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.     

Photofragment image analysis using the Onion-Peeling Algorithm

With the growing popularity of the velocity map imaging technique, a need for the analysis of photoion and photoelectron images arose. Here, a computer program is presented that allows for the analysis of cylindrically symmetric images. It permits the inversion of the projection of the 3D charged particle distribution using the Onion Peeling Algorithm. Further analysis includes the determination of radial and angular distributions, from which velocity distributions and spatial anisotropy parameters are obtained. Identification and quantification of the different photolysis channels is therefore straightforward. In addition, the program features geometry correction, centering, and multi-Gaussian fitting routines, as well as a user-friendly graphical interface and the possibility of generating synthetic images using either the fitted or user-defined parameters.

Program summary

Title of program: Glass OnionCatalogue identifier: ADRYProgram Summary URL:http://cpc.cs.qub.ac.uk/summaries/ADRYProgram obtainable from: CPC Program Library, Queen's University of Belfast, N. IrelandLicensing provisions: noneComputer: IBM PCOperating system under which the program has been tested: Windows 98, Windows 2000, Windows NTProgramming language used: Delphi 4.0Memory required to execute with typical data: 18 MwordsNo. of bits in a word: 32No. of bytes in distributed program, including test data, etc.: 9 911 434Distribution format: zip fileKeywords: Photofragment image, onion peeling, anisotropy parametersNature of physical problem: Information about velocity and angular distributions of photofragments is the basis on which the analysis of the photolysis process resides. Reconstructing the three-dimensional distribution from the photofragment image is the first step, further processing involving angular and radial integration of the inverted image to obtain velocity and angular distributions. Provisions have to be made to correct for slight distortions of the image, and to verify the accuracy of the analysis process.Method of solution: The “Onion Peeling” algorithm described by Helm [Rev. Sci. Instrum. 67 (6) (1996)] is used to perform the image reconstruction. Angular integration with a subsequent multi-Gaussian fit supplies information about the velocity distribution of the photofragments, whereas radial integration with subsequent expansion of the angular distributions over Legendre Polynomials gives the spatial anisotropy parameters. Fitting algorithms have been developed to centre the image and to correct for image distortion.Restrictions on the complexity of the problem: The maximum image size (1280×1280) and resolution (16 bit) are restricted by available memory and can be changed in the source code. Initial centre coordinates within 5 pixels may be required for the correction and the centering algorithm to converge. Peaks on the velocity profile separated by less then the peak width may not be deconvolved. In the charged particle image reconstruction, it is assumed that the kinetic energy released in the dissociation process is small compared to the energy acquired in the electric field. For the fitting parameters to be physically meaningful, cylindrical symmetry of the image has to be assumed but the actual inversion algorithm is stable to distortions of such symmetry in experimental images.Typical running time: The analysis procedure can be divided into three parts: inversion, fitting, and geometry correction. The inversion time grows approx. as R³, where R is the radius of the region of interest: for R=200 pixels it is less than a minute, for R=400 pixels less then 6 min on a 400 MHz IBM personal computer. The time for the velocity fitting procedure to converge depends strongly on the number of peaks in the velocity profile and the convergence criterion. It ranges between less then a second for simple curves and a few minutes for profiles with up to twenty peaks. The time taken for the image correction scales as R² and depends on the curve profile. It is on the order of a few minutes for images with R=500 pixels.Unusual features of the program: Our centering and image correction algorithm is based on Fourier analysis of the radial distribution to insure the sharpest velocity profile and is insensitive to an uneven intensity distribution. There exists an angular averaging option to stabilize the inversion algorithm and not to loose the resolution at the same time.     

Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography

Scanning transmission electron microscope tomography and atom-probe tomography are both three-dimensional techniques on the nanoscale. We demonstrate here the combination of the techniques by analyzing the very same volume of an Al-Ag alloy specimen. This comparison allows us to directly visualize the theoretically known artifacts of each technique experimentally, providing insight into the optimal parameters to use for reconstructions and assessing the quality of each reconstruction. The combination of the techniques for accurate morphology and compositional information in three dimensions at the nanoscale provides a route for a new level of materials characterization and understanding.     

Development of atom probe specimen preparation techniques for specific regions in steel materials

More elaborated specimen preparation techniques for atom probe analysis were developed using a focused ion beam with a sample lift-out system so as to expand the application field in steel materials. The techniques enable atom probe analysis of sample steel at site-specific regions of interest. The preferable form of the needle specimen was provided by electrostatic field calculation using a finite element method. The new techniques were applied to the observation of a bainite-ferrite interface in a low carbon steel, and atomic-scale partitioning and segregation of alloying elements at the phase interface were directly observed in three dimensions.     

A novel "ghost"-free tomographic image reconstruction method applicable to rotary-shadowed replica specimens

Electron tomography by conventional filtered back-projection is often seriously impaired by anisotropic resolution due to unavoidable limitation in specimen tilt-angles. We propose a new approach to overcome the problem for thin film-like replica-type specimens in which internal density is supposed as homogenous and contiguously distributed, by imposing a reasonable constraint of density-existing region in the reconstruction procedure. The objects were approximated as a distribution of binary voxels and the intensity of the projected images being proportional to the thickness along the projection ray. The new reconstruction algorithm consists of initial determination of approximate constraint region by a topographic analysis by stereo-photogrammetry, followed by iterative computation to find the unique solution of simultaneous equations, so that all the intensity distribution in tilt-series images are included within pre-determined voxel arrangement. During a trial run with a new methodology, we realized its significantly advantageous feature that much less number of projection images than conventional back-projection is required to perform the reconstruction of almost equivalent quality. Here, we show the performance of this novel algorithm by 3-D reconstruction of quick-freeze deep-etch replica specimens without any trace of spurious ghosting caused by missing-wedge problems.     

Application of simulated annealing for multispectral tomography

A new method based on simulated annealing is developed to obtain tomographic reconstructions based on multispectral absorption spectroscopy. The new method is able to exploit the spectral information content, to incorporate various a priori information, and to ameliorate the ill-posedness of the tomographic inversion problem. Numerical simulations are conducted to demonstrate the performance of this method for simultaneous temperature and species concentration imaging. This method is expected to enhance the practicality of multispectral tomography.     

Analyses of diverse mammals’ milk and lactoferrin glycans using five pathogenic bacterial lectins

Milk indigested glycans hamper infections by blocking pathogen adhesion to babies’ cells via lectins (sugar-binding proteins). This study describes usage of five pathogenic bacterial lectins and two plant lectins for analyses of alpaca, buffalo, camel, cow, dog, fallow deer, giraffe, goat, horse, human, rabbit, and sheep milks, and also commercial human and cow milk lactoferrins. The lectins used differentially reacted with the 12 milks – most strongly with humans’ ones. Most of them (excluding Pseudomonas aeruginosa galactophilic PA-IL) were also sensitive to the human and cow lactoferrins. The fucophilic bacterial lectins were most sensitive to human lactoferrin, while the mannophilic ones – to the cow’s. The actual function of bacterial lectins in pathogen adhesion and their non-glycosylated structures (evading non-specific interactions) are advantageous for such studies. This study shows the efficiency of the bacterial lectins for milk analyses: differentiating between the diverse milks, estimating their anti-infection potentials, and probing their active glycans.     

Atom probe analysis of titanium hydride precipitates

It is expected that the three-dimensional atom probe (3DAP) will be used as a tool to visualize the atomic scale of hydrogen atoms in steel is expected, due to its high spatial resolution and very low detection limit. In this paper, the first 3DAP analysis of titanium hydride precipitates in metal titanium is reported in terms of the quantitative detection of hydrogen. FIB fabrication techniques using the lift-out method have enabled the production of needle tips of hydride precipitates, of several tens of microns in size, within a titanium matrix. The hydrogen concentration estimated from 3DAP analysis was slightly smaller than that of the hydride phase predicted from the phase diagram. We discuss the origin of the difference between the experimental and predicted values and the performance of 3DAP for the quantitative detection of hydrogen.     

Three-dimensional atom probe analysis of heavily drawn steel wires by probing perpendicular to the pearlitic lamellae

Three-dimensional atom probe analysis of heavily drawn pearlitic steel wires was conducted by probing in the direction perpendicular to the pearlitic lamellae. A needle tip perpendicularly intersecting the lamellar structure was prepared using focused ion beam (FIB) milling combined with the lift-out method. The specimen preparation technique enabled the analysis of many lamellae and their interfaces with higher depth spatial resolution, which was suitable for drawn pearlitic steel wires having inhomogeneous and fine lamellar structure. Carbon concentration peaks at the cementite lamellae appeared higher and narrower than those obtained by probing parallel to the lamellae, which implies that the conventional analysis overestimated the extent of cementite decomposition in drawn pearlitic steel wires.     

The study of quantitativeness in atom probe analysis of alloying elements in steel

The quantitativeness in atom probe analysis of dilute solute alloying elements in steel was systematically investigated. The samples of binary Fe–Si, Fe–Ti, Fe–Cr, Fe–Cu, Fe–Mn and Fe–Mo alloys were prepared for present study. The apparent compositions of alloying elements were examined by three-dimensional atom probe (3DAP) under various experimental conditions. The temperature dependence of the apparent compositions varied largely with the alloys, which indicated that the degree of preferential evaporation or retention varied with the alloying elements. Furthermore, the analysis direction dependence of the apparent Mn composition was examined in the Fe–Mn alloy. The experimental results indicated that the order of the field evaporation rate of elements in steel was Cu>Cr>Mn∼Mo>Fe>Ti∼Si. The field evaporability of alloying elements in steel was discussed in terms of the solution enthalpy of the alloying elements and the phase types of the binary Fe alloys.