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At least 19 records

Bent crystal X-ray topography

A television X-ray topographic camera system was constructed. The system differs from the previous system in that it incorporates the X-ray TV imaging system and has a semi-automatic wafer loading system. Also the X-ray diffraction is in a vertical plane. This feature makes wafer loading easier and makes the system compatible with any commercial X-ray generating system. Topographs and results obtained from a study of the diffraction contrast variation with impurity concentration for both boron implanted and boron diffused silicon are included.

Parker, D. L.↗

X-ray topography study of complex silicon microcircuits

The correlation between the yield of silicon microcircuits wafers versus defects observed in X-ray topographs produced by a high speed curved wafer X-ray topographic camera was investigated. Most of the topographs were made after final wafer probe. Results indicated that most high volume silicon wafer processing does not need X-ray topography as a routine process control. It is further indicated that in changing any existing process or developing a new process the technique can be of significant benefit.

Parker, D. L.↗

Analysis of strain in ion implanted 4H-SiC by fringes observed in synchrotron X-ray topography

A novel high energy implantation system has been successfully developed to fabricate 4H-SiC superjunction devices for medium and high voltage via implantation of dopant atoms with multi-energies ranging from 13 to 66 MeV. The significantly higher levels of energy used compared to conventional implantation processes, necessitates detailed characterization of the lattice damage caused by implantation. To achieve this by employing the novel high energy system, 4H-SiC wafer with 12 μm epilayers were blanket implanted by 13.8–65.7 MeV Al atoms. The lattice damages induced by the implantation were primarily characterized by Synchrotron X-ray Plane Wave Topography (SXPWT) and Reciprocal Space Mapping (RSM). Topographs reveal fringe contrast akin to multiple asymmetric diffraction peaks with an angular separation of only 2″ (arcseconds) observed on rocking curves, indicating inhomogeneous strain distribution across the implanted layer. The strain profile of the implanted layer was extracted from the fringe contrast by applying Rocking-curve Analysis by Dynamical Simulation (RADS). In conclusion, the maximum strain value is similar to that measured on the RSM.

A1. Characterization↗

X-ray topography as a process control tool in semiconductor and microcircuit manufacture

A bent wafer camera, designed to identify crystal lattice defects in semiconductor materials, was investigated. The camera makes use of conventional X-ray topographs and an innovative slightly bent wafer which allows rays from the point source to strike all portions of the wafer simultaneously. In addition to being utilized in solving production process control problems, this camera design substantially reduces the cost per topograph.

Parker, D. L.↗

Analyzer-based X-ray phase contrast imaging using the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut crystal

An analyzer-based X-ray phase contrast imaging experiment employing the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut analyzer crystal has been implemented and tested in a geometry similar to that used in conventional radiography. The high angular stability requirements were overcome using specially designed crystals and a closed-loop feedback intensity system, monitoring the intensity of the diffracted h-beam. Analyzer-based images (ABis) taken at different angular positions on the forward-diffracted o-beam rocking curve show different contrasts, as expected. However, the ABis did not show sharp borders. This was closely investigated by X-ray topography and Δ d / d mapping and was attributed to the stresses caused by the analyzer crystal's own weight in the bulk. Further investigation of the crystal design using finite element analysis coupled with dynamical theory of X-ray diffraction is envisaged.

Honnicke, Marcelo Goncalves (ORCID:000000033276432↗

Cameras for semiconductor process control

The application of X-ray topography to semiconductor process control is described, considering the novel features of the high speed camera and the difficulties associated with this technique. The most significant results on the effects of material defects on device performance are presented, including results obtained using wafers processed entirely within this institute. Defects were identified using the X-ray camera and correlations made with probe data. Also included are temperature dependent effects of material defects. Recent applications and improvements of X-ray topographs of silicon-on-sapphire and gallium arsenide are presented with a description of a real time TV system prototype and of the most recent vacuum chuck design. Discussion is included of our promotion of the use of the camera by various semiconductor manufacturers.

Porter, W. A.↗

X-ray topographic observations of magnetic domains in Czochralski-grown nickel single crystals in anomalous transmission geometry

The anomalous transmission effect has been observed in nickel single crystals grown by the Czochralski technique. Sample crystals prepared for X-ray topography are 1.5 to 2.5 cm in diameter and thicker than 0.4 mm; the product of the ordinary linear absorption coefficient and thickness ranges from 17 to 45 for Cu K-alpha radiation. Topographs taken with an asymmetric-crystal-topographic (ACT) camera have revealed extremely straight line images and rectangular arrangements of short line-segment images, along with the images of crystal imperfections. The line images change their arrangement upon application of magnetic fields. These images are attributed to magnetic domains in the interior of crystals. The formation of domain walls near the crystal surface is also observed and distinguished clearly from magnetic domains in the bulk with the use of the ACT camera.

Kuriyama, M.↗

The effects of titanium impurities in N/+//P silicon solar cells

Microscopic and electrical measurements were performed to explain the degradation mechanisms associated with the presence of titanium impurities in silicon. The measurements included X-ray topography, transmission electron microscopy, and deep level transient spectroscopy, before and after processing. The results indicated the presence of TiO2 precipitates, the density of which increased after phosphorus diffusion. A majority carrier trapping level was observed in the wafers before processing. It was concluded that 10% of the Ti in the N(+)/P silicon solar cells formed electrically active centers which caused degradation of the cell junction. 14% of the remaining Ti precipitated out as TiO2, forming electrically active defects, which also caused junction degradation.

Salama, A. M.↗

Imaging surface topography with coherent x-ray reflectivity: Theory, kinematics, and simulations

A theoretical formalism is described for understanding coherent x-ray reflectivity (CXR) from the surface of a semi-infinite crystal having a variable surface topography, described by the height profile ℎ(𝑥,𝑦). The surface topography is imaged as a complex “effective density,” obtained from the phasing and inversion of the coherent x-ray reflectivity data, measured through a rocking scan centered at a vertical momentum transfer 𝑄$^{0}_{𝑧}$ and a vertical range Δ⁢𝑄 𝑧 . The formalism predicts that the effective density has an amplitude with a maximum located at the surface height for each position within the surface plane. The phase of the effective density has a lateral variation that is controlled by the surface height and a vertical variation that reflects a combination of the interfacial structure and specific choice of measurement conditions. This understanding enables direct observation of nanometer-scale interfacial topography, i.e., ℎ⁡(𝑥,𝑦)⁢𝑐 𝑠 (where 𝑐 𝑠 is the vertical substrate lattice parameter) with Å-scale sensitivity to surface height. Numerical simulations illustrate and confirm the theoretical results. These results show how the interpretation of the interfacial density phase obtained by CXR data inversion (i.e., surface topography with respect to a flat surface) is conceptually similar to that previously known for Bragg coherent diffraction imaging (BCDI) measurements of isolated nanoparticles (i.e., lattice displacements with respect to an ideal crystal lattice). This suggests that CXR can be thought of as a form of dark field imaging with respect to the bright field BCDI approach. An implication of these results is that interfacial imaging may bypass some of the significant challenges associated with BCDI imaging of multiple particles having different orientations.

X-ray imaging↗

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗

Status and new features of the topography beamline 1-BM after the Advanced Photon Source upgrade

The beamline 1-BM of the Advanced Photon Source (APS), a bending-magnet beamline with an effective X-ray beam size of ~100×4 mm2, has relatively comprehensive synchrotron topography and rocking curve imaging capabilities for characterization of crystals (particularly wide-bandgap semiconductors SiC, AlN, GaN, Ga2O3 etc). It is equipped with a white-beam topography stage for imaging large wafers up to 8 inches. It also has a double-crystal setup, of which the second stage can be used for monochromatic-beam topography. The first stage has different beam conditioners in the grazing-incidence geometry that can expand the vertical beam size from 4 to ~100 mm for double-crystal rocking curve imaging when it is combined with the second stage. Recently APS has been upgraded to a modern 4th-generation light source, and 1-BM has been recommissioned to its normal operation for general users with better performance. The upgraded APS leads to new features at 1-BM. The much smaller source size and higher X-ray coherence significantly improve the image resolution and contrast. The higher flux and brightness of the new source reduce exposure time, which mitigates the mechanical drifting and vibration issues. Here the main capabilities and status of 1-BM together with these new features are introduced.

X-ray topography↗

Fluid flow effects on crystalline perfection

Optimum solidification parameters for the production of highly perfect copper crystals by Czochralski growth are sought along with the documentation of crystal imperfections under various growth conditions. X-ray techniques which do not in their application produce defects and which allow the characterization of imperfections in single crystals are chosen to assess crystal perfection. The X-ray techniques employed ranged from ordinary Laue photography through Borrmann topography to double-crystal scanning diffractometry, thus allowing crystals with a wide variation in perfection to be studied. As a set of controllable solidification parameters, the rotation of the seed and of the melt and the diameter of the bottleneck are chosen. X-ray diffraction topographs are analyzed along with the data obtained from rocking curve measurements. Tables of growth conditions and quantitative data of rocking curve widths are presented.

Kuriyama, M.↗

Advanced Instrumentation for Metal Additive Manufacturing

Laser powder bed fusion (LPBF) is the most widely used process for metal additive manufacturing (AM), particularly where complex geometries provide performance advantages unattainable with traditional manufacturing techniques. However, LPBF is highly sensitive to innate variability in both the powder spreading and fusion steps, often leading to defects such as pores that are difficult to detect yet significantly impair component mechanical properties and fatigue life. This thesis presents a range of novel instruments enabling both precise assessment of powder layer characteristics and in-situ thermal metrology of metal AM to advance the quality control of LPBF. First, leveraging a custom X-ray microscope and a radiation-transport model developed through this work, transmission X-ray imaging is used to study spreading of thin metal powder layers. Effective layer depth is directly mapped at a process-relevant size scale, surpassing optical techniques that can only estimate local deposition from layer surface topography. Layer packing density and quality are shown to be influenced by powder flowability and particle size relative to nominal powder layer thickness. Layer quality is additionally connected to the geometry of the spreading implement and its velocity. This technique and its presented findings enable pairing feedstocks with spreading strategies that create layers with consistent packing density and uniformity. Second, a twofold approach is employed to optically interrogate the laser fusion step of LPBF for observing signatures of defect formation. Aperture division multiplexing is conceptualized, providing for simultaneous laser delivery and high-fidelity infrared (IR) process monitoring through a common optic. In-situ microscopy at 50 μm spatial resolution and at mid-wave IR wavelengths is proven readily achievable with the first purpose-built optic of this type. Next, a bespoke imaging spectrometer, along with a temperature-emissivity separation technique, is used to retrieve accurate process temperatures over a 1000 K range. Data from these instruments are correlated to porosity as fine as 4.3 μm in two LPBF test artifacts, as verified using computed tomography (CT), establishing the viability of robust optically-based component qualification.

Penny, Ryan↗

Understanding Fracture Aperture and Permeability Evolution due to Carbonate Mineralization Utilizing 3D Printing

Caprock formations are a crucial part of subsurface-engineered systems. Composed largely of shale, caprocks act as natural barriers that prevent the upward migration of fluids, thereby ensuring the containment of stored substances in subsurface formations. Fractures in these formations are potential leakage pathways for stored fluids. Mineral precipitation reactions in these fractures, particularly calcite, can significantly restrict the fluid permeability, reducing leakage potential. However, predictive capabilities of mineral precipitation in fractures and associated permeability evolution are limited due to a lack of fundamental understanding of such reactions in natural samples, complicated by mineral heterogeneity and the complexity of the fracture structure. In this study, 3D-printed fracture samples are used to understand the impact of carbonate mineralization on fracture aperture and permeability evolution. Samples were printed using a digital light processing (DLP) 3D printer and commercial liquid resin. Calcite precipitation was first tested on printed 2D films before conducting plug flow column experiments aimed to understand fracture permeability changes due to mineral precipitation. Contact angle measurement and Fourier transform infrared (FTIR) spectroscopy on printed 2D films show evidence of a substantial amount of surface energy for calcite nucleation and precipitation. Surface topography analysis of printed fractured surfaces reveals comparable values, highlighting the high replicability of the printed samples. During the column experiments, the permeability reduces exponentially due to a decrease in fracture aperture. Reductions in fracture aperture estimated from effluent concentration and 3D X-ray computed tomography (CT) show comparable results. Moreover, 3D X-ray CT images suggest the impact of local flow velocities on precipitation. The insights gained from this research contribute to a deeper understanding of the permeability evolution due to carbonate mineralization in caprock formations.

3D printing↗

Effect of surface topography on structural growth of thick sputtered films

Primarily thick sputtered S-Monel, silver, and 304 stainless steel coatings were deposited on mica, glass, and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. Compositional changes within the coating were analyzed by X-ray dispersion microscopy. Defects in the surface finish act as preferential nucleation sites and form isolated and complex nodules and various surface overgrowths in the coating. These nodules do not disappear after full annealing. Further, they have undesirable effects on mechanial properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces. These effects are illustrated by micrographs. Nodular growth within a coating can be minimized or eliminated by reducing the surface roughness.

Spalvins, T.↗

Effect of longitudinal surface finish on elastohydrodynamic lubrication

The effect of longitudinal-lay surface finish on the elastohydrodynamic film thickness and the percentage of film between rolling disks in contact were evaluated using a rolling disk apparatus. Film thickness was measured by transmitted X-rays, and percentage of film was monitored by an alternating-current continuity circuit. Disk finish was varied on both the crowned upper disk and the cylindrical lower disk. A type-2 ester and a synthetic paraffinic oil were used as lubricants. It was shown that the roughness with longitudinal lay has a deleterious effect on both film thickness and percentage of film. Measured film thicknesses for the two lubricants were comparable at equivalent test conditions. The percentage of film where a change in surface topography was observed was approximately 20 percent for the synthetic paraffinic oil and 10 percent for the type-2 ester.

Dow, T. A.↗

Temperature-dependent dielectric function of tantalum nitride formed by atomic layer deposition for tunnel barriers in Josephson junctions

Here, we report the dielectric functions of insulating tantalum nitride (TaN) films deposited by atomic layer deposition (ALD) on 300 mm Si/SiO 2 substrates to evaluate their suitability as tunnel barriers in tantalum-based Josephson junctions (JJs) for superconducting quantum circuits. Temperature-dependent ellipsometric angles were measured for ALD TaN films with nominal thicknesses of 13 and 25 nm at an incidence angle of 70°, over photon energy ranges of 0.03–0.7 eV (80–300 K) and 0.5–6.5 eV (80–600 K). These data were used to develop a dispersion model for insulating ALD TaN that incorporates a Tauc–Lorentz oscillator with an optical bandgap of 1.5–1.8 eV to describe interband transitions. The extracted dielectric function shows insulating behavior (mid-infrared transparency) at all temperatures and for both film thicknesses tested. In particular, ALD TaN does not exhibit infrared absorption due to free carriers, even at elevated temperatures, consistent with the insulating behavior required for a JJ tunnel barrier. Results from transmission electron microscopy (including selected area electron diffraction) and x-ray diffraction are also discussed. Sputter depth-profile x-ray photoelectron spectroscopy shows an N/Ta ratio of ∼1.2 throughout the film. The lower bandgap, low roughness, and thermal stability of ALD TaN compared to AlO x suggest the possibility of fabricating JJs with thicker barriers while achieving critical current densities required for qubits, enabling improved thickness and composition control, reduced topography, and resistance to aging.

36 MATERIALS SCIENCE↗