Mechanical elasticity of vapour-liquid-solid grown GaN nanowires

Mechanical elasticity of hexagonal wurtzite GaN nanowires with hexagonal cross sections grown through a vapour-liquid-solid (VLS) method was investigated using a three-point bending method with a digital-pulsed force mode (DPFM) atomic force microscope (AFM). In a diameter range of 57-135?nm, bending deflection and effective stiffness, or spring constant, profiles were recorded over the entire length of end-supported GaN nanowires and compared to the classic elastic beam models. Profiles reveal that the bending behaviour of the smallest nanowire (57.0?nm in diameter) is as a fixed beam, while larger nanowires (89.3-135.0?nm in diameter) all show simple-beam boundary conditions. Diameter dependence on the stiffness and elastic modulus are observed for these GaN nanowires. The GaN nanowire of 57.0?nm diameter displays the lowest stiffness (0.98?N?m(-1)) and the highest elastic modulus (400 ± 15?GPa). But with increasing diameter, elastic modulus decreases, while stiffness increases. Elastic moduli for most tested nanowires range from 218 to 317?GPa, which approaches or meets the literature values for bulk single crystal and GaN nanowires with triangular cross sections from other investigators. The present results together with further tests on plastic and fracture processes will provide fundamental information for the development of GaN nanowire devices.     

Estimation of wood stiffness and strength properties of hybrid larch by near-infrared spectroscopy

This work was undertaken to investigate the feasibility of near-infrared (NIR) spectroscopy for estimating wood mechanical properties, i.e., modulus of elasticity (MOE) and modulus of rupture (MOR) in bending tests. Two sample sets having large and limited density variation were prepared to examine the effects of wood density on estimation of MOE and MOR by the NIR technique. Partial least squares (PLS) analysis was employed and it was found that the relationships between laboratory-measured and NIR-predicted values were good in the case of sample sets having large density variation. MOE could be estimated even when density variation in the sample set was limited. It was concluded that absorption bands due to the OH group in the semi-crystalline or crystalline regions of cellulose strongly influenced the calibrations for bending stiffness of hybrid larch. This was also suggested from the result that both alpha-cellulose content and cellulose crystallinity showed moderate positive correlation to wood stiffness.     

Vibration-dependent morphology and crystal structure of isotactic polypropylene

A small homemade device was used to study the influence of mechanical vibration on the crystal structure and morphology of isotactic polypropylene (iPP) under different melting temperatures, vibration times, vibration frequencies, and cooling rates. The crystallite size, crystal structure, and crystallinity of iPP under or without vibration treatment were investigated by means of differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), and polarized microscopy observation (PLM). The crystallization of iPP varied with the length of vibration time, vibration frequency, cooling rate, and melt temperature. Compared with the data of conventional samples measured by DSC, vibration could increase the crystallinity of iPP, make melting peak of α-crystal move toward higher temperature and make that of β-crystal shift to lower temperature. Meanwhile, WAXD measurements showed that the vibration could reduce the content of β-crystal evidently, particularly at the lower vibration frequency, lower cooling rate, and higher melting temperature. Furthermore, PLM measurements showed that the vibration made the spherulite size smaller.     

PET/PC共混物配比对其高压结晶行为的影响

利用SEM及W AXD等测试手段研究了配比对PET/PC共混物高压结晶行为的影响。SEM观察表明,随PC比例的增加,共混物高压下主要结晶形态以伸直链晶体,生长成熟的立体开放球晶,大尺寸球晶的方式变化。拟合分峰法和W arren-A verbach傅氏分析法的计算结果表明,随PC含量的增加,高压结晶共混物的结晶度降低,PET的平均晶粒尺寸总体呈减小趋势,晶粒尺寸分布则变窄,而晶格畸变平均值在一定PC比例范围内达到极大值。     

Influence of certain media on properties of polycaprolactam

The kinetics of absorption of working media (water, benzene, kerosene) and the variation in the elasticity modulus in relation to the degree of absorption and degree of crystallinity of polycaprolactam were studied. It was shown that water produces a considerable reduction in the elasticity modulus of caprone, the effect becoming more pronounced with decreasing degree of crystallinity. In time the elasticity modulus becomes stable even though water continues to be absorbed. Benzine and kerosene appear to be inert with respect to caprone.     

SPM characterization of pulsed laser deposited nanocrystalline CrN hard coatings

Nanocrystalline CrN coatings, widely required for surface engineering application covering wear and corrosion resistance, need to be investigated for atomic scale morphology, surface roughness, local stiffness, phase uniformity, and homogeneity. Evolution of these properties as a function of thickness need to be studied. In this paper, we have attempted to address these issues through use of a multimode scanning probe microscope (SPM) equipped to carry out Atomic Force Microscopy (AFM) and Atomic Force Acoustic microscopy (AFAM) of Chromium nitride films (100-500 nm thick) on Si prepared under high vacuum by pulsed Laser Ablation using Nd-YAG Q-switched laser. Prior to SPM analysis, the coatings were annealed in N2 atmosphere at 700 degrees C for 30 minutes for improving crystallanity and coating substrate adhesion. The GIXRD patterns of these annealed specimens showed formation of nanocrystalline CrN. Also signature of amorphous phases was seen. The grain size was estimated to be less than 30 nm. Contact mode AFM imaging revealed a roughness value less than 50 nm. Local stiffness values were calculated from AFM force-distance curves. Imaging of frictional force and surface flaws are being investigated by Frictional Force Microscopy (FFM), resonance spectroscopy, and AFAM, respectively. The contrast in AFAM images is seen due to variation in surface elasticity in reference and CrN samples. Stiffness constant and elastic modulus were calculated for both the samples and compared.     

聚苯硫醚及其纤维增强复合材料的等温结晶形态

采用热台偏光显微镜技术观察了聚苯硫醚(PPS)及其玻璃纤维、 炭纤维及芳纶纤维增强复合材料等温结晶过程中球晶结构形态的变化。研究了等温结晶温度对PPS的晶体形态及球晶生长速率的影响。结果表明, 结晶温度对PPS的结晶影响非常明显。在235~265℃, 随着等温结晶温度的升高, 聚苯硫醚球晶形态发生了从细小而具有部分束状结构到大而完善再到细小而不完善的变化过程, 球晶的生长速率随着结晶温度的增大呈非线性下降。而纤维的存在使PPS的结晶形态发生了从球晶结构到横穿晶的变化, 且不同纤维诱导形成横穿晶的程度有所不同。其中玻璃纤维和芳纶纤维可以诱导形成较为明显的横穿晶形态, 而炭纤维则不能诱导形成明显的横穿晶。      

High molecular weight polyethylene nanospheres: synthesis physical and mechanical properties

The high molecular weight (MW) polyethylene (PE) particles of particle size varied from macro to micron to nanometer were synthesized by Grignard reagent. The microscopy analysis (scanning electron microscope, SEM; transmission electron microscope, TEM; and atomic force microscope, AFM) shows the spherical shape of PE particles. The effects of particle size, varies from macro to nanometer scale on crystal structure, crystallinity (chic), glass transition temperature (Tg), melting temperature (Tm), surface roughness and mechanical properties were studied. Differential scanning calorimetry (DSC) experiments show that the nanoparticles of PE are highly crystalline (chic approximately equal 72%). The crystal length of PE nanoparticles is found to be approximately 14 A. Although the Gibbs-Thomson equation is explained the depression of melting temperature (DeltaTm) by 5 degrees C, the impervious results of Tg are still not fully understood. The low roughness value (2 A) proves the presence of "atomic-scale-chain" folding at the surface of PE nanoparticles. A novel protocol is developed, and the elastic modulus of individual nanospherical PE particles is computed from 'force-distance' mapping curves of AFM. Hemispherical tungsten (W) tip was fabricated from focused ion beam and used as an indenter to measure the mechanical properties. It is found that the nano sized PE particles have higher elastic modulus (E = 1.2-1.4 GPa) compared to the bulk or macro sized PE (E = 0.6-0.7 GPa). The results corroborate the robustness of our experiments, since, the analogous results for macro sized particles match well with the literature.     

高取向聚乙烯的形态与晶体形变

采用ＳＥＭ和ＷＡＸＤ分析了高取向ＨＤＰＥ的形态,晶粒尺寸及结晶度,ＨＤＰＥ经口模拉伸,形态由台材料的微球状结构转变为纤维结构,随着拉伸比的提高,晶粒沿拉伸方向（ｃ轴）的尺寸增大,横向（ａ,ｂ轴）尺寸减小,有序性提高,结晶度增大,口模温度提高,晶粒沿ａ,ｂ,ｃ轴的尺寸均增大,有序性和结晶度提高,表明口模拉伸过程中既存在应力诱导的结晶过程,又存在温度诱导的二次重结晶过程。     

Mechanical properties of alkali treated plant fibres and their potential as reinforcement materials II. Sisal fibres

The tensile strength and Young’s modulus of sisal fibre bundles were determined following alkalisation. The results were then analysed with respect to the diameter and internal structure such as cellulose content, crystallinity index and micro-fibril angle. The tensile strength and stiffness were found to vary with varying concentration of caustic soda, which also had a varying effect on the cell wall morphological structure such as the primary wall and secondary wall. The optimum tensile strength and Young’s modulus were obtained at 0.16% NaOH by weight. The stiffness of the sisal fibre bundles obtained using the cellulose content also referred to as the micro-fibril content was compared with the stiffness determined using the crystallinity index. The stiffness obtained using the crystallinity index was found to be higher than that obtained using the cellulose content however, the difference was insignificant. Alkalisation was found to change the internal structure of sisal fibres that exhibited specific stiffness that was approximately the same as that of steel. These results indicates that the structure of sisal fibre can be chemically modified to attain properties that will make the fibre useful as a replacement for synthetic fibres where high stiffness requirement is not a pre-requisite and that it can be used as a reinforcement for the manufacture of composite materials.     

Estimation of modulus of elasticity of plastics and wood plastic composites using a Taber stiffness tester

This study measured the modulus of elasticity (MOE) of various plastics and composite materials with a Taber stiffness tester as an alternative to conventional universal testing machines. The proposed approach presents an expedited means to assess MOE for a wide range of plastics and wood plastic composites (WPCs) with various shapes. The Taber stiffness units and the geometry of the samples acted as the basis for the calculation of the MOE. The results showed a high correlation between the MOE calculated from Taber units and that obtained on a universal testing machine (Instron). Concurrently, Taber units showed the potential to assess stiffness of samples with irregular shapes, such as in the case of extruded rods, which exhibit this characteristic.     

Effect of annealing temperature on the tribological behavior of ZnO films prepared by sol-gel method

The tribological behavior of zinc oxide (ZnO) films grown on glass and silicon (100) substrates by sol-gel method was investigated. Particularly, the as-coated films were post-annealed at different temperatures in air to investigate the effect of annealing temperature. Crystal structural and surface morphology of the films were measured by X-ray diffraction (XRD) and Atomic Force Microscopy (AFM). XRD patterns and AFM images indicated that the crystallinity and grain size of the films were enhanced and increased, respectively, with temperature. The tribological behavior of films was evaluated by sliding the ZnO films against a Si₃N₄ ball under 0.5 gf normal load using a reciprocating pin-on-plate tribo-tester. The wear tracks of the films were measured by AFM to quantify the wear resistance of the films. The results showed that the wear resistance of the films could be improved by the annealing process. The wear resistance of the films generally increased with annealing temperature. Specifically, the wear resistance of the films was significantly improved when the annealing temperature was higher than 550° C. The increase in the wear resistance is attributed to the increase in hardness and modulus of the film with annealing temperature.     

In situ observation of the spherulite deformation in polybutene-1 (Modification I)

Stress-strain behaviour under uniaxial tension was determined for polybutene-1 specimens with various spherulite sizes and degrees of crystallinity. Samples with large spherulites and a high crystallinity level exhibited a very specific behaviour, characterized by a higher elastic modulus, a remarkably homogeneous deformation (absence of necking), a stress whitening phenomenon and a brittle intraspherulitic rupture. The deformation mechanisms have been analysed by means of in situ microscopic observations. It was shown that interlamellar separation, which occurred first in the equatorial regions perpendicular to the tensile axis, is mainly responsible for the observed phenomena.     

Effect of glass-fibre reinforcement and annealing on microstructure and mechanical behaviour of nylon 6,6

The effects of glass fibres and annealing on the microstructures and spherulitic morphology of a glass fibre-reinforced nylon 6,6 were investigated. The annealing effects on matrix crystallinity of nylon 6,6 composites with varying glass fibre contents were measured and the morphology of the composites were examined using both the microtomed bulk samples and thin composite films prepared by melt crystallization. It was found that fibre breakage during injection moulding was significant for composites with glass content higher than 20 wt%, and the spherulite size as well as the crystallinity were reduced by the additions of glass fibres. Upon annealing, the start of a log time rate increase of matrix crystallinity was delayed by the addition of glass fibres. Glass fibre-induced transcrystallinity was not observed in injection-moulded composites; however, columnar spherulites were found to develop along the glass fibres in melt-crystallized thin composite films. Differences in morphological observations between the two sample preparation methods are also discussed.     

Microhardness,chemical etching,SEM, AFM and SHG studies of novel nonlinear optical crystal – l-threonine formate

The crystal l-threonine formate, an organic NLO crystal was synthesized from aqueous solution by slow evaporation technique. The grown crystal surface has been analyzed by scanning electron microscopy (SEM), chemical etching and atomic force microscopy (AFM). SEM analysis reveals pyramidal shaped minute crystallites on the growth surface. The etching study indicates the occurrence of etch pit patterns like striations and step like pattern. The mechanical properties of LTF crystals were evaluated by mechanical testing which reveals certain mechanical characteristics like elastic stiffness constant (C₁₁) and young's modulus (E). The Vickers and Knoop microhardness studies have been carried out on LTF crystals over a range of 10–50 g. Hardness anisotropy has been observed in accordance with the orientation of the crystal. AFM image shows major hillock on growth surface. The second harmonic generation (SHG) efficiency has been tested by the Kurtz powder technique using Nd:YAG laser and found to be about 1.21 times in comparison with standard potassium dihydrogen phosphate (KDP) crystals.     

The influence of crystal habit on the prediction of dry powder inhalation formulation performance using the cohesive-adhesive force balance approach

The aim of this investigation was to study the influence of crystalline habit of active pharmaceutical ingredients on the cohesive-adhesive force balance within model dry powder inhaler (DPI) formulations and the corresponding affect on DPI formulation performance. The cohesive-adhesive balance (CAB) approach to colloid probe atomic force microscopy (AFM) was employed to determine the cohesive and adhesive interactions of micronized budesonide particles against the {102} and {002} faces of budesonide single crystals and crystalline substrates of different sugars (cyclodextrin, lactose, trehalose, raffinose, and xylitol), respectively. These data were used to measure the relative level of cohesion and adhesion via CAB and the possible influence on in vitro performance of a carrier-based DPI formulation. Varying the crystal habit of the drug had a significant effect on the cohesive measurement of micronized budesonide probes, with the cohesive values on the {102} faces being approximately twice that on the {002} crystal faces. However, although different CAB values were measured with the sugars with respect to the crystal faces chosen for the cohesive-based measurement, the overall influence on the rank order of the CAB values was not directly influenced. For these data sets, the CAB gradient indicated that a decrease in the dominance of the adhesive forces led to a concomitant increase in fine particle delivery, reaching a plateau as the cohesive forces became dominant. The study suggested that crystal habit of the primary drug crystals influences the cohesive interactions and the resulting force balance measurements of colloid probe CAB analysis.     

成核剂对聚丙烯结晶形态及冲击断裂行为的影响

对加入有效成核剂（加入量为0．1－2．0％）的聚丙烯材料进行了缺口冲击实验，发现其冲击强度在成核剂加入量0．4％处出现极大值，通过测定其结晶度和球晶尺寸的变化发现，当有效成核剂加入量小于0．4％时，随加入量增大，球晶尺寸呈下降趋势，结晶度呈上升趋势；当前有效成核剂加入量大于0．4％时，随加入量增大，球晶尺寸的下降趋势变小且逐渐趋于稳定，而结晶度仍呈上升趋势，另一方面，通过断口观察和分析发现，其断面形态特征参量－扩展区的断面分形维数值成核剂加入量的变化与结晶形态和冲击强度的变化相对应，即在成核剂0．4％加入量处出现极大值，实验结果分析表明，通过加入某种有效成核剂对PP共混，其结晶形态的变化与其冲击强度的变化相对应，并且这种对应关系通过断面特征形态尺寸的变化反映出来。     

Carbon-nanofibre-reinforced poly(ether ether ketone) fibres

Nano-reinforced fibres were spun from a semicrystalline high-performance poly(ether ether ketone) containing up to 10 wt% vapour-grown carbon nanofibres using conventional polymer processing equipment. Mechanical tensile testing revealed increases in nanocomposite stiffness, yield stress, and fracture strength for both as-spun and heat-treated fibres. X-ray and differential scanning calorimetry analyses were performed in order to investigate both the orientation of nanofibres within the polymer matrix and the matrix morphology. The carbon nanofibres were found to be well aligned with the direction of flow during processing. Significantly, the degree of crystallinity of the poly(ether ether ketone) matrix was found to increase with the initial addition of nanofibres although the crystal structure was not affected. The measured increase in composite tensile modulus is compared to injection-moulded nanocomposite samples made from the same blends. The results highlight the need to characterise the matrix morphology when evaluating nanocomposite performance and hence deducing the intrinsic properties of the nanoscale reinforcement.     

Non-isothermal crystallization of poly(ε-caprolactone)-grafted multi-walled carbon nanotubes

Non-isothermal crystallization behavior of poly(ε-caprolactone) (PCL)-grafted multi-walled carbon nanotubes (MWNTs) was studied in order to determine the effects of functionalized MWNTs (f-MWNTs) on its crystallization behavior. Differential scanning calorimeter measurements showed that an introduction of f-MWNTs into the PCL molecules induced heterogeneous nucleation and the crystal growth process was significantly affected. X-ray diffraction showed a decrease in the crystallinity of composites with the addition of f-MWNTs in PCL, likely due to the occurrence of more heterogeneous nucleation induced by f-MWNTs in the samples. The activation energy for crystallization of PCL drastically reduced with the presence of 2 wt.% f-MWNTs in the samples and increased slightly with increasing content of f-MWNTs. A spherulite structure of PCL-grafted MWNTs with MWNTs at the center was developed, clearly indicating the nucleating action of MWNTs in the crystallization process. The experimental data were also analyzed using various kinetic models e.g., Avrami, Tobin, Ozawa, etc.     

The Influence of Crystal Habit on the Prediction of Dry Powder Inhalation Formulation Performance Using the Cohesive–Adhesive Force Balance Approach

The aim of this investigation was to study the influence of crystalline habit of active pharmaceutical ingredients on the cohesive–adhesive force balance within model dry powder inhaler (DPI) formulations and the corresponding affect on DPI formulation performance. The cohesive–adhesive balance (CAB) approach to colloid probe atomic force microscopy (AFM) was employed to determine the cohesive and adhesive interactions of micronized budesonide particles against the {102} and {002} faces of budesonide single crystals and crystalline substrates of different sugars (cyclodextrin, lactose, trehalose, raffinose, and xylitol), respectively. These data were used to measure the relative level of cohesion and adhesion via CAB and the possible influence on in vitro performance of a carrier-based DPI formulation. Varying the crystal habit of the drug had a significant effect on the cohesive measurement of micronized budesonide probes, with the cohesive values on the {102} faces being approximately twice that on the {002} crystal faces. However, although different CAB values were measured with the sugars with respect to the crystal faces chosen for the cohesive-based measurement, the overall influence on the rank order of the CAB values was not directly influenced. For these data sets, the CAB gradient indicated that a decrease in the dominance of the adhesive forces led to a concomitant increase in fine particle delivery, reaching a plateau as the cohesive forces became dominant. The study suggested that crystal habit of the primary drug crystals influences the cohesive interactions and the resulting force balance measurements of colloid probe CAB analysis.