等离子体条件下PP／PS共混体系组成和相结构的关系

运用等离子体装置制备了聚苯乙烯预聚物(PSt)并对聚丙烯(PP)进行了表面处理,得到改性聚丙烯(gPP)。在密炼机中以间歇出料法制备了不同组成的聚丙烯(PP)/聚苯乙烯(PSt)和改性聚丙烯(gPP)/聚苯乙烯(PSt)共混物。针对扫描电镜图样,用投影面直径dp这一结构参数研究了组成对两个共混体系相尺寸的影响以及相应的相分散状况。利用分布函数求取了分散相聚苯乙烯(PSt)分形维数,对不同组成的相分散进行了研究。     

Dielectric method for detection of phase separation and its kinetics in TMPC/PS blends

A new method for the detection of phase separation and its kinetics through real-time measurements is presented using the dielectric technique. The kinetics of phase separation were determined for a blend of tetramethyl bisphenol-A polycarbonate TMPC and polystyrene PS at different temperatures. The temperature dependence of the rate constant of phase separation was determined. The activation energy of phase separation process is found to be equal to 46 kcal/mole. In addition, it was possible to determine the variation in the composition of the TMPC-rich phase with time. The results obtained were compared with the literature data and were found to be in good agreement.     

Morphology of PMMA/polyoxide blends and grafted copolymers using etching and staining techniques

The morphology of poly(methyl methacrylate), poly(ethylene oxide) blend and the grafted copolymer poly(methyl methacrylate-g-ethylene oxide) was observed by scanning electron microscopy. The contrast was obtained by an etching technique, removing the PEO phase out of the blend. The PEO phase of the copolymer was stained with OsO₄ and better contrast was observed using a back-scattering image. The PEO phase was shown to be distributed as spherical domains in the PMMA matrix for both the copolymer and the blend.     

Raman investigation of thermoplastic vulcanizates based on hydrogenated natural rubber/polypropylene blends

Raman spectroscopy including mapping technique appears as a powerful technique for the characterization of polymer blends like thermoplastic elastomers (TPEs) and thermoplastic vulcanizates (TPVs). The Raman spectra of polymers blends such as natural rubber/polypropylene (NR/PP) and 65% hydrogenated natural rubber/polypropylene (65%HNR/PP) were identified and the phase distribution was determined. The study was driven for the same type of blends in TPEs state and TPVs state obtained after to 2 different processes, either peroxide cure or sulfur cure. The morphology of TPEs and TPVs obtained by Raman spectroscopy were compared and confirmed using scanning electronic microscopy.Raman mapping shows that the phase morphology of NR/PP, 65%HNR/PP, were characterized as continuous rubber phase morphology of the thermoplastic elastomers (TPEs) and a fine dispersion of cross-linked rubber phase in a continuous matrix of the thermoplastic vulcanizates (TPVs). Raman spectroscopy is demonstrated to be a reference to determine the content ratio of each component in the TPVs. Moreover, Raman mapping could be used to calculate the phase size of cross-linked rubber phase dispersed in the thermoplastic vulcanizates (TPVs).     

Controlling the size of poly(hydroxybutyrate-co-hydroxyvalerate) nanoparticles prepared by emulsification–diffusion technique using ethanol as surface agent

Poly(hydroxybutyrate-co-hydroxyvalerate) (PHBHV) nanospheres and oily nanocapsules were prepared by emulsification–diffusion technique. Controlled particle sizes were obtained employing binary mixtures of solvents (chloroform:ethanol) in the organic phase. Ethanol was chosen because of its dipole–dipole interaction with chloroform and its hydrogen bond with water. The smallest particles (from 253 to 493 nm) were obtained using a mixture of solvents composed of 70% ethanol and 30% chloroform (v/v) in the organic phase, while the largest particles (from 896 to 1568 nm) were obtained using chloroform exclusively. Independently of the organic phase composition, the nanoparticles showed unimodal distributions. Optical microscopy showed that the size of the primary emulsion droplets of the nanosphere formulations decreased with increasing ethanol concentrations in the organic phase. A simple empirical equation was developed correlating the nanoparticle diameters with the surface tension gradient coefficient multiplied by the ethanol molar concentration in the organic phase. The strategy showed that the control of the nanoparticle diameters, using emulsification–diffusion technique, could be achieved by adjusting the surface tension of the organic phase.     

Preparation of insulin-loaded PLA/PLGA microcapsules by a novel membrane emulsification method and its release in vitro

Uniform-sized biodegradable PLA/PLGA microcapsules loading recombinant human insulin (rhI) were successfully prepared by combining a Shirasu Porous Glass (SPG) membrane emulsification technique and a double emulsion-evaporation method. An aqueous phase containing rhI was used as the inner water phase (w1), and PLA/PLGA and Arlacel 83 were dissolved in a mixture solvent of dichloromethane (DCM) and toluene, which was used as the oil phase (o). These two solutions were emulsified by a homogenizer to form a w1/o primary emulsion. The primary emulsion was permeated through the uniform pores of a SPG membrane into an outer water phase by the pressure of nitrogen gas to form the uniform w1/o/w2 droplets. The solid polymer microcapsules were obtained by simply evaporating solvent from droplets. Various factors of the preparation process influencing the drug encapsulation efficiency and the drug cumulative release were investigated systemically. The results indicated that the drug encapsulation efficiency and the cumulative release were affected by the PLA/PLGA ratio, NaCl concentration in outer water phase, the inner water phase volume, rhI-loading amount, pH-value in outer water phase and the size of microcapsules. By optimizing the preparation process, the drug encapsulation efficiency was high up to 91.82%. The unique advantage of preparing drug-loaded microcapsules by membrane emulsification technique is that the size of microcapsules can be controlled accurately, and thus the drug cumulative release profile can be adjusted just by changing the size of microcapsules. Moreover, much higher encapsulation efficiency can be obtained when compared with the conventional mechanical stirring method.     

Thermodynamic, kinetic and electrical switching studies on Si15Te85−xInx glasses: Observation of Boolchand intermediate phase

An interesting topic for quite some time is an intermediate phase observed in chalcogenide glasses, which is related to network connectivity and rigidity. This phenomenon is exhibited by Si-Te-In glasses also. It has been addressed here by carrying out detailed thermal investigations by using Alternating Differential Scanning Calorimetry technique. An effort has also been made to determine the stability of these glasses using the data obtained from different thermodynamic quantities and crystallization kinetics of these glasses. Electrical switching behavior by recording I-V characteristics and variation of switching voltages with indium composition have been studied in these glasses for phase change memory applications.     

Mesoscopic Simulation Assistant Design of Immiscible Polyimide/BN Blend Films with Enhanced Thermal Conductivity

The mesoscopic simulation technique was applied to describe the phase separation behavior of polyimide blends and used for design of immiscible polyimide/BN blend films with enhanced thermal conductivity. The simulation equilibrium morphologies of different poly(amic acid)(PAA) blend systems were investigated and compared with optical images of corresponding polyimide blend films obtained by experiment. The immiscible polyimide blend films containing nano-/micro-sized BN with vertical double percolation structure were prepared. The result indicated that the thermal conductivity of polyimide blend film with 25 wt% nano-sized BN reached1.16 W/(m·K), which was 236% increment compared with that of the homogenous film containing the same BN ratio. The significant enhancement in thermal conductivity was attributed to the good phase separation of polyimide matrix, which made the inorganic fillers selectively localized in one continuous phase with high packing density, consequently, forming the effective thermal conductive pathway.     

三维多孔碳纤维/聚乳酸/壳聚糖复合支架材料的体外细胞相容性评价

利用溶液共混法以及冷冻干燥法制备了三维多孔碳纤维/聚乳酸/壳聚糖(CF/PLA/CS)复合生物支架材料,通过相差显微镜和扫描电子显微镜检测了鼠骨髓基质细胞（BMSCs）与该材料的生物相容性,得到了MTT生长曲线,评价了材料的毒性。 结果表明,以实验组材料的浸提液培养细胞,8 d后细胞开始连片生长,没有观察到细胞变形、坏死现象;在实验组材料上培养4 d后细胞的SEM图像显示,细胞形貌正常,并已开始向孔隙深部生长;MTT法绘制的增值曲线表明,培养4 d后实验组的细胞增殖速度高出空白对照组30%。 以上细胞形态学观察法和细胞增殖法评价结果表明,三维多孔 CF/PLA/CS复合材料没有细胞毒性,并对细胞有良好的粘附、增殖能力,有望成为骨修复材料。     

Rapid Evaluation of Water-in-Oil (w/o) Emulsion Stability by Turbidity Ratio Measurements

In this Note, we investigated the turbidity ratio method for the evaluation of water-in-oil emulsion stability. The slope of turbidity ratio of water-in-oil emulsions with time was taken as an index of stability; the higher the slope, the less stable the system. Various factors affecting the stability of emulsion such as HLB of emulsifier, amount of emulsifiers, and water were tested using this technique. The results of the turbidity ratio technique for the evaluation of emulsion stability were well consistent with those obtained by the measurement of phase separation when incubated for 30 days at room temperature. Copyright 2000 Academic Press.     

Determination of the Phase Inversion Temperature of Orange Oil/Water Emulsions by Rheology and Microcalorimetry

Abstract

In low-energy emulsification processes, phase inversion occurs when the phases of a dispersion exchange, because of changes in the medium's properties. This paper reports experiments to determine the phase inversion temperature (PIT) of orange oil/water emulsions stabilized by nonionic surfactants. Two techniques were employed: rheology, which is already commonly used to obtain the PIT, and microcalorimetry, which has been proposed as a new technique. Continuous monitoring of the emulsions' viscosity permitted identifying different phenomena that occur while the temperature varies. For all the dispersions prepared, the rheological curves obtained showed two peaks, one attributed to the phase separation process and the other to the phase inversion phenomenon. The microcalorimetry technique showed two endothermic transitions as the dispersion's temperature increased. The initial temperatures were comparable to those obtained by rheology. The influence of the surfactant concentration and the hydrophilic-lipophilic balance (HLB) of the mixture of surfactants and the reduction in volume of the phases at the phase inversion temperature were also evaluated. In general, both methods used to evaluate the phase inversion of the orange oil/water systems (rheology and microcalorimetry) presented concordant results, both for the phase separation process and the phase inversion temperature.     

A fast synthesis for Zintl phase compounds of Na3SbTe3, NaSbTe2 and K3SbTe3 by microwave irradiation

The microwave irradiation technique was used to prepare three Zintl phase compounds Na₃SbTe₃, NaSbTe₂ and K₃SbTe₃. The as-prepared products were analyzed and characterized by XRD, EDX and SEM techniques. Higher microwave oven power and shorter irradiation time are required for the synthesis of Na₃SbTe₃, whereas lower oven power and longer irradiation time are needed for NaSbTe₂. Moderate microwave irradiation conditions facilitate the formation of pure K₃SbTe₃. Pure phase of Na₃SbTe₃ are directly obtained by this technique for the first time. Compared with the traditional high-temperature solid-state synthesis, the microwave reaction required a considerable shortened reaction time for the preparation of the three Zintl compounds. The initial driving force for these reactions originates from the interaction of microwave electric field with alkali metals (Na and K) and Sb powders.     

Separation of Th/IV/ and U/VI/ by extraction chromatography

Application of extraction chromatographic technique to the analytical separation of Th/IV/ and U/VI/ has been investigated. The stationary phase was a macroporous resin Amberlite XE-270 impregnated with undiluted trin-n-butylphosphate /TBP/ and the mobile phase was either 5.OM HNO₃ or 6M HCl. Separation of traces of Th/IV/ from large quantities of U/VI/ was achieved on a laboratory column by elution of the absorbed Th/IV/ with 6M HCl.     

Thermodynamic studies of mixed ionic/nonionic surfactant systems

Mixtures of alkyltrimethylammonium bromide (CnTAB, n=12, 14, 16, 18) and Triton X-100 were studied at a range of mole fractions of ionic surfactant per nonionic surfactant. For each mixture, the cmc obtained from surface tension measurements differed from that obtained using potentiometry. The behavior of these mixed-surfactant systems showed three different regions with increasing total surfactant concentration. From the surface tension and potentiometry data, we obtained the free monomer concentration of ionic surfactant (mi), the micellar mole fraction of surfactant (xi), and the degree of dissociation (alpha) of ionic surfactant. We also obtained the free monomer concentration of Triton X-100 (m2) using PFG-NMR technique. A new equation was introduced to evaluate the activity coefficient in the micellar phase. The excess free energy (GE) and the synergetic parameters of mixtures were determined at various mole fractions of CnTAB/Triton X-100. Finally, the complexity of the synergism parameters was investigated.     

Swift heavy ion induced effects at Mo/Si interface and silicide formation

Swift heavy ion (SHI) induced modification at metal/Si interfaces has emerged as an interesting field of research due to its large applications. In this study, we investigate SHI‐induced mixed molybdenum silicide film with ion fluences. The molybdenum thin films were deposited on silicon substrates using e‐beam evaporation at 10^?8 torr vacuum. Thin films were irradiated with Au ions of energy 120 MeV to form molybdenum silicide. The samples were characterized by grazing incidence X‐ray diffraction (GIXRD) technique for the identification of phase formation at the interface. Rutherford backscattering spectrometry (RBS) was used to investigate the elemental distribution in the films. The mixing rate calculations were made and the diffusivity values obtained lead to a transient melt phase formation at the interface according to thermal spike model. Irradiation‐induced effects at surface have been observed and roughness variations at the surface were calculated using atomic force microscopy (AFM) technique. Copyright © 2009 John Wiley & Sons, Ltd.     

An etching technique for morphological investigation of TPU/ABS blends by SEM

Blends of thermoplastic polyurethane elastomer (TPU) and ABS resin (acrylonitrile-butadiene-styrene) were observed by SEM (scanning electron microscopy) before and after their treatment with methyl ethyl ketone (MEK). Samples were treated with MEK for different periods of time and dried at two temperatures in order to optimize the etching conditions. It was found that 3 h of etching is adequate to reveal the phase morphology of these blends. In contrast, a 4 h period has provoked serious artifacts in the samples and no information about phase structure could be obtained. At appropriate conditions, this technique can be used to quantitatively estimate the component dispersion in these blends.     

Morphology-controlled synthesis of Al/Fe2O3 nano-composites via electrospinning

In this article, nano-scale Al/Fe₂O₃ composites with different morphologies were successfully obtained by a simple electrospinning technique, which is based on a surfactant (polyvinyl pyridine, PVP) in a mixture of N,N-dimethylformamide (DMF) and 2-propanol. The electrospun Al/Fe₂O₃ composites exhibited a crystal structure and phase composition by X-ray diffraction analysis. The different morphologies of the Al/Fe₂O₃ composites were also observed through scanning electron microscopy and transmission electron microscopy. It was found that the rather simple electrospinning method used to prepare the morphology-controlled Al/Fe₂O₃ composites may have the potential for preparation of propellants, explosives, and pyrotechnics in the future.     

Preparation of Mn2O3 and Mn3O4 nanofibers via an electrospinning technique

Thin PVA/manganese acetate composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibers, Mn₂O₃ and Mn₃O₄ nanofibers with a diameter of 50-200 nm could be successfully obtained. The fibers were characterized by TG-DTA, Scanning electron microscopy, FT-IR, WAXD, respectively. The results showed that the crystalline phase and morphology of nanofibers were largely influenced by the calcination temperature.     

Preparation and characterization of BiFeO3 ceramic

From the technological point of view, the mutual control of electric and magnetic properties is an attractive possibility, but the number of candidate materials is limited. One of them, BiFeO₃, has critical conditions for synthesizing single phase since the temperature stability range of the phase is very narrow. Hence, various aspects of BiFeO₃ system have to be studied.

Fine particles of BiFeO₃ are obtained using a wet chemical route (combustion technique) and compared with the same product prepared by classic solid state reaction. The sintering programs have been varied in order to investigate the mechanism reactions and to show the relation between the microstructures and the magnetoelectric behavior.

The samples are characterized by using various techniques: X-ray diffraction (XRD) study is carried out for phase determination and lattice parameter calculations; scanning electron microscopy (SEM-EDX) and TEM to find out grain size and morphology; differential thermal analysis (DTA) to determine transformations of the starting materials. The obtained bulk materials were characterized (density, porosity, etc.) and correlated with the phase composition present in the samples. Electric and magnetic properties were evaluated.

This study underlines the role of the preparation route on the structural and morphological characteristic of the obtained materials and their influence on the magnetoelectric behavior.     

Analysis of Precipitation Hardening of 6061/10% SiC Composite by Differential Scanning Calorimetry

The precipitation of a supersaturated 6061 Al alloy reinforced with 10% SiC_pwas monitored by using a DSC technique. DSC thermal curves were used to predict peak-aging temperatures and durations. The activation energies for precipitation of the β″ phase were found to increase with elevation of the solution temperature from 510 to 600°C, and hence the peak-aging temperature and duration also increased. Microstructural examination revealed an increase in grain size when a high solution temperature was applied. To compare predicted peak-aging temperatures and durations, hardness measurements were carried out after artificial aging. The studies revealed that peak-aging hardening was obtained when the aging temperatures and durations corresponded to about 95% to 97% precipitation of β″ phase from conversion plots. This revised version was published online in July 2006 with corrections to the Cover Date.