Doucet, Mathieu; Browning, James F.; Doyle, Barney L.; Charlton, Timothy R.; Ambaye, Haile; Seo, Joohyun; Mazza, Alessandro R.; Wenzel, John F.; Burns, George B.; Wixom, Ryan R.; Veith, Gabriel M.
Haynes 230 nickel alloy is one of the main contenders for salt containment in the design of thermal energy storage systems based on molten salts. A key problem for these systems is understanding the corrosion phenomena at the alloy–salt interface, and, in particular, the role played by chromium in these processes. In this study, thin films of Haynes 230, which is also rich in chromium, were measured with polarized neutron reflectometry and Rutherford backscattering spectrometry as a function of annealing temperature. Migration of chromium to the surface was observed for films annealed at 400 and 600 °C. Combining the two techniques determined that more than 60% of chromium comprising the as-prepared Haynes 230 layer moves to the surface when annealed at 600 °C, where it forms an oxide layer.
The National Nuclear Security Administration's Tritium Sustainment Program is responsible for the design, development, demonstration, testing, analysis, and characterization of tritium - producing burnable absorber rods (TPBARs) and their components used to produc e tritium for the nation's strategic stockpile. The FY1 9 call for proposals included the specific basic science research topic, "Demonstration and evaluation of advanced characterization methods, particularly for quantifying the concentration of lig ht isotopes ( 1 H, 3 H, 3 He , and 4 He, 6 Li and 7 Li ) in metal or ceramic matrices". Last year the same language appeared in the call for proposals, and a project IWO - 389859 was awarded to the Ion Beam Lab (IBL) at Sandia - NM which was successful using Elastic Recoil Detection, but in the future could have resulted in tritium contamination that jeopardized other equally important NNSA projects . An alternative approach using deuterium nuclear reaction analysis was proposed and funded in FY2019 which was also suc cessful and eliminated any possibility of contaminating the Ion Beam Laboratory with tritium, and will be described in this report . (page intentionally left blank)
This report documents work done at the Sandia Ion Beam Laboratory to develop a capability to produce 14 Me neutrons at levels sufficient for testing radiation effects on electronic materials and components. The work was primarily enabled by a laboratory directed research and development (LDRD) project. The main elements of the work were to optimize target lifetime, test a new thin- film target design concept to reduce tritium usage, design and construct a new target chamber and beamline optimized for high-flux tests, and conduct tests of effects on electronic devices and components. These tasks were all successfully completed. The improvements in target performance and target chamber design have increased the flux and fluence of 14 MV neutrons available at the test location by several orders of magnitude. The outcome of the project is that a new capability for testing radiation-effects on electronic components from 14 MeV neutrons is now available at Sandia National Laboratories. This capability has already been extensively used for many qualification and component evaluation and development tests.
Materials that incorporate hydrogen are of great interest for both scientific and technological reasons. The Ion Beam Laboratory at Sandia National Laboratories has developed techniques using micron to mm-size MeV ion beams to recoil H and its isotopes (Elastic Recoil Detection or ERD) that can very accurately make such measurements. However, there are many measurements that would benefit the field of materials science and technology that require much better resolution. To address these and many other issues, we have demonstrated that H can be recoiled through a thin film of Mylar by 70 keV electrons and detected with a channeltron electron multiplier (CEM). The electrons were steered away from the CEM by strong permanent magnets. This has proven the feasibility that the high energy electrons from a Transmission Electron Microscope-TEM can potentially be used to recoil and subsequently detect (e-ERD), quantify and map the concentration of H isotopes with nm resolution.
Diamond-like carbon (DLC) films were tribochemically formed from ambient hydrocarbons on the surface of a highly stable nanocrystalline Pt-Au alloy. A sliding contact between an alumina sphere and Pt-Au coated steel exhibited friction coefficients as low as μ = 0.01 after dry sliding in environments containing trace (ppb) organics. Ex situ analysis indicated that the change in friction coefficient was due to the formation of amorphous carbon films, and Raman spectroscopy and elastic recoil analysis showed that these films consist of sp2/sp3 amorphous carbon with as much as 20% hydrogen. Transmission electron microscopy indicated these films had thicknesses exceeding 100 nm, and were enhanced by the incorporation of worn Pt-Au nanoparticles. The result was highly wear-resistant, low-friction DLC/Pt-Au nanocomposites. Atomistic simulations of hydrocarbons under shear between rigid Pt slabs using a reactive force field showed stress-induced changes in bonding through chain scission, a likely route towards the formation of these coatings. This novel demonstration of in situ tribochemical formation of self-lubricating films has significant impact potential in a wide range of engineering applications.
The National Nuclear Security Administration's Tritium Sustainment Program is responsible for the design, development, demonstration, testing, analysis, and characterization of tritium-producing burnable absorber rods (TPBARs) and their components, in addition to producing tritium for the nation's strategic stockpile. The FY18 call for proposals included the specific basic science research topic, "Demonstration and evaluation of advanced characterization methods, particularly for quantifying the concentration of light isotopes (1H, 2H, and 4He, 6Li, and 7Li) in metal or ceramic matrices". A project IWO-389859 was awarded to the Ion Beam Lab (IBL) at Sandia-NM in FY18. This reports the success we had in developing and demonstrating such a method: 42 MeV Si+ 7 from the IBL' s Tandem was used to recoil these light isotopes into special detectors that separated all these isotopes by simultaneously measuring the energy and stopping power of these reoils. This technique, called Heavy Ion - Elastic Recoil Detection or HI-ERD, accurately measured the enriched 6 Li/Li-total of 0.246 +- 0.016, compared to the known value of 0.239. The isotopes 1H, 2H, 4He, 6Li and 7Li were also measured. (page intentionally left blank)
Materials that incorporate hydrogen and helium isotopes are of great interest at Sandia and throughout the NNSA and DOE. The Ion Beam Lab at SNL-NM has invented techniques using micron to mm-size MeV ion beams to recoil these light isotopes (Elastic Recoil Detection or ERD) that can very accurately make such measurements. However, there are many measurements that would benefit NW and DOE that require much better resolution, such as the distribution of H isotopes (and 3He) in individual grains of materials relevant to TPBARs, H and He-embrittlement of weapon components important to Tritium Sustainment Programs, issues with GTSs, batteries… Higher resolution would also benefit the field of materials science in general. To address these and many other issues, nm-scale lateral resolution is required. This LDRD demonstrated that neutral H atoms could be recoiled through a thin film by 70 keV electrons and detected with a Channeltron electron multiplier (CEM). The electrons were steered away from the CEM by strong permanent magnets. This proved the feasibility that the high energy electrons from a transmissionelectron- microscope-TEM can potentially be used to recoil and subsequently detect (e-ERD), quantify and map the concentration of H and He isotopes with nm resolution. This discovery could lead to a TEM-based H/He-isotope nanoprobe with 1000x higher resolution than currently available.
The Hecht equation can be used to model the nonlinear degradation of charge collection efficiency (CCE) in response to radiation-induced displacement damage in both fully and partially depleted GaAs photodiodes. CCE degradation is measured for laser-generated photocurrent as a function of fluence and bias in Al0.3Ga0.7As/GaAs/Al0.25Ga0.75As p-i-n photodiodes which have been irradiated with 12 MeV C and 7.5 MeV Si ions. CCE is observed to degrade more rapidly with fluence in partially depleted photodiodes than in fully depleted photodiodes. When the intrinsic GaAs layer is fully depleted, the 2-carrier Hecht equation describes CCE degradation as photogenerated electrons and holes recombine at defect sites created by radiation damage in the depletion region. If the GaAs layer is partially depleted, CCE degradation is more appropriately modeled as the sum of the 2-carrier Hecht equation applied to electrons and holes generated within the depletion region and the 1-carrier Hecht equation applied to minority carriers that diffuse from the field-free (non-depleted) region into the depletion region. Enhanced CCE degradation is attributed to holes that recombine within the field-free region of the partially depleted intrinsic GaAs layer before they can diffuse into the depletion region.
We propose here a novel device, called the Triassico, to microscopically study the entire surface of millimeter-sized spheres. The sphere dimensions can be as small as 1 mm, and the upper limit defined only by the power and by the mechanical characteristics of the motors used. Three motorized driving rods are arranged so an equilateral triangle is formed by the rod's axes, on such a triangle the sphere sits. Movement is achieved by rotating the rods with precise relative speeds and by exploiting the friction between the sphere and the rods surfaces. The sphere can be held in place by gravity or by an opposing trio of rods. By rotating the rods with specific relative angular velocities, a net torque can be exerted on the sphere which then rotates. No repositioning of the sphere or of the motors is needed to cover the full surface with the investigating tools. An algorithm was developed to position the sphere at any arbitrary polar and azimuthal angle. The algorithm minimizes the number of rotations needed by the rods, in order to efficiently select a particular position on the sphere surface. A prototype Triassico was developed for the National Ignition Facility, of the Lawrence Livermore National Laboratory (Livermore, California, USA), as a sphere manipulation apparatus for ion microbeam analysis at Sandia National Laboratories (Albuquerque, NM, USA) of Xe-doped DT inertial confinement fusion fuel spheres. Other applications span from samples orientation, ball bearing manufacturing, or jewelry.
This project was to use light ion beam induced charge (IBIC) to detect damage cascades generated by a single heavy ion, and thereby reveal details of the shape of the cascade and the physics of recombination of carriers that interact with the cluster. Further IBIC measurements using the hardware and software of this project will improve the accuracy of theoretical models used to predict electrical degradation in devices exposed to radiation environments. In addition, future use of light ion IBIC detection of single ion-induced damage could be used to locate single ion implantation sites in quantum computing applications. This project used Sandia's Pelletron and nanoImplanter (nI) to produce heavy ion-induced collision cascades in p-n diodes, simulating cascades made by primary knock-on atoms recoiled by neutrons. Si and Li beams from the nI were used to perform highly focused scans generating IBIC signal maps where regions of lower charge collection efficiency were observed without incurring further damage. The very first use of ion channeled beams for IBIC was explored to maximize ionization, improve contrast and provide very straight line trajectories to improve lateral resolution.
A MS Excel program has been written that calculates ion channeling half-angles and minimum yields in cubic bcc, fcc and diamond lattice crystals. All of the tables and graphs in the three Ion Beam Analysis Handbooks that previously had to be manually looked up and read from were programed into Excel in handy lookup tables, or parameterized, for the case of the graphs, using rather simple exponential functions with different power functions of the arguments. The program then offers an extremely convenient way to calculate axial and planar half-angles, minimum yields, effects on half-angles and minimum yields of amorphous overlayers. The program can calculate these half-angles and minimum yields for 〈uvw〉 axes and [hkl] planes up to (5 5 5). The program is open source and available at http://www.sandia.gov/pcnsc/departments/iba/ibatable.html.
Displacement damage reduces ion beam induced charge (IBIC) through Shockley-Read-Hall recombination. Closely spaced pulses of 200 keVions focused in a 40 nm beam spot are used to create damage cascades within areas. Damaged areas are detected through contrast in IBIC signals generated with focused ion beams of {200 ions and 60 keV ions. IBIC signal reduction can be resolved over sub-micron regions of a silicon detector damaged by as few as 1000 heavy ions.
Sandia journal manuscript; Not yet accepted for publication
Lemasson, Quentin L.; Kotula, Paul K.; Pichon, Laurent P.; Pacheco, Claire P.; Moignard, Brice M.; Doyle, Barney L.; Van Bennekom, Joosje V.
In the field of archaeometry, it is not uncommon to be presented with art objects that contain inscriptions, signatures and other writings that are nearly impossible to read. Scanned microbeam PIXE offers an attractive approach to attack this problem, but even then the distribution of characteristic X-rays of the element(s) used in these writings can remain illegible. We show in this paper that two methods were used to reveal the inscription: first the use of a GUPIXWin, TRAUPIXE and AGLAEMap software suite enables to make quantitative analysis of each pixel, to visualize the results and to select X-ray peaks that could enable to distinguish letters. Then, the Automated eXpert Spectral Image Analysis (AXSIA) program developed at Sandia, which analyzes the x-ray intensity vs. Energy and (X, Y) position “datacubes”, was used to factor the datacube into 1) principle component spectral shapes and 2) the weighting images of these components. The specimen selected for this study was a silver plaque representing a scroll from the so-called “MerkelscheTafelaufsatz,” a centrepiece made by the Nuremberg goldsmith Wenzel Jamnitzer in 1549. X-ray radiography of the plaque shows lines of different silver thicknesses, meaning that a text has been removed. The PIXE analysis used a 3-MeV proton beam focused to 50μm and scanned across the sample on different areas of interest of several cm². This analysis showed major elements of Cu and Ag, and minor elements such as Pb, Au, Hg. X-ray intensity maps were then made by setting windows on the various x-ray peaks but the writing on the centrepiece was not revealed even if the map of Cu after data treatment at AGLAE enabled to distinguish some letters. The AXSIA program enabled to factor two main spectral shapes from the datacube that were quite similar and involved virtually all of the X-rays being generated. Nevertheless, small differences between these factors were observed for the Cu K X-rays, Pb, Bi and Au L X-rays. The plot of the factor with the highest Au signal gave also information on the shape of some letters. The comparison of the results obtained by the two methods shows that they both drastically improve the resolution and contrast of such writings and that each of the method can also bring different information on the composition and thus the techniques used for the writing.
The recipients of the 2014 NSREC Outstanding Conference Paper Award are Nathaniel A. Dodds, James R. Schwank, Marty R. Shaneyfelt, Paul E. Dodd, Barney L. Doyle, Michael Trinczek, Ewart W. Blackmore, Kenneth P. Rodbell, Michael S. Gordon, Robert A. Reed, Jonathan A. Pellish, Kenneth A. LaBel, Paul W. Marshall, Scot E. Swanson, Gyorgy Vizkelethy, Stuart Van Deusen, Frederick W. Sexton, and M. John Martinez, for their paper entitled "Hardness Assurance for Proton Direct Ionization-Induced SEEs Using a High-Energy Proton Beam." For older CMOS technologies, protons could only cause single-event effects (SEEs) through nuclear interactions. Numerous recent studies on 90 nm and newer CMOS technologies have shown that protons can also cause SEEs through direct ionization. Furthermore, this paper develops and demonstrates an accurate and practical method for predicting the error rate caused by proton direct ionization (PDI).