Ion mixing at 20 keV: a comparison of the effects of Ga+, Ar+ and CF4+ ion irradiation

Medium-energy (some tens of keV) ion irradiation is frequently used in various technologies. It is well known that during this irradiation serious alterations are introduced to the material, changing its structure, composition, etc. While there are studies on the amorphization, no results have been reported on the medium-energy ion beam-induced mixing, however. In this work, we present Auger electron spectroscopy (AES) depth profiling measurements of Si/Cr multilayer samples, which were irradiated by various ions (Ga+, Ar+, CF4+) of 20 keV applying angles of incidence of 5 degrees (Ga+), 65 degrees (Ga+) and 75 degrees (Ar+, CF4+). The ion beam-induced mixing at the Si/Cr interface (the broadening of the interface) was measured as a function of the removed layer thickness. The weakest and strongest ion mixing (for a given removed layer thickness) were found for CF4+ and Ga+ 5 degrees irradiations, respectively. In the case of Ga+ irradiation, the larger the angle of incidence the weaker the ion mixing. The extent of mixing does not correlate with the corresponding projected range. Comparison of the experimentally measured ion mixed profiles with those given by dynamic TRIM simulations gave poor agreement for Ar+ and fails for Ga+ irradiations, respectively.     

Fast three-dimensional nanoscale metrology in dual-beam FIB–SEM instrumentation

A quantitative surface reconstruction technique has been developed for the geometric characterization of three-dimensional structures by using a combined focused ion beam—scanning electron microscopy (FIB–SEM) instrument. A regular pattern of lines is milled at normal incidence on the sample to be characterized and an image is acquired at a large tilt angle. By analyzing the pattern under the tilted view, a quantitative estimation of surface heights is obtained. The technique has been applied to a test sample and nanoscale resolution has been achieved. The reported results are validated by a comparison with atomic force microscopy measurements.     

Column-by-column compositional mapping by Z-contrast imaging

A phenomenological method is developed to determine the composition of materials, with atomic column resolution, by analysis of integrated intensities of aberration-corrected Z-contrast scanning transmission electron microscopy images. The method is exemplified for InAs_xP_1−x alloys using epitaxial thin films with calibrated compositions as standards. Using this approach we have determined the composition of the two-dimensional wetting layer formed between self-assembled InAs quantum wires on InP(0 0 1) substrates.     

Statistical analysis of atom probe data: Detecting the early stages of solute clustering and/or co-segregation

Statistical analysis of atom probe data has improved dramatically in the last decade and it is now possible to determine the size, the number density and the composition of individual clusters or precipitates such as those formed in reactor pressure vessel (RPV) steels during irradiation. However, the characterisation of the onset of clustering or co-segregation is more difficult and has traditionally focused on the use of composition frequency distributions (for detecting clustering) and contingency tables (for detecting co-segregation).     

Transmission electron microtomography without the "missing wedge" for quantitative structural analysis

A three-dimensional (3D) visualization and structural analysis of a rod-shaped specimen of a zirconia/polymer nanocomposite material were carried out by transmission electron microtomography (TEMT) with particular emphasis on complete rotation of the specimen (tilt angular range: +/-90 degrees ). In order to achieve such an ideal experimental condition for the TEMT, improvements in the specimen as well as the sample holder were made. A rod-shaped specimen was necessary in order to obtain a high transmission of the specimen upon tilting to large angles. The image resolution of the reconstructed tomogram was isotropic, in sharp contrast to the anisotropic image resolution of the conventional TEMT with a limited angular range (the "missing wedge" problem). A volume fraction of zirconia, phi, evaluated from the 3D reconstruction was in quantitative agreement with the known composition of the nanocomposite. A series of 3D reconstructions was made from the tilt series with complete rotation by limiting the maximum tilt angle, alpha, from which a couple of structural parameters, the volume fraction and surface area per unit volume, Sigma, of the zirconia, were evaluated as a function of alpha. It was confirmed from actual experimental data that both phi and Sigma slightly decreased with the increasing alpha and reached constant values at around alpha=80 degrees , suggesting that the specimen may have to be tilted to +/-80 degrees for truly quantitative measurements.     

Interpretation of Oxygen K pre-edge peak in complex oxides

A controversial pre-edge peak has often been observed at the O K-edge in absorption spectra from complex oxides. We study this feature in both K(2)O-SiO(2) glass and MgAl(2)O(4) spinel crystals. Our time-resolved energy-loss spectroscopy (EELS) results indicate that the pre-edge peak is due to radiation damage, rather than from any intrinsic feature of the material. It is assigned to the pi* peak due to the O-O interaction.     

Maximum diameter of the rod-shaped specimen for transmission electron microtomography without the "missing wedge"

In our recent study, the complete rotation of a rod-shaped specimen during transmission electron microscopy (TEM) has been successfully carried out, yielding a truly quantitative three-dimensional (3D) structure of a ZrO(2)/polymer nano-composite. This result allows the further development of transmission electron microtomography (TEMT) for materials science. The diameter of the rod-shaped specimen was about 150 nm, which may not be statistically large enough to evaluate structural parameters, e.g., volume fraction of Zr nano-particles. Thus, it is preferable to image rods with larger diameters in 3D. In this study, several rod-shaped specimens whose diameters ranged from 150 to 530 nm were subjected to the "distortion-free TEMT". The maximum diameters, l, observable under 200 and 300 kV-TEMTs were, respectively, 460-470 and 600-670 nm (corresponding the maximum relative diameters, l/lambda (lambda: mean free path), were ca. 2.2 and 2.7-3.0).     

Observation of three-dimensional elemental distributions of a Si device using a 360 degrees -tilt FIB and the cold field-emission STEM system

A technique for preparation of a pillar-shaped specimen and its multidirectional observation using a combination of a scanning transmission electron microscope (STEM) and a focused ion beam (FIB) instrument has been developed. The system employs an FIB/STEM compatible holder with a specially designed tilt mechanism, which allows the specimen to be tilted through 360 degrees [T. Yaguchi, M. Konno, T. Kamino, T. Hashimoto, T. Ohnishi, K. Umemura, K. Asayama, Microsc. Microanal. 9 (Suppl. 2) (2003) 118; T. Yaguchi, M. Konno, T. Kamino, T. Hashimoto, T. Ohnishi, M. Watanabe, Microsc. Microanal. 10 (Suppl. 2) (2004) 1030]. This technique was applied to obtain the three-dimensional (3D) elemental distributions around a contact plug of a Si device used in a 90-nm technology. A specimen containing only one contact plug was prepared in the shape of a pillar with a diameter of 200nm and a length of 5mum. Elemental maps were obtained from the pillar specimen using a 200-kV cold-field emission gun (FEG) STEM model HD-2300C equipped with the EDAX genesis X-ray energy-dispersive spectrometry (XEDS) system through a spectrum imaging technique. In this study, elemental distributions of minor elements with weak signals were enhanced by applying principal component analysis (PCA), which is a superior technique to extract weak signals from a large dataset. The distributions of elements, especially the metallization component Ti and minor dopant As in this particular device, were successfully extracted by PCA. Finally, the 3D elemental distributions around the contact plug could be visualized by reconstruction from the tilt series of maps.     

Characterisation of the early stages of solute clustering in 1Ni–1.3Mn welds containing Cu

Microstructural characterisation of neutron irradiated low alloy steels is important for developing mechanistic understanding of irradiation embrittlement. This work is focused on the early stages of irradiation-induced clustering in a low Cu (0.03 wt%), high Ni (∼1 wt%) weld. The weld was irradiated at a very high dose rate and then examined by atom probe (energy-compensated position-sensitive atom probe (ECOPoSAP) and local electrode atom probe (LEAP)) with supporting microstructural information obtained by small angle neutron scattering (SANS) and positron annihilation (PALA).     

Automated three-dimensional analysis of particle measurements using an optical profilometer and image analysis software

The automated collection of topographic images from an optical profilometer coupled with existing image analysis software offers the unique ability to quantify three‐dimensional particle morphology. Optional software available with most optical profilers permits automated collection of adjacent topographic images of particles dispersed onto a suitable substrate. Particles are recognized in the image as a set of continuous pixels with grey‐level values above the grey level assigned to the substrate, whereas particle height or thickness is represented in the numerical differences between these grey levels. These images are loaded into remote image analysis software where macros automate image processing, and then distinguish particles for feature analysis, including standard two‐dimensional measurements (e.g. projected area, length, width, aspect ratios) and third‐dimensional measurements (e.g. maximum height, mean height). Feature measurements from each calibrated image are automatically added to cumulative databases and exported to a commercial spreadsheet or statistical program for further data processing and presentation. An example is given that demonstrates the superiority of quantitative three‐dimensional measurements by optical profilometry and image analysis in comparison with conventional two‐dimensional measurements for the characterization of pharmaceutical powders with plate‐like particles.     

Site-specific fracture plane determination using the FIB/TEM

A new method for the determination of the crystallographic indices of planar fracture surfaces is described. The key innovation is the use of a focused ion beam instrument to extract two transmission electron microscopy (TEM) foils from the fracture surface. Selected area diffraction of these foils in the TEM allows the determination of the fracture plane from the cross product of two crystallographic line directions contained within the plane. This allows the indices to be determined from relatively small fracture surfaces, affording fracture plane determinations from facets on polycrystalline samples. The validation of this method using cleavage fracture in pure zinc is described.     

Imaging and analysis of 3-D structure using a dual beam FIB

The application of focused ion beam instrumentation in the generation of three-dimensional microstructural data is described. The methodologies used to acquire and manipulate this data are explained, and the technique is illustrated by a number of examples from the material sciences. The limitations of this method, and practical pointers to the generation of meaningful data, are also discussed.     

Atom probe specimen fabrication methods using a dual FIB/SEM

A dual FIB/SEM provides solutions to many challenges in atom probe specimen preparation. When combined with an in situ lift-out capability, the versatility of this tool allows almost any region of interest, in almost any geometry, to be placed at the apex of a specimen tip. Several preparation techniques have been developed in response to specific application requirements; for example, in cases where materials are not suitable for electropolishing, or where site-specific analysis is required. Two general techniques, with wide-ranging potential applications, are described in detail here. The first is a 'cut-out' technique that provides a relatively quick means of micro-tip specimen preparation from bulk material samples. The second method is a 'lift-out' technique that can be used in an in situ or ex situ mode and does not require the preparation of pre-sharpened mounting points.     

FIB preparation and SEM investigations for three-dimensional analysis of cell cultures on microneedle arrays

We report the investigation of the interfaces between microneedle arrays and cell cultures in patch-on-chip systems by using Focused Ion Beam (FIB) preparation and Scanning Electron Microscopy (SEM). First, FIB preparations of micro chips are made to determine the size and shape of the designed microneedles. In this essay, we investigate the cell-substrate interaction, especially the cell adhesion, and the microneedle's potential cell penetration. For this purpose, cross-sectional preparation of these hard/soft hybrid structures is performed by the FIB technology. By applying the FIB technology followed by high-resolution imaging with SEM, new insights into the cell-substrate interface can be received. One can clearly distinguish between cells that are only in contact with microneedles and cells that are penetrated by microneedles. A stack of slice images is collected by the application of the slice-and-view setup during FIB preparation and is used for three-dimensional reconstruction of cells and micro-needles.     

Analysis of defects on BN nano-structures using high-resolution electron microscopy and density-functional calculations

Cubic boron nitride (c-BN) nucleation takes place on hexagonal boron nitride (h-BN) layers growing perpendicular to the substrate surface during thin film synthesis. Studies focused on the nucleation of the cubic phase suggest the possibility that transient phases and/or defects on these h-BN structures have a role in sp3-bonded cubic phase nucleation. In this study, we have investigated the nature, energetics, and structure of several possible defects on BN basal planes, including point defects, 4-, and 5-fold BN rings, that may possibly match the experimentally observed transient phase fine structure. TEM image observations are used to build approximate atomic models for the proposed structures, and DFT calculations are used to relax these structures while minimizing their respective total energies. These optimized atomic geometries are then used to simulate TEM images, which are compared to the experimentally observed structures. Data from DFT calculations and analysis of simulated images from the proposed atomic structures suggest that 4-fold BN rings are more likely to exist on the transient phase possibly leading to c-BN nucleation.     

Triaxial joint moment estimation using a wearable three-dimensional gait analysis system

We developed a wireless sensor system composed of a mobile force plate system, three-dimensional (3D) motion sensor units and a wireless data logger. Triaxial joint moments of the ankle, knee and hip joints were calculated using measurements of the sensor system. The accuracy of the joint moment estimation is validated against results obtained from the reference measurement system composed of a camera based motion analysis system and force plates. Triaxial joint moments measured by the sensor system showed normalized root mean square error (NRMSE) and correlation coefficient (R) of less than 22% and more than 0.80 in comparison with the stationary system.     

General three-dimensional image simulation and surface reconstruction in scanning probe microscopy using a dexel representation

The ability to image complex general three-dimensional (3D) structures, including reentrant surfaces and undercut features using scanning probe microscopy, is becoming increasing important in many small length-scale applications. This paper presents a dexel data representation and its algorithm implementation for scanning probe microscope (SPM) image simulation (morphological dilation) and surface reconstruction (erosion) on such general 3D structures. Validation using simulations, some of which are modeled upon actual atomic force microscope data, demonstrates that the dexel representation can efficiently simulate SPM imaging and reconstruct the sample surface from measured images, including those with reentrant surfaces and undercut features.     

Study on effect of hydrogen treatment on amorphous carbon film using scanning probe microscopy

Amorphous carbon film was treated by hydrogen plasma. The change of surface structure, conductivity, and work function distribution is characterized by scanning probe microscope technique and local electron emission is also analyzed. We find that chemical effect of hydrogen plasma on the a-C film is small, but the etching effect is strong and the surface morphology and conductance are obviously changed after hydrogen treatment. Electron emission enhancement is not due to the decrease of work function or existence of sp² conductive channels, but from the mutual effect between sp² and sp³ phase. We suggest that the enhancement is due to the internal electron injection from the sp²-rich interface layer into the surface sp³-rich grains.     

Determination of the Fe content of embedded Cu-rich particles in ferritic alloys using energy-filtered TEM

A novel technique for the quantification of the iron content of copper precipitates in ferritic steels is presented. Energy-filtered (EF) imaging has been used to extract elemental maps with high spatial resolution. These maps contain enough information to attempt the quantification of the signal produced by the precipitates when either a line profile is measured across them or the whole image signal is integrated. Assumptions such as sphericity of the precipitates and composition variations are discussed. Special attention to the assessment of drift on the information extracted from EF images has been taken. Minimum detectability and optimum acquisition conditions are discussed.