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LDRD 226360 Final Project Report: Simulated X-ray Diffraction and Machine Learning for Optimizing Dynamic Experiment Analysis

Ao, Tommy A.; Donohoe, Brendan D.; Martinez, Carianne M.; Knudson, Marcus D.; Montes de Oca Zapiain, David M.; Morgan, Dane M.; Rodriguez, Mark A.; Lane, James M.

This report is the final documentation for the one-year LDRD project 226360: Simulated X-ray Diffraction and Machine Learning for Optimizing Dynamic Experiment Analysis. As Sandia has successfully developed in-house X-ray diffraction tools for study of atomic structure in experiments, it has become increasingly important to develop computational analysis methods to support these experiments. When dynamically compressed lattices and orientations are not known a priori, the identification requires a cumbersome and sometimes intractable search of possible final states. These final states can include phase transition, deformation and mixed/evolving states. Our work consists of three parts: (1) development of an XRD simulation tool and use of traditional data science methods to match XRD patterns to experiments; (2) development of ML-based models capable of decomposing and identifying the lattice and orientation components of multicomponent experimental diffraction patterns; and (3) conducting experiments which showcase these new analysis tools in the study of phase transition mechanisms. Our target material has been cadmium sulfide, which exhibits complex orientation-dependent phase transformation mechanisms. In our current one-year LDRD, we have begun the analysis of high-quality c-axis CdS diffraction data from DCS and Thor experiments, which had until recently eluded orientation identification.

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A compact x-ray diffraction system for dynamic compression experiments on pulsed-power generators

Review of Scientific Instruments

Ao, Tommy A.; Morgan, D.V.; Stoltzfus, Brian S.; Austin, Kevin N.; Usher, Joshua M.; Breden, E.; Pacheco, L.M.; Dean, S.; Brown, Justin L.; Duwal, Sakun D.; Fan, H.; Kalita, P.; Knudson, M.D.; Rodriguez, Mark A.; Lane, J.M.D.

Pulsed-power generators can produce well-controlled continuous ramp compression of condensed matter for high-pressure equation-of-state studies using the magnetic loading technique. X-ray diffraction (XRD) data from dynamically compressed samples provide direct measurements of the elastic compression of the crystal lattice, onset of plastic flow, strength-strain rate dependence, structural phase transitions, and density of crystal defects, such as dislocations. Here, we present a cost-effective, compact, pulsed x-ray source for XRD measurements on pulsed-power-driven ramp-loaded samples. This combination of magnetically driven ramp compression of materials with a single, short-pulse XRD diagnostic will be a powerful capability for the dynamic materials' community to investigate in situ dynamic phase transitions critical to equation of states. We present results using this new diagnostic to evaluate lattice compression in Zr and Al and to capture signatures of phase transitions in CdS.

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High pressure induced atomic and mesoscale phase behaviors of one-dimensional TiO2 anatase nanocrystals

MRS Bulletin

Meng, Lingyao; Duwal, Sakun D.; Lane, J.M.; Ao, Tommy A.; Stoltzfus, Brian S.; Knudson, Marcus D.; Park, Changyong; Chow, Paul; Xiao, Yuming; Fan, Hongyou F.; Qin, Yang

Abstract: Here, we report the high pressure phase and morphology behavior of ordered anatase titanium dioxide (TiO2) nanocrystal arrays. One-dimensional TiO2 nanorods and nanorices were synthesized and self-assembled into ordered mesostructures. Their phase and morphological transitions at both atomic scale and mesoscale under pressure were studied using in situ synchrotron wide- and small-angle x-ray scattering (WAXS and SAXS) techniques. At the atomic scale, synchrotron WAXS reveals a pressure-induced irreversible amorphization up to 35 GPa in both samples but with different onset pressures. On the mesoscale, no clear phase transformations were observed up to 20 GPa by synchrotron SAXS. Intriguingly, sintering of TiO2 nanorods at mesoscale into nano-squares or nano-rectangles, as well as nanorices into nanowires, were observed for the first time by transmission electron microscopy. Such pressure-induced nanoparticle phase-amorphization and morphological changes provide valuable insights for design and engineering structurally stable nanomaterials. Impact statement: The high pressure behavior of nanocrystals (NCs) continues to be of interest, as previous studies have demonstrated that an externally applied pressure can serve as an efficient tool to induce structural phase transitions of NC assemblies at both the atomic scale and mesoscale without altering any chemistry by manipulating NC interatomic and interparticle distances. In addition, the high pressure generated deviatoric stress has been proven to be able to force adjacent NCs to connect and fuse into new crystalline nanostructures. Although the atomic structural evolution of TiO2 NCs under pressure has been widely investigated in the past decades, open questions remain regarding the mesoscale phase transition and morphology of TiO2 NC assemblies as a function of pressure. Therefore, in this work, systemic high pressure experiments on ordered arrays of TiO2 nanorods and nanorices were conducted by employing wide/small angle x-ray scattering techniques. The sintering of TiO2 assemblies at mesoscale into various nanostructures under pressure were revealed by transmission electron microscopy. Overall, this high pressure work fills the current gap in research on the mesoscale phase behavior of TiO2 assemblies. The observed morphology tunability attained by applying pressure opens new pathways for engineering nanomaterials and optimizing their collective properties through mechanical compression stresses. Graphical abstract: [Figure not available: see fulltext.].

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A Platform-Independent X-ray Diffraction Diagnostic for Phase Transition Kinetics in Traditional and Synthetic Microstructure Materials (LDRD Project 213088 Final Report)

Ao, Tommy A.; Austin, Kevin N.; Breden, E.W.; Brown, Justin L.; Dean, Steven W.; Duwal, Sakun D.; Fan, Hongyou F.; Kalita, Patricia K.; Knudson, Marcus D.; Meng, Lingyao M.; Morgan, Dane D.; Pacheco, Lena M.; Qin, Yang Q.; Stoltzfus, Brian S.; Thurston, Bryce A.; Usher, Joshua M.; Lane, James M.

Pulsed-power generators using the magnetic loading technique are able to produce well-controlled continuous ramp compression of condensed matter for high-pressure equation-of-state studies. X-ray diffraction (XRD) data from dynamically compressed samples provide direct measurements of the elastic compression of the crystal lattice, onset of plastic flow, strength-strain rate dependence, structural phase transitions, and density of crystal defects such as dislocations. Here, we present a cost effective, compact X-ray source for XRD measurements on pulsed-power-driven ramp-loaded samples. This combination of magnetically-driven ramp compression of materials with single, short-pulse XRD diagnostic will be a powerful capability for the dynamic materials community. The success in fielding this new XRD diagnostic dramatically improves our predictive capability and understanding of rate-dependent behavior at or near phase transition. As Sandia plans the next-generation pulse-power driver platform, a key element needed to deliver new state-of-the-art experiments will be having the necessary diagnostic tools to probe new regimes and phenomena. These diagnostics need to be as versatile, compact, and portable as they are powerful. The development of a platform-independent XRD diagnostic gives Sandia researchers a new window to study the microstructure and phase dynamics of materials under load. This project has paved the way for phase transition research in a variety of materials with mission interest.

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Equation of State Measurements on Iron Near the Melting Curve at Planetary Core Conditions by Shock and Ramp Compressions

Journal of Geophysical Research: Solid Earth

Grant, S.C.; Ao, Tommy A.; Seagle, Christopher T.; Porwitzky, Andrew J.; Davis, Jean-Paul D.; Cochrane, Kyle C.; Dolan, Daniel H.; Lin, J.F.; Ditmire, T.; Bernstein, A.C.

The outer core of the Earth is composed primarily of liquid iron, and the inner core boundary is governed by the intersection of the melt line and the geotherm. While there are many studies on the thermodynamic equation of state for solid iron, the equation of state of liquid iron is relatively unexplored. We use dynamic compression to diagnose the high-pressure liquid equation of state of iron by utilizing the shock-ramp capability at Sandia National Laboratories’ Z-Machine. This technique enables measurements of material states off the Hugoniot by initially shocking samples and subsequently driving a further, shockless compression. Planetary studies benefit greatly from isentropic, off-Hugoniot experiments since they can cover pressure-temperature (P-T) conditions that are close to adiabatic profiles found in planetary interiors. We used this method to drive iron to P-T conditions similar to those of the Earth’s outer-inner core boundary, along an elevated-temperature isentrope in the liquid from 275 GPa to 400 GPa. We derive the equation of state using a hybrid backward integration – forward Lagrangian technique on particle velocity traces to determine the pressure-density history of the sample. Our results are in excellent agreement with SESAME 92141, a previously published equation of state table. With our data and previous experimental data on liquid iron we provide new information on the iron melting line and derive new parameters for a Vinet-based equation of state. The table and our parameterized equation of state are applied to provide an updated means of modeling the pressure, mass, and density of liquid iron cores in exoplanetary interiors.

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Scale and rate in CdS pressure-induced phase transition

AIP Conference Proceedings

Lane, J.M.D.; Thompson, Aidan P.; Srivastava, Ishan S.; Grest, Gary S.; Ao, Tommy A.; Stoltzfus, Brian S.; Austin, Kevin N.; Fan, H.; Morgan, D.; Knudson, Marcus D.

We describe recent efforts to improve our predictive modeling of rate-dependent behavior at, or near, a phase transition using molecular dynamics simulations. Cadmium sulfide (CdS) is a well-studied material that undergoes a solid-solid phase transition from wurtzite to rock salt structures between 3 and 9 GPa. Atomistic simulations are used to investigate the dominant transition mechanisms as a function of orientation, size and rate. We found that the final rock salt orientations were determined relative to the initial wurtzite orientation, and that these orientations were different for the two orientations and two pressure regimes studied. The CdS solid-solid phase transition is studied, for both a bulk single crystal and for polymer-encapsulated spherical nanoparticles of various sizes.

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A spherical crystal diffraction imager for Sandia’s Z Pulsed Power Facility

Review of Scientific Instruments

Ao, Tommy A.; Schollmeier, Marius; Kalita, Patricia K.; Gard, Paul D.; Smith, Ian C.; Shores, Jonathon S.; Speas, Christopher S.; Seagle, Christopher T.

Sandia’s Z Pulsed Power Facility is able to dynamically compress matter to extreme states with exceptional uniformity, duration, and size, which are ideal for investigating fundamental material properties of high energy density conditions. X-ray diffraction (XRD) is a key atomic scale probe since it provides direct observation of the compression and strain of the crystal lattice and is used to detect, identify, and quantify phase transitions. Because of the destructive nature of Z-Dynamic Material Property (DMP) experiments and low signal vs background emission levels of XRD, it is very challenging to detect a diffraction signal close to the Z-DMP load and to recover the data. We have developed a new Spherical Crystal Diffraction Imager (SCDI) diagnostic to relay and image the diffracted x-ray pattern away from the load debris field. The SCDI diagnostic utilizes the Z-Beamlet laser to generate 6.2-keV Mn–Heα x rays to probe a shock-compressed material on the Z-DMP load. Finally, a spherically bent crystal composed of highly oriented pyrolytic graphite is used to collect and focus the diffracted x rays into a 1-in. thick tungsten housing, where an image plate is used to record the data.

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X-ray diffraction of dynamically compressed matter on Sandia?s Z Pulsed Power Facility

Ao, Tommy A.; Schollmeier, Marius; Kalita, Patricia K.; Gard, Paul D.; Williams, James R.; Blada, Caroline B.; Hanshaw, Heath L.; Smith, Ian C.; Shores, Jonathon S.; Speas, Christopher S.; Seagle, Christopher T.

Sandia's Z Pulsed Power Facility is able to dynamically compress matter to extreme states with exceptional uniformity, duration, and size, which are ideal for investigations of fundamental material properties of high energy density conditions. X-ray diffraction (XRD) is a key atomic scale probe since it provides direct observation of the compression and strain of the crystal lattice, and is used to detect, identify, and quantify phase transitions. Because of the destructive nature of Z-Dynamic Materials Properties (DMP) experiments and low signal vs background emission levels of XRD, it is very challenging to detect the XRD pattern close to the Z-DMP load and to recover the data. We developed a new Spherical Crystal Diffraction Imager (SCDI) diagnostic to relay and image the diffracted x-ray pattern away from the load debris field. The SCDI diagnostic utilizes the Z-Beamlet laser to generate 6.2-keV Mn-He c , x-rays to probe a shock-compressed sample on the Z-DMP load. A spherically bent crystal composed of highly oriented pyrolytic graphite is used to collect and focus the diffracted x-rays into a 1-inch thick tungsten housing, where an image plate is used to record the data. We performed experiments to implement the SCDI diagnostic on Z to measure the XRD pattern of shock compressed beryllium samples at pressures of 1.8-2.2 Mbar.

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The effects of surface roughness on specular diagnostics in shocked experiments

Review of Scientific Instruments

Grant, Sean C.; Ao, Tommy A.

Many shock experiments, whether impact, laser, or magnetically driven, use reflected optical light from shocked samples to diagnose their material properties. Specifically, optical velocimetry diagnostics, which do not require absolute power measurements, are regularly used to obtain equation-of-state information of materials. However, new diagnostics will be necessary to expand the realm of measured material properties, and many useful diagnostic techniques do require absolute measurements. Thus, it is important to understand what happens at the reflective surface of shock experiments, and the effect scattering has on the light collection of optical probes. To this end, we present results from experiments done to observe the behavior of a reflected beam from a specular coating on an optical window during shock impact. We find that the specular condition of the coating is adversely affected by the shock front, but this can be mitigated by minimizing roughness on the surface preceding the coating.

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Polycapillary x-ray lenses for single-shot, laser-driven powder diffraction

Review of Scientific Instruments

Schollmeier, Marius; Ao, Tommy A.; Field, Ella S.; Galloway, B.R.; Kalita, Patricia K.; Kimmel, Mark W.; Morgan, D.V.; Rambo, Patrick K.; Schwarz, Jens S.; Shores, J.E.; Smith, Ian C.; Speas, C.S.; Benage, John F.; Porter, John L.

X-ray diffraction measurements to characterize phase transitions of dynamically compressed high-Z matter at Mbar pressures require both sufficient photon energy and fluence to create data with high fidelity in a single shot. Large-scale laser systems can be used to generate x-ray sources above 10 keV utilizing line radiation of mid-Z elements. However, the laser-to-x-ray energy conversion efficiency at these energies is low, and thermal x-rays or hot electrons result in unwanted background. We employ polycapillary x-ray lenses in powder x-ray diffraction measurements using solid target x-ray emission from either the Z-Beamlet long-pulse or the Z-Petawatt (ZPW) short-pulse laser systems at Sandia National Laboratories. Polycapillary lenses allow for a 100-fold fluence increase compared to a conventional pinhole aperture while simultaneously reducing the background significantly. This enables diffraction measurements up to 16 keV at the few-photon signal level as well as diffraction experiments with ZPW at full intensity.

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X-Ray Diffraction Measurements on Laser-Compressed Polycrystalline Samples Using a Short-Pulse Laser Generated X-Ray Source

Schollmeier, Marius; Ao, Tommy A.; Field, Ella S.; Galloway, B.R.; Kalita, Patricia K.; Kimmel, Mark W.; Long, Joel L.; Morgan, Dane D.; Rambo, Patrick K.; Schwarz, Jens S.; Seagle, Christopher T.

Existing models for most materials do not describe phase transformations and associated lattice dy- namics (kinetics) under extreme conditions of pressure and temperature. Dynamic x-ray diffraction (DXRD) allows material investigations in situ on an atomic scale due to the correlation between solid-state structures and their associated diffraction patterns. In this LDRD project we have devel- oped a nanosecond laser-compression and picosecond-to-nanosecond x-ray diffraction platform for dynamically-compressed material studies. A new target chamber in the Target Bay in building 983 was commissioned for the ns, kJ Z-Beamlet laser (ZBL) and the 0.1 ns, 250 J Z-Petawatt (ZPW) laser systems, which were used to create 8-16 keV plasma x-ray sources from thin metal foils. The 5 ns, 15 J Chaco laser system was converted to a high-energy laser shock driver to load material samples to GPa stresses. Since laser-to-x-ray energy conversion efficiency above 10 keV is low, we employed polycapillary x-ray lenses for a 100-fold fluence increase compared to a conventional pinhole aperture while simultaneously reducing the background significantly. Polycapillary lenses enabled diffraction measurements up to 16 keV with ZBL as well as diffraction experiments with ZPW. This x-ray diffraction platform supports experiments that are complementary to gas guns and the Z facility due to different strain rates. Ultimately, there is now a foundation to evaluate DXRD techniques and detectors in-house before transferring the technology to Z. This page intentionally left blank.

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Superfast assembly and synthesis of gold nanostructures using nanosecond low-temperature compression via magnetic pulsed power

Nature Communications

Li, Binsong; Bian, Kaifu B.; Lane, J.M.; Salerno, K.M.; Grest, Gary S.; Ao, Tommy A.; Hickman, Randy J.; Wise, Jack L.; Wang, Zhongwu; Fan, Hongyou F.

Gold nanostructured materials exhibit important size- and shape-dependent properties that enable a wide variety of applications in photocatalysis, nanoelectronics and phototherapy. Here we show the use of superfast dynamic compression to synthesize extended gold nanostructures, such as nanorods, nanowires and nanosheets, with nanosecond coalescence times. Using a pulsed power generator, we ramp compress spherical gold nanoparticle arrays to pressures of tens of GPa, demonstrating pressure-driven assembly beyond the quasi-static regime of the diamond anvil cell. Our dynamic magnetic ramp compression approach produces smooth, shockless (that is, isentropic) one-dimensional loading with low-temperature states suitable for nanostructure synthesis. Transmission electron microscopy clearly establishes that various gold architectures are formed through compressive mesoscale coalescences of spherical gold nanoparticles, which is further confirmed by in-situ synchrotron X-ray studies and large-scale simulation. This nanofabrication approach applies magnetically driven uniaxial ramp compression to mimic established embossing and imprinting processes, but at ultra-short (nanosecond) timescales.

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Development of Dynamic Ellipsometry for Measurements or Iron Conductivity at Earth's Core Conditions

Grant, Sean C.; Ao, Tommy A.; Davis, Jean-Paul D.; Dolan, Daniel H.; Seagle, Christopher T.; Lin, Jung-Fu L.; Bernstein, Aaron B.

The CHEDS researchers are engaged in a collaborative research project to study the properties of iron and iron alloys under Earth’s core conditions. The Earth’s core, inner and outer, is composed primarily of iron, thus studying iron and iron alloys at high pressure and temperature conditions will give the best estimate of its properties. Also, comparing studies of iron alloys with known properties of the core can constrain the potential light element compositions found within the core, such as fitting sound speeds and densities of iron alloys to established inner- Earth models. One of the lesser established properties of the core is the thermal conductivity, where current estimates vary by a factor of three. Therefore, one of the primary goals of this collaboration is to make relevant measurements to elucidate this conductivity.

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The Sandia Matlab AnalysiS Hierarchy (SMASH) toolbox

Dolan, Daniel H.; Ao, Tommy A.; Grant, Sean C.

The SMASH (Sandia Matlab AnalysiS Hierarchy) toolbox is a collection of MATLAB code for data analysis. The toolbox contains general purpose functions, custom class defini- tions, and self-contained programs aimed at the needs of experimental physicists working in pulsed power research. The initial release (version 1.0) supports file access, signal/image analysis, and user interface creation; custom graphics and generic system tools are also pro- vided. Much of the package is object oriented, encouraging users to build new capabilities from established classes. Future releases will continue this goal, expanding capabilities and streamlining application development.

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Demonstration of space-resolved x-ray Thomson scattering capability for warm dense matter experiments on the Z accelerator

High Energy Density Physics

Ao, Tommy A.; Harding, Eric H.; Bailey, James E.; Lemke, Raymond W.; Desjarlais, Michael P.; Hansen, Stephanie B.; Smith, Ian C.; Geissel, Matthias G.; Maurer, A.; Reneker, Joseph R.; Romero, D.; Sinars, Daniel S.; Rochau, G.A.; Benage, John F.

Experiments on the Sandia Z pulsed-power accelerator have demonstrated the ability to produce warm dense matter (WDM) states with unprecedented uniformity, duration, and size, which are ideal for investigations of fundamental WDM properties. For the first time, space-resolved x-ray Thomson scattering (XRTS) spectra from shocked carbon foams were recorded on Z. The large (>20 MA) electrical current produced by Z was used to launch Al flyer plates up to 25 km/s. The impact of the flyer plate on a CH2 foam target produced a shocked state with an estimated pressure of 0.75 Mbar, density of 0.52 g/cm3, and temperature of 4.3 eV. Both unshocked and shocked portions of the foam target were probed with 6.2 keV x-rays produced by focusing the Z-Beamlet laser onto a nearby Mn foil. The data are composed of three spatially distinct spectra that were simultaneously captured with a single spectrometer with high spectral (4.8 eV) and spatial (190 μm) resolutions. Detailed spectral information from three target locations is provided simultaneously: the incident x-ray source, the scattered signal from unshocked foam, and the scattered signal from shocked foam.

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Sandia Data Archive (SDA) file specifications

Dolan, Daniel H.; Ao, Tommy A.

The Sandia Data Archive (SDA) format is a specific implementation of the HDF5 (Hierarchal Data Format version 5) standard. The format was developed for storing data in a universally accessible manner. SDA files may contain one or more data records, each associated with a distinct text label. Primitive records provide basic data storage, while compound records support more elaborate grouping. External records allow text/binary files to be carried inside an archive and later recovered. This report documents version 1.0 of the SDA standard. The information provided here is sufficient for reading from and writing to an archive. Although the format was original designed for use in MATLAB, broader use is encouraged.

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Dynamic temperature measurements with embedded optical sensors

Dolan, Daniel H.; Seagle, Christopher T.; Ao, Tommy A.

This report summarizes LDRD project number 151365, \Dynamic Temperature Measurements with Embedded Optical Sensors". The purpose of this project was to develop an optical sensor capable of detecting modest temperature states (<1000 K) with nanosecond time resolution, a recurring diagnostic need in dynamic compression experiments at the Sandia Z machine. Gold sensors were selected because the visible re ectance spectrum of gold varies strongly with temperature. A variety of static and dynamic measurements were performed to assess re ectance changes at di erent temperatures and pressures. Using a minimal optical model for gold, a plausible connection between static calibrations and dynamic measurements was found. With re nements to the model and diagnostic upgrades, embedded gold sensors seem capable of detecting minor (<50 K) temperature changes under dynamic compression.

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SIRHEN : a data reduction program for photonic Doppler velocimetry measurements

Ao, Tommy A.; Dolan, Daniel H.

SIRHEN (Sandia InfraRed HEtrodyne aNalysis) is a program for reducing data from photonic Doppler velocimetry (PDV) measurements. SIRHEN uses the short-time Fourier transform method to extract velocity information. The program can be run in MATLAB (2008b or later) or as a Windows executable. This report describes the new Sandia InfraRed HEtrodyne aNalysis program (SIRHEN; pronounced 'siren') that has been developed for efficient and robust analysis of PDV data. The program was designed for easy use within Sandia's dynamic compression community.

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LIVA :

Ao, Tommy A.

LIVA (Line-Imaging Velocimetry Analysis) is a program for reducing data of a line-imaging optically recording velocity interferometer system (ORVIS) diagnostic. LIVA uses the Fourier transform method to extract phase information from recorded streak camera images. The extracted phase shift is used to infer target velocity as a function of space and time. The program can be run in any current version of MATLAB (2008a or later) or as a Windows XP executable.

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IWA : an analysis program for isentropic wave measurements

Ao, Tommy A.

IWA (Isentropic Wave Analysis) is a program for analyzing velocity profiles of isentropic compression experiments. IWA applies incremental impedance matching correction to measured velocity profiles to obtain in-situ particle velocity profiles for Lagrangian wave analysis. From the in-situ velocity profiles, material properties such as wave velocities, stress, strain, strain rate, and strength are calculated. The program can be run in any current version of MATLAB (2008a or later) or as a Windows XP executable.

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The VELOCE pulsed power generator for isentropic compression experiments

Ao, Tommy A.; Hickman, Randy J.; Hall, Clint A.; Baer, Melvin B.

Veloce is a medium-voltage, high-current, compact pulsed power generator developed for isentropic and shock compression experiments. Because of its increased availability and ease of operation, Veloce is well suited for studying isentropic compression experiments (ICE) in much greater detail than previously allowed with larger pulsed power machines such as the Z accelerator. Since the compact pulsed power technology used for dynamic material experiments has not been previously used, it is necessary to examine several key issues to ensure that accurate results are obtained. In the present experiments, issues such as panel and sample preparation, uniformity of loading, and edge effects were extensively examined. In addition, magnetohydrodynamic (MHD) simulations using the ALEGRA code were performed to interpret the experimental results and to design improved sample/panel configurations. Examples of recent ICE studies on aluminum are presented.

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117 Results
117 Results