DMF及热处理对常压制备Cu掺杂SiO2纳米复合气凝胶的影响

以正硅酸乙酯(TEOS)为硅源, 硝酸铜(Cu(NO3)2·3H2O)为铜源, 通过在复合溶胶体系中引入干燥控制化学添加剂(DCCA)N,N-二甲基甲酰胺(DMF)进行原位共溶胶-凝胶, 结合常压干燥工艺, 制备出具有高比表面积(560 m2·g-1)的Cu-SiO2纳米复合气凝胶(含铜质量分数为5%). 研究了DMF对凝胶时间、干燥过程和复合气凝胶形态结构的影响, 利用N2物理吸附, 全自动X射线衍射(XRD)仪, 傅立叶变换红外(FT-IR)光谱仪, 透射电子显微镜(TEM)等对样品的形貌结构进行了表征. 实验结果表明, DMF能有效防止凝胶的开裂, 抑制颗粒团簇的产生, 使所得复合气凝胶的粒径减小, 比表面积增加, 微观结构更趋完善. 高温热处理后, Cu-SiO2中的铜物种仍高度分散于骨架网络中, 复合气凝胶显示出良好的热稳定性.     

Novel coassembly route to Cu-SiO2 MCM-41-like mesoporous materials

A series of mesostructured Cu-SiO2 composites have been synthesized with sodium metasilicate (Na2SiO3) and cuprammonia nitrate (Cu(NH3)4(NO3)2) respectively used as Si and Cu sources. The synthetic procedures were conducted at room temperature, and cetyltrimethylammonia bromide was used as a template. Under our experimental conditions, ordered mesoporous Cu-SiO2 composites could be obtained with a copper content up to 16.8 wt %. Average pore diameters (2.80-3.15 nm), wall thickness (1.30-2.20 nm), and specific surface area (1020-690 m2/g) are found to vary linearly with copper content (0-16.8 wt %). Results of thermal gravimetry-differential thermal analysis reveal the collapse temperature of the order structure starts at approximately 1250 K for mesoporous Cu-SiO2 with 16.8 wt % copper content. As indicated by the outcomes of inductively coupled plasma and X-ray photoelectron spectroscopy studies, copper is mainly incorporated inside the pore wall rather than embedded on the wall surface. Copper species strongly interact with silica, and calcination at high temperatures cannot cause phase separation between silica and copper oxide. Cu status in mesoporous Cu-SiO2 composites is similar to that in copper silicate in neighboring structures. Based on the results, a S+ I- I+ I- mechanism is proposed in which copper entities are surrounded by silicon species during synthesis of the mesostructured composite.     

Dispersion of SiO2-based nanocomposites with high performance liquid chromatography

Core-shell structured Ag/SiO2 nanocomposite has been synthesized by a cyclohexane/Igepal/water reverse micelle system. The spherical nanocomposite particles were washed and concentrated with high performance liquid chromatography (HPLC) to remove the surfactant added during synthesis. Spherical SiO2 micrometer-scale particles were packed in the HPLC column as a stationary phase for the washing and dispersing of Ag/SiO2 nanocomposite particles. Surface modification of Ag/SiO2 nanocomposite particles and SiO2 microspheres with silane coupling agent enhanced the surface charge of the particles and improved the efficiency of washing with HPLC. Well-dispersed Ag/SiO2 stable suspensions were successfully attained in ethanol/water mixed solvents after HPLC washing. The state of dispersion for the Ag/SiO2 nanocomposite suspension was systematically assessed using dynamic light scattering (DLS) and transmission electron microscope (TEM) and spin coat/atomic force microscope (AFM) analyses. The mechanism of the enabling HPLC washing protocol for SiO2-based nanoparticles is discussed.     

Preparation and electrochemical properties of core-shell Si/SiO nanocomposite as anode material for lithium ion batteries

The Si/SiO nanocomposite was synthesized by a sol–gel method in combination with a following heat-treatment process. It was analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM), cyclic voltammetry (CV) and capacity measurement as anode material for lithium ion battery. Si nanoparticles were coated with SiO and a core-shell structured nanocomposite was formed. The core-shell Si/SiO nanocomposite displays better reversibility of lithium insertion/extraction and higher coulomb efficiency than virginal Si nanoparticles. The SiO shell envelops the Si nanoparticles to suppress the aggregation of the nanoparticles during cycling. As a result, the core-shell Si/SiO nanocomposite exhibits better capacity retention than virginal Si nanoparticles, indicating that this is a promising approach to improve the electrochemical performance of nano anode materials for lithium ion battery.     

Preparation and properties of low-cost cotton nanocomposite fabrics with in situ-generated copper nanoparticles by simple hydrothermal method

In this work, copper nanoparticles were in situ generated in cotton fabrics by simple hydrothermal method. These low-cost nanocomposite fabrics were characterized by scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction, thermogravimetric analysis, and antibacterial tests. The presence of spherical nanoparticles was visualized by SEM analysis. FTIR spectra did not show any differences between the peak positions of cotton fabrics and their nanocomposites. The crystallinity of cotton nanocomposites was enhanced by the copper nanoparticles. The cotton nanocomposite fabrics exhibited good antibacterial activity against Escherichia coli bacteria and hence can be considered for medical applications such as wound dressing, surgical aprons, hospital bed materials, etc.     

Synthesis and antibacterial property of hollow SiO2/Ag nanocomposite spheres

This paper presents a novel and facile method to fabricate hollow silica/sliver (SiO(2)/Ag) nanocomposite spheres. In this approach, the monodisperse hollow SiO(2) colloids bearing quantenary ammonium groups were prepared by dispersion polymerization combined sol-gel process and used as templates. The Ag(+) ions were first adsorbed onto the surfaces of the hollow SiO(2) beads via electrostatic interaction and then in situ reduced by the deprotonated silanol groups of the hollow SiO(2) beads, no extra reducing agents or catalysts were added during the reduction process. TEM, SEM and EDX analyses indicated that Ag nanoparticles were successfully deposited onto the surfaces of hollow SiO(2) beads. Some influencing parameters, such as the amount of quantenary ammonium groups in the inner wall of hollow SiO(2) colloids, Ag(+) ions concentration and reaction temperature, on the deposition of Ag nanoparticles onto SiO(2) colloids were investigated. Preliminary antibacterial tests indicated that these hollow nanocomposite spheres showed excellent antibacterial ability.     

In situ generation of silver nanoparticles in cellulose matrix using Azadirachta indica leaf extract as a reducing agent

In the present work, silver nanoparticles (AgNPs) were in situ generated in cellulose matrix using leaf extract of Azadirachta indica as a reducing agent. The cellulose/AgNP composite films prepared were characterized by FTIR, X-ray diffraction (XRD), scanning electron microscope, and antibacterial tests. The infrared spectra indicated the association of organic materials with silver nanoparticles to serve as capping agents. Scanning electron micrographs showed that synthesized silver nanoparticles were nearly uniform and spherical in shape with diameter in the range of 61–110?nm. XRD confirmed the formation of AgNPs and Ag–O nanoparticles. The nanocomposite films showed good antibacterial activity against Escherichia coli bacteria.     

CO2加氢合成甲醇Cu/ZrO2催化剂的失活因素

采用低温氮气吸脱附、X射线衍射(XRD)、电镜(TEM)以及热重差热(TG-DSC)等手段,对不同反应时间下Cu/ZrO₂催化剂的物理结构、微观形貌以及积炭情况进行了表征,分析了催化剂的失活原因。结果表明,造成催化剂失活的主要因素是活性组分烧结;其次,表面积炭覆盖其活性中心也造成催化剂活性在一定程度上的降低;而催化剂比表面积对其活性的影响较小。     

儿茶素-银纳米复合材料的制备及其应用

探索了以植物活性成分儿茶素作为还原剂和保护剂一步水热法合成儿茶素-银纳米复合材料,并进一步测试了纳米复合材料的抑菌活性。 紫外可见吸收光谱(UV-Vis)和红外光谱(FTIR)测定证明制备得到了儿茶素包裹的银纳米粒子。 透射电子显微镜(TEM)和X射线衍射(XRD)结果显示银纳米粒子的平均粒径为22.7 nm,并具有面心立方晶体结构。 抑菌活性实验结果表明,儿茶素-银纳米复合粒子对大肠杆菌、金黄色葡萄球菌以及白色念球菌都有很强抑制作用,尤其对白色念球菌的抑制作用最强,其最低抑制浓度(MIC)和最低杀菌浓度(MBC)分别为19.63和39.26 μg/mL。 儿茶素-银纳米粒子强抑菌活性可归因于其表面银离子的持续释放,有望应用于长效抑菌制剂产品。     

Studies on the mechanical and friction properties of polyamide 6-Cu/Si nanocomposites

Polyamide 6 nanocomposites reinforced with Cu/Si nanoparticles (PA6-Cu/Si) were prepared by the in-situ ring-opening polymerization of ?-caprolactam. The in-situ polymerization was critical for preventing the aggregation of Cu/Si nanoparticles. The Cu/Si nanoparticles in the nanocomposite retained their nano characteristics and were not oxidized by the amino groups in PA6. The structure of the as-fabricated PA6-Cu/Si nanocomposite was evaluated by transmission electron microscopy (TEM), X-ray diffraction (XRD), and ultraviolet-visible absorption spectroscopy (UV-vis). The friction and wear resistance, mechanical strength, and antistatic performance of PA6-Cu/Si were also evaluated. The PA6 polymer chains prevent the Cu/Si nanoparticles from aggregation by coating the surface of the Cu/Si nanoparticles via physical adsorption or an electrostatic effect. The mass fraction of the Cu/Si nanoparticles also had a significant effect on the crystalline form of PA6. The γ crystalline form of PA6 was predominant at a high mass fraction of Cu/Si to PA6. Moreover, PA6-Cu/Si with improved mechanical properties and wear resistance was generated by tuning the amount of nano-Cu/Si filler added during the polymerization. PA6-Cu/Si with a nano-Cu/Si content of 0.5% possesses the highest tensile strength and wear resistance and shows promise in applications as a functional polymer-matrix composite.     

One-step synthesis of monodisperse silver nanoparticles beneath vitamin E Langmuir monolayers

The monodisperse silver nanoparticles were synthesized by one-step reduction of silver ions in the alkaline subphase beneath vitamin E (VE) Langmuir monolayers. The monolayers and silver nanocomposite LB films were characterized by surface pressure-area (pi-A) isotherms, transmission electron microscopy (TEM), ultraviolet-visible spectroscopy (UV-vis), selected area electron diffraction (SAED), Fourier transform infrared transmission spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS), respectively. The results showed that the limiting area/VE molecule on different subphases varied. The phenolic groups in the VE molecules were converted to a quinone structure, and the silver ions were mainly reduced to ellipsoidal and spherical nanoparticles. The arrangement of the nanoparticles changed from sparseness to compactness with reaction time. The electron diffraction pattern indicated that the silver nanoparticles were face-centered cubic (fcc) polycrystalline. Silver nanocomposite LB films with excellent quality could be formed on different substrates, indicating that the transfer ratio of monolayer containing silver nanoparticles is close to unity. The dynamic process of reduction of silver ions by VE LB films was also studied through monitoring the conductivity of an Ag2SO4 alkaline solution.     

Pt负载复合氧化物催化剂的CO催化发光性能

采用非晶态络合物法制备了La0.9Cu0.1MnO3和LaCoO3钙钛矿催化剂, 并利用固定化溶胶工艺合成了Pt纳米粒子负载的Pt/La0.9Cu0.1MnO3和Pt/LaCoO3复合催化剂. 通过透射电镜(TEM)、X射线衍射(XRD)和X射线光电子能谱(XPS)等手段对催化剂的微观结构、形貌及Pt的价态进行了研究; 考察了催化剂的CO催化氧化发光性能. 结果表明, 若La0.9Cu0.1MnO3催化剂表面上负载的Pt纳米颗粒形成团聚, 则在其CO催化氧化发光谱中出现发光峰分裂的现象, 而在Pt纳米颗粒分散较好的Pt/LaCoO3体系中却没有出现这一情况. 因此可以利用CO催化发光谱来初步判断贵金属纳米颗粒在载体表面的分散状态.     

Fe-doped and ZnO-pillared titanates as visible-light-driven photocatalysts

Fe-doped cesium titanate was obtained by a solid state reaction with a mixture of Cs(2)CO(3), TiO(2), and Fe(2)O(3). ZnO-pillared doped titanate nanocomposite was successfully fabricated by exfoliating doped titanate and restacking its nanosheets with ZnO nanoparticles. The resulting nanocomposite was characterized by powder X-ray diffraction, scanning electron microscope, X-ray photoelectron spectroscopy, N(2) adsorption-desorption measurement, thermogravimetric analysis and UV-vis spectroscopy. It was revealed that the present nanocomposite exhibits greatly increased specific surface area with mesoporous texture and that there exists an electronic coupling between the host sheets and the guest nanoparticles in the pillared system. The results of degradation of methylene blue under visible light radiation suggest that doping iron ions improves the material spectral response region and that hybridizing with ZnO nanopillars can suppress the recombination of photogenerated electron-hole pairs.     

帽状锡纳米粒子的制备及其表面等离子的共振特性

采用真空热蒸发法在SiO2自组装单层膜上沉积金属锡, 制备了帽状锡纳米结构, 通过扫描电镜(SEM)、原子力显微镜(AFM)、X射线衍射(XRD)仪和Cary 5000紫外-可见-近红外(UV-Vis-NIR)分光光度计对其表面形貌、结构以及光谱特性进行了研究和表征. 结果表明, 制备的复合纳米粒子呈帽状, 表面等离子共振峰位具有明显的可调谐性, 随二氧化硅粒径的增大或锡帽层厚度的增加, 表面等离子共振吸收峰向长波方向移动.     

Synthesis and characterization of copper nanoparticles by reducing agent

Cu nanoparticles were synthesized by solution reduction process successfully. The influence of parameters on the size of Cu nanoparticles was studied and the referential process parameters were obtained. The morphology and structure of the synthesized Cu nanoparticles were characterized by transmission electron microscopy (TEM), powder X-ray diffraction (XRD), QELS data, infrared spectroscopy (IR) and solid state UV. The average size of nanoparticles was found between 15 ± 2 nm.     

Bifunctional single-crystalline rutile nanorod decorated heterostructural photoanodes for efficient dye-sensitized solar cells

A novel heterostructural TiO(2) nanocomposite, which consists of single-crystalline rutile TiO(2) nanorod decorated Degussa P25 nanoparticles, has been fabricated through a facile acidic hydrothermal method and successfully applied as the photoanodes for efficient dye-sensitized solar cells. The morphology, crystal structure, specific surface area and pore size distribution of the obtained nanocomposite were systematically investigated by X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM), selected-area electron diffraction patterns (SAED) and nitrogen adsorption-desorption measurements. Under standard illumination conditions (AM 1.5, 100 mW cm(-2)), devices with these hybrid anodes exhibited considerably enhanced photocurrent density and overall conversion efficiency in comparison with that of the commercial Degussa P25 electrodes, which can be partially attributed to the light scattering effect in the long-wavelength region as evidenced from the incident photon-to-current conversion efficiency (IPCE) response and the diffuse reflectance spectroscopy. More importantly, devices employing these hybrid anodes have demonstrated extended electron lifetimes and larger electron diffusion coefficient as validated by the intensity-modulated photocurrent/photovoltage spectroscopy measurements, which can be mainly ascribed to the fast electron transport and collection superiority of the single-crystalline nanorods.     

Novel Approach for the Decoration of Magnetic Carbon Nanospheres with Platinum Nanoparticles and Their Enhanced Peroxidase Activity for the Colorimetric Detection of H2O2

Pt/Fe3O4-DIB-DETA-CNS(PFDDC)nanocomposite(DIB=2,4-dihydroxybenzaldehyde;DETA=diethylenetfiamine;CNS=carbon nanosphere)was synthesized by dispersing Pt nanoparticles on magnetic carbon nanospheres. The structure,morphology and composition of the nanocomposite were studied by X-ray diffraction(XRD),transmission electron microscopy(TEM),energy-dispersive X-ray spectroscopy(EDX)and X-ray photoelectron spectroscopy(XPS). In addition,the nanocomposite showed superior peroxidase-like activity towards 3,3',5,5'-tetramethylbenzidine(TMB) with a visual color change in the presence of hydrogen peroxide(H2O2).Therefore,the PFDDC nanocomposite provides a sensing platform for the colorimetric detection of H2O2 with high sensitivity and selectivity.Furthermore,the nanocomposite can be conveniently preserved and separated.These features enable the nanocomposite to colorimetrically detect H2O2 for potential pharmaceutical,environmental and industrial applications.     

可磁分离的氮掺杂二氧化钛光催化剂的制备及光催化性能

将氮掺杂二氧化钛和通过液相催化相转化制备的磁性载体混合、煅烧制备了一种可磁分离的光催化剂TiO2-xNx/SiO2/NiFe2O4(TSN), 这种光催化剂显示出了典型的铁磁性和可见光活性(λ>400 nm). 对该光催化剂的XRD谱图和透射电镜照片进行分析. 结果表明, SiO2/NiFe2O4(SN)纳米粒子黏附在TiO2-xNx聚集体的表面形成了TSN复合光催化剂. 利用光催化降解甲基橙的效果来评价这种光催化剂的活性. 结果表明, 在NiFe2O4和TiO2-xNx之间包覆一层无定形的SiO2, 可以显著地提高催化剂的脱色效果.     

Comprehensive comparison of various techniques for the analysis of elemental distributions in thin films

The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 μm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.     

纳米结构TiO2／SiO2的逐层自组装

采用逐层自组装方法在二氧化硅球表面交替组装了十二烷基硫酸钠单分子膜和 二氧化钛纳米粒子膜，该复合多层膜经高温假烧后得到了核壳型纳米结构二氧化钛 ／二氧化硅复合颗粒．利用XRD，SEM，X射线能谱等对复合颗粒进行了表征．结果 表明：二氧化肽在复合颗粒表面排列紧密、均匀，粒径在50nm左右，为锐钛矿型结 构．复合颗粒中二氧化肽的含量随组装层数的增加而均匀增加．