In situ dynamic HR-TEM and EELS study on phase transitions of Ge2Sb2Te5 chalcogenides

The phase transition phenomena of Ge2Sb2Te5 chalcogenides were investigated by in situ dynamic high-resolution transmission electron microscopy (HR-TEM) and electron energy loss spectroscopy (EELS). A 300kV field emission TEM and a 1250kV high voltage TEM were employed for the in situ heating experiments from 20 to 500 degrees C for undoped and 3wt% nitrogen-doped Ge2Sb2Te5 thin films deposited by DC sputtering. Crystallization of amorphous Ge2Sb2Te5 to its cubic structure phase started at 130 degrees C and then rapid crystal growth developed from cubic to hexagonal phase in the range of 130-350 degrees C; finally, the hexagonal crystals started to melt at 500 degrees C. For nitrogen-doped Ge2Sb2Te5, its crystallization from amorphous film occurred at higher temperature of ca. 200 degrees C, and the cubic and hexagonal phases were usually formed simultaneously without significant growth of crystals at further heating to 400 degrees C. EELS measurements showed that the electronic structures of Ge, Sb and Te stayed almost the same regardless of the amorphous, FCC and hexagonal phases. The nitrogen doped in Ge2Sb2Te5 was confirmed to exist as a nitride. Also, the doped nitrogen distributed homogeneously in both amorphous and crystalline phases. Localization of doped nitrogen was not found in the grain boundary of crystallized phases. The dynamic process of phase transition was enhanced by high-energy electron irradiation. Peeling of atomic layers in nitrogen-doped Ge2Sb2Te5 film was detected during heating assisted with electron beam irradiation.     

Characterization of nanoscale recording mark on Ge2Sb2Te5 film

We have fabricated nanoscale recording marks on Ge(2)Sb(2)Te(5) (GST) films with conductive atomic force microscope (AFM). GST films were deposited on glass or polyimide film with thickness of 150-200nm by the rf-sputtering method. Through current-voltage (I-V) spectroscopy, good cantilevers for fabrication and characterization of nanoscale marks on GST were selected. A fresh and highly conductive tip showed voltage-switching characteristic in the I-V curve, where the threshold voltage was approximately 1.6V. Nanoscale dot and wire arrays of crystalline phases were successfully obtained by varying sample bias voltage from -10 to 10V. With highly conductive tips, nanowires having full-width at half-maximum of approximately 20nm could be fabricated, whereas nanowires could not be fabricated with bias voltage below -2V. The width of the nanoscale mark was increased by repetition of AFM lithography even with same applied voltage and lithography speed. For a thicker nanowire, the width measured in current-image (C-image) was observed to be approximately 2 times of that measured in topography-image (T-image). This result supports that current sensing provides an image of phase-changed GST area with higher resolution than topography sensing.     

A simple model for the prediction of thermal conductivity of Ge2Sb2Te5 thin film

A modified version of the Mayadas-Shatzkes (MS) model is proposed for the prediction of the thermal conductivity of both amorphous and crystalline of Ge₂Sb₂Te₅ (GST) phase-change materials at room temperature. The structural parameters of the original MS model are extended to describe the additional disorder scattering effects caused by the ternary components of the GST. The effect of disorder due to the alloy composition on the grain boundary scattering can be interpreted with the aid of thermal models. It is also found that for all phases of GST, the contribution of disorder scattering to the thermal resistance is nearly uniform. This is consistent with the fact that the GST phase changes without any destruction of the structural basis such as the building blocks.     

Scanning electron microscope design for quantitative multicontrast

Conceptual designs of scanning electron microscopes (SEMs) using a time-of-flight electron spectrometer are presented. The procedure for making quantitative measurements with such SEMs is shown to be much simpler and versatile than using conventional SEMs. SEMs which use an electron time-of-flight spectrometer are able to operate as multicontrast analytical probes, capable of simultaneously quantifying surface topography, voltage, and material type. In addition, it is demonstrated that these SEMs can be designed to have high spatial resolution, good signal-to-noise characteristics, and to be of compact table-top size.     

In situ transmission electron microscope study of single asperity sliding contacts

Direct observation of events taking place at the contacting interfaces is important to understand many tribological phenomena. Transmission electron microscope (TEM) has the ability to look through materials at very high magnifications. Most of the TEM observations are done long after the deforming loads and stresses have been relaxed and the material state is further disturbed during the specimen preparation. We have developed a specimen holder in which two electron transparent surfaces can be brought in contact and moved relative to each other in JEOL 2000FX microscope. This holder enables visualization of not only the contacting surfaces at nanoscale but also the subsurface deformation resulting from the contact interaction. Sliding experiments have been carried out mimicking a single asperity sliding contact. A sharp tungsten probe is moved laterally against a tip mounted on a cantilever. Magnitude of the contact instability, when the contact is broken is found to be dependent on the local geometry of the contact.     

Scanning electron microscope analysis of fretting fatigue damage

Scanning electron microscope examinations of surfaces damaged by fretting fatigue were performed to establish variations in microstructural and environmental effects on the fretting fatigue process of ferrite/pearlite and martensite microstructures of a $\text{.40}\text{.50}$ carbon steel. The observations suggest differences in fretting mechanisms in laboratory air and “vacuum” conditions as well as differences due to surface hardness.     

Scanning photoelectron microscope for nanoscale three-dimensional spatial-resolved electron spectroscopy for chemical analysis

In order to achieve nondestructive observation of the three-dimensional spatially resolved electronic structure of solids, we have developed a scanning photoelectron microscope system with the capability of depth profiling in electron spectroscopy for chemical analysis (ESCA). We call this system 3D nano-ESCA. For focusing the x-ray, a Fresnel zone plate with a diameter of 200 μm and an outermost zone width of 35 nm is used. In order to obtain the angular dependence of the photoelectron spectra for the depth-profile analysis without rotating the sample, we adopted a modified VG Scienta R3000 analyzer with an acceptance angle of 60° as a high-resolution angle-resolved electron spectrometer. The system has been installed at the University-of-Tokyo Materials Science Outstation beamline, BL07LSU, at SPring-8. From the results of the line-scan profiles of the poly-Si/high-k gate patterns, we achieved a total spatial resolution better than 70 nm. The capability of our system for pinpoint depth-profile analysis and high-resolution chemical state analysis is demonstrated.     

Automated jet polishing of transmission electron microscope specimens for in situ straining

A jet-polishing technique has been developed for use in the preparation of microtensile specimens for HVEM examination. The technique requires the use of a pair of Teflon sheet inserts with rectangular openings in a conventional specimen holder. When inserts with optimum opening dimensions are used, specimens having elliptical holes close to the center of the gauge section are produced with large electron-transparent areas at both ends of the long axis. Annealed metal specimens, such as brass or aluminum, prepared by this method are stronger, and can be handled more easily, than those prepared by conventional methods. An advantage of the technique is that reproducible electropolishing conditions and the automatic detection of perforation by a photocell can be used in the normal way.     

Scanning electron microscope charging effect model for chromium/quartz photolithography masks

We propose a new method for fitting a model of specimen charging to scanning electron microscope (SEM) images. Charging effects cause errors when one attempts to infer the size or shape of a specimen from an image. The goal of our method is to enable image analysis algorithms for measurement, segmentation, and three-dimensional (3-D) reconstruction that would otherwise fail on images containing charging effects. Our model is applied to images of chromium/quartz photolithography masks and may also work in the more general case of isolated metal islands on a flat insulating substrate. Unlike methods based on Monte Carlo simulation, our simulation method does not handle more general topographies or specimens composed entirely of an insulator; it is a crude approximation to the physical charging process described in more detail in Cazaux (1986) and Melchinger and Hofmann (1985), but can be fit with quantitative accuracy to real SEM images. We only consider changes in intensity and do not model charging-induced distortion of image coordinates. Our approach has the advantage over existing methods of enabling fast prediction of charging effects so it may be more practical for image analysis applications.     

In situ laser heating in an environmental scanning electron microscope

The environmental scanning electron microscope (ESEM) offers improved capabilities for coupling a scanning electron microscope (SEM) with an in situ laser device compared with conventional SEMs. Such coupling generally enables, for example, the observation of laser glazing effects or high-temperature behaviour as well as thermal shock behaviour of materials and devices. In an ESEM, decomposition caused by high-temperature gas reactions can additionally be studied while monitoring the gaseous environment online with a mass spectrometer attached to the specimen chamber. In this work, we demonstrate the capabilities of an in situ laser system suitable for heating specimen in an in situ deformation stage, thus enabling the further study of the mechanical properties of materials far beyond temperatures accomplished by thermal heating stages.     

Scanning electron microscope imaging in liquids – some data on electron interactions in water

The electron backscattering coefficient of liquid water has been determined for electrons in the energy range 15–30 keV using Quantomix^TM capsules. Values of the mean atomic number for water estimated from a fit to the backscatter yield, the mean ionization potential of water and from Monte Carlo simulations, show that the scattering behaviour of water is not anomalous despite the effects of hydrogen bonding. Computations of the electron range, and of the mean depth for backscattering, in water as a function of incident beam energy show that water and vitreous ice are good media for imaging purposes.     

电子显微镜在金属-半导体纳米线界面原位合金化中的应用

利用原位电子显微方法研究了金属-ZnSe半导体纳米线界面合金化过程,结果表明:在脉冲电流的作用下,ZnSe纳米线可以产生明显的焦耳热效应,导致金属-ZnSe纳米线界面发生合金化反应.通过调整纳米线与金属电极的接触面积,可将焦耳热效应准确控制在界面内,进而实现纳米尺度的合金化反应.     

High-voltage electron microscope high-temperature in situ straining experiments to study dislocation dynamics in intermetallics and quasicrystals

The dynamic behaviour of dislocations in several intermetallic alloys, studied by in situ straining experiments in a high-voltage electron microscope, is compared at room temperature and at high temperatures. In contrast to room temperature, the dislocations move viscously at high temperatures, which is explained by diffusion processes in the dislocation cores. In quasicrystals, the viscous dislocation motion can be interpreted by models on the cluster scale.     

Scanning reflection electron microscopy of surface topography by diffusely scattered electrons in the scanning electron microscope

In this paper, the technique of scanning reflection electron microscopy (SREM) by diffusely scattered electrons in the scanning electron microscope is described in detail. A qualitative account of the formation of image contrast in SREM is also described. It is assumed that, for grazing geometry, forward-scattered electrons reflect from regions close to the surface, following a few scattering events within the first few atomic layers, and lose very little energy in the process. The penetration depth of the primary electrons is very limited, resulting in strongly peaked envelopes of forward-scattered electrons. It is also assumed that a surface containing topographic features presents a range of tilt angles, resulting in different reflection coefficients. Tilt contrast results because each facet has a different scattering yield, which is dependent upon local surface inclination. Full details of the instrumentation designed for SREM are described, and to illustrate the technique, results recorded from an epitaxial GaAs on GaAs crystal, Pb₂(Zr,Ta)O₆ thin film on silicon, and SiO₂ amorphous film on silicon are presented.     

Scanning electron microscope localization of zinc granules in the oyster ostrea angasi by backscattered electron imaging

A method for rapid localization of the zinc granules in oyster tissue using SEM has been developed. The results are discussed in terms of electron backscattering coefficients η for tissue, carbon support and embedding medium. Also, the application of the presented method for marine environment pollution detection and monitoring is recommended.     

Transmission electron microscope in situ fatigue experiments: A computer-control approach

A computer-control procedure was developed to facilitate in situ fatigue experiments within an intermediate voltage transmission electron microscope using a goniometer-type straining holder. The procedure was designed to allow sine-wave tension-tension cyclic loading of a microfatigue specimen similar in geometry to a center-crack panel fatigue specimen. Computer control allows greater freedom for the operator to control the experiments while providing better reproducibility from one test to another. Further development of this procedure is possible by coupling this computer-control technique with computer-controlled stage motion and digitized TV imaging.