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At least 37 records · Page 2

Improved quantitation of SIMS depth profile measurements of niobium via sample holder design improvements and characterization of grain orientation effects

The importance of SIMS analyses for “N-doped” impurity alloyed niobium and other surface-alloyed materials continues to increase. A major hurdle is the uncertainty of instrument calibration due to changes in sample height either from sample surface topography or from the sample holder itself. The CAMECA sample holder design allows for many types of samples to be analyzed. However, a drawback is that the holder faceplate can bend, contributing an uncertainty in the relative sensitivity factor (RSF) used to quantify the SIMS results. Here, we describe an improved sample holder having a reinforced faceplate, which prevents deflection and reduces uncertainty. Simulations show that the new design significantly reduces deflection from 10 μm to 5 nm. Sample measurements show a reduction of RSF uncertainty from this source from 4.1% to 0.95%. Grain orientation has long been suspected to affect RSF measurement as well. A bicrystal implant standard, consisting of randomly oriented and [001] grains, was successively rotated 15° between analyses. It was observed that 20% of the analyses performed on the randomly oriented grain exhibited anomalously high RSF values as well as slow sputter rates. These features were associated with the changing grain normal orientation with respect to the primary Cs + beam. The grain orientation associated with the rise in RSF was simulated and determined to be the [101] crystallographic plane, thus indicating that ion channeling was responsible for the significantly increased RSF. Focused ion beam analysis confirmed slower sputter rates for the cardinal crystallographic orientations, indicating that ion channeling occurred for each.

43 PARTICLE ACCELERATORS↗

Sampling and Analysis of Impact Crater Residues Found on the Wide Field Planetary Camera-2 Radiator

After nearly 16 years in low Earth orbit (LEO), the Wide Field Planetary Camera-2 (WFPC2) was recovered from the Hubble Space Telescope (HST) in May 2009, during the 12 day shuttle mission designated STS-125. The WFPC-2 radiator had been struck by approximately 700 impactors producing crater features 300 microns and larger in size. Following optical inspection in 2009, agreement was reached for joint NASA-ESA study of crater residues, in 2011. Over 480 impact features were extracted at NASA Johnson Space Center's (JSC) Space Exposed Hardware clean-room and curation facility during 2012, and were shared between NASA and ESA. We describe analyses conducted using scanning electron microscopy (SEM) - energy dispersive X-ray spectrometry (EDX): by NASA at JSC's Astromaterials Research and Exploration Science (ARES) Division; and for ESA at the Natural History Museum (NHM), with Ion beam analysis (IBA) using a scanned proton microbeam at the University of Surrey Ion Beam Centre (IBC).

Kearsley, A. T.↗

Nuclear Microprobe using Elastic Recoil Detection (ERD) for Hydrogen Profiling in High Temperature Protonic Conductors

The interaction between hydrogen and various high temperature protonic conductors (HTPC) has not been clearly understood due to poor densification and unreacted secondary phases. the melt-processing technique is used in producing fully dense simple SrCe(0.9)Y (0.10) O(3-delta) and complex Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskites that can not be achieved by solid-state sintering. the possibilities of ion beam analysis have been investigated to quantify hydrogen distribution in HTPC perovskites subjected to water heat treatment. Nuclear microprobe technique is based on the interactions of a focused ion beam of MeV light ions (H-1, H-2, He-3, He-4,.) with the sample to be analyzed to determine local elemental concentrations at the cubic micrometer scale, the elastic recoil detection analysis technique (ERDA) has been carried out using He-4(+) microbeams and detecting the resulting recoil protons. Mappings of longitudinal sections of water treated SrCeO3 and Sr(Ca(1/3)Nb(2/3))O3 perovskites have been achieved, the water treatment strongly alters the surface of simple SrCe(0.9)Y(0.10)O(3-delta) perovskite. From Rutherford Back Scattering measurements (RBS), both Ce depletion and surface re-deposition is evidenced. the ERDA investigations on water treated Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskite did not exhibit any spatial difference for the hydrogen incorporation from the surface to the centre. the amount of hydrogen incorporation for Sr3Ca(1+x)Nb(2+x)O(9-delta) was low and required further development of two less conventional techniques, ERDA in forward geometry and forward elastic diffusion H-1(p,p) H-1 with coincidence detection.

Berger, Pascal↗

Sampling and Analysis of Impact Crater Residues found on the Wide Field Planetary Camera-2 Radiator

After nearly 16 years on orbit, the Wide Field Planetary Camera-2 (WFPC-2) was recovered from the Hubble Space Telescope in May 2009 during the 12 day shuttle mission designated STS-125. During that exposure to the low Earth orbit environment, the WFPC-2 radiator was struck by approximately 700 impactors producing crater features 300 micrometers and larger in size. Following an optical inspection of these features in 2009, an agreement was reached for the joint NASA-ESA examination and characterization of crater residues, the remnants of the projectile, in 2011. Active examination began in 2012, with 486 of the impact features being cored at NASA Johnson Space Center fs (JSC) Space Exposed Hardware cleanroom and curation facility. The core samples were subsequently divided between NASA and ESA. NASA's analysis was conducted at JSC fs Astromaterials Research and Exploration Science (ARES) Division, using scanning electron microscopy (SEM)/ energy dispersive X-ray spectrometry (EDS) methods, and ESA's analysis was conducted at the Natural History Museum (NHM) again using SEM/EDS, and at the University of Surrey Ion Beam Centre (IBC) using ion beam analysis (IBA) with a scanned proton microbeam. As detailed discussion of the joint findings remains premature at this point, this paper reports on the coring technique developed; the practical taxonomy developed to classify residues as belonging either to anthropogenic "orbital debris" or micrometeoroids; and the protocols for examination of crater residues. Challenges addressed in coring were the relative thickness of the surface to be cut, protection of the impact feature from contamination while coring, and the need to preserve the cleanroom environment so as to preclude or minimize cross-contamination. Classification criteria are summarized, including the assessment of surface contamination and surface cleaning. Finally, we discuss the analytical techniques used to examine the crater residues. We employed EDS from either electron excitation (SEM-EDS) and, in a minority of cases for cores assessed as "difficult" targets, proton excitation (IBA). All samples were documented by electron imagery: backscattered electron imagery in the SEM, and where appropriate, secondary electron imagery during IBA.

Kearsley, A. T.↗

A dual dynamic shutter system for accelerating ion irradiation sample throughput via lateral gas implantation gradients

Ion irradiation for material performance testing is limited due to its serial nature, which allows for only one value of the implantation (appm) versus dose (dpa) parameter space to be explored for each ion and experiment at a time. While ion irradiation can accelerate the process by up to three orders of magnitude compared to neutron irradiation experiments, the sample throughput for ion irradiation remains relatively low. To address these limitations, a novel capability has been developed at the Michigan Ion Beam Laboratory (MIBL), enabling for the creation of single- and two-dimensional lateral ion implantation gradients using recently installed motorized-controlled ion-beam shutters. This advancement can generate a wide scope of the two-dimensional (H+, He2+) implantation parameter space within a single sample. Integration of this new capability now allows for dual- and triple-ion beam experiments to be performed with full user control over not only the ion implantation depth, but also laterally across the sample by imposing ion implantation concentration gradients, thus providing researchers with a high-throughput means for material testing under various irradiation conditions. Furthermore, recent improvements in MIBL's microbeam ion-beam analysis (IBA) target station now allow for probing these concentration gradients in irradiated alloys with exceptional spatial resolution, down to 10 µm. These two approaches promise to significantly improve ion irradiation capabilities and increase the sample throughput by several orders of magnitude. The application of the shutter technique plus the subsequent microbeam characterization of the imposed implantation gradients are showcased by two proof-of-principle ion-irradiated experiments, one performed on single-crystal Si and the other on the fusion-candidate alloy F82H-IEA. These advancements mark a substantial leap in ion-beam technology, offering researchers a robust, high-throughput method to efficiently investigate candidate alloys with high technological readiness for both advanced fission and fusion reactor applications, in a time- and cost-effective manner.

36 - MATERIALS SCIENCE↗

Liquid lithium wetting and percolation in a porous tungsten/liquid Li plasma facing component (PFC)

This work explores the concept of a hybrid material system designed to protect the plasma from high-Z material emission while also protecting an underlying high-Z wall material from erosion by integrating a low-Z component in the liquid phase. Plasma-surface interaction properties of a porous tungsten (W)-liquid metal hybrid system, having the favorable bulk thermomechanical properties of W while serving as a scaffold for a liquid metal with self-healing and radiative vapor shielding characteristics, are examined. W-substrates with 70% density of bulk W and 1–5 μm sized pores have been fabricated with 50-nm W powders using spark plasma sintering. Enhanced lithium (Li) wettability, driven by percolation through the porous W architecture, is demonstrated with in-situ liquid Li drop measurements. Finally, results show complete wetting of liquid Li at 250 °C in the porous W, 100 °C lower temperature than what has been observed on traditional W surfaces. In operando ion beam analysis of Li films deposited on porous W substrates provides microscopic evidence of Li percolation into the substrate and a first look at D retention up to a depth of 100 nm after plasma exposure at a flux of 10 20 m –2 s –1 , 250 eV/amu D + plasma to a fluence of 1.16 × 10 23 m –2 at a temperature of 200 °C.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Improvement in the spatial resolution of heavy ion beam probe measurements through application of ion optics

A technique for more accurately modeling and improving the spatial resolution of heavy ion beam probe measurements is described. We use a set of particle trajectories to numerically determine the focusing properties of a complicated three-dimensional magnetic field and characterize those properties with a transfer matrix. We then modify the transfer matrix approach of traditional ion optics to include a parameter that describes the ionization location of the detected ions. The ion optics model calculated using this technique enables a more accurate description of the particle trajectories than previously feasible. The model also allows one to easily determine an initial beam focus that could be used during experimental operation to optimize the spatial resolution of measurements. The technique has been applied to the design of a heavy ion beam probe diagnostic for the Wendelstein 7-X stellarator and improvements in the modeled spatial resolution by a factor of about 2 over previous estimates are possible. As a result, the improved spatial resolution will enable measurements of plasma fluctuations with smaller wavelengths than would otherwise be possible.

43 PARTICLE ACCELERATORS↗

Tuning of the electronic and vibrational properties of epitaxial MoS 2 through He-ion beam modification

Abstract Atomically thin transition metal dichalcogenides (TMDs), like MoS 2 with high carrier mobilities and tunable electron dispersions, are unique active material candidates for next generation opto-electronic devices. Previous studies on ion irradiation show great potential applications when applied to two-dimensional (2D) materials, yet have been limited to micron size exfoliated flakes or smaller. To demonstrate the scalability of this method for industrial applications, we report the application of relatively low power (50 keV) 4 He + ion irradiation towards tuning the optoelectronic properties of an epitaxially grown continuous film of MoS 2 at the wafer scale, and demonstrate that precise manipulation of atomistic defects can be achieved in TMD films using ion implanters. The effect of 4 He + ion fluence on the PL and Raman signatures of the irradiated film provides new insights into the type and concentration of defects formed in the MoS 2 lattice, which are quantified through ion beam analysis. PL and Raman spectroscopy indicate that point defects are generated without causing disruption to the underlying lattice structure of the 2D films and hence, this technique can prove to be an effective way to achieve defect-mediated control over the opto-electronic properties of MoS 2 and other 2D materials.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Direct Analysis of Early Solar System Aqueous Fluids

We lack fundamental information on early solar system aqueous fluids. Fluid inclusions are present in carbonates, sulfides and halides in astro materials, whose characterization is finally becoming feasible. The ordinary chondrite regolith breccias Monahans 1998 (H5) and Zag (H3-6)contain fluid inclusion-bearing halite (NaCl) crystals dated at~4.5 billion years old. Freezing studies to measure the eutectic temperature demonstrated that the brines likely contain divalent cations(Ca, Mg, Fe). Halite is effective at preservation (at least 250 MY) of organic phases and structures. Thus, compositional data on fluid inclusions in halite will reveal unique information on the origin and activity of aqueous fluids in the early solar system, and interactions with organics. To measure fluid compositions from individual fluid inclusions we performed TOF-SIMS depth profiling a tultra-high vacuum at ~110 Kusing a 30 kVBi+analysis ion beam and a1 kVO2+sputtering ion beam. Halite fluid inclusion FI1 contains H2O, K,Na,Cl and NaCl•2H2O.FI2 contains H2O, K, Na, Cl, Al, Fe,Ca,NaCl•2H2O and C-N-O-H species originating from organic molecules. Mass overlap with NaOH species prevented definitive identification of Cain FI1.

M. E Zolensky↗

Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues

Meteoritics research is a major beneficiary of recent developments in analytical instrumentation [1,2]. Integrated studies in which multiple analytical techniques are applied to the same specimen are providing new insight about the nature of IDPs [1]. Such studies are dependent on the ability to prepare specimens that can be analyzed in multiple instruments. Focused ion beam (FIB) microscopy has revolutionized specimen preparation in materials science [3]. Although FIB has successfully been used for a few IDP and meteorite studies [1,4-6], it has yet to be widely utilized in meteoritics. We are using FIB for integrated TEM/NanoSIMS/synchrotron infrared (IR) studies [1].

Graham, G. A.↗

Statistical analysis of upflowing ion beam and conic distributions at DE 1 altitudes

Upflowing ion (UFI), beam, conic, and hybrid pitch angle distribution data obtained in the 8000-23,000-km altitude range by the energetic ion composition spectrometer of the DE 1 satellite during September 1981-June 1986 have been statistically analyzed. It is found that the source and transport mechanisms largely confine UFI to auroral field lines; no obvious one-to-one relationship is found between current direction and UFI source characteristics. O(+) is more efficiently accelerated than H(+) at the higher K(p) values.

Kondo, T.↗

Hybrid Simulation of Proton Cyclotron Waves Upstream of Mars Generated by Pickup Ion Beam Distribution

Linear instability analysis as well as a corresponding two‐dimensional hybrid simulation are performed to examine the excitation of the proton cyclotron waves observed upstream of Mars. The waves are believed to be excited by the pickup ions produced from the ionization of the Martian hydrogen exosphere. And previous statistical analysis of wave observations suggested that the waves are mostly related to pickup ion beam velocity distributions. While earlier linear instability analysis of pickup ion beam distributions has mainly been focused on the parallel unstable modes, our analysis reveals that the maximum growth rate occurs at very oblique propagation. The corresponding hybrid simulation confirms the linear analysis results and further demonstrates that the pickup ions are scattered toward an isotropic shell velocity distribution by the waves excited. Interestingly, the waves at oblique propagation gradually damp out and the system is eventually dominated by waves of quasi‐parallel propagation.

79 ASTRONOMY AND ASTROPHYSICS↗

Comparative Mechanical Properties Analysis of Triple Ion-Beam Irradiated and Neutron Irradiated Potential Plasma Facing Components

Abstract Several classes of materials are being proposed for use in fusion reactors including oxide dispersion strengthened (ODS) and reduced activation ferritic-martensitic (RAF/M) steels to withstand the severe and harsh conditions. In this work, the mechanical properties of a Fe-16Cr-4Al-2W-0.3Ti-0.3Y 2 O 3 (K3) (ODS) ferritic steel and a Fe-8.9Cr-1.1W-0.47Mn-0.2V-0.14Ta-0.11C (Eurofer 97) (RAF/M) steel) after triple ion beam irradiation were locally evaluated utilizing in-situ micro-pillar compression tests, and continuous stiffness/quasi-static nanoindentation. No change in mechanical properties was observed in the K3 ODS steel. However, the Eurofer 97 RAF/M steel exhibited radiation-induced effects via increases in yield strength. Micro-pillar techniques were expanded to neutron-irradiated materials via an in-situ testing technique employing lift-out methods on Fe-14Cr-0.9Ti-0.3Mo-0.25Y 2 O 3 (MA957) ODS ferritic steel. Both the non-irradiated and irradiated compressive yield stresses of the MA 957 micro-pillars were in good agreement with bulk yield stress values reported in the literature, suggesting that the lift-out micro-pillar compression testing technique is a promising method. The demonstration of these techniques on ion beam and neutron irradiated ODS steels and ion beam RAF/M steels gives information to inform models of the material degradation during use in a fusion device.

alloys↗

Probing elemental diffusion and radiation tolerance of perovskite solar cells via non-destructive Rutherford backscattering spectrometry

Mixed organic–inorganic halide perovskite-based solar cells have attracted interest in recent years due to their potential for both terrestrial and space applications. Analysis of interfaces is critical to predicting device behavior and optimizing device architectures. Most advanced tools to study buried interfaces are destructive in nature and can induce further degradation. Ion beam techniques, such as Rutherford backscattering spectrometry (RBS), is a useful non-destructive method to probe an elemental depth profile of multilayered perovskite solar cells (PSCs) as well as to study the inter-diffusion of various elemental species across interfaces. Additionally, PSCs are becoming viable candidates for space photovoltaic applications, and it is critical to investigate their radiation-induced degradation. RBS can be simultaneously utilized to analyze the radiation effects induced by He+ beam on the device, given their presence in space orbits. In the present work, a 2 MeV He+ beam was used to probe the evidence of elemental diffusion across PSC interfaces with architecture glass/ITO/SnO2/Cs0.05(MA0.17FA0.83)0.95Pb(I0.83Br0.17)3/spiro-OMeTAD/MoO3/Au. During the analysis, the device active area was exposed to an irradiation equivalent of up to 1.62 × 1015 He+/cm2, and yet, no measurable evidence (with a depth resolution ∼1 nm) of beam-induced ion migration was observed, implying high radiation tolerance of PSCs. On the other hand, aged PSCs exhibited indications of the movement of diverse elemental species, such as Au, Pb, In, Sn, Br, and I, in the active area of the device, which was quantified with the help of RBS.

14 SOLAR ENERGY↗

A high-temperature Rutherford Backscattering Spectrometry apparatus for in situ material characterization

A new methodology for high-temperature Rutherford Backscattering Spectrometry (HT-RBS) has been developed to enable in situ material characterization at elevated temperatures. A 3.5 MeV proton beam penetrates a 10-µm-thick 316L stainless steel foil mounted on a graphite substrate, with backscattered signals detected using an HT-RBS system. Conventional semiconductor detectors, primarily based on silicon, suffer significant performance degradation at temperatures higher than ~ 60 °C due to increased leakage current and noise, leading to signal distortion and failure. Here, to preserve spectral quality, a 5 µm aluminum foil shields the detector from thermal radiation, allowing reliable operation up to 900 °C at the target. A rotatable shutter provides additional thermal isolation during data collection pauses. In situ measurements of areal density changes of 316L stainless steel were conducted to validate the technique, revealing consistency with the known thermal expansion coefficient. The method facilitates seamless switching between irradiation and analysis, enabling continuous studies. This approach supports in situ investigations of diffusion, void swelling, creep, and corrosion, offering a versatile tool for advanced materials research.

36 MATERIALS SCIENCE↗

Characterization of the microstructure of yttrium hydride under proton irradiation

High moderation per unit volume solid moderator materials like yttrium hydride (YH x ) are necessary for compact nuclear microreactors. However, the phase stability and hydrogen transport processes of YH x under high-temperature irradiation are largely unknown. Proton irradiation was conducted on YH x at 300 °C and 580 °C to 0.2 dpa using 1 MeV or 2 MeV protons in a high-vacuum environment. The hydrogen concentration was determined before and after irradiation using elastic recoil detection analysis, and microstructural evolution was examined via post-irradiation scanning transmission electron microscopy and Raman spectroscopy. Dislocation loops and cavities were observed in all conditions; their distribution was correlated with the bombarding proton energy and ion irradiation temperature. This work revealed that hydrogen retention is proportional to the formation of traps for hydrogen gas atoms and identified pathways for hydrogen release. The relative contributions of bulk or fast diffusion paths, such as grain boundaries, delamination boundaries, and stacking faults are discussed; the primary mechanisms of hydrogen loss are likely based on diffusion, ruling out artefacts of the experimental design. In conclusion, the study suggests proton irradiation may be a strong surrogate to study hydrogen transport in hydride moderator materials under irradiation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗