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Study of Chromium Migration in a Nickel-Based Alloy Using Polarized Neutron Reflectometry and Rutherford Backscattering Spectrometry

Journal of Physical Chemistry C

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.

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Development of eXternal Nuclear Reaction Analysis (XNRA) Detection Technique for Quantifying Light Isotope Concentrations

Doyle, Barney L.

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)

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14 MeV DT Neutron Test Facility at the Sandia Ion Beam Laboratory

Wampler, William R.; Doyle, Barney L.; Vizkelethy, Gyorgy V.; Bielejec, Edward S.; Snow, Clark S.; Styron, Jedediah D.; Jasica, Matthew J.

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.

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Using high energy electrons for Elastic Recoil Detection of hydrogen

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Doyle, Barney L.; Van Deusen, S.B.; Briggs, S.

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.

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In situ tribochemical formation of self-lubricating diamond-like carbon films

Carbon

Argibay, Nicolas A.; Babuska, Tomas F.; Curry, John C.; Dugger, Michael T.; Lu, Ping L.; Adams, David P.; Nation, Brendan L.; Doyle, Barney L.; Pham, Minh P.; Pimentel, Adam S.; Mowry, Curtis D.; Hinkle, Adam H.; Chandross, M.

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.

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Development of Elastic Recoil Detection Technique for Quantifying Light Isotope Concentrations in Irradiated TPBAR Materials

Doyle, Barney L.; Taylor, Caitlin A.; Hattar, Khalid M.; Muntifering, Brittany R.

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)

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A Hydrogen and He Isotope Nanoprobe

Doyle, Barney L.; Van Deusen, Stuart B.

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.

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Modeling charge collection efficiency degradation in partially depleted GaAs photodiodes using the 1- and 2-carrier Hecht equations

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Auden, E.C.; Vizkelethy, Gyorgy V.; Serkland, Darwin K.; Bossert, David B.; Doyle, Barney L.

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.

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Triassico: A Sphere Positioning System for Surface Studies with IBA Techniques

Physics Procedia

Fontana, Cristiano L.; Doyle, Barney L.

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.

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The anatomy of the minority carrier - atomic cluster interaction in semiconductors

Doyle, Barney L.; Auden, Elizabeth C.; Bielejec, Edward S.; Abraham, John B.; Vizkelethy, Gyorgy V.

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.

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Parameterization of ion channeling half-angles and minimum yields

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Doyle, Barney L.

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.

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Sub-Micron Resolution of Localized Ion Beam Induced Charge Reduction in Silicon Detectors Damaged by Heavy Ions

IEEE Transactions on Nuclear Science

Auden, Elizabeth C.; Pacheco, Jose L.; Bielejec, Edward S.; Vizkelethy, Gyorgy V.; Abraham, John B.; Doyle, Barney L.

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.

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Deciphering a removed text on a 16th c. centrepiece: The benefits of using AGLAEMap and AXSIA to process PIXE maps

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.

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Outstanding conference paper award 2014 IEEE nuclear and space radiation effects conference

IEEE Transactions on Nuclear Science

Dodds, Nathaniel A.; Dodds, Nathaniel A.; Schwank, James R.; Schwank, James R.; Shaneyfelt, Marty R.; Shaneyfelt, Marty R.; Dodd, Paul E.; Dodd, Paul E.; Doyle, Barney L.; Doyle, Barney L.; Trinczek, M.C.; Trinczek, M.C.; Blackmore, E.W.; Blackmore, E.W.; Rodbell, K.P.; Rodbell, K.P.; Reed, R.A.; Reed, R.A.; Pellish, J.A.; Pellish, J.A.; LaBel, K.A.; LaBel, K.A.; Marshall, P.W.; Marshall, P.W.; Swanson, Scot E.; Swanson, Scot E.; Vizkelethy, Gyorgy V.; Vizkelethy, Gyorgy V.; Van Deusen, Stuart B.; Van Deusen, Stuart B.; Sexton, Frederick W.; Sexton, Frederick W.; Martinez, Marino M.; Martinez, Marino M.

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).

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Hardness assurance for proton direct ionization-induced SEEs using a high-energy proton beam

IEEE Transactions on Nuclear Science

Dodds, N.A.; Schwank, James R.; Shaneyfelt, Marty R.; Dodd, Paul E.; Doyle, Barney L.; Trinczek, M.; Blackmore, E.W.; Rodbell, K.P.; Gordon, M.S.; Reed, R.A.; Pellish, J.A.; LaBel, K.A.; Marshall, P.W.; Swanson, Scot E.; Vizkelethy, Gyorgy V.; Van Deusen, Stuart B.; Sexton, Frederick W.; Martinez, Marino M.

The low-energy proton energy spectra of all shielded space environments have the same shape. This shape is easily reproduced in the laboratory by degrading a high-energy proton beam, producing a high-fidelity test environment. We use this test environment to dramatically simplify rate prediction for proton direct ionization effects, allowing the work to be done at high-energy proton facilities, on encapsulated parts, without knowledge of the IC design, and with little or no computer simulations required. Proton direct ionization (PDI) is predicted to significantly contribute to the total error rate under the conditions investigated. Scaling effects are discussed using data from 65-nm, 45-nm, and 32-nm SOI SRAMs. These data also show that grazing-angle protons will dominate the PDI-induced error rate due to their higher effective LET, so PDI hardness assurance methods must account for angular effects to be conservative. We show that this angular dependence can be exploited to quickly assess whether an IC is susceptible to PDI.

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Mapping of radiation-induced resistance changes and multiple conduction channels in TaOx memristors

IEEE Transactions on Nuclear Science

Hughart, David R.; Pacheco, Jose L.; Lohn, Andrew L.; Mickel, Patrick R.; Bielejec, Edward S.; Vizkelethy, Gyorgy V.; Doyle, Barney L.; Wolfley, Steven L.; Dodd, Paul E.; Shaneyfelt, Marty R.; McLain, Michael L.; Marinella, Matthew J.

The locations of conductive regions in TaOx memristors are spatially mapped using a microbeam and Nanoimplanter by rastering an ion beam across each device while monitoring its resistance. Microbeam irradiation with 800 keV Si ions revealed multiple sensitive regions along the edges of the bottom electrode. The rest of the active device area was found to be insensitive to the ion beam. Nanoimplanter irradiation with 200 keV Si ions demonstrated the ability to more accurately map the size of a sensitive area with a beam spot size of 40 nm by 40 nm. Isolated single spot sensitive regions and a larger sensitive region that extends approximately 300 nm were observed.

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Displacement damage caused by gamma-rays and neutrons on Au and Se

Doyle, Barney L.

This report documents theoretical calculations of displacement damage produced by gamma rays and neutrons on various materials. The average energy of the gamma rays was 1.24 MeV and 1.0 MeV for the neutrons. The fluence of the gamma rays was 1.2e14 γ/cm2 , for the neutrons it was 1.0e12 n/cm2. The initial materials of interest were Au and Se. The total doses of the gamma ray exposures were in the 100 kRad range for both elements. An equivalent electron fluence was approximated to be the same as the gamma ray fluence over one gamma ray attenuation length in both materials and at the same 1.24 MeV energy. The maximum recoil energy of the Au and Se for these electrons was calculated relativisticaly to be 29 and 72 eV respectively. The relativisitic McKinley and Feshbach theory for the atomic recoil cross sections produced by the electrons were in the 10s of mbarn range and an upper limit for the concentration of Frenkel pairs for the gamma ray exposures for both elements was in the ppb range. The Robinson Energy Partioning Theory for non-ionizing energy loss (NIEL) of ions in solids was used to calculate the concentration of Frenkel pairs produced by the 1 MeV neutrons, and this concentration was also in the ppb range for both Au and Se. Low damage levels like this can have effects on minority carrier recombination in semiconductors, but are not expected to have any effect on metals like Au, or metalloids such as Se.

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Ion channeling revisited

Doyle, Barney L.; Corona, Aldo C.; Nguyen, Anh N.

A MS Excel program has been written that calculates accidental, or unintentional, ion channeling in cubic bcc, fcc and diamond lattice crystals or polycrystalline materials. This becomes an important issue when simulating the creation by energetic neutrons of point displacement damage and extended defects using beams of ions. 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 powers of the argument. The program then offers an extremely convenient way to calculate axial and planar half-angles and minimum yield or dechanneling probabilities, effects on half-angles of amorphous overlayers, accidental channeling probabilities for randomly oriented crystals or crystallites, and finally a way to automatically generate stereographic projections of axial and planar channeling half-angles. The program can generate these projections and calculate these probabilities for axes and [hkl] planes up to (555).

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Theory of using magnetic deflections to combine charged particle beams

Doyle, Barney L.; Steckbeck, Mackenzie K.

Several radiation effects projects in the Ion Beam Lab (IBL) have recently required two disparate charged particle beams to simultaneously strike a single sample through a single port of the target chamber. Because these beams have vastly different mass–energy products (MEP), the low-MEP beam requires a large angle of deflection toward the sample by a bending electromagnet. A second electromagnet located further upstream provides a means to compensate for the small angle deflection experienced by the high-MEP beam during its path through the bending magnet. This paper derives the equations used to select the magnetic fields required by these two magnets to achieve uniting both beams at the target sample. A simple result was obtained when the separation of the two magnets was equivalent to the distance from the bending magnet to the sample, and the equation is given by: Bs= 1/2(rc/rs) Bc, where Bs and Bc are the magnetic fields in the steering and bending magnet and rc/rs is the ratio of the radii of the bending magnet to that of the steering magnet. This result is not dependent upon the parameters of the high MEP beam, i.e. energy, mass, charge state. Therefore, once the field of the bending magnet is set for the low-MEP beam, and the field in the steering magnet is set as indicted in the equation, the trajectory path of any high-MEP beam will be directed into the sample.

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Rutherford forward scattering and elastic recoil detection (RFSERD) as a method for characterizing ultra-thin films

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Lohn, Andrew J.; Doyle, Barney L.; Stein, Gregory J.; Mickel, Patrick R.; Stevens, James E.; Marinella, Matthew J.

We present a novel ion beam analysis technique combining Rutherford forward scattering and elastic recoil detection (RFSERD) and demonstrate its ability to increase efficiency in determining stoichiometry in ultrathin (5-50 nm) films as compared to Rutherford backscattering. In the conventional forward geometries, scattering from the substrate overwhelms the signal from light atoms but in RFSERD, scattered ions from the substrate are ranged out while forward scattered ions and recoiled atoms from the thin film are simultaneously detected in a single detector. The technique is applied to tantalum oxide memristors but can be extended to a wide range of materials systems. © 2014 Published by Elsevier B.V.

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Effect of B+ Flux on the electrical activation of ultra-shallow B+ implants in Ge

ECS Transactions

Yates, B.R.; Darby, B.L.; Petersen, D.H.; Hansen, O.; Lin, R.; Nielsen, P.F.; Doyle, Barney L.; Kontos, A.; Jones, K.S.

The residual implanted dose of ultra-shallow B+ implants in Ge was characterized using elastic recoil detection and was determined to correlate well with simulations with a dose loss of 23% due to ion backscattering for 2 keV implants in Ge. The electrical characterization of ultra-shallow B+ implants at 2 keV to a dose of 5.0×1014 cm-2 at beam currents ranging from 0.4 to 6.4 mA has been studied using micro Hall effect measurements after annealing at 400°C for 60 s. It has been shown that the sheet number increases with beam current across the investigated range with electrical activation being 76% higher at 6.4 mA as compared to 0.4mA. However, at 6.4 mA, the electrically active fraction remained low at 11.4%. Structural characterization revealed that the implanted region remained crystalline and amorphization is not able to explain the increased activation. The results suggest the presence of a stable B:Ge cluster whose formation is altered by point defect recombination during high flux implantation which results in increased B activation. © The Electrochemical Society.

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Ion beam characterization of advanced luminescent materials for application in radiation effects microscopy

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Branson, J.V.; Hattar, K.; Rossi, P.; Vizkelethy, G.; Powell, Cody J.; Hernandez-Sanchez, Bernadette A.; Doyle, Barney L.

The ion photon emission microscope (IPEM) is a technique developed at Sandia National Laboratories (SNL) to study radiation effects in integrated circuits with high energy, heavy ions, such as those produced by the 88" cyclotron at Lawrence Berkeley National Laboratory (LBNL). In this method, an ion-luminescent film is used to produce photons from the point of ion impact. The photons emitted due to an ion impact are imaged on a position-sensitive detector to determine the location of a single event effect (SEE). Due to stringent resolution, intensity, wavelength, decay time, and radiation tolerance demands, an engineered material with very specific properties is required to act as the luminescent film. The requirements for this material are extensive. It must produce a high enough induced luminescent intensity so at least one photon is detected per ion hit. The emission wavelength must match the sensitivity of the detector used, and the luminescent decay time must be short enough to limit accidental coincidences. In addition, the material must be easy to handle and its luminescent properties must be tolerant to radiation damage. Materials studied for this application include plastic scintillators, GaN and GaN/InGaN quantum well structures, and lanthanide-activated ceramic phosphors. Results from characterization studies on these materials will be presented; including photoluminescence, cathodoluminescence, ion beam induced luminescence, luminescent decay times, and radiation damage. Results indicate that the ceramic phosphors are currently proving to be the ideal material for IPEM investigations.

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Fast neutron environments

Hattar, Khalid M.; Puskar, J.D.; Doyle, Barney L.; Boyce, Brad B.; Buchheit, Thomas E.; Foiles, Stephen M.; Lu, Ping L.; Clark, Blythe C.; Kotula, Paul G.; Goods, Steven H.

The goal of this LDRD project is to develop a rapid first-order experimental procedure for the testing of advanced cladding materials that may be considered for generation IV nuclear reactors. In order to investigate this, a technique was developed to expose the coupons of potential materials to high displacement damage at elevated temperatures to simulate the neutron environment expected in Generation IV reactors. This was completed through a high temperature high-energy heavy-ion implantation. The mechanical properties of the ion irradiated region were tested by either micropillar compression or nanoindentation to determine the local properties, as a function of the implantation dose and exposure temperature. In order to directly compare the microstructural evolution and property degradation from the accelerated testing and classical neutron testing, 316L, 409, and 420 stainless steels were tested. In addition, two sets of diffusion couples from 316L and HT9 stainless steels with various refractory metals. This study has shown that if the ion irradiation size scale is taken into consideration when developing and analyzing the mechanical property data, significant insight into the structural properties of the potential cladding materials can be gained in about a week.

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Heavy ion radiation effects studies with ion photon emission microscopy

Hattar, Khalid M.; Powell, Cody J.; Doyle, Barney L.

The development of a new radiation effects microscopy (REM) technique is crucial as emerging semiconductor technologies demonstrate smaller feature sizes and thicker back end of line (BEOL) layers. To penetrate these materials and still deposit sufficient energy into the device to induce single event effects, high energy heavy ions are required. Ion photon emission microscopy (IPEM) is a technique that utilizes coincident photons, which are emitted from the location of each ion impact to map out regions of radiation sensitivity in integrated circuits and devices, circumventing the obstacle of focusing high-energy heavy ions. Several versions of the IPEM have been developed and implemented at Sandia National Laboratories (SNL). One such instrument has been utilized on the microbeam line of the 6 MV tandem accelerator at SNL. Another IPEM was designed for ex-vacu use at the 88 cyclotron at Lawrence Berkeley National Laboratory (LBNL). Extensive engineering is involved in the development of these IPEM systems, including resolving issues with electronics, event timing, optics, phosphor selection, and mechanics. The various versions of the IPEM and the obstacles, as well as benefits associated with each will be presented. In addition, the current stage of IPEM development as a user instrument will be discussed in the context of recent results.

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Imaging penetrating radiation through ion photon emission microscopy

Hattar, Khalid M.; Villone, J.; Powell, Cody J.; Doyle, Barney L.

The ion photon emission microscope (IPEM), a new radiation effects microscope for the imaging of single event effects from penetrating radiation, is being developed at Sandia National Laboratories and implemented on the 88' cyclotron at Lawrence Berkeley National Laboratories. The microscope is designed to permit the direct correlation between the locations of high-energy heavy-ion strikes and single event effects in microelectronic devices. The development of this microscope has required the production of a robust optical system that is compatible with the ion beam lines, design and assembly of a fast single photon sensitive measurement system to provide the necessary coincidence, and the development and testing of many scintillating films. A wide range of scintillating material for application to the ion photon emission microscope has been tested with few meeting the stringent radiation hardness, intensity, and photon lifetime requirements. The initial results of these luminescence studies and the current operation of the ion photon emission microscope will be presented. Finally, the planned development for future microscopes and ion luminescence testing chambers will be discussed.

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Radiation microscope for SEE testing using GeV ions

Villone, J.; Hattar, Khalid M.; Doyle, Barney L.; Knapp, J.A.

Radiation Effects Microscopy is an extremely useful technique in failure analysis of electronic parts used in radiation environment. It also provides much needed support for development of radiation hard components used in spacecraft and nuclear weapons. As the IC manufacturing technology progresses, more and more overlayers are used; therefore, the sensitive region of the part is getting farther and farther from the surface. The thickness of these overlayers is so large today that the traditional microbeams, which are used for REM are unable to reach the sensitive regions. As a result, higher ion beam energies have to be used (> GeV), which are available only at cyclotrons. Since it is extremely complicated to focus these GeV ion beams, a new method has to be developed to perform REM at cyclotrons. We developed a new technique, Ion Photon Emission Microscopy, where instead of focusing the ion beam we use secondary photons emitted from a fluorescence layer on top of the devices being tested to determine the position of the ion hit. By recording this position information in coincidence with an SEE signal we will be able to indentify radiation sensitive regions of modern electronic parts, which will increase the efficiency of radiation hard circuits.

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Phosphors' lifetime measurement employing the Time Between Photons method

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Rossi, P.; Doyle, Barney L.; Brice, D.K.; Vizkelethy, G.; McDaniel, F.D.; Branson, J.V.

The Time Between Photons theory (hereafter TBP) is applied to the evaluation of the lifetime of phosphors employed in the Ion Photon Emission Microscope (IPEM). IPEM allows Radiation Effects Microscopy (REM) without focused ion beams and appears to be the best tool for the radiation hardness assessment of modern integrated circuit at cyclotron energies. IPEM determines the impact point of a single ion onto the sample by measuring the light spot produced on a thin phosphor layer placed on the sample surface. The spot is imaged by an optical microscope and projected at high magnification onto a Position Sensitive Detector (PSD). Phosphors, when excited by an ion, emit photons with a particular lifetime, which is important to evaluate. We measured the statistical distribution of the Time Between consecutive detected Photons (TBP) for several phosphors and have been able to link it to their lifetime employing a theory that is derived in this paper. The single-photon signals are provided by the IPEM-PSD, or faster photomultipliers when high-speed materials had to be assessed. © 2009 Elsevier B.V. All rights reserved.

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Ion beam analysis of targets used in controlatron neutron generators

AIP Conference Proceedings

Banks, James C.; Walla, Lisa A.; Walsh, David S.; Doyle, Barney L.

Controlatron neutron generators are used for testing neutron detection systems at Sandia National Laboratories. To provide for increased tube lifetimes for the moderate neutron flux output of these generators, metal hydride (ZrT 2) target fabrication processes have been developed. To provide for manufacturing quality control of these targets, ion beam analysis techniques are used to determine film composition. The load ratios (i.e. T/Zr concentration ratios) of ZrT 2 Controlatron neutron generator targets have been successfully measured by simultaneously acquiring RBS and ERD data using a He ++ beam energy of 10 MeV. Several targets were measured and the film thicknesses obtained from RBS measurements agreed within ±2% with Dektak profilometer measurements. The target fabrication process and ion beam analysis techniques will be presented. © 2009 American Institute of Physics.

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A dual neutron/gamma source for the Fissmat Inspection for Nuclear Detection (FIND) system

Antolak, Arlyn J.; Doyle, Barney L.; King, Michael K.; Provencio, P.N.; Raber, Thomas N.

Shielded special nuclear material (SNM) is very difficult to detect and new technologies are needed to clear alarms and verify the presence of SNM. High-energy photons and neutrons can be used to actively interrogate for heavily shielded SNM, such as highly enriched uranium (HEU), since neutrons can penetrate gamma-ray shielding and gamma-rays can penetrate neutron shielding. Both source particles then induce unique detectable signals from fission. In this LDRD, we explored a new type of interrogation source that uses low-energy proton- or deuteron-induced nuclear reactions to generate high fluxes of mono-energetic gammas or neutrons. Accelerator-based experiments, computational studies, and prototype source tests were performed to obtain a better understanding of (1) the flux requirements, (2) fission-induced signals, background, and interferences, and (3) operational performance of the source. The results of this research led to the development and testing of an axial-type gamma tube source and the design/construction of a high power coaxial-type gamma generator based on the {sup 11}B(p,{gamma}){sup 12}C nuclear reaction.

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Ion-luminescence properties of GaN films being developed for IPEM

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Rossi, Paolo R.; Doyle, Barney L.; Vizkelethy, G.; McDaniel, F.D.; Knapp, J.A.; Jauregui, H.; Villone, J.

Radiation effects microscopy (REM) for the next generation integrated circuits (ICs) will require GeV ions both to provide high ionization and to penetrate the thick overlayers in present day ICs. These ion beams can be provided by only a few cyclotrons in the world. Since it is extremely hard to focus these higher-energy ions, we have proposed the ion photon emission microscope (IPEM) that allows the determination of the ion hits by focusing the emitted photons to a position sensitive detector. The IPEM needs a thin luminescent foil that has high brightness, good spatial resolution and does not change the incident ion's energy and direction significantly. Available organic-phosphor foils require a large thickness to produce enough photons, which results in poor spatial resolution. To solve this problem, we have developed thin, lightly doped n-type GaN films that are extremely bright. We have grown high quality GaN films on sapphire using metal organic chemical vapor deposition (MOCVD), detached the films from the substrate using laser ablation, and made them self-supporting. The smallest foils have 1 mm2 area and 1 μm thickness. The optical properties, such as light yield, spectrum and decay times were measured and compared to those of conventional phosphors, by using both alpha particles from a radioactive source and 250 keV ions from an implanter. We found that the GaN performance strongly depends on composition and doping levels. The conclusion is that 1-2 μm GaN film of a 1 mm2 area may become an ideal ion position detector. © 2007 Elsevier B.V. All rights reserved.

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Photofission in uranium by nuclear reaction gamma-rays

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Morse, Daniel H.; Antolak, Arlyn J.; Doyle, Barney L.

The ideal photon source for active interrogation of fissile materials would use monoenergetic photons to minimize radiation dose to surroundings. The photon energy would be high enough to produce relatively large photofission signals, but below the photoneutron threshold for common cargo materials in order to reduce background levels. To develop such a source, we are investigating the use of low-energy, proton-induced nuclear reactions to generate monochromatic, MeV-energy gamma-rays. Of particular interest are the nuclear resonances at 163 keV for the 11B(p,γ)12C reaction producing 11.7 MeV gamma-rays, 340 keV for the 19F(p,αγ)16O reaction producing 6.13 MeV photons, and 441 keV for the 7Li(p,γ)8Be reaction producing 14.8 and 17.7 MeV photons. A 700 keV Van de Graaff ion accelerator was used to test several potential (p,γ) materials and the gamma-ray yields from these targets were measured with a 5″ × 5″ NaI detector. A pulsed proton beam from the accelerator was used to induce prompt (neutron) and delayed (neutron and gamma-ray) photofission signals in uranium which were measured with 3He and NaI detectors. We show that the accelerator data is in good agreement with Monte Carlo radiation transport calculations and published results.

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Particulate characterization by PIXE multivariate spectral analysis

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Antolak, Arlyn J.; Morse, Daniel H.; Grant, Patrick G.; Kotula, Paul G.; Doyle, Barney L.; Richardson, Charles B.

Obtaining particulate compositional maps from scanned PIXE (proton-induced X-ray emission) measurements is extremely difficult due to the complexity of analyzing spectroscopic data collected with low signal-to-noise at each scan point (pixel). Multivariate spectral analysis has the potential to analyze such data sets by reducing the PIXE data to a limited number of physically realizable and easily interpretable components (that include both spectral and image information). We have adapted the AXSIA (automated expert spectral image analysis) program, originally developed by Sandia National Laboratories to quantify electron-excited X-ray spectroscopy data, for this purpose. Samples consisting of particulates with known compositions and sizes were loaded onto Mylar and paper filter substrates and analyzed by scanned micro-PIXE. The data sets were processed by AXSIA and the associated principal component spectral data were quantified by converting the weighting images into concentration maps. The results indicate automated, nonbiased, multivariate statistical analysis is useful for converting very large amounts of data into a smaller, more manageable number of compositional components needed for locating individual particles-of-interest on large area collection media.

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Damage equivalence of heavy ions in silicon bipolar junction transistors

IEEE Transactions on Nuclear Science

Bielejec, E.; Vizkelethy, G.; Kolb, N.R.; King, Donald B.; Doyle, Barney L.

Results of displacement damage correlation between neutrons, light ions and heavy ions in bipolar junction transistors are presented. Inverse gain degradation as the function of fluence was measured. The inverse gain degradation due to heavy ion irradiation followed the Messenger-Spratt equation, while some deviation was found for light ions. © 2006 IEEE.

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Simulation of neutron displacement damage in bipolar junction transistors using high-energy heavy ion beams

Bielejec, Edward S.; Doyle, Barney L.; Buller, Daniel L.; Fleming, Robert M.; Hjalmarson, Harold P.

Electronic components such as bipolar junction transistors (BJTs) are damaged when they are exposed to radiation and, as a result, their performance can significantly degrade. In certain environments the radiation consists of short, high flux pulses of neutrons. Electronics components have traditionally been tested against short neutron pulses in pulsed nuclear reactors. These reactors are becoming less and less available; many of them were shut down permanently in the past few years. Therefore, new methods using radiation sources other than pulsed nuclear reactors needed to be developed. Neutrons affect semiconductors such as Si by causing atomic displacements of Si atoms. The recoiled Si atom creates a collision cascade which leads to displacements in Si. Since heavy ions create similar cascades in Si we can use them to create similar damage to what neutrons create. This LDRD successfully developed a new technique using easily available particle accelerators to provide an alternative to pulsed nuclear reactors to study the displacement damage and subsequent transient annealing that occurs in various transistor devices and potentially qualify them against radiation effects caused by pulsed neutrons.

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Strain fields around high-energy ion tracks in α-quartz

Journal of Applied Physics

Follstaedt, D.M.; Norman, A.K.; Doyle, Barney L.; McDaniel, F.D.

Transmission electron microscopy has been used to image the tracks of high-energy 197Au +26 (374 MeV) and 127I +18 (241 MeV) ions incident in a nonchanneling direction through a prethinned specimen of hexagonal α-quartz (SiO 2). These ions have high electronic stopping powers in quartz, 24 and 19 keV/nm, respectively, which are sufficient to produce a disordered latent track. When the tracks are imaged with diffraction contrast using several different reciprocal lattice vectors, they exhibit a radial strain extending outward from their disordered centerline approximately 16 nm into the crystalline surroundings. The images are consistent with a radial strain field with cylindrical symmetry around the amorphous track, like that found in models developed to account for the lateral expansion of amorphous SiO 2 films produced by irradiation with high-energy ions. These findings provide an experimental basis for increased confidence in such modeling. © 2006 American Institute of Physics.

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PIXE-quantified AXSIA: Elemental mapping by multivariate spectral analysis

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Doyle, Barney L.; Provencio, P.N.; Kotula, Paul G.; Antolak, Arlyn J.; Ryan, C.G.; Campbell, J.L.; Barrett, K.

Automated, nonbiased, multivariate statistical analysis techniques are useful for converting very large amounts of data into a smaller, more manageable number of chemical components (spectra and images) that are needed to describe the measurement. We report the first use of the multivariate spectral analysis program AXSIA (Automated eXpert Spectral Image Analysis) developed at Sandia National Laboratories to quantitatively analyze micro-PIXE data maps. AXSIA implements a multivariate curve resolution technique that reduces the spectral image data sets into a limited number of physically realizable and easily interpretable components (including both spectra and images). We show that the principal component spectra can be further analyzed using conventional PIXE programs to convert the weighting images into quantitative concentration maps. A common elemental data set has been analyzed using three different PIXE analysis codes and the results compared to the cases when each of these codes is used to separately analyze the associated AXSIA principal component spectral data. We find that these comparisons are in good quantitative agreement with each other. © 2006 Elsevier B.V. All rights reserved.

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Heavy ion beam induced current/charge (IBIC) through insulating oxides

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Vizkelethy, Gyorgy; Brice, David K.; Doyle, Barney L.

Model experiments were performed on MOS (metal-oxide semiconductor) capacitors to study ion beam induced charge generation in silicon-on-insulator (SOI) devices. Surprisingly large induced charge was found and a lateral non-uniformity of the induced charge was discovered across the top electrode of the capacitor. In this paper we will give a simple model for the charge induction in MOS structures and an explanation of the lateral changes in the amount of induced charge. © 2006 Elsevier B.V. All rights reserved.

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Ion-induced gammas for photofission interrogation of HEU

Doyle, Barney L.; Morse, Daniel H.; Provencio, P.N.

High-energy photons and neutrons can be used to actively interrogate for heavily shielded special nuclear material (SNM), such as HEU (highly enriched uranium), by detecting prompt and/or delayed induced fission signatures. In this work, we explore the underlying physics for a new type of photon source that generates high fluxes of mono-energetic gamma-rays from low-energy (<500 keV) proton-induced nuclear reactions. The characteristic energies (4- to 18-MeV) of the gamma-rays coincide with the peak of the photonuclear cross section. The source could be designed to produce gamma-rays of certain selected energies, thereby improving the probability of detecting shielded HEU or providing a capability to determine enrichment inside sealed containers. The fundamental physics of such an interrogation source were studied in this LDRD through scaled ion accelerator experiments and radiation transport modeling. The data were used to assess gamma and neutron yields, background, and photofission-induced signal levels from several (p,{gamma}) target materials under consideration.

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Fabrication of phosphor micro-grids using proton beam lithography

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Auzelyte, V.; Elfman, M.; Kristiansson, P.; Pallon, J.; Wegdén, M.; Nilsson, C.; Malmqvist, K.; Doyle, Barney L.; Rossi, P.; Hearne, Sean J.; Provencio, P.N.; Antolak, Arlyn J.

A new nuclear microscopy technique called ion photon emission microscopy or IPEM was recently invented. IPEM allows analysis involving single ions, such as ion beam induced charge (IBIC) or single event upset (SEU) imaging using a slightly modified optical microscope. The spatial resolution of IPEM is currently limited to more than 10 μm by the scattering and reflection of ion-induced photons, i.e. light blooming or spreading, in the ionoluminescent phosphor layer. We are developing a "Microscopic Gridded Phosphor" (also called Black Matrix) where the phosphor nanocrystals are confined within the gaps of a micrometer scale opaque grid, which limits the amount of detrimental light blooming. MeV-energy proton beam lithography is ideally suited to lithographically form masks for the grid because of high aspect ratio, pattern density and sub-micron resolution of this technique. In brief, the fabrication of the grids was made in the following manner: (1) a MeV proton beam focused to 1.5-2 μm directly fabricated a matrix of pillars in a 15 μm thick SU-8 lithographic resist; (2) 7:1 aspect ratio pillars were then formed by developing the proton exposed area; (3) Ni (Au) was electrochemically deposited onto Cu-coated Si from a sulfamate bath (or buffered CN bath); (4) the SU-8 pillars were removed by chemical etching; finally (5) the metal micro-grid was freed from its substrate by etching the underlying Cu layer. Our proposed metal micro-grids promise an order-of-magnitude improvement in the resolution of IPEM. © 2005 Elsevier B.V. All rights reserved.

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Performance of an Alpha-IPEM

Doyle, Barney L.

The ion photon emission microscope, or IPEM, is the first device that allows scientists to microscopically study the effects of single ions in air on semiconductors, microchips and even biological cells without having to focus the beam. Reported here is a prototype, the size of a conventional optical microscope, developed at Sandia. The alpha-IPEM, that employs alpha particles from a radioactive source, represents the first example of IBA imaging without an accelerator. The IPEM resolution is currently limited to 10 {micro}m, but we also report a gridded-phosphor approach that could improve this resolution to that of the optical microscope, or {approx} 1 {micro}m. Finally, we propose that a simple adaptation of the alpha-IPEM could be the only way to maintain the high utility of radiation effects microscopy into the future.

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Direct single ion machining of nanopores

Follstaedt, D.M.; Norman, Adam K.; Doyle, Barney L.

The irradiation of thin insulating films by high-energy ions (374 MeV Au{sup +25} or 241 MeV I{sup +19}) was used to attempt to form nanometer-size pores through the films spontaneously. Such ions deposit a large amount of energy into the target materials ({approx}20 keV/nm), which significantly disrupts their atomic lattice and sputters material from the surfaces, and might produce nanopores for appropriate ion-material combinations. Transmission electron microscopy was used to examine the resulting ion tracks. Tracks were found in the crystalline oxides quartz, sapphire, and mica. Sapphire and mica showed ion tracks that are likely amorphous and exhibit pits 5 nm in diameter on the surface at the ion entrance and exit points. This suggests that nanopores might form in mica if the film thickness is less than {approx}10 nm. Tracks in quartz showed strain in the matrix around them. Tracks were not found in the amorphous thin films examined: 20 nm-SiN{sub x}, deposited SiOx, fused quartz (amorphous SiO{sub 2}), formvar and 3 nm-C. Other promising materials for nanopore formation were identified, including thin Au and SnO{sub 2} layers.

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A low power ultra-fast current transient measuring device

Doyle, Barney L.; Foltynowicz, Robert J.; Sullivan, John P.; Zutavern, Fred J.

We have studied the feasibility of an innovative device to sample 1ns low-power single current transients with a time resolution better than 10 ps. The new concept explored here is to close photoconductive semiconductor switches (PCSS) with a Laser for a period of 10 ps. The PCSSs are in a series along a Transmission Line (TL). The transient propagates along the TL allowing one to carry out a spatially resolved sampling of charge at a fixed time instead of the usual timesampling of the current. The fabrication of such a digitizer was proven to be feasible but very difficult.

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Radiation effects microscopy for failure analysis of microelectronic devices

Doyle, Barney L.; Dodd, Paul E.; Shaneyfelt, Marty R.; Schwank, James R.

Microelectronic devices in satellites and spacecraft are exposed to high energy cosmic radiation. Furthermore, Earth-based electronics can be affected by terrestrial radiation. The radiation causes a variety of Single Event Effects (SEE) that can lead to failure of the devices. High energy heavy ion beams are being used to simulate both the cosmic and terrestrial radiation to study radiation effects and to ensure the reliability of electronic devices. Broad beam experiments can provide a measure of the radiation hardness of a device (SEE cross section) but they are unable to pinpoint the failing components in the circuit. A nuclear microbeam is an ideal tool to map SEE on a microscopic scale and find the circuit elements (transistors, capacitors, etc.) that are responsible for the failure of the device. In this paper a review of the latest radiation effects microscopy (REM) work at Sandia will be given. Different SEE mechanisms (Single Event Upset, Single Event Transient, etc.) and the methods to study them (Ion Beam Induced Charge (IBIC), Single Event Upset mapping, etc.) will be discussed. Several examples of using REM to study the basic effects of radiation in electronic devices and failure analysis of integrated circuits will be given.

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High-energy ion tracks in thin films

Follstaedt, D.M.; Norman, Adam K.; Rossi, Paolo R.; Doyle, Barney L.

High-energy ion tracks (374 MeV Au{sup 26+}) in thin films were examined with transmission electron microscopy to investigate nanopore formation. Tracks in quartz and mica showed diffraction contrast. Tracks in sapphire and mica showed craters formed at the positions of ion incidence and exit, with a lower-density track connecting them. Direct nanopore formation by ions (without chemical etching) would appear to require film thicknesses less than 10 nm.

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An annular Si drift detector mu PIXE system using AXSIA analysis

Proposed for publication in X-Ray Spectrometry.

Doyle, Barney L.; Walsh, David S.; Rossi, Paolo R.; Kotula, Paul G.

Sandia and Rontec have developed an annular, 12-element, 60 mm{sup 2}, Peltier-cooled, translatable, silicon drift detector called the SDD-12. The body of the SDD-12 is only 22.8 mm in total thickness and easily fits between the sample and the upstream wall of the Sandia microbeam chamber. At a working distance of 1 mm, the solid angle is 1.09 sr. The energy resolution is 170 eV at count rates <40 kcps and 200 eV for rates of 1 Mcps. X-ray count rates must be maintained below 50 kcps when protons are allowed to strike the full area of the SDD. Another innovation with this new {mu}PIXE system is that the data are analyzed using Sandia's Automated eXpert Spectral Image Analysis (AXSIA).

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Ion beam induced luminescence of doped yttrium compounds

Proposed for publication in Nuclear Instruments & Methods in Physics Research Section B.

Rossi, Paolo R.; Seager, Carleton H.; Doyle, Barney L.

Rare earth doped yttrium oxide (yttria) and silicate, Y{sub 2}O{sub 3}:Eu and Y{sub 2}SiO{sub 5}:Tb, are the most promising phosphors for advanced devices such as flat panel field-emission-displays. However, their light yield for electron excitation has proven to be lower than that predicted by early models. New experimental data are needed to improve the theoretical understanding of the cathodoluminescence (CL) that will, in turn, lead to materials that are significantly brighter. Beside the existing CL and photo luminescence (PL) measurements, one can provide new information by studying ion-induced luminescence (IL). Ions penetrate substantially deeper than electrons and their light yield should therefore not depend on surface effects. Moreover, the energy density released by ions can be much higher than that of electrons and photons, which results in possible saturation effects, further testing the adequacy of models. We exposed the above yttrium compounds to three ion beams, H (3 MeV), C (20 MeV), Cu (50 MeV), which have substantially different electronic stopping powers. H was selected to provide an excitation close to CL, but without surface effects. The C and Cu allowed an evaluation of saturation effects because of their higher stopping powers. The IL experiments involved measuring the transient light intensity signal radiating from thin phosphor layers following their exposure to {approx}200 ns ion beam pulses. We present the transient yield curves for the two materials and discuss a general model for this behavior.

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Cross-sections for the elastic recoil of hydrogen isotopes for high energy helium ions

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Browning, J.F.; Banks, J.C.; Wampler, W.R.; Doyle, Barney L.

Cross-sections for the elastic recoil of hydrogen isotopes, including tritium, have been measured for 4He2+ ions in the energy range of 9.0-11.6 MeV. These cross-sections have been measured at a scattering angle of 30° in the laboratory frame. Cross-sections were measured by allowing a 4He2+ beam to fall incident on solid targets of ErH2, ErD2 and ErT2, each of 500 nm nominal thickness and known areal densities of H, D, T and Er. The uncertainty in each cross-section is estimated to be ±3.2%. Published by Elsevier B.V.

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Round robin analyses of hydrogen isotope thin films standards

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Banks, J.C.; Browning, J.F.; Wampler, W.R.; Doyle, Barney L.; LaDuca, C.A.; Tesmer, J.R.; Wetteland, C.J.; Wang, Y.Q.

Hydrogen isotope thin film standards have been manufactured at Sandia National Laboratories for use by the materials characterization community. Several considerations were taken into account during the manufacture of the ErHD standards, with accuracy and stability being the most important. The standards were fabricated by e-beam deposition of Er onto a Mo substrate and the film stoichiometrically loaded with hydrogen and deuterium. To determine the loading accuracy of the standards two random samples were measured by thermal desorption mass spectrometry and atomic absorption spectrometry techniques with a stated combined accuracy of ∼1.6% (1σ). All the standards were then measured by high energy RBS/ERD and RBS/NRA with the accuracy of the techniques ∼5% (1σ). The standards were then distributed to the IBA materials characterization community for analysis. This paper will discuss the suitability of the standards for use by the IBA community and compare measurement results to highlight the accuracy of the techniques used. © 2004 Elsevier B.V. All rights reserved.

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Monte Carlo simulations of multiple scattering effects in ERD measurements

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Arstila, K.; Knapp, J.A.; Nordlund, K.; Doyle, Barney L.

Multiple scattering effects in ERD measurements are studied by comparing two Monte Carlo simulation codes, representing different approaches to obtain acceptable statistics, to experimental spectra measured from a HfO2 sample with a time-of-flight-ERD setup. The results show that both codes can reproduce the absolute detection yields and the energy distributions in an adequate way. The effect of the choice of the interatomic potential in multiple scattering effects is also studied. Finally the capabilities of the MC simulations in the design of new measurement setups are demonstrated by simulating the recoil energy spectra from a WCxNy sample with a low energy heavy ion beam. Published by Elsevier B.V.

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Elastic recoil detection analysis of 3He

Knapp, J.A.; Knapp, J.A.; Wampler, William R.; Banks, J.C.; Doyle, Barney L.

We give the results of a study using Monte Carlo ion interaction codes to simulate and optimize elastic recoil detection analysis for {sup 3}He buildup in tritide films. Two different codes were used. The primary tool was MCERD, written especially for simulating ion beam analysis using optimizations and enhancements for greatly increasing the probabilities for the creation and the detection of recoil atoms. MPTRIM, an implementation of the TRIMRC code for a massively parallel computer, was also used for comparison and for determination of absolute yield. This study was undertaken because of a need for high-resolution depth profiling of 3He and near-surface light impurities (e.g. oxygen) in metal hydride films containing tritium.

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Radiation-Induced Prompt Photocurrents in Microelectronics: Physics

Dodd, Paul E.; Walsh, David S.; Buller, Daniel L.; Doyle, Barney L.

The effects of photocurrents in nuclear weapons induced by proximal nuclear detonations are well known and remain a serious hostile environment threat for the US stockpile. This report describes the final results of an LDRD study of the physical phenomena underlying prompt photocurrents in microelectronic devices and circuits. The goals of this project were to obtain an improved understanding of these phenomena, and to incorporate improved models of photocurrent effects into simulation codes to assist designers in meeting hostile radiation requirements with minimum build and test cycles. We have also developed a new capability on the ion microbeam accelerator in Sandia's Ion Beam Materials Research Laboratory (the Transient Radiation Microscope, or TRM) to supply ionizing radiation in selected micro-regions of a device. The dose rates achieved in this new facility approach those possible with conventional large-scale dose-rate sources at Sandia such as HERMES III and Saturn. It is now possible to test the physics and models in device physics simulators such as Davinci in ways not previously possible. We found that the physical models in Davinci are well suited to calculating prompt photocurrents in microelectronic devices, and that the TRM can reproduce results from conventional large-scale dose-rate sources in devices where the charge-collection depth is less than the range of the ions used in the TRM.

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Diffusion-time-resolved ion-beam-induced charge collection from stripe-like test junctions induced by heavy-ion microbeams

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Guo, B.N.; El Bouanani, M.; Renfrow, S.N.; Nigam, M.; Walsh, David S.; Doyle, Barney L.; Duggan, J.L.; McDaniel, F.D.

To design more radiation-tolerant integrated circuits (ICs), it is necessary to design and test accurate models of ionizing-radiation-induced charge collection dynamics. A new technique, diffusion-time-resolved ion-beam-induced charge collection (DTRIBICC), is used to measure the average arrival time of the diffused charge, which is related to the average time of the arrival carrier density at the junction. Specially designed stripe-like test junctions are studied using a 12 MeV carbon microbeam with a spot size of ∼1 μm. The relative arrival time of ion-generated charge and the collected charge are measured using a multiple parameter data acquisition system. A 2-D device simulation code, MEDICI, is used to calculate the charge collection dynamics on the stripe-like test junctions. The simulations compare well with experimental microbeam measurements. The results show the importance of the diffused charge collection by junctions, which is especially significant for single-event upsets (SEUs) and m ultiple-event upsets (MEUs) in electronic devices. The charge sharing results also indicate that stripe-like junctions may be used as position-sensitive detectors with a resolution of ∼0.1 μm. © 2001 Elsevier Science B.V. All rights reserved.

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Luminescent layers for ion-photon emission microscopy

Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms

Yang, C.; Doyle, Barney L.; Rossi, P.; Nigam, M.; El Bouanani, M.; Duggan, J.L.; McDaniel, F.D.

Ion beam induced luminescence (IBIL) combined with ion beam induced charge collection (IBICC) is applied in a quantitative study of the IBIL generation yield and detection efficiency for several plastic phosphor materials. The main purpose of this study is to search for strongly luminescence materials that can be used to easily coat samples to be studied with ion-photon emission microscopy (IPEM). A special focus is given to plastic scintillation materials because thin films are easily prepared, and such films have already been used for single event triggering. The emission yield was found to be low for typical Bicron plastic phosphors (only ∼70 photons/ion/μm). The total collection, transmission and photon detection efficiency of the optical microscope used in this study was determined to be only ∼0.00003. For thin film plastic phosphors ∼20 μm thick, the detection efficiency was only 0.04 photons/ion. This means that using these plastics, IPEM would need to be performed with ∼20× more beam fluence to obtain data, such as IBICC, similar to a standard scanned nuclear microprobe. Improvements are discussed. © 2001 Elsevier Science B.V. All rights reserved.

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The Study of Phosphors Efficiency and Homogeneity using a Nuclear Microprobe

Doyle, Barney L.; Doyle, Barney L.

Ion Beam Induced Luminescence (IBIL) and Ion Beam Induced Charge Collection (IBICC) have been applied in the study of the luminescence emission efficiency and investigation of the homogeneity of the luminescence emission in phosphors. The IBIL imaging was performed by using sharply focused ion beams or broad/partially-focused ion beams. The luminescence emission homogeneity in samples was examined to reveal possible distributed crystal-defects that may lead to the inhomogeneity of the luminescence emission in samples.The purpose of the study is to search for suitable luminescent thin films that have high homogeneity of luminescence emission, large IBIL efficiency under heavy ion excitation, and can be placed as a thin layer on the top of microelectronic devices to be analyzed with Ion Photon Emission Microscopy (IPEM). The emission yield was found to be low for organic materials, due to saturation of the light output dependence on the energy deposition of heavy ions. The emission yield of a typical Bicron plastic scintillator is about 70 photons/ion/micron. Inorganic materials may have higher IBIL yield under high-energy and heavy-ion excitation, but the challenging problem is the inhomogeneity of the IBIL emission. The IBIL image techniques are applied in the investigation of the homogeneity of a GaN epitaxial thin film, a zircon single crystal and a thin layer coated by Thiogallate(EuII) ceramic.

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Nuclear microprobe studies of the electronic transport properties of cadmium zinc telluride (CZT) radiation detectors

Proceedings of SPIE - The International Society for Optical Engineering

Vizkelethy, G.; Doyle, Barney L.; Walsh, David S.; James, R.B.

Ion Beam Induced Charge Collection (IBICC) is a proven albeit relatively new method to measure the electronic transport properties of room temperature radiation detectors. Using an ion microbeam, the charge collection efficiency of CZT detectors can be mapped with submicron resolution and maps of the electron mobility and lifetime can be calculated. The nuclear microprobe can be used not only for characterizing detectors but also with the use of Time Resolved IBICC (TRIBICC) and lateral IBICC/TRIBICC we can deduce information about the electron and hole mobility and lifetime profiles, and about the variation of electric field along the detectors' axes. The Sandia Nuclear Microprobe has been and is being used routinely to characterize CZT detectors and measure their electronic transport properties. In this paper we will present the results of these measurements for different detectors. Furthermore the damage effects caused by the probing beam will be discussed and a simple model will be presented to explain the characteristic charge collection efficiency pattern observed after high dose irradiation. © 2000 SPIE.

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Microbeam Studies of Diffusion Time Resolved Ion Beam Induced Charge Collection from Stripe-Like Junctions

Applied Physics Letters

Walsh, David S.; Walsh, David S.; Doyle, Barney L.

To design more radiation tolerant Integrated Circuits (ICs), it is essential to create and test accurate models of ionizing radiation induced charge collection dynamics within microcircuits. A new technique, Diffusion Time Resolved Ion Beam Induced Charge Collection (DTRIBICC), is proposed to measure the average arrival time of the diffused charge at the junction. Specially designed stripe-like junctions were experimentally studied using a 12 MeV carbon microbeam with a spot size of 1 {micro}m. The relative arrival time of ion-generated charge is measured along with the charge collection using a multiple parameter data acquisition system. The results show the importance of the diffused charge collection by junctions, which is especially significant in accounting for Multiple Bit Upset (MBUs) in digital devices.

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Time resolved ion beam induced charge collection

Sexton, Frederick W.; Walsh, David S.; Doyle, Barney L.; Dodd, Paul E.

Under this effort, a new method for studying the single event upset (SEU) in microelectronics has been developed and demonstrated. Called TRIBICC, for Time Resolved Ion Beam Induced Charge Collection, this technique measures the transient charge-collection waveform from a single heavy-ion strike with a {minus}.03db bandwidth of 5 GHz. Bandwidth can be expanded up to 15 GHz (with 5 ps sampling windows) by using an FFT-based off-line waveform renormalization technique developed at Sandia. The theoretical time resolution of the digitized waveform is 24 ps with data re-normalization and 70 ps without re-normalization. To preserve the high bandwidth from IC to the digitizing oscilloscope, individual test structures are assembled in custom high-frequency fixtures. A leading-edge digitized waveform is stored with the corresponding ion beam position at each point in a two-dimensional raster scan. The resulting data cube contains a spatial charge distribution map of up to 4,096 traces of charge (Q) collected as a function of time. These two dimensional traces of Q(t) can cover a period as short as 5 ns with up to 1,024 points per trace. This tool overcomes limitations observed in previous multi-shot techniques due to the displacement damage effects of multiple ion strikes that changed the signal of interest during its measurement. This system is the first demonstration of a single-ion transient measurement capability coupled with spatial mapping of fast transients.

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176 Results
176 Results