Lock-in technique applied to cathodoluminescence of biomedical specimens in the SEM

Very low signals or disturbances by unwanted, foreign signals often lead to a restriction in the application of the cathodoluminescence (CL) method in the scanning electron microscope (SEM). This is even true if one uses an optimal CL detection system. We, therefore, introduced the lock-in-amplification technique, which has proved very successful in investigations of semiconductor materials into the biomedical field. After attaching the lock-in system to our SEM which has a special CL equipment, we found that this technique could remove the disturbance caused by the light emitted from the heated filament, which can be reflected into the CL detector. Specimens on polished Al-stubs or on Au-coated glass slides could be imaged with improved contrast. The same was true if we measured the wavelengths of the CL. A general improvement of the signal-to-noise ratio in all specimens could not be detected. However, the beam current could often be reduced when using the lock-in technique without a decrease in the quality of the CL image. A disadvantage of the commercially available lock-in amplifier is that pictures need a longer exposure time than without lock-in amplification.     

Cathodoluminescence study of semiconductor oxide micro- and nanostructures grown by vapor deposition

Nano- and microstructures of SnO(2), In(2)O(3) and ZnO have been grown during thermal treatment of compacted powders under argon flow. Indium-doped SnO(2) tube-shaped structures with rectangular cross-section are obtained by adding a fraction of In(2)O(3) to the starting SnO(2) powder. In-rich nanoislands were found to grow on some edges of the tubes. ZnO nanostructures doped with Sn or Eu were grown by adding SnO(2) and Eu(2)O(3) powder, respectively, to the ZnO precursor powder. All the samples have been characterized by the emissive and cathodoluminescence (CL) modes of scanning electron microscopy. CL images from SnO(2):In and In(2)O(3):Sn tubes and islands show a higher emission from the Sn-rich structures related to oxygen deficiency. CL of doped ZnO enables to detect the presence of dopant in specific regions or structures. CL appears to be a useful technique to study optical and electronic properties of semiconductor oxide nanostructures.     

Cathodoluminescence and computer graphics in materials science

The combination of cathodoluminescence (CL) in scanning electron microscopy (SEM) with computer graphics is proposed for studying semiconductors and dielectric materials. Spatial distribution of several types of defects that occurred naturally and by design in crystals, can be sorted out and visualized in CL mapping and in three-dimensional images reconstructed in scanning cathodoluminescence microscopy. The possibilities of this method are illustrated on magnesium oxide single crystals indented with a Vickers diamond pyramid.     

Multiscale iterative voting for differential analysis of stress response for 2D and 3D cell culture models

Focused ion beam-scanning electron microscope (FIB-SEM) tomography is a powerful application in obtaining three-dimensional (3D) information. The FIB creates a cross section and subsequently removes thin slices. The SEM takes images using secondary or backscattered electrons, or maps every slice using X-rays and/or electron backscatter diffraction patterns. The objective of this study is to assess the possibilities of combining FIB-SEM tomography with cathodoluminescence (CL) imaging. The intensity of CL emission is related to variations in defect or impurity concentrations. A potential problem with FIB-SEM CL tomography is that ion milling may change the defect state of the material and the CL emission. In addition the conventional tilted sample geometry used in FIB-SEM tomography is not compatible with conventional CL detectors. Here we examine the influence of the FIB on CL emission in natural diamond and the feasibility of FIB-SEM CL tomography. A systematic investigation establishes that the ion beam influences CL emission of diamond, with a dependency on both the ion beam and electron beam acceleration voltage. CL emission in natural diamond is enhanced particularly at low ion beam and electron beam voltages. This enhancement of the CL emission can be partly explained by an increase in surface defects induced by ion milling. CL emission enhancement could be used to improve the CL image quality. To conduct FIB-SEM CL tomography, a recently developed novel specimen geometry is adopted to enable sequential ion milling and CL imaging on an untilted sample. We show that CL imaging can be manually combined with FIB-SEM tomography with a modified protocol for 3D microstructure reconstruction. In principle, automated FIB-SEM CL tomography should be feasible, provided that dedicated CL detectors are developed that allow subsequent milling and CL imaging without manual intervention, as the current CL detector needs to be manually retracted before a slice can be milled. Due to the required high electron beam acceleration voltage for CL emission, the resolution for FIB-SEM CL tomography is currently limited to several hundreds of nm in XY and up to 650 nm in Z for diamonds. Opaque materials are likely to have an improved Z resolution, as CL emission generated deeper in the material is not able to escape from it.     

A cathodoluminescent study of quartz sand grains

Surfaces and cross sections of individual quartz sand grains have been examined in both the emissive and cathodoluminescent (CL) modes using a scanning electron microscope. The cathodoluminescent micrographs reveal sub-surface information not seen in the emissive mode micrographs. The CL features are generally associated with previous stressing, fracturing or abrasion of the grains, and are probably related to the formation of disrupted-lattice and/or amorphous quartz. The sequence of events during the formation of these features can be identified on many grains by studying the spatial distribution of the most common form of CL contrast—narrow dark bands. On other grains, irregularly distributed dark patches are generally observed to be a surface phenomenon, but the distribution, depth and intensity of these features can be studied by examining cross sections of grains. While it is common for the banded features to cross the entire specimen, it is rare for the diffuse areas to penetrate more than 30 μm. Some grains when experimentally heated above the α-β transition temperature show a marked change and even a complete reversal in CL contrast. Such studies of grains in cathodoluminescence can supplement the environmental information obtained from emissive mode micrographs of geological materials.     

Origin and significance of the SEM cathodoluminescence from zircon

In geochronological investigations, zircons are used frequently as a geological clock because of the small amounts of radioactive U isotopes and their decay products, e.g. Pb, incorporated into the crystal structure. However, the U or Pb concentration of zircon is not only dependent on the radioactive decay. One factor is the presence of old, inherited zircon cores in younger igneous zircons. This polyphase structure often cannot be recognized by conventional imaging methods, such as light microscopy. Dating such zircons, can therefore lead to ambiguous age results. However, zircons can be selected for dating purposes using cathodoluminescence (CL) in the scanning electron microscope. It is shown that zircon phases of different ages can be identified by their specific CL properties. Moreover, conclusions on the origin and on the development of the inherited phases can be drawn by comparison with detrital zircons. The zircon CL is formed by the superpostion of several broad bands. The shape of the spectra is dependent on the zircon genesis. By fitting the spectra with Gaussian curves, the individual CL bands can be separated. Using this methodology, it is possible to trace back the essential parts of the zircon CL to a superpostion of the quartz and zirconia (ZrO₂) CL. In addition, CL phenomena due to dysprosium impurities can be separated from intrinsic zircon CL properties.     

Direct metal laser fabrication: machine development and experimental work

A novel modification of the freeform technique selective laser sintering machine via system integration to develop a direct metal laser fabrication machine suitable for both nonmetal and metal materials is put forward in this paper, the aim of which is to establish an experiment platform for studying the direct metal laser fabrication (DMLF) as a variant of selective laser sintering (SLS). The system integration of two machines is realized by use of the low-power SLS Machine (CO₂, 50 W) and high-power laser processing machine (CO₂, 2,000 W) in our institute after the improvement or rebuilding of light route system, functional units, machinery and electrical system, and control software in the primary SLS machine, which means that direct metal laser fabrication machine with the laser power up to 1,000 W has been developed successfully. Functional tests of two machines and DMLF experiments of a large number of metal powders including Cu-based mixture and 316L-based mixture of powder have been done in detail. The results show that the material suitable for direct metal laser fabrication machine ranges from nonmetal powders to metal powders, including polystyrene, polyamide, polycarbonate, sands, and a large number of metal powders. At the same time, the primary functions or performances of both low-power SLS Machine and high-power laser processing machine are preserved entirely. Metal samples based on copper and 316L powders can be fabricated with the relative density of about 80% and 100%, respectively, by use of developed DMLF machine. The macro appearance and microstructure and processing mechanisms of DMLF are analyzed minutely. The academic application of DMLF machine for metal powders with high melting point has been making its mark.     

Application of a new detector for cathodoluminescence measurements in the wavelength range to 1.8 μm

The energetic gap structure of semiconductors or insulators can strongly be influenced by the local appearance of inhomogenities, impurities, dopants or vacancies. A high spatial resolution cathodoluminescence (CL) measuring technique makes it possible to investigate this gap structure via spectral analysis of the emitted CL. This can lead to a detailed knowledge of the local defect distribution. The wavelength range which could be detected by CL measurements has, up to the present, been limited to values less than 1 μm, because no detectors were available for higher wavelengths. By use of a new germanium detector, the measuring range could be extended to 1.8 μm. This makes it possible to analyse the CL properties, both of materials with small gap energies and of deep impurities. The detector properties which are important for CL measurements are presented. The efficiency of the detector is demonstrated by CL investigations of barium titanate ceramics and silicon. The results are discussed and compared to results obtained using conventional detectors.     

Material analysis with cathodoluminescence standard spectra

There are several cases where x-ray analyses of material cannot yield the desired results (e.g., if materials of nearly identical chemical composition are considered.) Spectral cathodoluminescence (CL) investigations can be used to overcome these difficulties. For this purpose, CL standard spectra of different standard substances are presented here. The validity of these spectra is demonstrated by spectral analysis of a fireproof ceramic consisting of Al₂O₃ and of quartz and by an attempt to explain the origin of the CL properties of magmatic Zircon which is of significant importance in the field of geochronological investigations.     

Developments in tribological materials in the next millennium

The materials needed for tribological contact systems in the next millennium will depend on the trend and pace of technological development, and environmental policy. The latter will certainly demand lower pollution and energy consumption, so materials should preferably be light, and work in most friction systems without lubrication, but with low friction, and no wear. The following properties, or requirements, of future tribomaterials can be conceived of in such a scenario: it seems likely that micro‐mechanical systems will achieve great importance, but silicon must be either surface protected or replaced by an optimised material; light metal alloys must be conditioned by surface treatment or coating; coatings must be improved, e.g., by nanomaterials; ceramic materials sintered at low temperatures from nano‐powders will be ductile and machinable, but retain the other beneficial properties of ceramics; and ultra‐precise surface finishing of materials may lead to nearly friction‐free and wearproof tribocontacts.     

The application of heat‐deproteinization to the morphological study of cortical bone: A contribution to the knowledge of the osteonal structure

Observation of heat‐deproteinized cortical bone specimens in incident light enabled the high definition documentation of the osteonal pattern of diaphyseal Haversian bone. This prompted a study to compare these images with those revealed by polarized light microscopy, carried out either on decalcified or thin, undecalcified, resin‐embedded sections. Different bone processing methods can reveal structural aspects of the intercellular matrix, depending on the light diffraction mode: birefringency in decalcified sections can be ascribed to the collagen fibrils orientation alone; in undecalcified sections, to both the ordered layout of collagen and the inorganic phase; in the heat‐deproteinized samples, exclusively to the hydroxyapatite crystals aggregation mode. The elemental chemical analysis documented low content of carbon and hydrogen, no detectable levels of nitrogen and significantly higher content of calcium and phosphorus in heat‐deproteinized samples, as compared with dehydrated controls. In both samples, the X‐ray diffraction (XRD) pattern did not show any significant difference in pattern of hydroxyapatite, with no peaks of any possible decomposition phases. Scanning electron microscopic (SEM) morphology of heat‐deproteinized samples could be documented with the fracturing technique facilitated by the bone brittleness. The structure of crystal aggregates, oriented in parallel and with marks of time periods, was documented. Comparative study of deproteinized and undecalcified samples showed that the matrix inorganic phase did not undergo a coarse grain thermal conversion until it reached 500°C, maintaining the original crystals structure and orientation. Incident light stereomicroscopy, combined with SEM analysis of deproteinized bone fractured surfaces, is a new enforceable technique which can be used in morphometric studies to improve the understanding of the osteonal dynamics. Microsc. Res. Tech. 79:691–699, 2016. © 2016 Wiley Periodicals, Inc.     

State-of-the-art of non-destructive measurement of sub-surface material properties and damages

The possibilities of common non-destructive measuring techniques are reviewed in this paper for their applications in precision engineering. The grazing X-ray technique is believed to be a powerful improvement of the conventional X-ray techniques under both the diffraction mode and the fluorescent mode. Information of the crystallographic structure and chemical composition can be obtained to a nanometre resolution. Ultrasound can be used in scanning acoustic microscopy to give information on the physical or even chemical nature of superficial layers. Raman spectroscopy has now become an important tool for studying superficial structures, chemical composition and stresses in cyrstalline and amorphous materials: it is recommended to use this method especially for the investigation of monocrystalline silicon and germanium. The instrumented microindentation technique is a quasi- non-destructive technique for evaluating mechanical material properties like hardness and Young's modulus in a nanometre range. It can be used on any material that does not require special surroundings like a vacuum. Photothermal microscopy has been developed recently for the non-destructive testing of the local thermal properties of materials. By using the Mirage effect and its local measurement above the surface, a non-destructive depth profiling of surface damages can be obtained.     

Electroless silver coating of rod-like glass particles

An electroless silver coating of rod-like glass particles was performed and silver glass composite powders were prepared to impart electrical conductivity to these non-conducting glass particles. The low density Ag-coated glass particles may be utilized for manufacturing conducting inorganic materials for electromagnetic interference (EMI) shielding applications and the techniques for controlling the uniform thickness of silver coating can be employed in preparation of biosensor materials. For the surface pretreatment, Sn sensitization was performed and the coating powders were characterized by scanning electron microscopy (SEM), focused ion beam microscopy (FIB), and atomic force microscopy (AFM) along with the surface resistant measurements. In particular, the use of FIB technique for determining directly the Ag-coating thickness was very effective on obtaining the optimum conditions for coating. The surface sensitization and initial silver loading for electroless silver coating could be found and the uniform and smooth silver-coated layer with thickness of 46nm was prepared at 2mol/l of Sn and 20% silver loading.     

数值模拟分析在近净成形中的运用

近净成形是零件成形后,对其进行少量加工或不加工就可以作为构件使用的技术。该技术建立在新材料、新能源、机电一体化、精密模具技术、计算机技术、自动化技术、数值模拟和分析技术等多学科和技术的基础上,改变了传统的毛坯成形方式,是使粗糙成形变成优质、高效、高精度和低成本的成形技术。本文讨论的数值模拟分析技术只是其中的一个方面,随着制造业的转型和升级,数值模拟分析技术在工艺优化中的作用将会越来越重要。     

Adaptive Gregory Patch Approximation to Z-Map Data

A method is proposed for Gregory surface approximation to 3D array data points. Surface approximation is the process of constructing a compact representation to model an object surface based on a fairly large number of measured 3D data points. Based on an adaptive subdivision technique, the proposed method begins with a rough initialisation of the surface and progressively refines it in successive steps in the regions where the data is poorly approximated. The method has been implemented using piecewise bicubic Gregory patches with G 1 continuity. An advantage of this approach is that the refinement is essentially local, reducing the computational requirements that permit the processing of a large number of data points This method, combined with the inverse offsetting method, can be used to obtain an offset surface without self-interference. The offset surface can be used to generate gouging-free CL tool paths for machining compound surfaces on milling machines.     

Thermogravimetric characterization of tyrosine and catechol adsorbed on montmorillonite

Thermogravimetric analysis is suggested as an essential methodology for studying the interaction between montmorillonite-type clays and organic molecules such as amino acids and phenolic compounds. In this work, two commercial clays, a bentonite and a montmorillonite commercially called K10, were separately put in contact with solutions of catechol and tyrosine. After the contact with the organic molecules, the powders were characterized by X-ray diffraction, infrared spectroscopy, nitrogen adsorption at 77?K, scanning electron microscopy, and thermogravimetric analysis. The thermal stability of the organic molecules on the particles’ surface depended mainly on the type of the montmorillonite clay used. This characteristic can be associated with the adsorption strength. The results show the importance of the thermogravimetric analysis for choosing the appropriate clay to be used in environmental studies or in the elaboration of industrial materials.     

An automated image alignment system for the scanning electron microscope

We have developed an automated image alignment system for the scanning electron microscope (SEM). This system enables specific locations on a sample to be located and automatically aligned with submicron accuracy. The system comprises a sample stage motorization and control unit together with dedicated imaging electronics and image processing software. The standard SEM sample stage is motorized in the X and Y axes with stepping motors which are fitted with rotary optical encoders. The imaging electronics are interfaced to beam deflection electronics of the SEM and provide the image data for the image processing software. The system initially moves the motorized sample stage to the area of interest and acquires an image. This image is compared with a reference image to determine the required adjustments to the stage position or beam deflection. This procedure is repeated until the area imaged by the SEM matches the reference image. A hierarchical image correlation technique is used to achieve submicron alignment accuracy in a few seconds. The ability to control the SEM beam deflection enables the images to be aligned with an accuracy far exceeding the positioning ability of the SEM stage. The alignment system may be used on a variety of samples without the need for registration or alignment marks since the features in the SEM image are used for alignment. This system has been used for the automatic inspection of devices on semiconductor wafers, and has also enabled the SEM to be used for direct write self-aligned electron beam lithography.     

Study on drug powder acceleration in a micro shock tube

Recently, micro shock tubes have been widely used in the medical engineering. The needle-free drug delivery device which mainly consists of a micro shock tube and an expanded nozzle has been produced to inject drug powders into human and animal bodies without any sharp metal needles. The drug powders were delivered by obtaining high momentum, which can be done by accelerating drug powders in the micro shock tube and supersonic nozzle. The particle-gas flows are induced by the incident shock wave developing by rupturing the diaphragm in the micro shock tube and again accelerated in the supersonic nozzle. The momentum of injected drug particles should be strictly controlled otherwise patients will suffer from skin injury or hurt. Even though micro shock tubes have been investigated in the past several decades, the detailed studies on particle-gas flows in the micro shock tube were rare to date due to the micro size and difficult experimental operation on micro shock tubes. In this paper, the experimental and numerical studies were carried out on investigating particle-gas flows in a designed micro shock tube. Particle tracking velocimetry (PTV) was performed to calculated particle average velocity at the exit of the supersonic nozzle. The nozzle flows were analyzed by obtaining instantaneous particle fields. The particle number density ratio was also investigated in the test section. The numerical simulations were performed by calculating unsteady Naver-Stokes equations on compressible flows and using fully implicit finite volume schemes. Discrete phase model (DPM) was used for simulating particle-gas flows in the micro shock tube. Particle diameter and density were varied to investigate their effects on the particle-gas flows. Unsteady particle-gas flows and shock wave propagation were obtained in details in the micro shock tube for present experimental and numerical studies.     

Fuzzy-Logic Based Knowledge Representation for Water Jet Cutting of Light-Weight Composites

The process of water jet cutting has advantages over laser beam cutting, especially in the case of temperature-sensitive materials. Together with the foam and cellulose material processing, the processing of composite materials of lightweight structures is becoming more and more important. In order to meet given requirements, these sandwich constructions can have various types of cover layers (defined by e.g., sheet thickness and material) and consist of core materials (differing e.g., in geometry or in structure).

Unlike simple sheets, multilayer structures have greater influence on the cutting result. When the process is planned, the CAD/CAM-systems must take all sheets of the composite material into account in order to avoid manufacturing problems. Due to the great variety of composite materials and desired contours, the necessary knowledge or experience must be efficiently represented. There is no universal system model for all these variations. This paper suggests a fuzzy-logic theory to build up a knowledge base for the water jet cutting of composite materials. The knowledge contained within the fuzzy-logic base proves to be efficient, due to the relatively high speed at which it can be acquired and due to the possibility to apply it to different structures. Development and structure of the necessary linguistic rule base are presented using sinusoidal composite material made of aluminium as an example. The expert system optimized according to the given design parameters determines the optimal cutting speed for the desired cutting contour.     

Fuzzy‐Logic Based Knowledge Representation for Water Jet Cutting of Light‐Weight Composites

The process of water jet cutting has advantages over laser beam cutting, especially in the case of temperature‐sensitive materials. Together with the foam and cellulose material processing, the processing of composite materials of lightweight structures is becoming more and more important. In order to meet given requirements, these sandwich constructions can have various types of cover layers (defined by e.g., sheet thickness and material) and consist of core materials (differing e.g., in geometry or in structure).

Unlike simple sheets, multilayer structures have greater influence on the cutting result. When the process is planned, the CAD/CAM‐systems must take all sheets of the composite material into account in order to avoid manufacturing problems. Due to the great variety of composite materials and desired contours, the necessary knowledge or experience must be efficiently represented. There is no universal system model for all these variations. This paper suggests a fuzzy‐logic theory to build up a knowledge base for the water jet cutting of composite materials. The knowledge contained within the fuzzy‐logic base proves to be efficient, due to the relatively high speed at which it can be acquired and due to the possibility to apply it to different structures. Development and structure of the necessary linguistic rule base are presented using sinusoidal composite material made of aluminium as an example. The expert system optimized according to the given design parameters determines the optimal cutting speed for the desired cutting contour.