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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Helium Ion Microscopy

Nanotechnology research led to the development of various instruments to be used for imaging or fabrication. The helium ion microscope (HIM) became available in 2006 but quickly gained popularity. Its unique gas field ion source enables high-resolution imaging, nanofabrication, direct write, and the recent combination with a secondary ion mass spectrometer offers chemical imaging with ~15 nm resolution. Particularly attractive are the small interaction volume of He and Ne (the two gases offered), small beam spot size, and a moderate sputtering rate. Additionally, the HIM is an excellent imaging tool for insulating samples in soft, polymeric, and biological materials. It can be expected that helium ion microscopy will continue to have a strong influence on broad range of scientific disciplines, including chemistry, materials science, and biology.This chapter aims at providing an overview of the current status of HIM for imaging, analysis, and nanofabrication. It introduces the reader to key components of the instrument, theoretical background, and latest results in the areas of imaging, material fabrication, and chemical analysis capabilities of helium ion microscopy.

Belianinov, Alex↗
DOE OSTI2022

Multi-scale imaging of high-pressure hydrogen induced damage in EPDM rubber using X-ray microcomputed tomography, helium-ion microscopy and transmission electron microscopy

Ethylene propylene diene (EPDM) rubber has gained increasing interest for use in hydrogen infrastructure due to its excellent sealing performance and low temperature properties. However, severe structural damage has been observed in EPDM O-rings after exposure to high-pressure hydrogen. The origination and propagation mechanisms of this damage are poorly understood. Here, to address this knowledge gap, multi-scale imaging leveraging X-ray micro-computed tomography (micro-CT), helium ion microscopy (HeIM), and transmission electron microscopy (TEM) were used in this work to study a series of sulfur-cured ethylene propylene diene (EPDM) rubber materials with varying additives that were exposed to different hydrogen environments. Micro-CT captured the substantial structural damage due to hydrogen exposure; it revealed an association between zinc oxide (ZnO) particles and damage initiation. Further studies by TEM and scanning TEM with energy dispersive X-ray spectroscopy (EDS) were focused on these particles at the micro-to nano-scale range. TEM indicated that hydrogen causes void formation at the interface between ZnO and the rubber matrix. HeIM enabled imaging of surface morphology of the material at high resolution pre- and post-hydrogen exposure while providing information on chemical composition and that cannot be captured by either micro-CT or TEM.

08 HYDROGEN↗
DOE OSTI2021

Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ~14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Altogether, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

High-efficiency single-junction p-i-n GaAs solar cell on roll-to-roll epi-ready flexible metal foils for low-cost photovoltaics

We demonstrate the fabrication and characterization of high-efficiency, single-junction p-i-n GaAs solar cells, on flexible metal foil with epi-ready buffer via roll-to-roll fabrication. Single-junction p-i-n GaAs solar cells were fabricated using metal–organic chemical vapor deposition (MOCVD). Furthermore, an efficiency greater than 13% was obtained at 1 sun, which is the highest reported efficiency on GaAs photovoltaics directly deposited on metal tapes. This exceeds our previously reported study showcasing 11.5% efficiency on single-junction p-n solar cell structure. Improved morphology of p-i-n structure compared with p-n is explained by atomic force microscopy (AFM), scanning electron microscopy (SEM), and helium ion microscopy (HIM) measurements. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis showed reduced Zn diffusion in p-i-n cell compared with the p-n cell. We attribute the improvement in efficiency of p-i-n cells on flexible metal tapes to the quality of the junction, surface morphology, controlled diffusion of species within the active layers, and increase in absorption due to the optimized intrinsic layer thickness.

14 SOLAR ENERGY↗
DOE OSTI2020

Quantitative investigation of surface structure and interatomic potential with impact-collision ion scattering spectroscopy

Helium ion beam interactions with materials have important implications for magnetic confinement fusion, material modification, and helium ion microscopy. These interactions depend on the precise physics of how helium ions channel into the materials, which can vary greatly based on the local crystalline orientation. Here, we performed a dedicated experiment to investigate helium ion channeling in a well-characterized tungsten single crystal. Time-of-flight impact-collision ion scattering spectroscopy was used to obtain multi-angle maps of the backscattering intensity for 3 keV He + → W(111). We found that the backscattering intensity profile arising from helium ion channeling could be well described by a shadow cone analysis. This analysis revealed that subsurface W atoms as deep as the ninth monolayer contributed to the backscattering intensity profile. Binary collision approximation simulations were performed with MARLOWE to model the experimental maps with sufficient accuracy to allow for quantitative comparisons using reliability factors. These quantitative comparisons were applied to investigate how the W lattice structure and He–W interatomic potential affect the multi-angle maps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Direct Write of 3D Nanoscale Mesh Objects with Platinum Precursor via Focused Helium Ion Beam Induced Deposition

The next generation optical, electronic, biological, and sensing devices as well as platforms will inevitably extend their architecture into the 3rd dimension to enhance functionality. In focused ion beam induced deposition (FIBID), a helium gas field ion source can be used with an organometallic precursor gas to fabricate nanoscale structures in 3D with high-precision and smaller critical dimensions than focused electron beam induced deposition (FEBID), traditional liquid metal source FIBID, or other additive manufacturing technology. In this work, we report the effect of beam current, dwell time, and pixel pitch on the resultant segment and angle growth for nanoscale 3D mesh objects. We note subtle beam heating effects, which impact the segment angle and the feature size. Additionally, we investigate the competition of material deposition and sputtering during the 3D FIBID process, with helium ion microscopy experiments and Monte Carlo simulations. Our results show complex 3D mesh structures measuring ~300 nm in the largest dimension, with individual features as small as 16 nm at full width half maximum (FWHM). These assemblies can be completed in minutes, with the underlying fabrication technology compatible with existing lithographic techniques, suggesting a higher-throughput pathway to integrating FIBID with established nanofabrication techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Deciphering the influence of high-flux helium plasma exposure on tungsten nanostructure growth using real-time, in situ spectroscopic ellipsometry

In situ analysis of surfaces during high-flux plasma exposure represents a long-standing challenge in the study of plasma–material interactions. While post-mortem microscopy can provide a detailed picture of structural and compositional changes, in situ techniques can capture the dynamic evolution of the surface. In this study, we demonstrate how spectroscopic ellipsometry can be applied to the real-time characterization of W nanostructure (also known as “fuzz”) growth during exposure to low temperature, high-flux He plasmas. Strikingly, over a wide range of sample temperatures and helium fluences, the measured ellipsometric parameters (Ψ,Δ) collapse onto a single curve that can be directly correlated with surface morphologies characterized by ex situ helium ion microscopy. The initial variation in the (Ψ,Δ) parameters appears to be governed by small changes in surface roughness (<50 nm) produced by helium bubble nucleation and growth, followed by the emergence of 50 nm diameter W tendrils. This basic behavior appears to be reproducible over a wide parameter space, indicating that the spectroscopic ellipsometry may be of general practical use as a diagnostic to study surface morphologies produced by high-flux He implantation in refractory metals. An advantage of the methods outlined here is that they are applicable at low incident ion energies, even below the sputtering threshold. As an example of this application, we apply in situ ellipsometry to examine how W fuzz growth is affected both by varying ion energy and the temperature of the surface.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2020

In-situ spectroscopic ellipsometry for real-time characterization of the effects of high-flux helium plasmas on tungsten surfaces

Tungsten samples were exposed to He plasmas generated by an RF source (Γ i = 3.5 x 10 16 He cm -2 s -1 , ion energy = 92 eV.) The range of exposure conditions selected here is conducive to the growth of nearsurface He bubbles, and at higher fluence, the formation of W nanotendrils ranging between 50 — 100 nm in diameter. The evolution of these surface features was probed using a fixed-angle ellipsometer (280 — 1000 nm wavelength range) with direct line-of-sight to the sample. Over the parameter space explored here, changes in the two angles (p, S) that define the polarization of the reflected light followed a distinct trajectory with increasing plasma fluence. Ex-situ ellipsometry of 22 additional tungsten specimens tested at a wide range of plasma fluences and temperatures mapped onto these in-situ results well. We used helium ion microscopy and focused ion beam profiling to provide a direct calibration of the ellipsometry measurements. Our results indicate that for a reproducible process such as the growth helium-induced surface morphologies, ellipsometry is a practical in-situ diagnostic to study how fusion plasmas modify materials. To study more general effects of plasmas on surfaces, including co-deposition and sputtering, different approaches to modelling the optical properties of the exposed surfaces are also considered.

36 MATERIALS SCIENCE↗
DOE OSTI2020

The superior hydrothermal stability of Pd/SSZ-39 in low temperature passive NOx adsorption (PNA) and methane combustion

We successfully synthesized uniform SSZ-39 with an average crystal size of about a micron. Pd (0.7 - 3 wt%) was supported on SSZ-39 with Si/Al ratio ~12. The as-synthesized materials were characterized by FTIR, XRD, Helium Ion Microscopy, HAADF-STEM imaging, 27 Al, 29 Si and H solid state NMR spectroscopic techniques. FTIR studies with CO and NO probe molecules reveal that the 0.7 wt% Pd/SSZ-39 material with Si/Al ~12 has the majority of Pd dispersed atomically as isolated Pd(II) and Pd(II)-OH centers, and thus can be used as a low-temperature passive NOx adsorber. Pd(II)-NO, Pd(II)(OH)(NO) and Pd(II)(CO)(NO) complexes form during PNA in this material. We compare this PNA material directly with the Pd/SSZ-13 system (with Si/Al ratio ~12) and show its superior hydrothermal stability. Remarkably, Pd/SSZ-39 with Si/Al ratio ~12 survives hydrothermal aging up to 815 ºC in 10% H 2 O/Air vapor for 16 hours without significant loss in activity. The SSZ-39 crystal structure remains intact during hydrothermal aging up to 1,000 ºC as we elucidate it with XRD and HAADF-STEM imaging/EDS mapping. However, changes to the framework during such harsh hydrothermal treatment significantly change the NOx release profiles during PNA as evidenced by high-field 27 Al NMR on fresh and aged Pd/SSZ-39 samples as well as PNA performance measurements. Besides PNA application, these hydrothermally very stable materials (3 wt% Pd on SSZ-39 with Si/Al ratio ~12) can be used as a robust methane combustion catalyst under industrially relevant conditions (GHSV~600,000hr -1 ). This catalyst shows minimal deactivation after both harsh hydrothermal aging at 750 and 800 ºC, and prolonged time on stream (105 hrs) at 425 °C. In contrast, both 3wt% Pd/alumina and 3wt% SSZ-13 supported samples lose a significant portion of their activity. Our study opens new avenues to prepare the most hydrothermally stable known Pd/zeolite materials with applications for adsorption and catalytic hydrocarbon combustion under industrially relevant conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

H-Mat Hydrogen Compatibility of Polymers and Elastomers

The H2@Scale program of the U.S. Department of Energy (DOE) Fuel Cell Technologies Office is supporting work on the hydrogen compatibility of polymers to improve the durability and reliability of materials for hydrogen infrastructure. The hydrogen compatibility program (H-Mat) seeks “to address the challenges of hydrogen degradation by elucidating the mechanisms of hydrogen-materials interactions with the goal of providing science-based strategies to design materials, (micro)structures, and morphology with improved resistance to hydrogen degradation.” This research has observed interactions of hydrogen and pressure with model rubber-material compounds resulting in volume change and compression-set differences in the materials. The materials were investigated using helium-ion microscopy (HeIM), which revealed significant morphological changes in the plasticizer-incorporating compounds after exposure, as evidenced by time-of-flight secondary ion mass spectrometry. Additional studies using transmission electron microscopy and nuclear magnetic resonance were performed to correlate morphological change to potential chemical change in the materials.

08 HYDROGEN↗
DOE OSTI2026

Retention and surface morphology evaluation of fine-grain dispersion-strengthened tungsten for plasma-facing component applications

This study exposed novel fine-grain dispersion-strengthened tungsten (W) to high fluence, low energy deuterium (D) and helium (He) plasmas to evaluate how material microstructure and composition affect hydrogen retention and surface morphology. Tested materials included fine-grain dispersion-strengthened tungsten (DSW) with 3 wt% zirconium carbide (ZrC) dispersoids, fine-grain dense W without any dispersoids (FGW), and coarse-grained polycrystalline ‘ITER-grade’ W. Samples were exposed to D 2 + and He + plasmas at fusion-relevant fluences (∼10 25 m -2 ) and ion energies (75 eV) over a range of temperatures (200 °C, 300 °C, 450 °C for D, 850 °C for He). Helium ion microscopy was performed on the exposed samples to evaluate surface morphology changes and material integrity. After D plasma exposure, the ZrC dispersoids showed near-surface degradation at exposure temperatures above 300 °C, but no detrimental morphology changes were observed for the adjacent W grains. After He plasma-exposure, nano-structured fuzz formation was observed in the tungsten matrix of all samples. The ZrC dispersoids maintained their integrity despite the surrounding fuzz growth, with clear delineation between the W fuzz and dispersoid regions. Thermal desorption spectroscopy showed that ZrC DSW consistently retained more D than the FGW by about a factor of 2 across all temperatures. At 200 °C and 300 °C, the ITER-W displayed lower D retention than both the DSW and FGW, however at 450 °C ITER-W showed the highest retention, about 50% more than DSW. He retention was comparable across all samples, with the highest retention observed in the fine-grain W, only 26% higher than in ITER-W. These insights on retention behavior will inform further optimization of these novel fine-grained tungsten materials with and without dispersoid additives.

Dispersion-strengthened tungsten↗
DOE OSTI2020

Atomistic Positioning of Defects in Helium Ion Treated Single-Layer MoS 2

Structuring materials with atomic precision is the ultimate goal of nanotechnology and is becoming increasingly relevant as an enabling technology for quantum electronics/spintronics and quantum photonics. Here, we create atomic defects in monolayer MoS 2 by helium ion (He-ion) beam lithography with a spatial fidelity approaching the single-atom limit in all three dimensions. Using low-temperature scanning tunneling microscopy (STM), we confirm the formation of individual point defects in MoS 2 upon He-ion bombardment and show that defects are generated within 9 nm of the incident helium ions. Atom-specific sputtering yields are determined by analyzing the type and occurrence of defects observed in high-resolution STM images and compared with Monte Carlo simulations. Both theory and experiment indicate that the He-ion bombardment predominantly generates sulfur vacancies.

Two-dimensional materials↗
DOE OSTI2021

Nanoscale friction of CVD single-layer MoS 2 with controlled defect formation

Two-dimensional (2D) layered nanomaterials such as graphene, molybdenum disulfide (MoS 2 ), or tungsten disulfide offer a promising solution in areas of solid-state lubrication, due to their excellent mechanical properties as well as low friction. However, defects can influence their friction and reduce their superior tribological properties. Thus, it is crucial to understand the effects of defects on sliding behavior in 2D nanomaterials, to foster a functional strategy for utilizing 2D nanomaterials as solid-state tribological films. In this study, frictional effects of defects, grain boundaries, and atomic-scale structural defects were explored on chemical vapor deposition (CVD) grown single layer MoS 2 . Selective patterning of defects into MoS 2 was accomplished via controlled irradiation of helium ions with varying ion doses. The friction of MoS 2 was characterized by friction force microscopy (FFM) and was found that friction depends on the defect formation controlled by helium ion irradiation. This approach offers a correlation between surface topography, defects and friction. Understanding the relative friction of MoS 2 in the presence of different levels of defects is foundational to studying tribological properties of a single layer MoS 2 at both nanoscales and macroscales.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ transmission electron microscopy with dual ion beam irradiation and implantation

To study the helium effects and their interactions with displacement damage in irradiated materials, an in situ dual-ion beam irradiation capability with transmission electron microscopy was recently established at the IVEM-Tandem Facility at Argonne National Laboratory. Pure nickel was irradiated in situ individually with 1 MeV Kr ions for displacement damage study, 16 keV He ions for helium implantation, and simultaneously with 1 MeV Kr ions and 16 keV He ions at the rate of 1 at.% He/dpa to study the interaction of helium and displacement damage at 500 degrees C. Helium bubbles were formed and segregated within dislocation loops during the He implantation experiment and no bubbles were observed outside the loops. The loop size increased with increasing helium concentration. In contrast, helium bubbles were formed uniformly in the matrix when nickel was irradiated simultaneously with 1 MeV Kr ions and 16 keV He ions. Overall, it is suggested that the uniformly-distributed defect clusters formed under 1 MeV Kr ion irradiation serve as trapping sites of helium atoms resulting in homogeneous nucleation of helium bubbles under the dualion beam irradiation in nickel.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Compositional Effects of Additively Manufactured Refractory High-Entropy Alloys under High-Energy Helium Irradiation

High-Entropy Alloys (HEAs) are proposed as materials for a variety of extreme environments, including both fission and fusion radiation applications. To withstand these harsh environments, materials processing must be tailored to their given application, now achieved through additive manufacturing processes. However, radiation application opportunities remain limited due to an incomplete understanding of the effects of irradiation on HEA performance. In this letter, we investigate the response of additively manufactured refractory high-entropy alloys (RHEAs) to helium (He) ion bombardment. Through analytical microscopy studies, we show the interplay between the alloy composition and the He bubble size and density to demonstrate how increasing the compositional complexity can limit the He bubble effects, but care must be taken in selecting the appropriate constituent elements.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The dependence of tungsten fuzz layer thickness and porosity on tungsten deposition rate and helium ion fluence

Abstract Fuzz formation on a heated tungsten surface in the presence of a helium-containing plasma and tungsten deposition source was investigated. Tungsten samples were exposed at 1123 K to pure helium plasma with ion incident energy of 76 eV, W/He ion flux ratio of ∼ 0.4 × 10 − 4 , and varied helium ion fluence from 0.18 to 3.4 × 10 26 m −2 . Fuzz thickness was measured by cross-sectional scanning electron microscopy to increase from 0.22 to 15 µ m with increasing helium ion fluence. No indication of saturation in fuzz thickness at high fluence was observed, in contrast to fuzz produced on a tungsten surface without tungsten deposition. Additional tungsten samples were exposed at 1123 K to pure helium plasma with ion incident energy of 76 eV, helium ion fluence of ∼ 3.4 × 10 26 m −2 , and varied W/He ion flux ratio from 0.26 to 3.0 × 10 − 4 . Fuzz thickness increased from 7.5 to 120 µ m with increasing W/He ion ratio. A final sample exposed at 1123 K to a mixed helium-deuterium plasma with ion incident energy of 76 eV, helium ion fluence of 0.18 × 10 26 m −2 , and W/He ion flux ratio of 2.2 × 10 − 4 developed nearly identical fuzz structures to that developed in a pure He plasma. As a function of deposited tungsten fluence, all results were found to trace out a single layer-growth curve given by a power law relation, indicating that fuzz thickness is independent of the W/He ion flux ratio in the range investigated and independent of any deuterium present in the plasma. As a result, for tungsten plasma facing walls in magnetic fusion devices at 1000–2000 K with 10 −4 W/He ion flux ratio, fuzz with thicknesses greater than hundreds of microns may form in as little as 10 4 s (in the absence of ELM-induced erosion or annealing), and may more significantly affect its thermophysical properties than fuzz generated without a tungsten deposition source.

Physics↗