A portable cryo-storage system for low-temperature scanning electron microscopy,suitable for international transport of cryo-specimens

A cryo-specimen storage system for low-temperature scanning electron microscopy (LTSEM) specimens is described, which: liberates multi-specimen experiments from sampling restrictions imposed by the rate at which LTSEM specimens can be examined in the SEM; provides security against experiment loss resulting from breakdown of the SEM or cryo-system; enables collection of specimens in the field or in laboratories remote from the SEM laboratory; and facilitates international air transport of LTSEM specimens. The components of the system, which has a capacity of 98 stub-mounted specimens, are readily made in a laboratory workshop. The details of the design may be altered to suit particular specimen types or experimental approaches.     

On the applied stress dependence of the subgrain size

The present work studies the collection of experimental data from which Raj and Pharr (Mater. Sci. Eng., 81 (1986) 217) deduced a universal empirical dependence of the subgrain size on the applied stress. In accord with their result and some theoretical predictions the normalized subgrain size d_s/b was ssumed to be proportional to G/σ (G is the shear modulus, b the Burgers vector length, σ the applied stress). The evaluated factor of proportionality K₁, having the value within the interval from 0.76 to 180 in the inspected data sets, was discussed from the point of view of various factors which can influence the experimental data.     

The effect of particle distribution on damage formation in particulate reinforced metal matrix composites deformed in compression

Image analysis results are reported on the generation of damage in particulate reinforced metal matrix composites during compressive deformation. The technique allows the automated collection of data on the incidence of particle fracture and void formation in the matrix as a function of important microstructural parameters such as local particle volume fraction and particle size. There is a strong relationship between damage and the local volume fraction of the reinforcement proving that damage formation is accentuated in regions of particle clustering. With the SiC reinforced materials examined, there was observed to be a change in dominance of damage mechanism from particle fracture at low local volume fractions to void formation in the matrix within strongly clustered regions. The results are compared with finite element (FE) modelling of the compressive deformation of clustered particles using a simple cluster of equi-spaced particles. The FE results suggest that plastic flow is generally inhibited in clustered regions. In certain highly clustered configurations shielding is such that flow does not occur in the heart of the cluster even at high levels of average plastic strain. The modelling suggests that the change in dominance of damage mechanism is related to the dramatic increase in tensile hydrostatic stresses in the matrix with higher levels of particle clustering.     

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。     

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.     

Structure of soya glycinin and conglycinin gels

Gels of glycinin and conglycinin formed at various heating temperatures, in the absence and presence of 0.2M sodium chloride were characterised by transmission electron microscopy. In distilled water both proteins formed gels consisting of strands with a thickness of 10–15 nm. The strands of glycinin were very regular and cross sections of strands showed a hollow cylindrical structure. In the presence of sodium chloride, glycinin formed an aggregated gel structure at 85°C, but at 95°C an ordered strand structure was formed. Dissociation of the quaternary structure on heating and reassociation of subunits into regular strands were considered the most probable mechanisms for strand formation from glycinin. The aggregated structure at 85°C was interpreted as a transient state prior to dissociation. Conglycinin rich gels were less regular and more crosslinked than gels of glycinin. Also, the strands of conglycinin showed a complex mode of aggregation possibly in the form of double spirals. The addition of sodium chloride caused a denser and more aggregated structure at 75 and 85°C, but the effects were not as drastic as in the case of glycinin. Heating temperature had only minor effects on the gel structure in the range studied.     

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.     

A novel technique to prepare LiNbO3 at low temperature

Fresh niobium hydroxide was first precipitated from NbF₅ solution using an aqueous ammonium hydroxide under basic conditions. Then a simple procedure of mixing lithium and niobium hydroxides together and heating at a low temperature (400 °C) produced pure ultrafine single phase LiNbO₃ (LN). In the literature, this is the lowest temperature so far reported on the formation of LN. The phase content and lattice parameters are determined by X-ray diffraction (XRD). The average particle size and morphology were studied by transmission electron microscopy (TEM).