射、光电子能谱、透射电镜、紫外-可见吸收光谱和光致发光光谱,对核-壳结构的发光纳米粒子的结构及光学性质进行了表征.结果表明,以较宽带隙的ZnSe在较窄带隙的CdSe纳米粒子表面形成的壳层有效地钝化了CdSe纳米粒子的表面缺陷,明显地提高了室温下CdSe纳米粒子的光致发光效率.X射线粉末衍射表明随着Zn²⁺的不断注入,CdSe/ZnSe的衍射峰逐渐移向ZnSe衍射峰.光电子能谱数据显示,Zn2p的双峰分别位于1020,1040eV附近,通过与体材料ZnO相比,确定为Zn²⁺的光电子发射,说明Zn是以共价键形式存在于CdSe纳米粒子的表面.透射电镜照片显示纳米粒子具有良好的单分散性,核-壳结构的发光纳米粒子直径较CdSe核的直径明显增加.     

纳米硫化锌的制备及光谱分析

采用超重力反应结晶法制备了纳米硫化锌粒子,并通过透射电子显微镜(TEM)、X射线粉末衍射仪(XRD)、X射线光电子能谱仪(XPS)、傅里叶红外光谱仪(FTIR)、紫外-可见光分光光度计(UV-Vis)和X射线能谱仪(EDX)对纳米硫化锌的形貌、结构、组成和光谱性能进行了细致分析。结果表明：超重力反应结晶法制备的纳米硫化锌粒子为球形,平均粒径为42 nm;XRD图谱表明纳米硫化锌呈现较好的闪锌矿晶型; XPS能谱表明纳米硫化锌的S(2p)的电子结合能为162.6 eV,Zn的2p_3/2,2p_1/2的电子结合能分别为1021.4, 1044.6eV。红外光谱研究表明纳米硫化锌在400～4 000cm-1范围内具有良好的红外透过率。紫外-可见光谱研究发现纳米硫化锌在200～340nm的紫外区域有较强的吸收,其禁带宽度为3.57eV。EDX能谱表明该法制备的纳米硫化锌具有较高的纯度。     

X射线光电子能谱法研究硅纳米线的能带结构

制备了氧辅助热分解法,以一氧化硅为原料,以氩气为载气,维持管内压强为1000Pa,在高温炉中于1250℃下反应5 h后得到硅纳米线。硅纳米线经5%氢氟酸水溶液处理5 min后,与1×10-3 mol·L-1的氯化金溶液中反应5 min,在硅纳米线的表面上修饰了金纳米粒子,用X射线粉末衍射表征了产物的结构,同时观察到单质硅和金的XRD图谱;用电子扫描和透射显微镜观察了产物的形貌,表明氧辅助方法可制得大量均匀的硅纳米线,修饰在硅纳米线上的金纳米点形状整齐,尺寸均匀,平均直径约8 nm;并用X射线光电子能谱分析了修饰过程中能带结构的变化。结果表明,金纳米粒子表面带负电,它在施主能级和受主能级上都有电子存在;由于氧杂质的存在,硅纳米线的费米能级移向价带顶。     

脉冲激光沉积Ag:BaTiO3纳米复合薄膜及其光学特性

在MgO(100)基片上利用脉冲激光沉积技术制备了掺有Ag纳米颗粒的BaTiO₃复合薄膜.通过X射线衍射对薄膜的结构进行了表征,利用透射电子显微镜对Ag纳米颗粒的尺寸、形态进行了观测,X射线光电子能谱结果表明Ag呈金属态.在410—500nm范围内观测到了Ag纳米颗粒引起的等离子振荡峰,随着后处理温度和Ag颗粒浓度的增加,吸收峰发生红移,并出现了双峰现象. 关键词： 金属纳米复合薄膜 激光沉积 光吸收     

脉冲激光沉积Ag:BaTiO3纳米复合薄膜及其光学特性

在MgO(100)基片上利用脉冲激光沉积技术制备了掺有Ag纳米颗粒的BaTiO3复合薄膜.通过X射线衍射对薄膜的结构进行了表征,利用透射电子显微镜对Ag纳米颗粒的尺寸、形态进行了观测,X射线光电子能谱结果表明Ag呈金属态.在410-500 nm范围内观测到了Ag纳米颗粒引起的等离子振荡峰,随着后处理温度和Ag颗粒浓度的增加,吸收峰发生红移,并出现了双峰现象.     

水溶性CdTe纳米晶的制备和发光性质的研究

在水相中以巯基乙酸作为稳定剂制备了CdTe纳米晶,用X射线粉末衍射和X射线光电子能谱对其进行了表征,用荧光光谱研究了CdTe纳米晶的生长过程,结果表明,随着回流时间的增加,CdTe半导体纳米晶的粒径和半高全宽逐渐变大,纳米晶的荧光颜色也从绿色逐渐过渡到红色.     

温和的苯热溶剂条件下GaP纳米棒的形成机理研究

采用金属Na，白磷和GaCl₃为原料，在温和的苯热溶剂条件下制备了直径为20—40nm，长度为200—500nm的GaP纳米棒和直径为20—40nm的球形颗粒.利用X射线衍射(XRD)、透射电子显微镜(TEM)和X射线光电子能谱(XPS)研究了反应条件对产物结晶性和形貌的影响.实验结果表明，当反应温度低于250℃时，产物基本上为GaP纳米棒，并随着反应温度升高，产物逐渐转化为球形纳米颗粒；当反应温度超过280℃时，产物完全为规则的球形.同时，GaP纳米棒的生长遵循SLS生长机理. 关键词： 纳米GaP 苯热 SLS生长机理     

Sonochemical synthesis of silver vanadium oxide micro/nanorods: Solvent and surfactant effects

In this investigation, a facile sonochemical route has been developed for the preparation of silver vanadium oxide (SVO) micro/nanorods by using silver salicylate and ammonium metavanadate as silver and vanadate precursor, respectively. Here, silver salicylate, [Ag(HSal)], is introduced as a new silver precursor to fabricate AgVO₃ nanorods. The effect of numerous solvents and surfactants on the morphology and sonochemical formation mechanism of AgVO₃ nanorods was studied. AgVO₃ nanorods were characterized by SEM and TEM images, XRD patterns, FT-IR, XPS, and EDS spectroscopy. SEM, TEM, and XRD results showed that AgO nanoparticles were formed onto AgVO₃ nanorods in the presence of ethanol, cyclohexanol, dimethylsulfoxide (DMSO), and acetone. By using polyethylene glycol (PEG-6000) and N,N-dimethylformamide (DMF) as organic additives, the thickness of AgVO₃ nanorods decreased.     

Green synthesis of silver nanoparticle-decorated porous reduced graphene oxide for antibacterial non-enzymatic glucose sensors

A simple and environmentally friendly approach was developed to fabricate silver nanoparticle (Ag NP)-decorated porous reduced graphene oxide (grGO) using glucose as a crosslinking and reducing agent. Physicochemical analysis, such as X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission-scanning electron microscopy (FE-SEM) were used to confirm the structural, morphological characteristics of the as-prepared samples. The electrocatalytic activity of Ag/grGO towards glucose oxidation was examined by cyclic voltammetry and amperometry. The fabricated sensor showed excellent sensitivity of 725.0 μA cm^?2 mM^?1 with a rapid response time of 11 s. Furthermore, the hybrids showed significant antibacterial activity against Escherichia coli with 99.76% antibacterial efficiency after 18 h.     

Fabrication of surface‐enhanced Raman scattering‐active ZnO/Ag composite microspheres

We show in this paper how zinc oxide (ZnO)/silver (Ag) composite microspheres can be prepared by the reduction of Ag(NH₃)₂⁺ with the reducing agent formaldehyde in aqueous solution on the surface of ZnO microspheres. During the preparation, Sn²⁺ was absorbed on the surface of ZnO microspheres for sensitization and activation, and then Ag(NH₃)₂⁺ was reduced to Ag nanoparticles by the reducing agent to obtain ZnO/Ag composite microspheres. SEM and TEM images revealed silver nanoparticles with a diameter ranging from tens to 100 nm. X‐Ray photoelectron spectra (XPS), X‐ray diffraction (XRD) patterns and UV‐vis spectra were used to characterize the structure of the ZnO/Ag composite microspheres. The origin of the surface‐enhanced Raman scattering properties was traced to the surface of the ZnO/Ag composite microspheres. The enhancement factor was estimated in detail, and the enhancement mechanism for the SERS effect was also investigated. Copyright © 2007 John Wiley & Sons, Ltd.     

Preparation of In2S3 nanopraricle by ultrasonic dispersion and its tribology property

In this paper, we describe a facile and rapid method for preparing In2S3 nanoparticles via ultrasound dispersion. This method allows us to prepare In2S3 nanoparticles from bulk indium and sulfur with ease and without using expensive agents and in a short time. The possible growing mechanism of the In2S3 nanoparticles was presented. In addition, we provide detailed characterizations including TEM, XRD, TG-DTA, and XPS to study the shape, composition and structure of In2S3 nanoparticles. We also studied the tribology property of In2S3 nanoparticles made using this novel recipe.     

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N,N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA–Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA–Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus (S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli (E. coli) by the disc diffusion susceptibility test. The HA–Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.     

掺磷TiO_2优化TiO_2/MBA/Ag三明治结构的SERS性能

本文以磷酸为磷源,通过溶胶水热法制备磷掺杂TiO_2,利用Lee和Meisel的方法制备银溶胶,以4-巯基苯甲酸(MBA)为探针分子,通过构建TiO_2/MBA/Ag三明治结构,研究磷掺杂二氧化钛对该基底表面增强拉曼(SERS)性能的提升。通过TEM、XRD、XPS、DRS和拉曼光谱图表征二氧化钛的形貌结构、化学组成、光学和拉曼性能,结果表明,制备出的磷掺杂二氧化钛为锐钛矿型纳米颗粒,粒径范围6~12nm,XPS显示磷以P~(5+)替代了Ti~(4+),形成O-P-O键掺入TiO_2的晶格中,当磷的掺杂量在1.77%时,TiO_2/MBA/Ag三明治体系具有最佳的SERS信号,这是因为适量的磷掺杂降低了TiO_2的能带间隙,丰富TiO_2的表面态,这能促进TiO_2向MBA分子的电荷转移。     

Synthesis of thiolate-protected silver nanocrystal superlattices from an organometallic precursor and formation of molecular di-<Emphasis Type="Italic">n</Emphasis>-alkyldisulfide lamellar phases

Abstract  

Silver nanocrystal superlattices (NCSs) stabilized by hexadecanethiol have been prepared through reduction of [Ag(hexadecanethiolate)] _n , formed in situ by reaction of the organometallic precursor [Ag(C₆F₅)] and hexadecanethiol. The nanostructures have been characterized by transmission electron microscopy (TEM) and X-ray diffractometry (XRD). Several reaction parameters such as solvent (anisole or toluene), reaction temperature (150 or 120 °C) or silver:thiol ratio (1:1 or 2:1) have been studied. The NCSs are formed by silver nanoparticles which sizes range from 3.7 to 5.1 nm, depending on the reaction conditions. The formation a of lamellar phase of di-n-hexadecyldisulfide by oxidation of the hexadecanethiolate ligands bonded to Ag(I) is detected by XRD.     

Fabrication and characterization of silver/titanium dioxide composite nanoparticles in ethylene glycol with alkaline solution through sonochemical process

This paper aims to study fabrication and characterization of silver/titanium oxide composite nanoparticle through sonochemical process in the presence of ethylene glycol with alkaline solution. By using ultrasonic irradiation of a mixture of silver nitrate, the dispersed TiO₂ nanoparticle in ethylene glycol associated with aqueous solution of sodium oxide yields Ag/TiO₂ composite nanoparticle with shell/core-type geometry. The powder X-ray diffraction (XRD) of the Ag/TiO₂ composites showed additional diffraction peaks corresponding to the face-centered cubic (fcc) structure of silver crystallization phase, apart from the signals from the cores of TiO₂. Transmission electron microscopy (TEM) images of Ag/TiO₂ composites, which average particle size is roughly 80 nm, reveal that the titanium oxide coated by Ag nanoparticle with a grain size of about 2–5 nm. Additionally, the formation of silver nanoparticles on TiO₂ was monitored by ultraviolet visible light spectrophotometer (UV–Vis). As measured the optical absorption spectra of as-synthesized Ag nanoparticle varying with time, the mechanism of surface formatting silver shell on the cores of TiO₂ could be explored by autocatalytic reaction; the conversion of Ag particle from silver ion is 98% for the reaction time of 1000 s; and the activity energy of synthesizing Ag nanoparticles on TiO₂ is 40 kJ/mol at temperature ranging from 5 to 25 °C. Hopefully, this preliminary investigation could be used for mass production of composite nanoparticles assisted by ultrasonic chemistry in the future.     

Preparation of ZnS nanoparticles by ultrasonic radiation method

2 S solution. ZnS nanoparticles were synthesized under ultrasonic radiation. They were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV spectrophotometry, and X-rayphotoelectron spectrometry (XPS). XRD revealed that the ZnS nanoparticles prepared have a zincblende structure. TEM observations showed that the ZnS nanoparticles are in a spherical form with an average diameter of 40 nm. XPS results proved that, for our sample, the binding energies of Zn 2p and S 2p are the same as those of bulk single-crystal, but the full widths at half maximum of the XPS peaks are larger than those of bulk single-crystal. Received: 22 September 1997/Accepted: 5 January 1998