Preparation of polyimide-epoxy composites

The formation of a three dimensional network of crosslinked epoxy leads all unmodified epoxies to have inherent brittleness and relatively low degradation temperatures. Polyimides, on the other hand, are widely used for applications that require high degrees of flexibility and thermal resistance. Here, we have focused on the preparation of epoxy systems cured with polyamic acids instead of traditional amino-group-containing hardening agents. The cure behavior and potential reaction mechanisms of EPON 828 resin and polyamic acid mixtures were evaluated by DSC and TGA. Thermal analysis showed a complex reaction sequence taking place in the mixture and also determined the extent of reaction of the polyamic acid with itself and the competitive reaction of the polyamic acid with the epoxy. The compositions of the mixtures were varied to see the dependence of the cure behavior on component concentrations. Solutions of the two components did not phase separate and also phase separation was not apparent either optically or microscopically in the cured samples. This phase behavior was attributed to a unique in situ reaction. A novel solvent system for the polyamic acid precursor was also used.     

激光扫描共焦荧光显微镜的电子控制系统研究

介绍了激光扫描共焦荧光显微镜的电子控制系统，为了提高激光扫描器的定位精度，在系统中提出采用基于闭环象素时钟发生器的检流计振镜所固有的扫描非线性失真补偿方案，减少输出图象的枕形畸变，实现行扫描空间位置的均匀性。在以细分梯形波电流驱动反应式步进电机情况下，根据实测θｉ曲线，用反插法求得与步进电机运行非均匀性相补偿的相电流波，从而获得在小电流情况下高角度均匀的步进电机细分运行特性。     

Minimizing sample evaporation in the environmental scanning electron microscope

The ElectroScan environmental scanning electron microscope (ESEM) enables wet samples to be observed by eliminating air but allowing water vapour into the sample chamber. However, evaporation from, and condensation on, the sample may occur during the pumpdown sequence used to reach this state, which means that the sample may not be in its natural state when viewed if due care is not taken. In this paper, the pumping system of the ESEM is described mathematically and expressions are derived for the evaporation and condensation. This treatment is then used to calculate the optimum pumpdown sequence. The importance of using the optimized procedure is illustrated by micrographs of fat emulsions.     

The As-prepared surfaces of C-axis-oriented Nd1Ba2Cu3Oy thin films characterized using scanning probe microscopes

Recently, superconducting Nd₁Ba₂Cu₃O_y (Ndl23) thin films with high superconducting transition temperature (T _c) have been successfully fabricated at our institute employing the standard laser ablation method. In this paper, we report the results of surface characterization of the Nd123 thin films using an ultrahigh vacuum scanning tunneling microscope/spectroscopy (UHV-STM/STS) and an atomic force microscope (AFM) system operated in air. Clear spiral pattern is observed on the surfaces of Nd123 thin films by STM and AFM, suggesting that films are formed by two-dimensional island growth mode. Contour plots of the spirals show that the step heights of the spirals are not always the integer or half-integer number of thec-axis parameter of the structure. This implies that the surface natural termination layer of the films may not be unique. This result is supported byI-V STS measurements. The surface morphology of the Nd123 thin films is compared with that of thec-axis-oriented Y₁Ba₂Cu₃S_y thin films. Surface atomic images of the as-prepared Nd123 thin films are obtained employing both STM and AFM. STS measurements show that most of the surfaces are semiconductive. The results of STS measurements together with the fact that we are able to see the surface atomic images using scanning probe microscopes suggest that exposure to air does not cause serious degradation to the as-prepared surfaces of Nd123 thin films.     

Laser scanning path generation considering photopolymer solidification in micro-stereolithography

It is essential to automate the scanning path generation process to effectively implement the micro-stereolithography. However, a scanning path that is generated based only on a 3D CAD model introduces dimensional inaccuracies. In micro-stereolithography, the photopolymer solidification is affected by fabrication conditions, such as the optical properties (laser power, laser scanning speed, laser scanning pitch focusing condition, etc.) and material properties of the photopolymer. Thus, the photopolymer solidification phenomena must be considered when generating a laser scanning path. In this paper, a scanning path generation algorithm that uses 3D CAD data and considers the photopolymer solidification phenomena is proposed to improve the dimensional accuracy in micro-stereolithography. Multi-line photopolymer solidification experiments were performed for various laser scanning conditions to examine the photopolymer solidification phenomena. From these experiments, linear relations between the solidification length (width) and scanning length (width) were acquired and stored in a database. Subsequently, these data were utilized to compensate the scanning path of the laser beam. In addition, experiments for determining the layer thickness in the z-direction were performed and these results were also used in the scanning path generation algorithm.This research was supported by the Highly Advanced National Project (http://www.most.go.kr), which performs some of the National R&D Program, and sponsored by the Korean Ministry of Science and Technology under the contract project code M10214000116-02B1500-02010.     

An Investigation of Milk Powders Produced by a Laboratory-Scale Spray Dryer

A mini spray dryer has been used to investigate morphological changes that occur to milk particles during the spray drying process. We have found that the mini spray dryer is ideal for such investigations, because phenomena such as skin and vacuole formation in particles can be analyzed without the added complication of particle agglomeration, which only occurs in much larger spray dryers where particle number concentrations are higher. We have confirmed observations made by various researchers that the bulk density of spray-dried milk powder is greatly affected by the drying temperature, due to the strong influence of the latter on the porosity of the particles. In addition, we have attempted to explain observations made by various workers that fat accumulates preferentially at the surface of a particle during drying by postulating that fluid fat is transported towards the surface, via a network of cracks and pores, by the development of a vacuole overpressure which is also responsible for the inflation of the particle. Finally, we have shown that milk powders can be spray dried a second time, by reconstitution with water, with no change to the thermodynamic characteristics of the resultant powder. Thus, milk concentrates for spray drying research can be prepared from already-spray-dried milk powders rather than using the more arduous evaporation method to concentrate unprocessed milk.     

自聚焦共焦探测系统轴向分辨率的影响因素

从微小内尺度测量角度出发，研究了针孔尺寸、探测器位置、透镜的数值孔径、放大倍率和杂散光等对自聚焦共焦式探测系统轴向分辨率的影响。结果表明，为提高系统的轴向分辨率，需将有效针孔尺寸控制在≤2.5；探测器需配以精密微调整装置以实现横向精确定位；选用差动共焦光路及大数值孔径和大放大倍率的自聚焦透镜，同时，偏振光路的使用将有效的提高系统的信噪比。     

低温聚合物结构松弛的数值研究

为了获得低温聚合物的参数和升降温速率对连续升降温无量纲比热容的影响,应用差示扫描量热法(DSC)和TNM的结构松弛模型作出简单的数值研究.结果表明,变换不同比率的升降温速率及不同参数值得到的DSC曲线图形变化能够对聚合物的结构松弛研究有一点参考作用.     

Scanning electron microscope electron detector with a radial type discrete dynode electron multiplier

A discrete dynode electron multiplier with radial flux of electrons was built and tested in the range of low‐voltage scanning electron microscopy as a backscattered electron detector of topographic contrast. The multiplier collects backscattered electron emitted in a specific range of take‐off angles and over the whole azimuth angular range enabling large solid collection angle. Multipliers with different dynode shapes were studied theoretically with the use of the software for particle optics and three assemblies were built and tested experimentally. The gain estimation, assessment of the type of detected electrons (secondary electron or backscattered electron), imaging the spatial collection efficiency and signal‐to‐noise measurements were performed.     

The use of the scanning electron microscope in the determination of the mineral composition of Ballachulish slate

Slate is a fine-grained, low-grade metamorphic rock derived from argillaceous sediments or occasionally volcanic ash. Although most slates contain mainly quartz, chlorite and white mica, they vary considerably in their durability, some lasting centuries while others fail after a few years of service. A detailed characterisation of their mineralogy is required for the assessment of performance, and to establish the provenance of a used slate. A combination of methods was used to examine Ballachulish slates; XRD analysis to determine the principal minerals present, XRF analysis to determine the total chemical composition, and scanning electron microscopy to determine the chemical composition of individual minerals. It was found that the white mica in Ballachulish slate is phengite and the chlorite is ripidolite. Feldspar is present as albite and carbonate as ferroan dolomite. Several accessory minerals were also identified, including chloritoid, monzonite and zircon. There was considerable variation in the ratio of the principal minerals, making it impossible to identify used slates by this criterion. Instead, chemical composition of the individual minerals, and possibly key accessory minerals, should be used to determine the provenance of slates.