W/O微乳液技术与纳米粒子的控制合成

分析了W／O微乳液的形成机理、结构特征以及用W／O微乳液法合成纳米粒子的基本原理。讨论了制备条件如水与表面活性剂的比值,反应物、表面活性剂、助表面活性剂的浓度以及焙烧条件对纳米粒子特征的影响。指出应该加强对纳米粒子生成反应动力学的研究,加强微乳液法与其它纳米粒子制备技术的耦合研究,并注意改善非极性溶剂和表面活性剂的回收率以降低制备成本。     

Ag/Co/Au三金属纳米粒子的合成及表征

反胶束是指由介于油和水界面的表面活性剂分子来稳定的,且均匀分散于连续油介质中的微液滴,由于微液滴的尺寸限制和其在油介质中的良好分散性,它可以作为"微反应器"合成纳米材料。以AOT为阴离子表面活性剂,采用反胶束法合成了Ag/Co/Au纳米粒子。采用紫外-可见(UV-Vis)吸收光谱、傅立叶红外光谱(FT-IR)对产物进行表征。研究结果表明,反胶束法合成Ag/Co/Au纳米粒子粒径均匀,分散性好、稳定性好。     

水包油微乳法合成氧化铝纳米粒子

为了探索绿色、无污染的微乳法合成途径,采用水包油微乳法制备了氧化铝纳米粒子。Tween-80和醇作为表面活性剂和助表面活性剂,用超纯水来代替反相微乳液中大量的有机相,既经济又环保。研究了反应温度和反应物的浓度对反应产物的影响。实验结果表明:用水包油微乳液制备的氧化铝纳米粒子粒径小、分散性好。     

溶剂热法制备Fe_3O_4纳米粒子的研究进展

四氧化三铁是一种重要的功能材料,因其具有优异的磁性能和较高的化学稳定性而被广泛应用于水体净化、磁流体和靶向药物等领域。四氧化三铁的合成方法主要有共沉淀法、热分解法、微乳液法及溶剂热法。其中,溶剂热法因流程简单、所得产物形貌多样、规整度高而得到广泛关注。该法所用的溶剂、矿化剂、表面活性剂等对Fe_3O_4纳米粒子的形貌及性能有较大影响。基于此,本文对溶剂热法制备Fe_3O_4纳米粒子进行了回顾,阐述了溶剂热法合成空心Fe_3O_4纳米粒子的机理。结果表明:在合成过程中,溶剂不仅作为还原剂,还提供合成所需的液相环境;矿化剂可促使铁前体的溶解,从而保证合成反应顺利进行;表面活性剂可与Fe_3O_4晶面作用,其种类和浓度不同,作用的晶面不同,进而诱导Fe_3O_4生长为不同形貌的纳米粒子。最后,本文对溶剂热法合成Fe_3O_4纳米粒子今后的发展趋势进行了展望,指出在空心Fe_3O_4纳米粒子的基础上,通过选择黏度较大的溶剂和表面活性剂合成多层壳状Fe_3O_4纳米粒子是研究者努力的方向。     

微乳液法制备无定形纳米二氧化硅

采用Triton X-100／正己醇／环己烷／氨水体系配制反相微乳液，在碱性条件下正硅酸乙酯在反相微乳液中发生受控水解，合成了具有无定形结构的球形二氧化硅纳米粒子。通过红外光谱（FT-IR）、X衍射（XRD）、透射电镜（TEM）分别对样品的结构及形貌尺寸进行了表征和分析。结果表明：改变表面活性剂加入量可以得到不同粒径（50～110nm）、不同粒度分布及不同分散程度的球形二氧化硅纳米粒子。随着表面活性剂在微乳液中体积分数的增大，二氧化硅纳米粒子的粒径先减小后增大，团聚程度也呈现先减小后增大的趋势。当表面活性剂在微乳液体系中的体积分数为20％时，所合成的二氧化硅纳米粒子粒径最小（50nm），粒度均匀且呈现出良好的分散性。     

纳米硫化铜的非水溶剂法合成及其光学性能研究

以无水乙醇为溶剂,SDBS为表面活性剂,采用一种便利的非水溶剂法,在常温常压下合成了硫化铜纳米球和纳米棒.实验结果表明,表面活性剂SDBS对控制产物形貌起决定作用,通过改变SDBS的量可以有效控制纳米硫化铜的形貌.对产物进行表征,XRD结果证实产物为六方晶系的硫化铜且纯度较高:TEM分析表明产物分散性好,粒径分布范围窄.利用荧光光谱仪测定室温下产物的荧光特性,发现产物具有较强的荧光效应,在可见光区域内存在两强发射峰;将产物制成CuS/PVA复合膜并测试其紫外吸收特性,结果表明纳米CuS在260 nm处有强吸收峰.     

微乳液法制备纳米氧化锌粒子

采用微乳液法制备了纳米ZnO粒子,探讨了影响纳米ZnO粒子生成的因素.结果表明,最佳工艺条件为主表面活性剂与助表面活性剂之比为3:1、煅烧温度600℃、煅烧时间3 h.并用红外光谱、透射电子显微镜(TEM)等对产物进行了表征,所制备的纳米ZnO粒子粒径为20nm左右,形貌为球型或类球型.     

乳液法制备聚合物纳米粒子的研究进展

综述了乳液法制备聚合物纳米粒子的研究进展,详细介绍了采用新型乳化剂,即高分子表面活性剂与反应性表面活性剂,和以超声波辐照技术为主的新技术制备聚合物纳米粒子方面的研究成果。     

水热合成CuS/GO纳米复合材料及光催化降解有机污染物的研究

以醋酸铜 Cu(Ac)2 和硫化钠（Na2S）以及氧化石墨烯 (GO) 为原料，去离子水作溶剂，十六烷基三甲基溴化铵 (CTMAB) 为表面活性剂，在水热条件下合成CuS/GO纳米复合材料。并对其进行了XRD，FT-IR，XPS，SEM和 TEM 表征，发现具有10~20nm左右CuS纳米粒子均匀的负载在氧化石墨烯上。CuS/GO纳米复合材料在可见光照射下对有机物四环素(TC)和罗丹明B (Rh-B)表现优异的光催化活性，在可见光照射120分钟后分别对TC和Rh-B降解速率达到63%和85%。通过-ln(C/C0) 对反应时间呈现线性关系说明样品在降解TC和Rh-B过程遵循一级动力学原理。     

表面活性剂在纳米材料制备领域的研究概况

表面活性剂是用途非常广泛的一类两亲分子,现如今已运用在纳米粒子模板,有机化学制备等诸多领域。而纳米材料的微乳液合成方法是一项日趋完善的技术,它可以用于控制许多有机和无机材料的粒子尺寸。本文将对表面活性剂,以及表面活性剂在溶液中形成的微乳液制备纳米材料的应用趋势做详细的介绍。     

Very slow formation of copper sulfide and cobalt sulfide nanoparticles in montmorillonite

Intercalation of semiconductor nanoparticles, copper sulfide or cobalt sulfide, into montmorillonite was carried out by solid–solid reactions of Cu(II)- or Co(II)-montmorillonite with sodium sulfide at room temperature. The intercalation compounds were characterized by X-ray diffraction, thermal analysis, transmission electron microscopy, Raman, UV–visible and photoluminescence spectroscopy. The photoluminescent copper sulfide and cobalt sulfide nanoparticles in the interlayer spaces formed after the sample storage at room temperature for several months.     

Chemical and morphological characterization of mesoporous material supported copper oxide nanoparticles for potential application

SBA-15 supported nano-scaled copper oxide was synthesized by impregnation method via ultrasonic-assisted route. The removal test from gas mixture containing 0.1 vol.% hydrogen sulfide was carried out over this material at atmospheric conditions. The effects of the chemical nature of copper oxide and the textural properties of the material on removal capacity were studied. The materials before and after the removal test were analyzed by nitrogen adsorption, X-ray diffraction, Transmission Electron Microscope, X-ray photoelectron Spectroscopy, Fourier Transform Infrared Spectrometer and Inductive Coupled Plasma. The results showed that copper species are located predominantly in mesopore channels, existing as copper oxide nanoparticles. Mesopores are active sites for removal reaction. The outstanding performance of hydrogen sulfide uptake capacity is attributed to a combination of the nature of the active centers and the well-proportioned distribution of active phase inside the mesoporous material.     

A short but glorious porcelain glaze of Early Ming Dynasty: New finding of raw material and colorants in the copper red glaze

Copper red glaze is considered to be Chinese unique high-temperature copper colored glaze. The sample of Hongwu underglaze red of the Ming Dynasty was analyzed by scanning electron microscopy (SEM), synchrotron radiation micro-X-ray fluorescence spectroscopy (SR-μ-XRF), synchrotron radiation micro-X-ray diffraction (SR-μ-XRD) and transmission electron microscopy (TEM), the results show that there are nano-scale metal copper particles in the diffusion layer of the glaze, and irregular copper sulfide particles at the bottom layer. The presence of metal copper nanoparticles shows the glaze red, but under the influence of black copper sulfide, the appearance of underglaze red is relatively dull and dark. It is assumed that the pigments in Hongwu underglaze red are natural copper ores due to the existence of irregular particles. Referring to the record of "Bright red clay" in ancient literatures, a mixture of cuprite and chalcopyrite are probably the raw materials, the exhaustion of which may be the main reason for the interruption of copper red glaze after the mid-Ming Dynasty.     

Synthesis,characterization, and conductivity studies of polypyrrole/copper sulfide nanocomposites

Nanocomposites of polypyrrole (PPy) containing copper sulfide (CuS) were synthesized by an in situ chemical oxidative polymerization. The nanocomposites were characterized by FTIR, SEM, XRD, DSC, TGA, and conductivity studies. The FTIR spectra ascertained the chemical interlinking of polypyrole with metal sulfide nanoparticles. Morphological analysis showed that the nanoparticles were uniformly covering the entire substrate. The XRD pattern reveals that the nanoparticle incorporated polypyrrole showed a crystalline nature and the crystallinity of the polymer increases with increase in concentration of CuS nanoparticles. From DSC, an increase in glass transition temperature shows the increased orderness in the polymer composite than in the pure polypyrrole. Thermal analysis (TGA) of the composite showed a progressive increase in the thermal stability with increase in content of CuS. The frequency dependent electrical properties (a.c. conductivity) of the nanocomposites were higher than that of polypyrrole. The d.c. electrical conductivity increased with increase in amount of nanoparticles in the polymer matrix. The results obtained for these composites have greater scientific and technological interest. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

铜铟硫纳米粒子的溶剂热合成及表征

采用溶剂热法,以二乙基二硫代氨基甲酸铜和二乙基二硫代氨基甲酸铟配合物为前体,油胺为配体,合成了铜铟硫纳米粒子。研究了配体与前体的配比、反应时间、反应温度以及添加剂对产物的影响,采用XRD、SEM等测试方法对产物进行了表征。结果表明,在配体和铜的物质的量比为5∶1,180℃反应,反应时间为8 h,能够得到具有较好的粒度和晶度的铜铟硫纳米粒子。     

Plasmon-enhanced upconversion luminescence with the hybrid structure of semiconductor-insulator-semiconductor

High-quality hexagonal NaYF₄:Er/Yb particles and monodisperse copper(I) sulfide nanoparticles (NPs) were obtained with the solvothermal method and the hot-injection method, respectively. The hybrid structure of semiconductor-insulator-semiconductor (SIS) was constructed for upconversion luminescence (UCL). The results showed that compared with that of NaYF₄:Er/Yb-SiO₂ particles, the luminous intensity of SIS was promoted by 12.5 folds, and the quantum yield of SIS can reach to 0.89%. Furthermore, the optical field distribution in the vicinity of hybrid structure of SIS was numerically simulated based on the finite-time domain-difference method (FDTD). The UCL enhancement of the SIS originates from the amplified optical field, which was attributed to the localized surface plasmon resonance (LSPR) effect of copper(I) sulfide NPs and the local effect of the copper(I) sulfide film on the excited light.     

Unconventional 0-, 1-, and 2-dimensional single-crystalline copper sulfide nanostructures

We report the synthesis of several unconventional 0-, 1- and 2-dimensional copper sulfide nanostrucutures by the chemical vapor deposition method. The key factor for morphology and structure control of a variety of copper sulfide products is the tuning of deposition and growth temperature to fit for the surface energy barriers and promote different growth directions. At a high growth temperature (480 °C) that provides enough thermal energy, a 0-D octahedral copper sulfide single crystal structure was synthesized. At a slightly lower growth temperature (460 °C), a new 1-D copper sulfide nanorod structure with a nanocrystal head was discovered for the first time. At a much lower growth temperature (150 °C), 2-D copper sulfide nanoflakes with a single crystal hexagonal structure were obtained. These novel structural varieties of copper sulfide can lead to discovering more unconventional material structures and growth mechanisms of other transitional metal chalcogenides, and may allow for new copper sulfide based devices and applications.     

Synthesis,characterization, and properties of new conducting polyaniline/copper sulfide nanocomposites

This article reports the facile synthesis of copper sulfide (CuS)/polyaniline (PANI) nanocomposites by in situ polymerization. The composites were characterized by scanning electron microscopy (SEM), UV–visible and Fourier transform infrared (FTIR) spectroscopy, X‐ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). SEM analysis showed that the metal sulfide nanoparticles were uniformly dispersed in the polymer matrix. The characteristic peaks in FTIR and UV–vis spectra of PANI were found to be shifted to higher wave numbers in PANI/CuS composite, which is attributed to the interaction of CuS nanoparticles with PANI chain. XRD pattern revealed the structurally ordered arrangement of polymer composite and this regularity increases with increase in concentration of nanoparticles. Glass transition temperature of the nanocomposite increased with increase in the concentration of nanoparticles and it indicated the ordered arrangement of the polymer composite than PANI. TGA studies indicated excellent thermal stability of polymer nanocomposite. The electrical properties of nanocomposites were studied from direct current and alternating current resistivity measurement. Conductivity, dielectric constant, and dissipation factor of the nanocomposite were significantly increased with the increase in CuS content in the nanocomposite. The enhancement of these properties suggests that the proposed PANI/CuS nanocomposites can be used as multifunctional materials for nanoelectronic devices. POLYM. ENG. SCI., 54:438–445, 2014. © 2013 Society of Plastics Engineers     

纳米硫化铁在环境保护中的应用研究进展

总结了近二十年来纳米硫化铁在环境中的应用报道,综述了纳米硫化铁的合成方法、污染物去除效果和机理以及溶液组分对材料本身和污染物去除的影响。介绍了纳米硫化铁目前在环境中主要用于重金属离子去除(如镉、汞、铀、锝等)、氯代有机物的脱氯和难降解有机物的高级氧化等过程,其对污染物的去除机理主要包括吸附、(共)沉淀、还原、催化氧化。指出虽然纳米硫化铁在污染物处理方面取得了良好的效果,但是依然存在问题,如溶液中共存的阴阳离子和腐植酸会对材料的团聚、腐蚀以及污染物的吸附行为和处理效果产生不同的影响。提出目前国内外对于纳米硫化铁材料自身性能研究尚未深入,材料在反应过程中及实际环境中的迁移、转化及其对污染物去除的影响值得深入。     

1-甲基-3丁基咪唑氯离子液体中片状硫化铜纳米结构研究

以1-甲基-3丁基咪唑氯离子液体为溶剂直接溶解氯化铜,硫化钠水溶液作为沉淀剂快速制得片状硫化铜纳米颗粒.对比实验揭示,离子液体对于片状硫化铜纳米结构的形成具有决定性的影响.UV-Vis光谱检测显示其在240到600 nm处有较宽的吸收峰.