浓硝酸处理前后多壁碳纳米管的荧光特性研究

对浓硝酸处理前后多壁碳纳米管的荧光特性进行了研究,结果发现多壁碳纳米管在浓硝酸处理前后都能产生荧光;与浓硝酸处理前相比,浓硝酸处理后的多壁碳纳米管的荧光有所增强,且荧光谱峰向短波长方向发生蓝移。碳纳米管产生的荧光与碳纳米管在其缺陷处捕获激发光的能量以及最低空轨道和最高占有轨道之间的能隙有关。多壁碳纳米管在浓硝酸处理前后都有缺陷,因而都能在其缺陷处捕获激发光能量而产生荧光;浓硝酸处理引起多壁碳纳米管的缺陷增多、捕获激发光能量增加因而荧光也随之增强。碳纳米管的最低空轨道和最高占有轨道之间的能隙随其长度减小而增大,浓硝酸处理引起多壁碳纳米管被削短导致其最低空轨道和最高占有轨道之间的能隙增大,因而引起多壁碳纳米管的荧光谱峰向短波方向蓝移。     

一种基于MEMS微硅多狭缝分光光度计

研制出了一种采用后分光技术,微硅片多狭缝进行像元分割,硅光电二极管阵列为探测器的微型分光光度计。分析了光谱带宽对测试得到的溶液吸光度线性相关性的影响,讨论了分光前后狭缝宽度与分光光度计光谱带宽之间的关系,为分光光度计前后狭缝的设计提供了理论依据。采用MEMS(微机电系统)工艺制造出了体积小、精度高、厚度薄的一体式微硅片狭缝,并将其应用于分光光度计中。采用此分光光度计对线性吸光度溶液进行测试,结果表明线性相关系数大于0.999,说明所研制的采用微硅片狭缝的分光光度计具有高度线性相关性。     

磁性碳纳米管吸附去除水中甲基橙的研究

采用高温催化裂解法制备碳纳米管,对其用浓硝酸氧化法进行纯化处理,并用化学共沉淀方法制备了磁性碳纳米管(简称磁性管)。利用场发射扫描电子显微镜对磁性管进行了表征。将磁分离技术应用于碳纳米管吸附性能研究,探索碳纳米管负载磁性颗粒后对甲基橙的吸附性能,寻找最佳实验条件,对吸附质溶液进行紫外-可见吸收光谱分析。同时,进行了磁性管的脱附和再吸附性能研究。     

Photocatalytic Degradation of Phenol over MWCNTs-TiO2 Composite Catalysts with Different Diameters

采用溶胶-凝胶法制备了不同管径的多壁碳纳米管-二氧化钛(MWCNTs-TiO₂)催化剂．应用热重分析、N₂等温吸附和BET比表面、X射线衍射、扫描电镜以及漫反射紫外可见吸收光谱等对样品进行了表征．选择光催化降解苯酚反应对光催化剂性能进行了测试,结果表明,MWCNTs-TiO₂催化剂在苯酚降解反应中表现出明显的协同效应,并分别采用表观反应速率常数、总有机碳消除和光子效率对此协同效应进行了评价     

氢在多壁碳纳米管中的吸附储存

利用巨正则系综蒙特卡罗(GCMC)的方法模拟了氢在多壁碳纳米管中的吸附,氢气分子之间、氢气分子和碳原子之间的相互作用势能采用Lennard-Jones势能模型。模拟了不同结构参数(管内径、管壁数、管壁间距)的多壁碳纳米管在77K和298K下的吸附等温线,分析了多壁碳纳米管的管内径、管壁数以及管壁间距对吸附性能的影响。模拟结果表明:多壁碳纳米管的管壁数和管壁间距对吸附性能的影响较明显;管壁数越少,管壁间距越大,其吸附性能越好;多壁碳纳米管的管内径对其吸附性能的影响甚微。     

碳纳米管及其H_2吸附体系的Raman光谱

利用紫外Raman光谱技术 ,对分别以CO和CH4为碳源、由化学催化法制备的两种多壁碳纳米管以及它们的H2 吸附体系进行Raman光谱表征 ,观测到可分别归属于类石墨结构的基频模G (1 5 80cm- 1 )和D (1 41 6cm- 1 ,缺陷诱导 ) ,以及它们的二阶和三阶组合频 2D(2 83 2cm- 1 ) ,D +G (2 996cm- 1 ) ,2G (3 1 6 0cm- 1 )和 2D +G (441 2cm- 1 )的Raman峰 ;H2在这些多壁碳纳米管上吸附有两种形式 :非解离吸附分子氢H2 (a)和解离吸附生成含氢表面物种CHX(x =3 ,2 ,1 ) ,所观测在 2 85 0 ,2 96 7和 3 95 0cm- 1 处的Raman谱峰可分别归属于表面CH2 基的对称C -H伸缩模 ,CH3基的不对称C -H伸缩模 ,以及吸附态分子氢H2 (a)的H -H伸缩模     

多壁碳纳米管/铋膜修饰电极示差脉冲溶出伏安法测定水中镉和铅

制备多壁碳纳米管/壳聚糖纳米复合物修饰玻碳电极,用于同位镀铋膜法连续测定水中镉和铅离子的含量.将多壁碳纳米管分散在壳聚糖溶液中,滴涂在玻碳电极表面制得修饰电极;在含铋的溶液中,采用示差脉冲溶出伏安法测定了镉、铅离子的浓度;考察了沉积电位、富集时间对溶出电流的影响.在优化的实验条件下,对浓度在0-0.2μmol/L范围内...     

季铵盐改性四钛酸钾晶须及其吸附性能

通过季铵盐改性四钛酸钾晶须,应用X射线衍射分析、红外光谱,紫外-可见漫反射光谱对改性前后的四钛酸钾晶须进行表征,并初步研究了不同季铵盐改性的四钛酸钾晶须对苯酚吸附性能的研究。实验结果表明,改性前后的四钛酸钾晶须在紫外光区均有较强的光吸收,而在可见光区其吸收则较弱。改性前后四钛酸钾晶须的结构没有改变,季铵盐能够进入层状化合物的层板间,使改性后的层间距稍微增大。与改性前相比,改性后的四钛酸钾晶须对苯酚的吸附量和吸附率有了明显的提高。     

热丝和射频等离子体化学气相沉积法制备定向碳纳米管薄膜

采用热丝和射频等离子体复合化学气相沉积设备(PE-HF-CVD),以CH4、H2和N2为反应气体.在较低衬底温度下(500℃),用简单的催化剂制备方法--旋涂法在硅片上涂覆Ni(NO3)2溶液,经热处理及H2还原后的Ni颗粒为催化剂,在硅衬底上制备出了垂直于硅片且定向生长的碳纳米管薄膜.扫描电子显微镜(SEM)和透射电子显微镜(TEM)结果显示,1 mol/l的硝酸镍溶液旋涂硅片所得催化剂制得的碳纳米管管径为30～50 nm,长度超过4μm,定向性好.并用拉曼光谱(Raman)对不同摩尔浓度Ni(NO3)2溶液条件下制备的碳纳米管薄膜样品进行了表征.     

纳米银粒子对表面吸附罗丹明B的光谱学性质的影响及电解质效应研究

基于贵金属纳米粒子的局域场增强效应,利用透射电子显微镜、紫外-可见分光光度计和荧光分光光度计等分析手段研究了纳米银粒子对表面吸附罗丹明B的光谱学性质的影响以及罗丹明B-纳米银体系中加入电解质离子后,电解质离子与纳米银、染料分子间的相互关系和作用.研究结果表明,当罗丹明B溶液的浓度小于0.6μmol·L-1时,微量纳米银...     

Functional and unmodified MWNTs for delivery of the water-insoluble drug Carvedilol - A drug-loading mechanism

The purpose of this study was to develop carboxyl multi-wall carbon nanotubes (MWNTs) and unmodified MWNTs loaded with a poorly water-soluble drug, intended to improve the drug loading capacity, dissolubility and study the drug-loading mechanism. MWNTs were modified with a carboxyl group through the acid treatment. MWNTs as well as the resulting functionalized MWNTs were investigated as scaffold for loading the model drug, Carvedilol (CAR), using three different methods (the fusion method, the incipient wetness impregnation method, and the solvent method). The effects of different pore size, specific surface area and physical state were systematically studied using scanning electron microscopy (SEM), thermogravimetric analysis (TGA), Fourier transformation infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), nitrogen adsorption, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The functional MWNTs allowed a higher drug loading than the unmodified preparations. The methods used to load the drug had a marked effect on the drug-loading, dissolution, and physical state of the drug as well as its distribution. In addition, the solubility of the drug was increased when carried by both MWNTs and functional MWNTs, and this might help to improve the bioavailability.     

L-天冬氨酸在银胶体中吸附状态的表面增强拉曼光谱研究

利用表面增强拉曼光谱 (Surface EnhancedRamanScattering,SERS)研究了L 天冬氨酸在银溶胶体中的吸附状态及其浓度变化对表面增强拉曼散射效应的影响 ,并探讨了L 天冬氨酸在银溶胶表面的吸附作用特点和规律。实验结果表明 ,L 天冬氨酸在银溶胶中有明显的SERS信号 ,经过分析表明 ,该化合物能够吸附在银表面 ,这种吸附是通过羧基和氨基中的氮原子与银结合来实现的 ,L 天冬氨酸分子中带有负电荷的羧基和氨基中带有孤对电子的氮原子都能与银原子配位 ,其中羧基在银表面的增强为电荷转移机制增强 ,具有化学吸附的特征 ;氨基在银表面的增强为电磁场增强机制 ,为物理吸附。而且SERS强度随着L 天冬氨酸浓度的变化而改变 ,当其浓度为 10 - 3mol·L- 1 时增强效果较好 ,当浓度降低 ,增强作用也逐步变弱     

Fabrication of multiwalled carbon nanotubes in the channels of iron loaded three dimensional mesoporous material by catalytic chemical vapour deposition technique

The growth of multiwalled carbon nanotubes (MWNTs) was successfully achieved in the channels of three dimensional (3D) iron loaded mesoporous matrices (KIT-6) by employing catalytic chemical vapour deposition (CCVD) technique. The synthesised MWNTs, which were characterised by SEM, TEM and Raman spectroscopy, consist of thick graphene layers of about 10 nm composed of 29 graphene sheets with inner and outer diameter of ∼17 nm and ∼37 nm, respectively. The Raman spectrum showed the formation of well-graphitised MWNTs with significantly higher I_G/I_D ratio of 1.47 compared to commercial MWNTs. Comparatively, 2 wt% Fe loaded KIT-6 material produced a better yield of 91%, which is also highest compared with the report of MWNTs synthesis using mesoporous materials reported so far.     

Ultrasound promoted regioselective nitration of phenols using dilute nitric acid in the presence of phase transfer catalyst

Phenols are selectively nitrated to o-nitrophenol along with rate enhancement using dilute nitric acid (6 wt%)/tetra butyl ammonium bromide (TBAB) under sonication. The selectivity can also be reversed to p-nitrophenol using NaBr as a catalyst. Kinetic analysis of nitration of phenol both with and without sonication has been investigated by variation of reaction parameters such as catalyst, nitric acid and substrate concentration.     

Enhanced mechanical properties and morphological characterizations of poly(vinyl alcohol)-carbon nanotube composite films

Tensile tests were carried out on free-standing composite films of poly(vinyl alcohol) (PVA) and multiwall carbon nanotubes (MWNTs) for different loading levels. Results show that overall mechanical properties of the composite were greatly improved as compared to the neat PVA film. For PVA-based materials at significant high loading level such as 9.1 wt.% MWNTs, considerable increases in Young's modulus, tensile strength and toughness by factors of 4.5, 2.7 and 4.1, respectively, were achieved. Raman, SEM, TEM, and DSC techniques were used to evaluate the PVA/MWNTs composite system. Strong acid-modification of the pristine MWNTs and the subsequent ultrasonication processing allowed good distribution of the nanotubes in the matrix. SEM together with DSC result shows apparent good wetting of the nanotubes by the PVA matrix, which are supportive of good interfacial bonding between the modified carbon nanotubes and the hosting polymer matrix.     

Electrical properties of boron-doped MWNTs synthesized by hot-filament chemical vapor deposition

We have synthesized a large amount of boron-doped multiwalled carbon nanotubes (MWNTs) by hot-filament chemical vapor deposition. The synthesis was carried out in a flask using a methanol solution of boric acid as a source material. The scanning electron microscopy, transmission electron microscopy, and micro-Raman spectroscopy were performed to evaluate the structural properties of the obtained MWNTs. In order to evaluate the electrical properties, temperature dependence of resistivity was measured in an individual MWNTs with four metal electrodes. The Raman shifts suggest carrier injection into the boron-doped MWNTs, but the resistivity of the MWNTs was high and increased strongly with decreasing temperature. Defects induced by the plasma may cause this enhanced resistivity.     

Amino Functionalization of MWNTs and Their Effect on ILSS of Hybrid Nanocomposites

Multi-walled carbon nanotubes (MWNT) were oxidized by treatment with a mixture of sulfuric and nitric acids to introduce carboxyl groups on their surfaces. Triethylene tetraamine (TETA) was then grafted onto the oxidized MWNTs via a thionyl chloride route to obtain the amino-functionalized MWNTs (f-MWNT). The presence of amino functional groups on the MWNTs was confirmed using FT-IR, and scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to compare the morphology of pristine MWNT (p-MWNT) and f-MWNT. Both the p-MWNT and f-MWNT were dispersed in epoxy resin using ultrasonic agitation and the suspensions were injected into E-glass fiber woven fabric using a specialized vacuum assisted resin transfer molding (VARTM) process in which a flow flooding chamber (FFC) was used to re-direct the suspension flow. Control samples were fabricated using the same E-glass fiber mat and unmodified epoxy resin following the same procedure. Compression shear testing (CST) was performed on all the manufactured samples to determine their Inter laminar shear strength (ILSS). Results show 41% increase in ILSS for hybrid composites containing p-MWNTs and a 61% increase for samples containing f-MWNTs relative to the control samples without MWCNT.     

Environmentally superior cleaning of diatom frustules using sono-Fenton process: Facile fabrication of nanoporous silica with homogeneous morphology and controlled size

Existing techniques for the preparation of silica structures from diatom cells include cleaning of frustules through baking at high temperature and oxidant cleaning using concentrated sulfuric acid, hydrogen peroxide, nitric acid, or sodium dodecyl sulfate (SDS)/ethylenediaminetetraacetic acid (EDTA). In this study, sono-Fenton (SF) process was examined to prepare nanoporous silica through cleaning diatom frustules, while preserving their structural features. Single colonies of Cyclotella sp. were cultivated in batch mode f/2-enriched seawater. Combination of Fenton process with ultrasonication was found to be more efficient than the sum of individual processes in the removal of organic compounds from Cyclotella sp. structure. The optimized amounts of operational parameters were determined as suspension pH of 3, diatom cell density of 4.8 × 10⁵ cell mL⁻¹, H₂O₂ concentration of 60 mM, Fe²⁺ concentration of 15 mM, ultrasound irradiation power of 400 W and the temperature of 45 °C. The results of energy-dispersive X-ray spectroscopy (EDX) and thermal gravimetry (TG) analyses proved that organic materials covering the cell wall were significantly removed from the frustules through SF process. Scanning electron microscopy (SEM) images showed that after SF treatment, silica nanostructures were produced having uniform pores less than 15 nm in diameter. N₂ adsorption–desorption isotherms demonstrated that almost non-porous structure of diatom frustules became mesoporous during removing the organic matrix. Lipids, amino acids, carbohydrates and organic acids or their oxidized products were identified using GC–MS analysis as the main organic compounds released from diatom cells to the solution after SF treatment. Treated frustules exhibited adsorption capability of 91.2 mg/g for Methylene Blue, which was almost 2.5 times higher than that of untreated frustules (34.8 mg/g).     

Comparative study on modification of multi-walled carbon nanotubes by a hydrophilic polymer with different approaches

The multi-walled carbon nanotubes (MWNTs) modified by a hydrophilic polymer were prepared with polymerization and blending approaches. The differences of both modified MWNTs were compared by Fourier transform infrared and Raman spectroscopies, thermogravimetric analysis and transmission electron microscopy. Chemical grafting reaction had occurred between MWNTs and polyvinyl pyrrolidone (PVP) after modification with polymerization and blending approaches. Polymerization modification can graft more PVP on the surface of MWNTs compared with blending modification. Polymerization modification of MWNTs belongs to the “grafting from” mechanism, while blending modification belongs to the “grafting to” mechanism. Modified MWNTs exhibit remarkable solubility in water, ethanol and dimethyl formamide.