Poly(lactic acid)/poly(butylene succinate)/calcium sulfate whiskers biodegradable blends prepared by vane extruder: Analysis of mechanical properties,morphology, and crystallization behavior

Ternary blends of PLA/PBS/CSW with different weight fractions were prepared using a vane extruder. The mechanical properties, morphology, crystallization behavior and thermal stability of the blends were investigated. For the PLA/CSW blend, the tensile strength decreased, the flexural strength and modulus increased compared with pure PLA. For PBS, the addition of CSW had little influence on the mechanical properties. For the ternary blends PLA/PBS/CSW, the tensile strength, flexural strength and modulus decreased compared with pure PLA, while the elongation at break and the impact strength increased significantly. The brittle-ductile transition of the blends took place when the PBS weight fraction reaching 30 wt%. As a soft component in the blends, PBS was beneficial to improve the tensile ductility and the toughness of PLA. SEM measurements reveal that PLA/PBS/CSW blends were immiscible. When the weight fraction of PBS was 50 wt%, significant phase separation was observed, and CSW had preferential location in the PBS phase of the blend. DSC measurement and POM observation reveal that CSW had a heterogeneous nucleation effect on PLA and PBS matrix. The addition of PBS improved the crystallization of PLA and the thermal resistance of the PLA/PBS/CSW blends significantly.     

Mineralization of simulated flue gas to prepare CaCO3 whisker using suspended CaSO4

CaCO₃ whiskers were synthesized controllably by introducing simulated flue gas containing CO₂ and N₂ into a CaSO₄ suspension. The effects of solution pH, reaction temperature, and simulated flue gas on the formation of CaCO₃ whiskers were studied. The growth mechanism and growth model of CaCO₃ whiskers had also been provisionally recommended. The reaction product was characterized by scanning electron microscopy analysis, thermogravimetric analysis, and X-ray diffraction analysis. CaCO₃ whiskers with 97% purity were synthesized at pH 7.5, 80°C, 0.1 L/min CO₂ flow rate, and 16.7% CO₂ purity, with a length between 15 and 20 μm and an aspect ratio of about 12.     

Dynamic mechanical analysis of the interphase in bacterial polyester/cellulose whiskers natural composites

Nanocomposite materials were prepared from an elastomeric poly(hydroxyoctanoate) (PHO) latex as a fully amorphous or semi-crystalline matrix using a colloidal suspension of hydrolyzed cellulose whiskers as natural and biodegradable filler. After stirring, the preparations were cast and evaporated. High performance materials were obtained from these systems, preserving the natural character of PHO. Interfacial phenomena were assumed to be noticeable owing to the high specific area of this filler. Dynamic mechanical analysis was performed on these systems to test the influence of the interphase on the molecular mobility of the amorphous phase. To quantify the distance away from the surface at which the molecular mobility is restricted, a physical model was used to predict the mechanical loss angle. This allows removal of the filler reinforcement effect keeping only the interfacial effect. It was shown that the local motion at the filler-matrix interface of amorphous PHO chains is strongly affected when an amorphous PHO was used as the matrix. No significant change was observed when a semi-crystalline PHO was used as the matrix. This result was ascribed to a possible trancrystallization phenomenon of semi-crystalline PHO in contact with cellulose whisker surface, which prevents any contact between amorphous PHO chains and filler surface.     

莫来石晶须/堇青石表面层的制备及准超疏水性能

采用溶胶-凝胶法制备了硅铝混合凝胶粉体, 再通过熔盐反应在堇青石陶瓷基体上生长莫来石晶须, 制得莫来石晶须/堇青石表面层微结构. 表征结果表明, 莫来石晶须紧密生长在堇青石基体上, 晶须直径为100~300 nm, 长度可达几个微米. 莫来石晶须表面含有大量Si—OH和Al—OH极性亲水基团, 采用十二烷基三甲氧基硅烷与活性基团间的偶联反应将非极性基团引入莫来石晶须表面, 获得了静态润湿角为146°的莫来石晶须/堇青石表面层. 动态润湿研究表明, 合成的莫来石晶须增大了堇青石陶瓷的表面粗糙度, 使亲水的莫来石晶须/堇青石表面更加亲水, 而硅烷偶联剂修饰的堇青石/莫来石晶须表面则成为准超疏水表面.     

Properties and Morphology of Poly(Lactic Acid)/Calcium Carbonate Whiskers Composites Prepared by a Vane Mixer based on an Extensional Flow Field

Binary composites of poly(lactic acid) (PLA)/calcium carbonate whiskers (CCW) with different weight fractions were prepared with a vane mixer based on extensional rheology. The mechanical properties, thermostability, crystallization behavior, rheology behaviors and micromorphology of the composites were analysed to study the effect of the CCW fibers on the composite's properties; a pure PLA sample was also prepared for comparison. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) revealed that the CCW fibers had excellent compatibility with the PLA matrix and the CCW fibers were dispersed and distributed evenly in the PLA matrix under the action of the extensional flow field produced by the vane mixer. Differential scanning calorimetric (DSC) analysis showed that introducing a vane mixer into the PLA processing could increase the degree of crystallization (χ_c) of the composites significantly, and moderate CCW fibers adding could further increase its χ_c value. Thermogravimetric analysis (TGA) revealed that adding the CCW fibers reduced the thermostability of the composites. The G′, G″, η* and the torque, T_N, of the composites, obtained from rheology analyses, declined obviously, because of the hydrolysis and chains scission induced by residual water and fatty acid when the CCW content less than 4%. Tensile tests proved that filling moderate amounts of CCW fibers into PLA could increase its tensile strength and strain at break, increasing by 5% and 29.6%, respectively.     

T-ZnO晶须化学镀铜复合粉体的制备及其电磁性能的研究

采用化学镀的方法制备了Cu包覆四脚状氧化锌晶须(T-ZnO晶须)的复合粉体.使用X射线衍射分析仪(XRD)进行了物象分析,扫描电镜(SEM)观察了粉体的形貌.运用能谱仪(EDS)进行了成份分析.结果表明,晶须为纯氧化锌,晶体结构为六方晶系纤锌矿结构,镀层为纯铜. SEM观察晶须外观形貌为四脚状结构.同时使用波导法对T-ZnO晶须和化学镀铜得到的Cu/T-ZnO晶须复合粉体进行了电磁参数的测量.微波电磁性能试验表明,化学镀后晶须的微波吸收性能明显增加,在频率为13 GHz处反射率可达－12 dB左右,而且最大吸收峰的频率随铜析出量的不同而发生改变,这样有利于实现吸收频带的展宽.     

Synthesis and characterization of superhydrophobic magnesium oxysulfate whiskers

Superhydrophobic materials have attracted much attention for their special wettability. In this study, magnesium oxysulfate (MOS) whiskers were surface modified by vinyltrimethoxysilane (VTMS) and prepared as superhydrophobic materials, which are expected to be widely used in self-cleaning, corrosion prevention, and oil-water separation. The factors of silane concentration, hydrolysis time, reaction temperature, and reaction time were investigated. The superhydrophobic MOS whiskers were synthesized. SEM and XRD turned out that there were no apparent changes in the morphology and crystallization behavior of whiskers before and after modification, while the surface was uniformly coated with a layer of non-crystal material, and the surface of the whiskers employed a chemical bond Si–O–Mg covalently connected. The thermogravimetric analysis ultimately demonstrated that surface modification was beneficial to the improvement of the thermal stability of MOS whiskers. Superhydrophobic MOS whiskers showed good compatibility with organic solvents through oil-water separation experiments, and demonstrated excellent self-cleaning performance. The methodology for the surface treatment of MOS whiskers to prepare superhydrophobic whiskers in this work may be extended for other whiskers or fillers, which may be promising for the preparation of superhydrophobic materials.     

Surface treatment of magnesium oxysulfate whiskers through plasma polymerization

The surface of magnesium oxysulfate (MOS) whiskers was treated through plasma polymerization to increase the compatibility between the MOS whiskers and a polymer matrix. Different plasma parameters were chosen to determine the most hydrophobic coating. The surface structure of the plasma-treated MOS whiskers was examined. The MOS whiskers retained their crystal structure after plasma treatment, as shown by X-ray powder diffraction (XRD) analyses. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy analyses revealed that a polymer sheath was formed on the surface of the MOS whiskers, and interfacial chemical bonds were generated between the polymer sheath and the MOS whiskers. The thin-layer polymer sheath was uniform around the entire surface of the MOS whiskers and exhibited a typical amorphous structure, as determined by transmission electron microscopy (TEM) combined with selected area electron diffraction (SAED) analyses. The possible reaction mechanism on the surface of the MOS whiskers under plasma treatment was then proposed. Finally, the effect of surface treatment was evaluated by scanning electron microscopy (SEM), measurement of the contact angle and contact angle hysteresis, and torque rheometer. Results showed that plasma treatment could markedly increase the hydrophobicity of the MOS whiskers' surface, effectively reducing the agglomeration and improving the dispersibility of the MOS whiskers in the matrix, which results in the improved compatibility between the MOS whiskers and the polyvinyl matrix, as well as the processability of the composites.     

Preparation of copper aluminum borate whiskers via flux method

Single‐crystal and uniform copper aluminum borate whiskers have been synthesized by heating a mixture of boric acid, copper sulfate and aluminum sulfate with potassium sulfate as flux at 870 °C for 4 h. The synthesized whiskers exhibit a well‐crystallized, one‐dimensional structure with diameters ranging from 100 nm to 5 μm, lengths from 5 to 100 μm. Heating temperature and flux addition affect the aspect ratio and morphology of the copper aluminum borate whiskers. A possible growth mechanism of the whiskers is proposed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)