Preparation of nanoalumina/EPDM composites with good performance in thermal conductivity and mechanical properties

In this paper, nanoalumina (Al₂O₃) highly filled ethylene propylene diene monomer (EPDM) composites are prepared, and the mechanical (static and dynamic) properties and thermal conductivity are investigated systemically through various characterization methods. Furthermore, influences of in situ modification (mixing operation assisted by silane at high temperature for a certain time) with the silane‐coupling agent bis‐(3‐triethoxy silylpropyl)‐tetrasulfide (Si69) and stearic acid (SA) pretreatment on the nano‐Al₂O₃ filled composites are as well investigated. The results indicate that nano‐Al₂O₃ particles can not only perform well in reinforcing EPDM, but also improve the thermal conductivity significantly. Assisted by in situ modification with Si69, the mechanical properties (especially dynamic mechanical properties) of the nano‐Al₂O₃ filled composites are improved obviously, without influencing the thermal conductivity. By comparing to the traditional reinforcing fillers, such as carbon black (grade N330) and silica, in situ modified nano‐Al₂O₃ filled composites exhibit excellent performance in mechanical (static and dynamic) properties as well as better thermal conductivity, especially lower compression heat build‐up and better fatigue resistance. In general, our work indicates that nano‐Al₂O₃, as the novel thermal conductive reinforcing filler, is suitable to prepare rubber products serving in dynamic conditions, with the longer expected service life. Copyright © 2010 John Wiley & Sons, Ltd.     

Nanoscale polyoxometalate‐based inorganic/organic hybrids

The latest advances in the area of polyoxometalate (POM)‐based inorganic/organic hybrid materials prepared by self‐assembly, covalent modification, and supramolecular interactions are presented. This Review is composed of five sections and documents the effect of organic cations on the formation of novel POMs, surfactant encapsulated POM‐based hybrids, polymeric POM/organic hybrid materials, POMs‐containing ionic crystals, and covalently functionalized POMs. In addition to their role in the charge‐balancing, of anionic POMs, the crucial role of organic cations in the formation and functionalization of POM‐based hybrid materials is discussed. DOI 10.1002/tcr.201100002     

Efficient organic monoliths prepared by γ-radiation induced polymerization in the evaluation of histone deacetylase inhibitors by capillary(nano)-high performance liquid chromatography and ion trap mass spectrometry

New monolithic HPLC columns were prepared by γ-radiation-triggered polymerization of hexyl methacrylate and ethylene glycol dimethacrylate monomers in the presence of porogenic solvents. Polymerization was carried out directly within capillary (250-200 μm I.D.) and nano (100-75 μm I.D.) fused-silica tubes yielding highly efficient columns for cap(nano)-LC applications. The columns were applied in the complete separation of core (H2A, H2B, H3, and H4) and linker (H1) histones under gradient elution with UV and/or electrospray ionization (ESI) ion trap mass spectrometry (MS) detections. Large selectivity towards H1, H2A-1, H2A-2, H2B, H3-1, H3-2 and H4 histones and complete separation were obtained within 8 min time windows, using fast gradients and very high linear flow velocities, up to 11 mm/s for high throughput applications. The method developed was the basis of a simple and efficient protocol for the evaluation of post-translational modifications (PTMs) of histones from NCI-H460 human non-small-cell lung cancer (NSCLC) and HCT-116 human colorectal carcinoma cells. The study was extended to monitoring the level of histone acetylation after inhibition of Histone DeACetylase (HDAC) enzymes with suberoylanilide hydroxamic acid (SAHA), the first HDAC inhibitor approved by the FDA for cancer therapy. Attractive features of our cap(nano)-LC/MS approach are the short analysis time, the minute amount of sample required to complete the whole procedure and the stability of the polymethacrylate-based columns. A lab-made software package ClustMass was ad hoc developed and used to elaborate deconvoluted mass spectral data (aligning, averaging, clustering) and calculate the potency of HDAC inhibitors, expressed through a Relative half maximal Inhibitory Concentration parameter, namely R_IC(50) and an averaged acetylation degree.     

Preparation of uniform and nano‐sized NaA zeolite using silatrane and alumatrane precursors

Nano‐sized Na A zeolite was successfully synthesized via the sol–gel process and microwave techniques. The synthesis parameters, such as hydroxide ion concentration, seed amount, as well as heating time and temperature, were studied to obtain the most uniform and very small sized NaA zeolite using the composition of SiO₂:Al₂O₃:xNa₂O:410H₂O; 3 ≤ x ≤ 6. It was found that hydroxide ion concentration affects the crystal size and heating time, whereas a higher amount of seed provides smaller sized NaA zeolite. The zeolite product can be synthesized using a higher temperature for a shorter time or lower temperature for a longer time. The best conditions for synthesizing the smallest size, 0.1–0.2 µm, and the most homogeneous NaA zeolite is to use the composition of SiO₂:Al₂O₃:3Na₂O:410H₂O and 3 wt% crystal seed at 80 °C microwave heating for 6 h. The synthesized NaA zeolite was characterized using XRD and SEM. Copyright © 2006 John Wiley & Sons, Ltd.     

NiMn2O4纳米粉体的相变过程和晶粒生长行为研究

采用溶胶凝胶法（Ｓｏｌ－Ｇｅｌ）制备ＮｉＭｎ２Ｏ４纳米粉体．用Ｘ射线衍射（ＸＲＤ）法，热分析仪研究ＮｉＭｎ２Ｏ４纳米粉体的相变过程．用Ｘ射线衍射线线宽法，透射电子显微镜（ＴＥＭ）研究晶粒长大行为．研究结果表明：热处理温度小于６７０°Ｃ，存在非晶晶化过程和向ＮｉＭｎ２Ｏ４尖晶石主晶相转变等相变过程，晶粒尺寸缓慢增大，热处理温度在于６７０°Ｃ，粉体的相结构为ＮｉＭｎ２Ｏ４尖晶石相．晶粒尺寸较快增长．相变过程严重影响了晶粒长大行为．     

Hybrid Siloxane-Based Nano Building Blocks for Optical Applications: Optimization of the Synthetic Procedures by Spectroscopic Analysis

Diphenylsilanediol (DPDO) reacts with triethoxysilane (TREOS) in anhydrous conditions and in the presence of pyridine, to form complex mixtures of linear and cyclic condensation products which were identified by ²⁹Si NMR and ATR/FTIR spectroscopies. The distribution of products can be varied by modifying the reaction conditions. Spectroscopic analysis allowed to identify the optimal reagents ratio and concentration for the production of hetero-condensation products minimizing the number of residual –OH groups whose presence would affect the performance of optical waveguides based on the synthesised nano building blocks.     

孔雀石绿在自组装纳米银膜上的SERS

电解法制备了自组装纳米银膜。用紫外可见分光光度计和透射电镜对电解出的银胶进行了观测,并且用扫描电镜对制备好的银膜进行了表征,发现银膜上的纳米银颗粒是银胶中颗粒的二聚体和三聚体。我们得到了孔雀石绿的SERS谱,发现自组装纳米银膜对于用SERS检测孔雀石绿具有很好的增强效果,检测的下限是10-10M。另外,我们对所测不同浓度的孔雀石绿的指纹峰面积进行了分析,发现峰面积随浓度的变化有很好的线性关系,这对以后进行定量分析打下了基础。本实验说明用电解法制备的自组装纳米银膜对于检测孔雀石绿具有很好的应用前景。     

Structure, room-temperature magnetic and optical properties of Mn-doped TiO2 nano powders prepared by the sol-gel process

TiO 2 nano powders with Mn concentration of 0 at%-12 at% were synthesized by the sol-gel process,and were annealed at 500 C and 800 C in air for 2 hrs.X-ray diffraction (XRD) measurements indicate that the Mn-TiO 2 nano powders with Mn concentration of 1 at% and 2 at% annealed at 500 and 800 C are of pure anatase and rutile,respectively.The scanning electron microscope (SEM) observations reveal that the crystal grain size increases with the annealing temperature,and the high resolution transmission electron microscopy (HRTEM) investigations further indicate that the samples are well crystallized,confirming that Mn has doped into the TiO 2 crystal lattice effectively.The room temperature ferromagnetism,which could be explained within the scope of the bound magnetic polaron (BMP) theory,is detected in the Mn-TiO 2 samples with Mn concentration of 2 at%,and the magnetization of the powders annealed at 500 C is stronger than that of the sample treated at 800 C.The UV-VIS diffuse reflectance spectra results demonstrate that the absorption of the TiO 2 powders could be enlarged by the enhanced trapped electron absorption caused by Mn doping.     

Effect of citric acid concentration as emulsifier on perovskite phase formation of nano‐sized SrMnO3 and SrCoO3 samples

In this study the effects of citric acid concentration, used as organic emulsifier, on the perovskite phase formation of the nano strontium manganite or cobaltite samples were studied. Stoichiometric perovskites in the absence and presence of citric acid were prepared by drying a solution containing molar ratio of Sr(NO₃)₂/Mn(NO₃)₂·4H₂O and Sr(NO₃)₂/Co(NO₃)₂·6H₂O = 1 followed by calcination at 900 °C for 5 h. Citric acid concentration, selected to be 0.0, 0.3, 0.6, 1.0, 1.3, 2.5 and 5 times of the total number of moles of the nitrate ions. The results revealed that increase in the citric acid concentration, larger than number of moles of the nitrate ions equivalent, deteriorates the perovskite phase formation. Instead, a new phase of carbonates and metal oxides are appeared. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Comparison Between Different Syntesis Methods of PMMA/HA Using Ultrasonic Radiation

Summary: The use of PMMA as dental and osseous cement and also in the fabrication of intraocular lenses has been widely reported. The combination of its excellent properties with those of hydroxyapatite (HA) to form a composite material, can result in very interesting properties as a biomaterial. The key is to obtain a good filler dispersion and interface bonding. Ultrasonic radiation seems to be a very versatile method for the synthesis of these materials, since the use of conventional initiators can be avoided, the filler dispersion improved and the interface interaction can be promoted. In the present work PMMA/HA composite materials were prepared by three different synthesis routes using ultrasonic radiation, in order to study the effect of the synthesis method on the final microstructure. Method I : in situ synthesis of PMMA and HA, under ultrasonic radiation by emulsion polymerization of MMA and HA precursors. Method II : in situ synthesis of HA, (from its precursors) by high frequency ultrasound in commercial PMMA solution Method III : in situ polymerization of MMA under high frequency ultrasonic radiation and adding HA to the solution and Method IV Mixing of hydroxyapatite nanocrystals, in different proportions, in a solution of commercial PMMA, by different periods from 10 min to 7 h, under low frequency (conventional) ultrasonic radiation, to compare the effect of high frequency and conventional ultrasound radiation. The different materials were characterized by FTIR, SEM, TEM, DRX, ¹H NMR and TGA. The results showed that, all the composites prepared by in situ synthesis showed an interaction between HA and PMMA, manifested by a bonding of the phosphate groups with the polar groups of the polymer matrix observed by FTIR. On the other hand, when the synthesis was carried out simultaneously adding HA and PMMA precursors a inhibition of the polymerization reaction of MMA was observed.