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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

High–Yield Deterministic Focused Ion Beam Implantation of Quantum Defects Enabled by In Situ Photoluminescence Feedback

Focused ion beam implantation is ideally suited for placing defect centers in wide bandgap semiconductors with nanometer spatial resolution. However, the fact that only a few percent of implanted defects can be activated to become efficient single photon emitters prevents this powerful capability to reach its full potential in photonic/electronic integration of quantum defects. Here an industry adaptive scalable technique is demonstrated to deterministically create single defects in commercial grade silicon carbide by performing repeated low ion number implantation and in situ photoluminescence evaluation after each round of implantation. An array of 9 single defects in 13 targeted locations is successfully created—a ≈70% yield which is more than an order of magnitude higher than achieved in a typical single pass ion implantation. The remaining emitters exhibit non-classical photon emission statistics corresponding to the existence of at most two emitters. This approach can be further integrated with other advanced techniques such as in situ annealing and cryogenic operations to extend to other material platforms for various quantum information technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Direct Synthesis of Layer-Tunable and Transfer-Free Graphene on Device-Compatible Substrates Using Ion Implantation Toward Versatile Applications

Direct synthesis of layer-tunable and transfer-free graphene on technologically important substrates is highly valued for various electronics and device applications. State of the art in the field is currently a two-step process: a high-quality graphene layer synthesis on metal substrate through chemical vapor deposition (CVD) followed by delicate layer transfer onto device-relevant substrates. Here, we report a novel synthesis approach combining ion implantation for a precise graphene layer control and dual-metal smart Janus substrate for a diffusion-limiting graphene formation to directly synthesize large area, high quality, and layer-tunable graphene films on arbitrary substrates without the post-synthesis layer transfer process. Carbon (C) ion implantation was performed on Cu–Ni film deposited on a variety of device-relevant substrates. A well-controlled number of layers of graphene, primarily monolayer and bilayer, is precisely controlled by the equivalent fluence of the implanted C-atoms (1 monolayer ~4 × 10 15 C-atoms/cm 2 ). Upon thermal annealing to promote Cu-Ni alloying, the pre-implanted C-atoms in the Ni layer are pushed toward the Ni/substrate interface by the top Cu layer due to the poor C-solubility in Cu. As a result, the expelled C-atoms precipitate into a graphene structure at the interface facilitated by the Cu-like alloy catalysis. After removing the alloyed Cu-like surface layer, the layer-tunable graphene on the desired substrate is directly realized. The layer-selectivity, high quality, and uniformity of the graphene films are not only confirmed with detailed characterizations using a suite of surface analysis techniques but more importantly are successfully demonstrated by the excellent properties and performance of several devices directly fabricated from these graphene films. Molecular dynamics (MD) simulations using the reactive force field (ReaxFF) were performed to elucidate the graphene formation mechanisms in this novel synthesis approach. With the wide use of ion implantation technology in the microelectronics industry, this novel graphene synthesis approach with precise layer-tunability and transfer-free processing has the promise to advance efficient graphene-device manufacturing and expedite their versatile applications in many fields.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Imaging and speciation of intracellular metallic implant debris using synchrotron-based X-ray fluorescence micro-spectroscopy: a study of two cases

Debris generated from total hip arthroplasty (THA) components made from metal alloys can cause, in some cases, inflammatory cell (e.g., macrophages) responses that lead to adverse local tissue reactions (ALTR) and implant failure. The lack of information on intracellular chemical alterations of metal debris has hindered the understanding of the pathogenesis of ALTR. The goal of this study was to characterize intracellular debris within macrophages using Synchrotron imaging and spectroscopy. We studied periprosthetic tissues of two retrieved THAs with (1) a metal-on-metal (MoM) articulation and (2) a metal-on-polyethylene (MoP) articulation exhibiting corrosion of the metal femoral head. The MoM-THA exhibited different valence states of chromium- and cobalt-containing debris, suggesting three different moieties: Cr 2 O 3 , CrPO 4 , and an alloy-oxide mixture. The findings further suggest that Cr 2 O 3 formed in the tribological interfaces of the implant, while CrPO 4 is a by-product of the phagocytosis process of cobalt alloy-containing debris. Titanium debris appeared to occur in a mixed crystalline/amorphous oxide state. It remains unclear if this chemical state results from the tribochemical processes at the implant surface or intracellular alterations. The MoP-THA specimen exhibited no intracellular particulate debris associated with macrohpages, indicating that the ALTR may be entirely triggered by metal ionic species in this case. A better understanding of in vivo chemical alteration of implant debris will aid in assessing the risk for ALTR during implant design and material choice. However, various techniques are needed to accurately determine the interaction between metal particles and the inta- and extra-cellular environment.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2020

Efficacy of dalbavancin against MRSA biofilms in a rat model of orthopaedic implant-associated infection

Abstract Objectives The aim of this study was to evaluate the efficacy of dalbavancin against MRSA biofilm-related infection in orthopaedic implants in vivo. Methods One MRSA strain isolated from human osteomyelitis was used to promote biofilm formation on the surface of screws. The implants were inserted in the proximal tibia under general anaesthesia. Thirty-nine Wistar rats were divided into three groups [control group (no treatment), Group 1 (7 days of treatment) and Group 2 (14 days of treatment)]; both treatment groups were administered dalbavancin intraperitoneally and euthanized after treatment. cfu of bacteria present in both the tibia and the implant were quantified. The infection severity was assessed by histopathology and scored from 0 (no infection) to 4 (severe infection). Results The high number of cfu/g and cfu/mL present in the control group indicated a well-established infection. There was a significant reduction in cfu in rats treated with dalbavancin both in the tibia (2.8 × 105 cfu/g) and the implant (1.1 × 106 cfu/mL) in Group 1 (1.8 × 103 cfu/g and 2.4 × 105 cfu/mL, respectively) and in Group 2 (8.2 cfu/g and 8.2 × 103 cfu/mL, respectively). Most animals from the control group presented an infection scored as 3 (severe). At the end of the experiment, most rats from Groups 1 and 2 presented an infection scored as 2 (moderate) and 0 (no infection), respectively. Conclusions Although there was a marked decrease in cfu number, signs of biofilm-induced infection prevailed after 14 days of treatment. Further studies should be carried out to evaluate the potential of dalbavancin in the treatment of bone and orthopaedic implant-associated MRSA infections.

Silva, Vanessa↗
DOE OSTI2023

Correlated characterization of 20 Ne-implanted targets using nuclear reaction analysis, Rutherford backscattering spectrometry, and ion transport modeling

In this article, we present the preparation and characterization of a large sample of implanted noble gas targets for use in precision nuclear astrophysics measurements with intense proton beams. Tantalum and titanium backings were prepared using wet-acid etching, outgassed via resistive heating, and implanted with 20 Ne + beams from differing ion sources. These experimental targets were investigated using both nuclear reaction analysis techniques on the 1169-keV resonance in 20 Ne(p, $\gamma$) 21 Na and Rutherford backscattering spectrometry analysis with 2-MeV α-particle beams. Results from these analyses reveal small target-to-target variations in stoichiometry, while exhibiting excellent agreement independent of ion-beam analysis method. We also present a self-consistent validation of the nuclear reaction analysis results using ion transport simulations in TRIM-2013 that rely on input parameters from SIMNRA scattering-yield fits to Rutherford backscattering spectra. In addition to a complete description of the implantation profile, this analysis method provides an alternate solution for characterizing a large sample of implanted targets when no suitable resonances are available for nuclear reaction analysis.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

A methodology for customizing implantation profiles of light ions using a single thin foil energy degrader

We report a method was developed to quantify the spatial distribution and implantation depth of energy-degraded light ions with a thin foil rotating energy degrader for use during multiple ion beam irradiation. The methodology covers three physical phenomena: ions passing through the thin foil, ions travelling through the vacuum to the target, and ion implantation into the target, and accounts for the distribution of ions both in depth and in plane. The processes of energy straggling and scattering were calculated using SRIM. The effects of raster-scanning, and the geometry of the system were implemented in scripts handling the SRIM output files. Elastic backscattering (EBS) using 2.38 MeV H+ protons was used to measure the helium depth profiles after implantation with and without thin foil energy degradation. Defect analysis with transmission electron microscopy confirmed the implantation profiles measured with EBS and calculated with SRIM.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Silicon implantation and annealing in β -Ga 2 O 3 : Role of ambient, temperature, and time

Optimizing thermal anneals of Si-implanted β-Ga 2 O 3 is critical for low resistance contacts and selective area doping. Here we report the impact of annealing ambient, temperature, and time on the activation of room temperature ion-implanted Si in β-Ga 2 O 3 at concentrations from 5 × 10 18 to 1 × 10 20 cm −3 , demonstrating full activation (>80% activation, mobilities >70 cm 2 /V s) with contact resistances below 0.29 Ω mm. Homoepitaxial β-Ga 2 O 3 films, grown by plasma-assisted molecular beam epitaxy on Fe-doped (010) substrates, were implanted at multiple energies to yield 100 nm box profiles of 5 × 10 18 , 5 × 10 19, and 1 × 10 20 cm −3 . Anneals were performed in an ultra-high vacuum-compatible quartz furnace at 1 bar with well-controlled gas compositions. To maintain β-Ga 2 O 3 stability, p O2 must be greater than 10 −9 bar. Anneals up to p O2 = 1 bar achieve full activation at 5 × 10 18 cm −3, while 5 × 10 19 cm −3 must be annealed with p O2 ≤ 10 −4 bar, and 1 × 10 20 cm −3 requires p O2 < 10 −6 bar. Water vapor prevents activation and must be maintained below 10 −8 bar. Activation is achieved for anneal temperatures as low as 850 °C with mobility increasing with anneal temperatures up to 1050 °C, though Si diffusion has been reported above 950 °C. At 950 °C, activation is maximized between 5 and 20 min with longer times resulting in decreased carrier activation (over-annealing). This over-annealing is significant for concentrations above 5 × 10 19 cm −3 and occurs rapidly at 1 × 10 20 cm −3 . Rutherford backscattering spectrometry (channeling) suggests that damage recovery is seeded from remnant aligned β-Ga 2 O 3 that remains after implantation; this conclusion is also supported by scanning transmission electron microscopy showing retention of the β-phase with inclusions that resemble the γ-phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2022

Synthesis of Nano-Oxide Precipitates by Implantation of Ti, Y and O Ions in Fe-10%Cr: Towards an Understanding of Precipitation in Oxide Dispersion-Strengthened (ODS) Steels

The properties of oxide dispersion-strengthened steels are highly dependent on the nature and size distribution of their constituting nano-oxide precipitates. A fine control of the processes of synthesis would enable the optimization of pertinent properties for use in various energy systems. This control, however, requires knowledge of the precise mechanisms of nucleation and growth of the nanoprecipitates, which are still a matter of debate. In the present study, nano-oxide precipitates were produced via the implantation of Y, Ti, and O ions in two different sequential orders in an Fe-10%Cr matrix that was subsequently thermally annealed. The results show that the oxides that precipitate are not necessarily favoured thermodynamically, but rather result from complex kinetics aspects related to the interaction between the implanted elements and induced defects. When Y is implanted first, the formation of nanoprecipitates with characteristics similar to those in conventionally produced ODS steels, especially with a core/shell structure, is evidenced. In contrast, when implantation starts with Ti, the precipitation of yttria during subsequent high-temperature annealing is totally suppressed, and corundum Cr 2 O 3 precipitates instead. Moreover, the systematic involvement of {110} matrix planes in orientation relationships with the precipitates, independently of the precipitate nature, suggests matrix restriction effects on the early stages of precipitation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Strain Recovery and Defect Characterization in Mg‐Implanted Homoepitaxial GaN on High‐Quality GaN Substrates

The evolution of defects due to high‐pressure annealing of magnesium ion‐implanted epitaxial GaN grown on high‐quality GaN substrates is investigated. Changes in the implant‐induced strain are quantified as a function of annealing temperature and time. After annealing at 1300 °C for 10 min, the implant‐induced strain is fully relieved and accompanied by the presence of extended defects such as basal plane stacking faults and prismatic loops. Approximately one‐third of the original implant‐induced strain remains after annealing at 700 °C, and 5% of the original strain remains at 1000 °C for 100 min. In all cases, nearly all of the recovered strain occurs within first few minutes of annealing. A prominent increase in the asymmetric (104) triple axis X‐ray rocking curve full width at 0.01 maximum (FW0.01M) is observed after annealing at 1300 °C for 10 min. After annealing at 1300 °C for 100 min, a subsequent decrease in FW0.01M is correlated with a reduction of the extended defect density from 4 × 10 8 to 3 × 10 7 cm −2 , determined through transmission electron microscope (TEM) measurements. Further reduction in the density of the extended defects by optimizing annealing temperature and time is expected to improve the performance of GaN‐based vertical power devices.

Wang, Yekan↗
DOE OSTI2021

Arrays of Si vacancies in 4 H -SiC produced by focused Li ion beam implantation

Point defects in SiC are an attractive platform for quantum information and sensing applications because they provide relatively long spin coherence times, optical spin initialization, and spin-dependent fluorescence readout in a fabrication-friendly semiconductor. The ability to precisely place these defects at the optimal location in a host material with nano-scale accuracy is desirable for integration of these quantum systems with traditional electronic and photonic structures. Here, we demonstrate the precise spatial patterning of arrays of silicon vacancy (${V}_{Si}$) emitters in an epitaxial 4H -SiC (0001) layer through mask-less focused ion beam implantation of Li + . We characterize these arrays with high-resolution scanning confocal fluorescence microscopy on the Si-face, observing sharp emission lines primarily coming from the ${V1}^{{\prime}}$ zero-phonon line (ZPL). The implantation dose is varied over 3 orders of magnitude, leading to ${V}_{Si}$ densities from a few per implantation spot to thousands per spot, with a linear dependence between ZPL emission and implantation dose. Optically-detected magnetic resonance (ODMR) is also performed, confirming the presence of V2 ${V}_{Si}$. Our investigation reveals scalable and reproducible defect generation.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Domain state exchange bias in a single layer FeRh thin film formed via low energy ion implantation

Modern spintronics relies heavily on the exchange bias effect to pin the orientation of ferromagnetic layers in magnetic tunnel junctions. The current implementations of exchange bias in magnetic tunnel junctions employ pristine interfaces between antiferromagnetic and ferromagnetic layers. Here we reveal an interfacial exchange bias introduced by a single-step, low-energy ion implantation process in a single layer FeRh thin film. Both 1 keV He + ions and 5 keV Fe + were investigated, their energy selected to ensure the ions would stop within the FeRh film. The ions reduce the metamagnetic transition temperature through defect generation to form a surface layer with ferromagnetic ordering. Temperature dependent magnetism measurements reveal a room temperature exchange bias between the ferromagnetic surface and the antiferromagnetic bulk of ~41 Oe in 5 keV Fe + implanted samples and ~36 Oe for 1 keV He + implanted samples. We directly scrutinize this exchange bias effect in magnetic depth profiles obtained by polarized neutron reflectometry which clearly show a pinned ferromagnetic layer adjacent to the disordered layer created by low energy Fe + ion implantation. These results reveal a novel method to implement exchange bias in an antiferromagnetic layer that can have direct application in the field of spintronics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Effect of thermal oxidation on helium implanted 316L stainless steel

The effect of thermal oxide layer on He implanted 316L stainless steel was studied to evaluate experimentally how thermal oxidation affects the diffusion and distribution of He in the material. In the case of thermal oxidation of a He implanted sample, with an increase in oxidation time, the max swelling height increases logarithmically as a function of time and finally saturates for all samples except for the lowest dose of implanted He. Concerning TEM results, two void regions are identified. Similar to the calculation, the total irradiated depth was around 250 nm and the large void region was formed around 100–150 nm depth. On the other hand, the small void region was observed immediately under oxide layer from the thermal oxidation. In contrast, there were no voids in the altered zone near the metal/oxide interface in the non-thermal oxidized/He implanted sample. This description of the phenomena was justified using the Kirkendall effect and the Point Defect Model.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Dissolution of Mg-enriched defects in implanted GaN and increased p-type dopant activation

Annealing Mg-implanted homoepitaxial GaN at temperatures above 1400 °C eliminates the formation of inversion domains and leads to improved dopant activation efficiency. Extended defects, in the form of inversion domains, contain electrically inactive Mg after post-implantation annealing at temperatures as high as 1300 °C (one GPa N 2 overpressure), which results in a low dopant activation efficiency. Triple-axis x-ray data reveal that implant-induced strain is fully relieved after annealing at 1300 °C for 10 min, indicating that strain-inducing point defects formed during implantation have reconfigured and inversion domains are formed. However, annealing at temperatures of 1400–1500 °C (one GPa N 2 overpressure) eliminates the presence of the inversion domains. While residual defects, such as dislocation loops, still exist after annealing at and above 1400 °C, chemical analysis at multiple dislocation loops shows no sign of Mg segregation. Meanwhile, an overall decreasing trend in the dislocation loop density is observed after annealing at the higher temperatures and longer times. Additionally, once inversion domains are formed and the samples are cooled to room temperature, they are shown to dissolve with subsequent annealing above 1400 °C. While such defects have been observed before, the important finding that such defects can be dissolved with a short, higher temperature step is key. Earlier work [Breckenridge et al., J. Appl. Phys. Lett. 118, 022101 (2021)] addressing electrical measurements of these types of samples showed that annealing at 1400 °C leads to a dopant activation efficiency that is an order of magnitude higher than that observed at 1300 °C. In conclusion, this work complements earlier work by identifying the inversion domains, which incorporate Mg, and points to the benefits, in terms of defect density and p-type dopant activation, of using higher temperature (>1400 °C) annealing cycles to activate Mg in GaN, even if the Mg-containing inversion domains had been formed during lower temperature annealing.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Overcoming the doping limit in GaAs by ion implantation and pulsed laser melting

Most semiconductors exhibit a saturation of free carriers when heavily doped with extrinsic dopants. This carrier saturation or “doping limit” is known to be related to the formation of native compensating defects, which, in turn, depends on the energy positions of their conduction band minimum and valence band maximum. Here, we carried out a systematic study on the n-type doping limit of GaAs via ion implantation and showed that this doping limitation can be alleviated by the transient process of pulsed laser melting (PLM). For n-type doping, both group VI (S) and amphoteric group IV (Si and Ge) dopants were implanted in GaAs. For comparison, p-type doping was also studied using Zn as the acceptor. Implanted dopants were activated by the PLM method, and the results are compared to rapid thermal annealing (RTA). Our results reveal that for all n-type dopants, while implantation followed by the RTA results in a similar saturation electron concentration of 2–3 × 10 18 cm –3 , the transient PLM process is capable of trapping high concentration of dopants in the substitutional site, giving rise to a carrier concentration of >10 19 cm –3 , exceeding the doping limit of GaAs. However, due to scatterings from point defects generated during PLM, the mobility of n-type GaAs after PLM is low (~80–260 cm 2 /V s). Subsequent RTA after PLM (PLM + RTA) is able to remove these point defects and recover the mobility to ~1000–2000 cm2/V s. The carrier concentrations of these PLM + RTA samples are reduced but are still a factor of 3 higher than RTA only GaAs. This can be understood as the dopants are already incorporated in the substitutional site after PLM; they are less likely to be “deactivated” by subsequent RTA. This work is significant to the understanding of doping mechanisms in semiconductors and provides a means for device applications, which require materials with ultra-high doping.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2025

Field-dependent carrier transport in implanted isolation region of GaN lateral power devices

Among GaN lateral power devices, with proper E-field management, the breakdown occurs in the device isolation region rather than the active region. In this paper, we investigate field-dependent carrier transport in the isolation structures. Isolation test structures with variations in buffer doping, un-intentionally doped (UID) GaN thickness, and implantation conditions were fabricated. Electrical characterization was performed over a wide range of voltage and temperature. With varying UID GaN thickness and buffer doping, the leakage current and breakdown characteristics remain the same for a specific implantation condition, indicating that the leakage conduction and breakdown are governed by the implanted GaN region. Analysis of the temperature-dependent I–V reveals that carrier transport in the implanted GaN can be well explained by hopping conduction, involving three distinctive regions of operation depending on the E-field. At low E-field, carrier transport is ohmic, consistent with variable range hopping, driven by thermal activation. At medium E-field, a field enhanced thermally activated hopping is observed, following σ ∼ σ(T)exp(E). At high E-field, activation-less hopping is visible, following σ ∼ exp(−1/E), which occurs above a critical E-field limited by localization length.

Sadek, Mansura (ORCID:0000000322588338)↗
DOE OSTI2020

Implanted satellite transmitters affect sea duck movement patterns at short and long timescales

Abstract Studies of the effects of transmitters on wildlife often focus on survival. However, sublethal behavioral changes resulting from radio-marking have the potential to affect inferences from telemetry data and may vary based on individual and environmental characteristics. We used a long-term, multi-species tracking study of sea ducks to assess behavioral patterns at multiple temporal scales following implantation of intracoelomic satellite transmitters. We applied state-space models to assess short-term behavioral patterns in 476 individuals with implanted satellite transmitters, as well as comparing breeding site attendance and migratory phenology across multiple years after capture. In the short term, our results suggest an increase in dispersive behavior immediately following capture and transmitter implantation; however, behavior returned to seasonally average patterns within ~5 days after release. Over multiple years, we found that breeding site attendance by both males and females was depressed during the first breeding season after radio-marking relative to subsequent years, with larger relative decreases in breeding site attendance among males than females. We also found that spring and breeding migrations occurred later in the first year after radio-marking than in subsequent years. Across all behavioral effects, the severity of behavioral change often varied by species, sex, age, and capture season. We conclude that, although individuals appear to adjust relatively quickly (i.e. within 1 week) to implanted satellite transmitters, changes in breeding phenology may occur over the longer term and should be considered when analyzing and reporting telemetry data.

Lamb, Juliet S.↗
DOE OSTI2022

Noninvasive Detection, Tracking, and Characterization of Aerogel Implants Using Diagnostic Ultrasound

Medical implants are routinely tracked and monitored using different techniques, such as MRI, X-ray, and ultrasound. Due to the need for ionizing radiation, the two former methods pose a significant risk to tissue. Ultrasound imaging, however, is non-invasive and presents no known risk to human tissue. Aerogels are an emerging material with great potential in biomedical implants. While qualitative observation of ultrasound images by experts can already provide a lot of information about the implants and the surrounding structures, this paper describes the development and study of two simple B-Mode image analysis techniques based on attenuation measurements and echogenicity comparisons, which can further enhance the study of the biological tissues and implants, especially of different types of biocompatible aerogels.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Wireless power transfer to biomedical implants

Various examples are provided for wireless power transfer to implants. In one example, a system includes a radio frequency (RF) power source and a transmitter (TX) array comprising an excitation coil and resonant coils distributed about the excitation coil. The TX array can transfer power from the RF power source to a biomedical implant inserted below a skin surface of a subject when the TX array is positioned on the skin surface adjacent to the biomedical implant. A receiver (RX) coil of the biomedical implant can inductively couple with the TX array for the power. The resonant coils can allow power transfer when the RX coil is not aligned with the excitation coil.

Lin, Jenshan↗