Influence of accelerated ageing on methacrylate‐based denture resins heterogeneity as viewed by ESR‐spin‐probe method

The electron‐spin‐resonance (ESR) spin‐probe method, was used to study the heterogeneity of denture resins based on poly(methyl methacrylate). Results for three resins processed by microwave energy, conventional curing and cold curing (depending on the curing procedure and exposed to ageing in various environmental conditions) were compared. All three cured resins were stored over the same time (1200 h) in distilled water at ambient temperature and in artificial saliva at 348 K. The temperature‐dependent ESR spectra of a spin probe dispersed in the denture resins are analyzed in terms of line‐shapes and line‐widths. The appearance of two spectral components was taken as an indication of resin heterogeneity. The results reveal that the cold‐cured resin has a lower local density in comparison with microwave and conventionally cured resin. The amount of residual monomer also contributes to the local motion of polymer segments. The change of denture resins exposed to ageing is influenced both by the structure of the original resin and the ageing conditions. Restricted motion of a spin probe incorporated into the acrylic resins exposed to accelerated ageing suggests additional crosslinking of polymer chains. The differences are observed for all the investigated resins, but the highest change is observed with the cold‐cured resin. The ESR results are accompanied by T_g and T_m measurements. Copyright © 2005 Society of Chemical Industry     

Investigation of Centreline Segregation and Centreline Porosity in CC ‐ Slabs

Improvements of solidification processing in conventional or near net shape casting depend on sophisticated methods of macroscopic examination of central unsoundness and inhomogeneity of the cast material. As long as remarkable deviations referring to the quality features exist between the slab centre and the bulk material such methods should be looked after. Two semi‐macroscopic methods of segregation analysis are discussed in this paper: firstly, the potential of the emission spectral analysis combined with sectioning of a sample and secondly, the computer aided micro‐probe analysis. Both methods are restricted to small local areas. The proneness of elements and steel grades with respect to micro‐ and macrosegregation as well as distribution‐ and segregation coefficients are determined. The effect of a diffusion anneal on homogenisation of segregation is studied. Last not least the precipitation of sulphides, phosphides or carbonitrides is estimated. Ultrasonic detection of the central unsoundness of conventional slabs or thin slabs is a new approach towards a quantitative macroscopic examination. The sample size is 400 mm x 300 mm x 30 mm. To achieve a low ultrasonic noise using a 5 MHz‐transducer the samples are heat treated for grain refinement. “Dog bone porosity”, macroscopic topographical misfit between the upper and lower solidifying shells, periodical corner cracks or systematic transverse centre cracks are detected. Obviously, segregations do not reflect the ultrasonic beam. However, it can be presumed that an interrelation exists between porosity and segregation, although these might be locally apart from each other. This new ultrasonic test of the central unsoundness of continuous cast (c.c.) slabs gives valuable arguments to machine builders and maintenance people to decide on the right concepts for strand guidance, support rollers and secondary cooling. Soft reduction can be optimized and variations in casting speed counteracted by dynamic means. R&D service of this kind can help steelmakers when decisions are impending to build new casting machines or revamp old ones.     

A new stereological principle for test lines in three-dimensional space

A new principle is presented to generate isotropic uniform random (IUR) test lines hitting a geometric structure in three-dimensional space (3D). The principle therefore concerns the estimation of surface area, volume, membrane thickness, etc., of arbitrary structures with piecewise smooth boundary. The principle states that a point-sampled test line on an isotropic plane through a fixed point in 3D is effectively an invariant test line in 3D. Particular attention is devoted to the stereology of particles, where an alternative to the surfactor method is obtained to estimate surface area. An interesting case arises when the particle is convex. The methods are illustrated with synthetic examples.     

Measurement of specimen charging in scanning electron microscopy with a kelvin probe

A vibrating Kelvin probe in form of a platinum wire loop is used to measure the surface potential U_s on electron-irradiated free-floating metal and insulator specimens as a function of electron energy E. This allows an accurate measurement of the critical electron energy E₂ for no charging. At energies below E₂, the positive charging increases with decreasing energy to U_s=2–5 eV at E=0.5 keV and switching off the collector bias of the Everhart-Thornley detector. A two-to threefold increase of U_s is observed when the bias is switched on. For E > E₂, the strong increase of a negative surface potential can be measured. Insulating films free-supported on a conductive substrate show a steep decrease to small positive and negative U_s when the film thickness becomes lower than the electron range at a critical energy E₃ > E₂. At insulating specimen the temporal decrease of charging can be measured when the electron beam is switched off.     

方块电阻测试中的有限元理论

介绍了用有限元方法计算半导体方块电阻四探针测试中二维点电流势场的模型并且证明了其正确性。由于有限元方法对边界没有限制，该方法为方块电阻测试中精确确定边界修正系数，更重要的是为微样品测试结构确定提供直接明了的理论依据。     

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.     

小型微/纳米级三坐标测量机的研制

介绍一套低成本小型三维坐标测量机的研制过程，作为微/纳米级超精密测量设备，整体机台结构采用花岗岩材料；X／Y轴的移动平台利用压电材料摩擦驱动与挠性变形原理，长短两行程可达25mm范围及5nm的微位移，藉自行研发的衍射干涉激光尺，位置回馈测量系统可具有0．025nm的分辨率；测量探头在一般DVD光读取头的自动聚焦原理基础上改装，最佳分辨率可达2．5nm，该雏形机适于测量微机电组件、微型器件及膜厚等。     

基于SPM技术的纳米信息存储薄膜的研究进展

扫描探针显微技术SPM可以在原子或分子尺度上对表面进行表征和修饰，应用SPM技术可以在薄膜表面形成纳米级的信息点阵，特别适合发展超高密度的信息存储，是一种非常有希望代替传统磁存储，光存储的纳米级存储技术，本文介绍了纳米信息存储薄膜的研究进展，并对其制备技术和读写机制进行了初步的探讨。     

用二次离子质谱和扩展电阻探针技术测量硅中注入硼的深度分布及扩展电阻探针技术分辨率的估算

利用二次离子质谱和扩展电阻探针技术测量了硅中注入硼的深度分布 .在适当的测量深度 ,用扩展电阻探针技术测得的结果对二次离子质谱技术测量的结果进行了标定 ,从而得到硅片中硼原子的深度分布 .用近似模型估算了扩展电阻探针针尖半径对测试分辨率的影响 .若探针针尖半径为r0 ,测量斜面的角度为 ξ ,在用扩展电阻探针技术测量载流子浓度的深度分布时 ,可以近似认为深度分辨率为 7 86r0 sinξ.还定性讨论了样品表面耗尽层对扩展电阻探针技术的影响.     

微区电阻测试方法及新测试仪研制

文章对国内外开展微区薄层电阻测试的方法进行了综述，特别对改进范德堡四探针技术方法的测试原理、测试过程与测试结果进行了论述与分析，对微区电阻测试方法的进一步发展提出了一种可操作的方法，并研制出新型四探针测试样机。