ZnO/ZnS复合材料的制备、表征及其光学性能研究

通过简便的两步水热法成功合成了ZnO/ZnS复合材料,通过X射线衍射(XRD)、扫描电镜(SEM)、透射电子显微镜(TEM)、荧光光谱(FTR)和紫外-可见分光光度计(UV-vis)对所得产物进行表征.结果表明:复合物由大量针状的六方纤锌矿氧化锌结构和立方相硫化锌纳米粒子组成,并且ZnS纳米粒子成功的组装在针状ZnO纳米单体的表面,成功合成了ZnO/ZnS复合材料.光学性能研究表明,复合物ZnO/ZnS比ZnO单体表现出更为优异的光致发光性及紫外吸收性能.     

CNTs-Pt甲醛传感器和CNTs-Au葡萄糖传感器的研究

采用化学气相沉积(CVD)技术,通过CH4裂解法制备了碳纳米管(CNTs).使用旋转圆盘处理机(SDP)自组装技术,将纳米Pt和纳米Au电沉积在CNTs上对其进行修饰.随后,通过将铂粒子电化学沉积在CNTs修饰的玻碳电极(GCE)上以及利用静电效应将葡萄糖氧化酶固定在金电极上,制备了CNTs-Pt/GCE和CNTs-A...     

葡聚糖修饰的超顺磁性氧化铁纳米粒子的制备及表征

以乙酰丙酮铁为铁源,聚乙二醇为溶剂,采用高温热分解法制备了超顺磁性氧化铁纳米粒子,得到聚乙二醇修饰的超顺磁性氧化铁纳米粒子,进一步修饰葡聚糖.苯酚-浓硫酸显色法表明葡聚糖修饰在SPIONs表面,获得葡聚糖修饰的氧化铁纳米粒子.采用透射电镜、纳米粒度和Zeta电位分析仪、超导量子干涉仪和热重对产物进行检测.葡聚糖/聚乙二醇修饰的超顺磁性氧化铁纳米粒子的平均粒径为8.7±1.5 nm;水合动力学粒径33 nm,Zeta电位为13mV.葡聚糖/聚乙二醇修饰的超顺磁性氧化铁纳米粒子为超顺磁性,饱和磁化强度为21 emu/g;热重分析表明约有42wt;的葡聚糖和30wt;的PEG修饰在SPIONs表面,计算得到纯氧化铁纳米粒子的饱和磁化强度为75 emu/g.     

亲水性氧化锌纳米粒子控制合成及光学性质研究

采用溶剂热分解法,以乙酰丙酮锌为原料,在亲水性有机溶剂聚乙二醇(PEG-600)、聚乙二醇单甲醚(MPEG-1000)、三甘醇(TEG)中合成了氧化锌纳米粒子.X-射线衍射(XRD)分析表明氧化锌纳米粒子为纤锌矿晶体结构.透射电镜(TEM)形貌观察结果表明,在不同溶剂PEG-600、MPEG-1000和TEG中合成的氧化锌纳米粒子其形状分别为短棒状、颗粒状以及由小晶粒团聚而成的球状粒子.合成的氧化锌纳米粒子表面修饰有亲水性有机分子,可以稳定分散于水溶液中.紫外-可见光吸收光谱和光致发光光谱研究显示,合成的氧化锌纳米粒子具有很强的紫外带隙吸收和发光性能,表明制备的氧化锌纳米粒子结晶性好,光学性能优异.     

软模板法制备二氧化钛纳米晶及表征

以钛酸丁酯为原料,正负表面活性剂自组装形成的囊泡为软模板,制备了二氧化钛纳米晶.采用XRD,TEM,TG-DSC,SEM和EDS,XPS等对二氧化钛纳米晶的微观结构进行表征.结果表明:二氧化钛纳米晶在囊泡双层膜内部,双层膜之间和外部均有析出;150℃,450℃,500℃,750℃,830℃焙烧得到锐钛矿相和金红石相二氧化钛纳米晶,并且随温度升高,锐钛矿相二氧化钛含量先增后减,500℃焙烧产物锐钛矿相二氧化钛含量最高,950℃焙烧产物只含有金红石相二氧化钛,二氧化钛纳米粒子呈不规则五边形,尺寸在80～110 nm之间.750℃焙烧产物对活性艳红具有较好的光催化活性.     

氧化锌纳米粒子的合成及其表面功能化修饰

以三甘醇(TEG)为溶剂,高温热分解乙酰丙酮锌合成了氧化锌纳米粒子.为改善氧化锌纳米粒子表面性能和生物应用性能,分别用硅烷偶联剂(KH550)和聚酰胺-胺(PAMAM)进行表面修饰,在氧化锌纳米粒子表面接枝了-NH2活性官能团.分别采用X射线衍射仪(XRD)、透射电镜(TEM)、红外光谱(FT-IR)、X射线光电子能谱、动态光散射(DSL)和紫外可见分光光度计(UV-Vis)对样品进行了表征测试.XRD结果表明纳米氧化锌的平均晶粒尺寸为10 nm,并具有较好的结晶性.TEM观察表明,其形貌为颗粒状和小晶粒团聚成的球状粒子.FT-IR、XPS、DSL和Zeta电位测试结果表明氨基官能团成功修饰在氧化锌纳米粒子表面,增强了粒子的表面功能.UV-Vis光谱表明,氨基活性基团修饰后的纳米氧化锌仍然具有较强紫外带隙吸收.     

离子液体辅助超声法合成Zn1-xCdxS纳米粒子及光催化性能研究

以硝酸锌,氯化镉和硫代乙酰胺为原料,以离子液体的水溶液为溶剂,用超声法成功合成了Zn1-xCdxS(x=0～1)纳米粒子.用XRD,SEM,以及UV-Vis等手段对所制备样品的晶型、形貌和光学特性进行了表征;以紫外光为光源、罗丹明B为目标降解物质评价了Zn1-xCdxS纳米粒子的光催化活性.结果表明,通过调整Zn和Cd的配比可获得不同粒径的Zn1-xCdxS纳米粒子,随着x值的增大纳米粒子的吸收带边发生红移,光催化降解罗丹明B的能力变强,Zn0.25Cd0.75S拥有最高的光催化性能.对比实验表明,离子液体和超声的协同作用可获得较小粒径的纳米粒子和较强的光催化活性,这可能源于离子液体在初生纳米粒子上的吸附和超声作用下的快速成核作用.     

Al-Fe3O4体系在机械力化学过程中的物理化学变化

将纳米磁性粒子嵌入到绝缘基体中形成的磁性复合粒子,在许多方面具有重要意义.本文利用Al-Fe3O4通过机械力化学方法原位生成Fe/Al2O3 磁性复合粒子.通过对球磨不同时间的Al-Fe3O4粉末进行X射线衍射(XRD)和示差扫描量热(DSC)分析,结果表明Al-Fe3O4混合粉末通过机械力化学方法可获得Fe/Al2O3复合粒子.同时较为详细地研究了上述体系在机械力化学过程中的物理化学变化,并提出了机械力化学过程中Al-Fe3O4体系固相反应的方式.     

直接合成法制备CdSe@SiO2荧光纳米材料

以3-巯基丙基三甲氧基硅烷(MPS)为修饰剂,直接法制备得到闪锌矿结构的CdSe@SiO2核-壳型量子点,该方法简化了制备硅烷化核-壳型量子点的流程,缩短了制备的时间.用荧光分光光度计,透射电子显微镜,X射线粉末衍射仪等分析测试方法对得到的核-壳型核-壳型量子点的性能进行表征.结果表明:n(Cd2+):n(SeSO2-3)和反应体系Ph值,对纳米晶的光学性质具有显著影响.在最佳合成条件下得到的CdTe@SiO2纳米粒子的平均粒径约为20nm,其大小均匀.与CdSe纳米粒子相比,CdSe@SiO2核-壳型量子点光化学性能较稳定,常温下可以放置半年以上.SiO2包覆的CdSe纳米粒子有效地提高了核-壳型量子点的稳定性,大大增强了其抗光漂白性能.     

退火温度对CuNps@ZnO纳米复合薄膜结构与光学性能的影响

使用磁控溅射结合惰性气体冷凝的方法制备了Cu纳米粒子,通过将Cu纳米粒子沉积与ZnO离子束溅射原位复合的方法制得了CuNps@ZnO纳米复合薄膜,并研究了退火温度对CuNps@ZnO纳米粒子复合薄膜的结构和光学性能的影响.通过对样品的表征发现所得产物中存在着低温条件下难以形成的立方相、岩盐结构的ZnO.并且,样品的微观形貌、结晶性和光学性能随着退火温度的变化而发生显著地变化.     

Cadmium ions adsorption in simulated wastewater using structured alumina–silica nanoparticles

Some results on the removal of cadmium ions from simulated industrial wastewater using sol–gel structured nanoparticles of silica and alumina are presented. Two different core-shell nanoparticles were prepared: Al–Si particles (alumina core surrounded by a silica shell) with a molar composition Al:Si of 1:5, and Si–Al particles (silica core and alumina shell) with a molar composition Si:Al of 1:5. Different amounts of cadmium ions were added and the flocculation process of these particles, induced by the ions adsorption, was followed using dynamic light scattering. The efficiency of the ions adsorption was determined using atomic absorption spectroscopy. The results show that it is possible to reduce the cadmium concentration from 140 ppm to less than 5 ppb using Si–Al particles, meeting some international regulations for this contaminant (New European Directive 98-83). The Al–Si particles were not so efficient because the cadmium was only reduced from 125 ppm to less than 90 ppb. The sol–gel technique allows to synthesize model nanoparticles with different morphologies to be used as a prototypes, allowing to choose the better morphology and scaling this knowledge to an industrial level using commercially available silica and alumina nanoparticles chemically modified on the surface.     

Production and Study of Silver Nanoparticles by 532 nm Laser Pulse Ablation in NaCl Solution

In this experimental research, silver nanoparticles are produced in NaCl solution by the laser ablation method. Our aim was to investigate the effect of the amount of NaCl in the ablation medium on the characteristics of nanoparticles. A 7 ns pulsed Neodymium YAG laser (Nd:YAG) at 5 J/cm2 fluence and 532 nm wavelength was employed to produce Ag nanoparticles in distilled water with four different concentrations of NaCl. The optical properties, size distribution, and agglomeration of nanoparticles were investigated by several diagnostics. The UV–Visible absorption spectra of the Ag nanoparticles exhibit absorptions in the UV region because of surface plasmon resonance. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to study the size distribution and morphology of nanoparticles. Dynamic light scattering (DLS) was employed to measure the hydrodynamic size of nanoparticles in suspensions. With X-ray diffraction (XRD) pattern, the lattice structure of nanoparticles was studied. Fourier transform infrared (FTIR), photoluminescence (PL) spectra were obtained to observe the molecular structure and atomic energy levels of particles.     

氧化镍纳米晶体的制备及其过程分析

为了开发一种新型纳米氧化镍催化剂,能有效地应用于生物质气化过程中去除焦油,本文采用均匀沉淀法成功地制备了纳米氧化镍晶体,并利用TGA、FTIR、XRD、BET、YEM等分析手段对前驱体和产品的性能进行了表征.同时,对前驱体的分解过程进行了全面的分析.分析结果表明前驱体是水合碱式碳酸镍,其分子式为NiCO3·Ni(OH)2·nH2O,它能在360℃下完全分解转化为纳米NiO,同时煅烧条件对合成纳米NiO的晶体粒径影响很大.实验证实所得纳米NiO颗粒呈球形,分散性好,纯度较高,属立方晶系结构,平均粒径约为7.5nm,其BET表面积为187.98m2/g,这显示纳米NiO晶体具有作为高效催化材料的应用可行性.     

Ordered structures based on self-organized Au and CdSe nanoparticles

Methods for obtaining cadmium selenide and gold nanoparticles have been developed. The sizes of the nanoparticles are determined and the morphology, structure, and chemical composition of these nanoparticles and their ensembles are studied by a complex of structural methods: electron diffraction, X-ray diffraction, energy-dispersive X-ray analysis, high-resolution transmission electron microscopy, and small-angle X-ray scattering. Gold nanoparticles are mainly spherical and have an average size of 10 nm. They are single-phase and have an fcc crystal structure. Samples of synthesized CdSe nanoparticles contain monodisperse spherical particles 12 nm in size with a wurtzite structure. The deposition of nanoparticles on a carbon substrate is accompanied by their self-organization into a closely packed two-dimensional structure with a pronounced texture in which all nanoparticles are oriented in the [001] direction perpendicularly to the carbon substrate plane.     

Characterization of single phase copper selenide nanoparticles and their growth mechanism

The high quality Cu₃Se₂ phase of copper selenide nanoparticles was synthesized through the solution-phase chemical reaction between copper and selenium. In this synthesis process, hydrazine hydrate acts as reducing agent whereas ethylene glycol controls the nucleation and growth of particles. An effort has been made to explain the growth mechanism to form copper selenide nanoparticles through the coordination of selenium to the Cu²⁺ complexes with OH groups of ethylene glycol. Result indicates the formation of Cu₃Se₂ single phase nanoparticles. The particles with the average particle size 25 nm are spherical in shape having tetragonal structure. The particles are well crystallized having 94% degree of crystallinity. An effort has also been made to determine the energy band gap of copper selenide nanoparticles through the absorption spectra.     

TiOCl2溶液微波加热制备金红石型TiO2纳米粒子

本文报道了一种由TiOCl2液相直接合成金红石型TiO2纳米粒子的新方法,即微波诱导沸腾回流强迫水解法,用该法制备出常规条件下不能得到的产品.所得产物用粉末X射线衍射仪和透射电子显微镜表征,证明产物为金红石型,粒子尺寸5～30nm可控.研究表明,产物物相取决于Ti4+的初始水解速率,水解速率越快,越有利于金红石相成核;通过控制初始Ti4+的浓度,可改变纳米TiO2的粒径.另外还讨论了该金红石型TiO2纳米粒子的成核机理.     

核壳结构CdS@C纳米复合材料的光催化性能研究

采用水热碳化法成功制备了不同碳含量的CdS@C纳米颗粒,同时对CdS@C的晶体结构、形貌、光学性能、光电化学和光催化性能进行了研究。实验结果表明本方法制备的碳包覆CdS纳米颗粒外壳为碳层,内核为六方纤锌矿结构CdS颗粒。CdS@C颗粒分散性良好,颗粒形貌主要为类球形,粒度均匀。X射线光电子能谱(XPS)证实CdS@C颗粒表面负载的碳主要以非晶碳形式存在。紫外-可见光光谱(UV-Vis)表明CdS@C纳米晶中表面碳的敏化作用提高了可见光响应范围,使得能隙变窄。光致发光光谱(PL)表明碳包覆CdS@C纳米颗粒的发光强度比纯CdS弱,有效抑制了光生载流子的复合。瞬态光电流响应和电化学阻抗谱(EIS)说明CdS@C纳米复合材料更有效促进电子-空穴对分离和提高转移效率。CdS@C纳米复合材料在可见光辐射下表现出良好的光催化活性和稳定性,其中·O₂^-和h⁺在光催化中起主要作用。     

Application of a conproportionation reaction to a synthesis of shape-controlled gold nanoparticles

Synthesis of gold nanoparticles with multiple shapes by a modified seeding growth method is reported. The optical extinction spectra of a mixture of the seed and growth solutions indicate that the seed particle size decreases during stirring the mixture by a conproportionation reaction of Au metal with Au(III) ions. This conproportionation reaction is used to investigate the effects of variation in seed particle size on the resultant gold nanoparticle shape. When single crystalline and multiply twinned particles are used as the seed particles, they grow into gold nanorods and nanobipyramids, respectively. By letting the seed particles experience the conproportionation reaction before the particle growth to decrease the size, the surface of resultant nanoparticles roughens. Increasing the conproportionation reaction time up to 5 min, multi-branched gold nanoparticles with many lattice defects grow from both of the seed particles. This indicates that the conproportionation reaction is useful to generate lattice defects during the particle growth, which lead to the formation of gold nanoparticles with complex shapes.     

Optical properties of nanocomposites with iron core-iron oxide shell structure

Iron nanoparticles of diameter ∼5 nm were produced within a gel-derived silica glass by reducing a suitable gel composition. By heating these composites in the temperature range 573-973 K, Fe₃O₄ shells of a few nanometer thickness were grown around the iron nanoparticles. Three peaks were observed in the optical absorption spectra of the nanocomposites when they were dispersed in ethyl alcohol. The first one around 300 nm was caused by plasma resonance absorption of unoxidized iron particles; the second was shown to be due to the core-shell structure with different permittivities of the two regions and the third one was ascribed to a d-d transition. Detailed analyses of the second peak showed that the extracted values of electrical conductivity were below Mott’s minimum metallic conductivity for iron in the case of particles with diameters below ∼2.5 nm.     

Studying the Molecular Mechanisms of Interaction of Nanoaerosol Particles with a Model Membrane

An X-ray study of the interaction of Langmuir monolayers with nanoparticles under the conditions when nanoparticles arrive at the monolayer from the side of the air medium has been performed for the first time. Measurements by the X-ray standing-wave method and two-dimensional diffraction have made it possible to investigate the transport of nanoaerosol particles through a lipid monolayer and observe the structural changes occurring in it. Nanoaerosol particles were formed by electrohydrodynamic sputtering of desalted solutions of ferritin. It was shown that nanoaerosol particles pass through the monolayer without disrupting the two-dimensional packing of lipid molecules. The ferritin molecules penetrating the aqueous subphase after sputtering are found to be adsorbed under the monolayer.