One-pot hydrothermal synthesis of MoS2 nanosheets/C hybrid microspheres

Uniform MoS₂ nanosheets/C hybrid microspheres with mean diameter of 320 nm have been successfully synthesized via a facile one-pot hydrothermal route by sodium molybdate reacting with sulfocarbamide in d-glucose solutions. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). XRD patterns showed that the MoS₂ was kept as a two-dimensional nanosheet crystal and C was retained as amorphous even after their annealing treatment at 800 °C. TEM and SEM images indicated that the MoS₂ nanosheets were uniformly dispersed in the amorphous carbon. The experiment results also revealed that the appropriate amount of d-glucose had an obvious effect on the formation of uniform MoS₂ nanosheets/C hybrid microspheres. A possible formation process of MoS₂ nanosheets/C hybrid microspheres was preliminarily presented.     

Preparation of ZnO nanorod by solvothermal reaction of zinc acetate in various alcohols

Solvothermal reaction of zinc acetate in various alcohols resulted in the formation of zinc oxide (ZnO) nanorods. The effects of reaction conditions on the product morphology as well as crystallization mechanism were investigated by using X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM) techniques. It was found that average diameter and length of the nanorods increased with an increase in reaction temperature or the initial concentration of zinc acetate. On the contrary, the aspect ratio of the product depended upon type of alcohol used as the reaction medium. The aspect ratio of ZnO nanorods increased from 1.7 to 5.6 when the alcohol was changed from 1-butanol to 1-decanol. An investigation of the reaction mechanism suggested that the formation of ZnO nanorods was initiated from the esterification reaction between zinc acetate precursor and alcohol to form ZnO seeds.     

氧化铟纳米棒的气敏特性

以非离子表面活性剂烷基苯酚聚氧乙烯醚OP-10为形貌控制剂合成In2O3纳米棒.用热重-差示扫描量热法、X射线衍射和透射电镜对In2O3纳米棒的热分解过程、晶体结构和微观形貌进行表征.对纳米棒制得的气敏元件进行气敏性能测试,同时用扫描电子显微镜及比表面积和孔隙度分析仪对元件的表面形貌和材料的介孔结构进行了分析.结果表明:制得的In2O3为立方晶型的纳米棒,直径约20 nm,长度约120 nm.与In2O3纳米颗粒气敏性能相比,In2O3 纳米棒对三甲胺具有更高的灵敏度和选择性.用In2O3纳米棒制的气敏元件对三甲胺在一定的浓度范围内的灵敏度与浓度呈现良好的双对数线性关系.棒状材料中形成的大量介孔对气敏性能的提高有着重要的作用.     

Hot pressing sintering of zinc sulfide microsphere decorated with nanorods synthesized by the simple refluxing method

A zinc sulfide microsphere decorated with nanorods was synthesized using the refluxing method. Then, the as-obtained ZnS nanostructures were consolidated via the hot pressing (HP) technique. X-ray diffraction, Fourier transforms infrared spectroscopy, high-resolution transmission electron microscopy, field emission scanning electron microscopy (FESEM), diffuse reflectance spectroscopy, and X-ray mapping analyzes were used to characterize the ZnS sample. The effects of various factors such as pH, temperature, and reaction time were investigated on the morphology and particle size of ZnS nanostructures. The formation of sphalerite phase of ZnS nanoparticles was confirmed by the XRD analysis. FESEM also revealed that ZnS nanostructures with the molar ratio 1:1.3 (zinc: sulfur) had a spherical morphology decorated with sulfur nanorods. The ZnS nanostructures were consolidated by hot pressing technique at 860 °C for 2h under vacuum atmosphere. XRD analysis indicated that the sintered ceramic had a sphalerite phase. FESEM study demonstrated that ZnS ceramic had a grain size diameter within the range of 1–3 μm.     

Graphene oxide-anchored reactive sulfonated copolymer via simple one pot condensation polymerization: proton-conducting solid electrolytes

A rapid and efficient post-polymerization functionalization of poly(urea-co-urethane) (PUU) onto the graphene oxide (GO) nanosheets has been developed to produce super-acidic polymer/GO hybrid nanosheets. Thus, the surface of GO nanosheets were functionalized with 3-(triethoxysilyl)propyl isocyanate (TESPIC) from hydroxyl groups to yield isocyanate functionalized graphene oxide nanosheets. Then, sulfonated polymer/GO hybrid nanosheets were prepared by condensation polymerization of isocyanate-terminated pre-polyurea onto isocyanate functionalized graphene oxide nanosheets through the formation of carbamate bonds. FTIR and TGA results indicated that TESPIC modifier agent and poly(urea-co-urethane) were successfully grafted onto the GO nanosheets. The grafting efficiency of poly(urea-co-urethane) polymer onto the GO nanosheets was estimated from TGA thermograms to be 205.9%. Also, sulfonated polymer/GO hybrid nanosheets showed a proton conductivity as high as 3.7 mS cm^?1. Modification and morphology of GO nanosheets before and after modification processes were studied by scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD).     

Enhanced gas sensing properties of hierarchical SnO2 nanoflower assembled from nanorods via a one-pot template-free hydrothermal method

Well-defined three-dimensional (3D) hierarchical tin dioxide (SnO₂) nanoflowers with the size of about 200 nm were successfully synthesized by a simple template-free hydrothermal method. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂ adsorption-desorption analyses were used to characterize the structure and morphology of the products. The as-synthesized full crystalline and large specific surface area SnO₂ nanoflowers were assembled by one-dimensional (1D) SnO₂ nanorods with sharp tips. A possible self-assembly mechanism for the formation the SnO₂ nanoflowers was speculated. Moreover, gas sensing investigation showed the sensor based on SnO₂ nanoflowers to exhibit high response and fast response-recovery ability to detect acetone and ethanol at an operating temperature lower than 200 °C. The enhancement of gas sensing properties was attributed to their 3D hierarchical nanostructure, large specific surface area, and small size of the secondary SnO₂ nanorods.     

Internal morphologies of diblock copolymer nanorods fabricated from regular and irregular pores of anodized aluminum oxide templates

Internal nanostructures in nanorods of polystyrene-poly(4-vinyl pyridine) (PS-PVP) diblock copolymers fabricated from pores having regular or irregular contours in AAO templates were investigated by cross-sectional transmission electron microscopy. When nanorods of PS-PVP copolymers were produced from pores with regular contours, a typical morphology of concentric cylinders was observed due to the strong affinity of the PVP block to the surface of the AAO pores. In the case of PS-PVP nanorods obtained from pores with irregular contours, a concentric cylindrical morphology was not induced. Instead, a nanostructure of lamellae mostly parallel to the axis of the nanorods was observed with a similar period of lamellae to the bulk lamellar period. In addition, nanorods having a functional coaxial nanostructure were fabricated by synthesizing Au nanoparticles in concentric cylinders of the nanorods to demonstrate the utilization of self-assembled internal nanostructures in nanorods.     

Synthesis, characterization and morphology of polyanthranilic acid micro- and nanostructures

Polyanthranilic acid (PANA) nanofibres, nanorods, nanospheres and microspheres were synthesized by polymerization of anthranilic acid using ammonium peroxydisulfate (APS) as oxidant without hard or soft templates. Polymerization of anthranilic acid was carried out in aqueous solutions of strong (hydrochloric) and weak (acetic) acids. The influence of synthetic parameters such as oxidant, initiator, dopant acid and its concentration, redox initiator, and reaction medium on the morphology and particle size of PANA have been investigated. PANA nanofibres and nanorods were obtained via redox polymerization of anthranilic acid initiated by FeSO₄ as redox initiator. PANA nanospheres and nanofibres were also obtained when used aromatic amines as initiators. When polymerization carried out in the solution of weak (acetic) acid the microsphere morphology obtained and the particle size increase with increasing the concentration of weak acid. PANA nanorods were obtained also by polymerization of anthranilic in ethanol-water mixture unlike interfacial polymerization of anthranilic acid (in chloroform-water) that give PANA microspheres. The morphology and particle size of PANA was studied by scanning electron microscope (SEM) and transmission electron microscope (TEM). The average diameter of nanostructures obtained ≤100 nm. The optical bandgap of microspheres and nanofibers polymeric products were determined using UV-vis spectroscopic technique and found to be 2.0 eV and 1.6 eV, respectively. The bandgap decreased with decreasing the particle size. IR spectrum confirmed the structure of PANA nanofibres (synthesized with FeSO₄ as redox initiator) in emeraldine form. The thermal stability of polymer obtained was determined by thermal gravimetric analysis (TGA). The molecular weight was determined also by gel permeation chromatography (GPC).     

丝素-羟丙基壳聚糖微球的结构和释药性能

以胰岛素为目标药物,以丝素(SF)和羟丙基壳聚糖(HPCS)为包药材料,复凝聚法制备SF-HPCS载药微球。采用红外光谱(FTIR)、扫描电镜(SEM)、X射线衍射(XRD)、热重分析(TGA)等对载药微球的结构、外部形貌及热性能等进行了表征。结果表明,所制备的载药微球表面密实,平均粒径22.4μm,呈正态分布;载药微球对胰岛素的包埋率达73.6%,大于HPCS载药微球(64.3%)及壳聚糖(CS)载药微球(57.1%);SF-HPCS载药微球在人工胃液中4h内累计释药率为21.3%,在人工肠液中24h内累计释药率达81.2%,48h累计释药率为92.2%,释放过程平稳、缓慢。     

Walnut-like In2S3 microspheres: ionic liquid-assisted solvothermal synthesis, characterization and formation mechanism

Walnut-like In(2)S(3) microspheres were synthesized through an ionic liquid-assisted solvothermal method for the first time. The crystal structure and morphology of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (DRS) and nitrogen adsorption-desorption measurement. It was found that the additional amount of ionic liquid, solvothermal temperature and time played crucial roles in controlling the structure and morphology of the In(2)S(3) microspheres. A possible formation mechanism of the walnut-like In(2)S(3) microsphere was proposed on the basis of the experimental results.     

Syntheses of PAM microgel surfacely covered with alkyl quaternary ammonium surfactant/Keggin‐type polyoxometalate complexes

The composite microspheres of poly(lacrylamide) microgels (PAM) surfacely covered with [2‐(methacryloyloxy)ethyl]dodecyldimethylammonium (MEDDAB)‐tungstophosphate (HPW) complexes (MEDDAB‐HPW) were synthesized by using ion‐exchange reaction between MEDDAB located within the porous PAM microgels and HPW in aqueous solution. The morphology and component of the composite microspheres were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis, respectively. The results indicated that PAM/MEDDAB‐HPW composite microsphere with different hierarchical surface structures could be obtained by controlling the weight ratio of MEDDAB to HPW in the microgels and cross‐linking degree of PAM microgels. Although the surface morphologies of the composite microspheres prepared in different conditions were different, a general feature was that the composite microspheres have the core‐shell structure and the wrinkly surface covered with the particles of MEDDAB‐HPW complexes. The formation of the wrinkly surface is attributed to the difference in shrinkage between inside and outside of PAM microgel frameworks due to deposition of MEDDAB‐HPW on the surface, and the formation of MEDDAB‐HPW small particles originates from the reaction between MEDDAB aggregation and HPW. For this composite microsphere, PAM hydrogel core is suitable to store water‐soluble substances, and the shell composed of the surfactant/Keggin‐type polyoxometalate complexes is not only amphiphilic but also catalytic. Additionally, PAM/MEDDAB‐HPW composite microspheres with big size and MEDDAB‐HPW particles with small size make the composite microspheres not only easy for separation but also beneficial for catalysis. This material provides an example to construct microreactors with new structure used in diphase catalytic reaction. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

A simple additive-free approach for the synthesis of uniform manganese monoxide nanorods with large specific surface area

A simple additive-free approach is developed to synthesize uniform manganese monoxide (MnO) one-dimensional nanorods, in which only manganese acetate and ethanol were used as reactants. The as-synthesized MnO nanorods were characterized in detail by X-ray diffraction, scanning and transmission electron microscopy (TEM) including high-resolution TEM and selected-area electron diffraction, Fourier transform infrared spectrum, and nitrogen adsorption isotherm measurements. The results indicate that the as-synthesized MnO nanorods present a mesoporous characteristic with large specific surface area (153 m² g⁻¹), indicating promising applications in catalysis, energy storage, and biomedical image. On the basis of experimental results, the formation mechanism of MnO one-dimensional nanorods in the absence of polymer additives was also discussed.     

Synthesis of silver/polymer colloidal composites from surface-functional porous polymer microspheres

This study presents a different colloidal silver (Ag)/polymer system where Ag nanoparticles are deposited uniformly onto surface-functional porous poly(ethylene glycol dimethacrylate-co-acrylonitrile) (poly(EGDMA-co-AN)) microspheres. The formation and morphology of the composite microspheres were characterized from electron microscopy and X-ray diffraction analyses. The significance of the present report is that owing to the high affinity between Ag and nitrile group (CN) on the large surface of the microspheres, the Ag nanoparticles having a face-centered cubic phase were incorporated evenly into the deep pores of the microspheres with fine size and size distribution. In the preservation test, the Ag/poly(EGDMA-co-AN) composite microspheres obtained showed an excellent anti-bacterial performance, elucidating a high applicability for a new preservative.     

Comparative study of photocatalytic performance of titanium oxide spheres assembled by nanorods,nanoplates and nanosheets

TiO₂ spheres assembled by nanorods, nanoplates and nanosheets were fabricated by facile hydrothermal/solvothermal methods. The three samples were thoroughly characterised by scanning electron microscopy, X-ray diffraction, the Brunauer–Emmett–Teller method and UV spectroscopy. The surface area of spheres assembled by nanosheets was 83.9 m²g^–1, which is larger than that obtained for nanorods (10.8 m²g^–1) and nanoplates (6.31 m²g^–1). Their photocatalytic performance was evaluated in terms of the decomposition rate of methyl orange in these three samples under UV irradiation. The best photoactivity was observed in the samples constructed from nanosheets.     

Hierarchical heterostructure of porous NiO nanosheets on flower-like ZnO assembled by hexagonal nanorods for high-performance gas sensor

A novel hierarchical heterostructure consisting of porous NiO nanosheets and flower-like ZnO assembled by hexagonal nanorods was successfully fabricated by a simple two-step hydrothermal approach. Flower-like ZnO was obtained by the first step hydrothermal method. Through the second step hydrothermal method, porous NiO nanosheets grew on the surface of flower-like ZnO to realize integration of ZnO and NiO, so the p-n heterostructure between ZnO and NiO formed. The samples were investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and energy dispersive X-ray (EDX). Gas sensing test results showed that the sensor based on NiO/ZnO composite exhibited superior sensing properties to acetone. The sensor response to 100 ppm acetone was about 205.14 at the optimum working temperature of 240 °C, and the response and recovery times were about 7 and 20 s, respectively. The enhanced response might be attributed to heterojunction and larger specific surface area provided by attached porous NiO nanosheets. The rapid response and recovery characteristics and improved selectivity attributed to the porous structure and good catalytic actions of NiO nanosheets.     

Preparation and characterization of porous titanium dioxide sulfonated polystyrene composite microspheres with amphiphilicity

Porous particles with amphiphilicity were prepared by a nonpolymeric pore‐formation process with the sulfonation of polystyrene microspheres. Nano titanium dioxide (TiO₂) particles were then grafted onto the surface via a sol–gel method to finally form the composite particles. The effects of the mass ratio of ethanol (EtOH) to water, temperature, and solubility parameter on the pore‐formation process is discussed in detail. The morphology, porous structure, and wetting properties of the particles were studied by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FTIR) spectroscopy, and contact angle measurement. The results show that porous sulfonated polystyrene (SP) microspheres could be fabricated at 60°C with a 1 : 1 mass ratio of EtOH–water and a solubility parameter of 29.69 MPa^1/2. The TiO₂ particles were determined to be grafted onto the SP microspheres by physical‐bond interaction on the basis of FTIR analysis. The contact angles for both water (aqueous‐phase) and various organic solvent (oil‐phase) droplets with different polarities on the surface of compressed tablets of TiO₂–SP powder were all lower than 30°; this indicated excellent amphiphilicity in the composite particles. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

铁掺杂二氧化钛空心球的制备及性能

以TiF₄为钛源、九水合硝酸铁为掺杂前体,采用水热法制备铁掺杂的TiO₂空心微球。采用SEM、TEM、XRD、BET、XPS等技术对样品的形貌、结构、晶型、比表面积、元素组成等进行表征,以亚甲基蓝（MB）的光催化降解为目标反应,评价其光催化活性。结果表明,160℃下水热反应生成的纳米TiO₂空心微球晶型为锐钛矿,少量掺铁并不影响微球的形貌及晶体结构。光催化实验表明,160℃下水热反应12 h生成的TiO₂空心微球样品均匀性好、光催化活性最佳;铁掺杂能显著提高TiO₂空心微球的催化活性,当铁钛比为1.5:100时,所得样品粒径最小,比表面积最大,光催化活性最高。     

Morphological development of polypropylene in immiscible blends with cellulose acetate butyrate

Isotactic polypropylenes (iPP) with different melt flow indexes were melt blended with cellulose acetate butyrate (CAB) and then prepared into microspheres or nanofibers following a novel process of producing well dispersed CAB/iPP immiscible blends and subsequent removal of the CAB matrix. The morphologies of iPP microspheres were investigated by a scanning electron microscopy, and the dimensions of iPP microspheres were evaluated. The melt viscosities of iPP, CAB, and CAB/iPP blends were measured by using a capillary rheometer. The influences of the viscosity, viscosity ratio, and composition ratio of iPP/CAB on the morphology formation of iPP in CAB matrix were studied.     

Synthesis and characterization of exfoliated polystyrene grafted hexagonal boron nitride nanosheets and their potential application in heat transfer nanofluids

Three different methods were used to develop surface-modified hexagonal boron nitride (h-BN) nanosheets, and polystyrene grafting was performed by an indirect covalent bond formation between modified h-BN nanosheets and styrene molecules through surface initiated atom transfer radical polymerization (SI-ATRP) approach. In all methods, an alkyl bromide as the ATRP-initiating site was first introduced on h-BN nanosheets and an SI-ATRP reaction of styrene from the initiator immobilized h-BN surface was achieved. The structure of synthesized PS grafted h-BN nanosheets (PS-g-h-BN) was identified and characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, field emission scanning electron microscopy, transmission electron microscopy, and atomic force microscopy methods. The functionalization promoted the exfoliation of h-BN layered structure into few layer sheets where the thickness of the sheets was dependent on the modification technique and the content of polymer grafted on nanosheets. The highest grafting content of PS-g-h-BN nanosheets was obtained around 20% which could enhance thermal conductivity of mineral oil-based nanofluids with the minimum concentration of the nanofiller (0.01 wt%). The electrical and physical properties of the nanofluid were also investigated. According to the results, the dielectric loss reduced by increase in nanofiller concentration was an indication of the enhanced dielectric nature of nanofluid. In addition, exfoliated PS-g-h-BN nanosheets dispersions were shown to be stable in mineral oil up to 2 months and this stability was linked to the presence of polymer chains followed by the formation of van der Walls interactions between the grafted polymer and the fluid.     

制备工艺对ATO纳米棒形貌结构的影响

以SnCl4·5H2O和SbCl3为原料,采用化学共沉淀法成功制备了高含量棒状纳米级掺锑二氧化锡(ATO)导电粉体,研究了掺锑量、热处理温度及热处理时间对纳米棒形貌结构的影响。初步探讨了ATO纳米棒的形成机理,并用热重分析(TG)、透射电镜(TEM)、X-射线衍射(XRD)、比表面法(BET)对棒结构进行了表征。