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At least 1,459 records · Page 81

New Directions in Focused Ion Beam Induced Deposition for the Nanoprinting of Functional 3D Heterostructures

The focused ion beam (FIB) microscope is well established as a high-resolution machining instrument capable of site-selectively removing material down to the nanoscale. Beyond subtractive processing, however, the FIB can also add material via a technique known as focused ion beam induced deposition (FIBID). Using FIBID, the FIB can thus be employed for the direct-write of complex nanostructures. This work explores new directions in three-dimensional FIBID nanoprinting, harnessing unique features of helium and neon FIBs. In particular, the superior spatial resolution of these novel FIBs is leveraged to fabricate precise multimaterial architectures, an isotope effect is used to create satellite deposits, and dose-controlled implantation of the gaseous ions is used to engineer internal voids. In the context of voids, the fabrication of hollow nanopillars by helium-FIBID due to concurrent milling (as shown previously by others) is revisited. Insight into the chemical and structural composition of the nanostructures is obtained using advanced electron microscopy, accurately revealing buried interfaces, crystallite distributions, chemical compositions, and material transformations. Next-generation devices and technologies that could be enabled by the novel heterostructures demonstrated here are discussed, setting the stage for the potential evolution of FIBID into a versatile platform for functional nanomaterials design and fabrication.

FIBID↗

An inductively heated hot cavity catcher laser ion source

An inductively heated hot cavity catcher has been constructed for the production of low-energy ion beams of exotic, neutron-deficient Ag isotopes. A proof-of-principle experiment has been realized by implanting primary {sup 107}Ag{sup 21+} ions from a heavy-ion cyclotron into a graphite catcher. A variable-thickness nickel foil was used to degrade the energy of the primary beam in order to mimic the implantation depth expected from the heavy-ion fusion-evaporation recoils of N = Z {sup 94}Ag. Following implantation, the silver atoms diffused out of the graphite and effused into the catcher cavity and transfer tube, where they were resonantly laser ionized using a three-step excitation and ionization scheme. Following mass separation, the ions were identified by scanning the frequency of the first resonant excitation step while recording the ion count rate. Ion release time profiles were measured for different implantation depths and cavity temperatures with the mean delay time varying from 10 to 600 ms. In addition, the diffusion coefficients for silver in graphite were measured for temperatures of 1470 K, 1630 K, and 1720 K, from which an activation energy of 3.2 ± 0.3 eV could be determined.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Spatially Enhanced Electrostatic Doping in Graphene Realized via Heterointerfacial Precipitated Metals

Forming heavily-doped regions in 2D materials, like graphene, is a steppingstone to the design of emergent devices and heterostructures. Here, a selective-area approach is presented to tune the work-function and carrier density in monolayer graphene by spatially synthesizing sub-monolayer gallium beneath the 2D-solid. The localized metallic gallium is formed via precipitation from an underlying diamond-like carbon (DLC) film that is spatially implanted with gallium-ions. By controlling the interfacial precipitation process with annealing temperature, spatially precise ambipolar tuning of the graphene work-function is achieved, and the tunning effect preserved upon cooling to ambient conditions. Consequently, charge carrier densities from ≈1.8 × 10 10 cm -2 (hole-doped) to ≈7 × 10 13 cm -2 (electron-doped) are realized, confirmed by in situ and ex situ measurements. The theoretical studies corroborated the role of gallium at the heterointerface on charge transfer and electrostatic doping of the graphene overlayer. Specifically, sub-monolayer gallium facilitates heavy n-doping in graphene. Extending this doping strategy to other implantable elements in DLC provides a new means of exploring the physics and chemistry of highly-doped 2D materials.

36 MATERIALS SCIENCE↗

In Situ Electron Microscopy of Helium Bubble Implantation in Metal Hydrides

Here we investigated the microstructural response of various Pd physically vapor deposited films and Er and ErD 2 samples prepared from neutron Tube targets to implanted He via in situ ion irradiation transmission electron microscopy and subsequent in situ annealing experiments. Small bubbles formed in both systems during implantation, but did not grow with increasing fluence or a short duration room temperature aging (weeks). Annealing produced large cavities with different densities in the two systems. The ErD 2 showed increased cavity nucleation compared to Er. The spherical bubbles formed from high fluence implantation and rapid annealing in both Er and ErD 2 cases differed from microstructures of naturally aged tritiated samples. Further work is still underway to determine the transition in bubble shape in the Er samples, as well as the mechanism for evolution in Pd films.

36 MATERIALS SCIENCE↗

Growth and characterization of ferromagnetic Ga 2 O 3 :(Cr, Mn)

The goal of this Exploratory Express project was to explore the possibility of tunable ferromagnetism in Mn or Cr incorporated epitaxial Ga 2 O 3 films. Tunability of magnetic properties can enable novel applications in spintronics, quantum computing, and magnetism-based logics by allowing control of magnetism down to the nanoscale. Carriers (electrons or holes) mediated ferromagnetic ordering in semiconductor can lead to tunable ferromagnetism by leveraging the tunability of carrier density with doping level, gate electric field, or optical pumping of the carriers. The magnetic ions (Cr or Mn) in Ga 2 O 3 act as localized spin centers which can potentially be magnetically coupled through conduction electrons to enable ferromagnetic ordering. Here we investigated tunable ferromagnetism in beta Ga 2 O 3 semiconductor host with various n-doping levels by incorporating 2.4 atomic percent Mn or Cr. The R&D approach involved growth of epitaxial Ga 2 O 3 film on sapphire or Ga 2 O 3 substrate, implantation of Mn or Cr ions, annealing of the samples post implantation, and magnetic measurements. We studied magnetic behavior of Mn:Ga 2 O 3 as a function of different n-doping levels and various annealing temperatures. The vibrating sample magnetometry (VSM) measurement exhibited strong ferromagnetic signals from the annealed Mn:Ga 2 O 3 sample with n-doping level of 5E19 cm -3 . This ferromagnetic behavior disappears from Mn:Ga 2 O 3 when the n-doping level is reduced to 5E16 cm -3 . Although these results are to be further verified by other measurement schemes due to the observation of background ferromagnetism from the growth substrate, these results indicate the possibility of tunable ferromagnetism in Mn:Ga 2 O 3 mediated by conduction electrons.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanoindentation study of the mechanical behavior of TiO{sub 2} nanotube arrays

Titanium dioxide (TiO{sub 2}) nanotube arrays are attracting increasing attention for use in solar cells, lithium-ion batteries, and biomedical implants. To take full advantage of their unique physical properties, such arrays need to maintain adequate mechanical integrity in applications. However, the mechanical performance of TiO{sub 2} nanotube arrays is not well understood. In this work, we investigate the deformation and failure of TiO{sub 2} nanotube arrays using the nanoindentation technique. We found that the load–displacement response of the arrays strongly depends on the indentation depth and indenter shape. Substrate-independent elastic modulus and hardness can be obtained when the indentation depth is less than 2.5% of the array height. The deformation mechanisms of TiO{sub 2} nanotube arrays by Berkovich and conical indenters are closely associated with the densification of TiO{sub 2} nanotubes under compression. A theoretical model for deformation of the arrays under a large-radius conical indenter is also proposed.

36 MATERIALS SCIENCE↗

Activation and thermal stability of ultra-shallow B{sup +}-implants in Ge

The activation and thermal stability of ultra-shallow B{sup +} implants in crystalline (c-Ge) and preamorphized Ge (PA-Ge) following rapid thermal annealing was investigated using micro Hall effect and ion beam analysis techniques. The residual implanted dose of ultra-shallow B{sup +} implants in Ge was characterized using elastic recoil detection and was determined to correlate well with simulations with a dose loss of 23.2%, 21.4%, and 17.6% due to ion backscattering for 2, 4, and 6 keV implants in Ge, respectively. The electrical activation of ultra-shallow B{sup +} implants at 2, 4, and 6 keV to fluences ranging from 5.0 Multiplication-Sign 10{sup 13} to 5.0 Multiplication-Sign 10{sup 15} cm{sup -2} was studied using micro Hall effect measurements after annealing at 400-600 Degree-Sign C for 60 s. For both c-Ge and PA-Ge, a large fraction of the implanted dose is rendered inactive due to the formation of a presumable B-Ge cluster. The B lattice location in samples annealed at 400 Degree-Sign C for 60 s was characterized by channeling analysis with a 650 keV H{sup +} beam by utilizing the {sup 11}B(p, {alpha})2{alpha} nuclear reaction and confirmed the large fraction of off-lattice B for both c-Ge and PA-Ge. Within the investigated annealing range, no significant change in activation was observed. An increase in the fraction of activated dopant was observed with increasing energy which suggests that the surface proximity and the local point defect environment has a strong impact on B activation in Ge. The results suggest the presence of an inactive B-Ge cluster for ultra-shallow implants in both c-Ge and PA-Ge that remains stable upon annealing for temperatures up to 600 Degree-Sign C.

36 MATERIALS SCIENCE↗

Glancing-incidence focussed ion beam milling: A coherent X-ray diffraction study of 3D nano-scale lattice strains and crystal defects

Here, this study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strains have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of Burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Quantifying Low Energy ICP-MS Isotope Deposition

Mass spectrometry (MS) offers an alternative approach to chemical or chromatographic separations to selectively isolate and collect individual isotopes of an element for analytical purposes. During this MS isotopic isolation process, the amount of material deposited on to a target can be conveniently tracked by measuring ion current or accumulated charge. In this paper we report the first study comparing measurment of isotope deposition amount with separated isotope ion current for isotopes of six different elements (88Sr, 107Ag, 133Cs, 140Ce, 175Lu and 205Tl). These isotopes were sequentially deposited on a conductive substrate located in place of the standard electron multiplier in a quadrupole inductively coupled plasma MS. The results indicate good correlation between measured ion current and deposited mass as measured by quantitative analysis. This empirically confirms a means to quantify total mass deposition by ion charge measurements at implantation energies of 5 – 10 eV.

Liezers, Martin↗

Cavity evolution at grain boundaries as a function of radiation damage and thermal conditions in nanocrystalline nickel

Enhanced radiation tolerance of nanostructured metals is attributed to the high density of interfaces that can absorb radiation-induced defects. Here, cavity evolution mechanisms during cascade damage, helium implantation, and annealing of nanocrystalline nickel are characterized via in situ transmission electron microscopy (TEM). Films subjected to self-ion irradiation followed by helium implantation developed evenly distributed cavity structures, whereas films exposed in the reversed order developed cavities preferentially distributed along grain boundaries. Post-irradiation annealing and orientation mapping demonstrated uniform cavity growth in the nanocrystalline structure, and cavities spanning multiple grains. Furthermore, these mechanisms suggest limited ability to reduce swelling, despite the stability of the nanostructure.

36 MATERIALS SCIENCE↗

Subsurface Synthesis and Characterization of Ag Nanoparticles Embedded in MgO

Metal nanoparticles exhibit localized surface plasmon resonance (LSPR) which is very sensitive to the size and shape of the nanoparticle and the dielectric medium surrounding it. LSPR causes field enhancement near the surface of the nanoparticle making them interesting candidates for plasmonic applications. In particular, partially exposed metallic nanoparticles distributed in a dielectric matrix form hotspots which are prime locations for LSPR spectroscopy and sensing. This study involves synthesizing partially buried Ag nanoparticles in MgO and investigating the characteristics of this material system. Ag nanoparticles of different shapes and size distributions were synthesized below the surface of MgO by implanting 200 keV Ag+ ions followed by annealing at 10000C for 10 and 30 hours. A detailed optical and structural characterization was carried out to understand the evolution of Ag nanoparticle microstructure and size distribution inside the MgO matrix. Micro x-ray diffraction (MicroXRD) was employed to investigate the structural properties and estimate the crystallite size. The nanoparticles evolved from a spherical to faceted morphology with annealing time, assuming an octahedral shape truncated at the (001) planes as seen from aberration corrected transmission electron microscopy (TEM) images. The nanoparticles embedded in MgO were shown to be pure metallic Ag using atom probe tomography (APT). The nanoparticles were partially exposed to the surface employing plasma etch techniques to remove the overlaying MgO. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to study the surface morphology and obtain a height distribution for the partially exposed nanoparticles.

Environmental Molecular Sciences Laboratory↗

Superconductive silicon nanowires using gallium beam lithography.

This work was an early career LDRD investigating the idea of using a focused ion beam (FIB) to implant Ga into silicon to create embedded nanowires and/or fully suspended nanowires. The embedded Ga nanowires demonstrated electrical resistivity of 5 m -cm, conductivity down to 4 K, and acts as an Ohmic silicon contact. The suspended nanowires achieved dimensions down to 20 nm x 30 nm x 10 m with large sensitivity to pressure. These structures then performed well as Pirani gauges. Sputtered niobium was also developed in this research for use as a superconductive coating on the nanowire. Oxidation characteristics of Nb were detailed and a technique to place the Nb under tensile stress resulted in the Nb resisting bulk atmospheric oxidation for up to years.

Henry, Michael David↗

Rare gases in etched 10084 ilmenite - A search for trapped solar-flare rare gases

Results are presented of rare-gas analyses of 10084 ilmenite samples which have been etched to depths of about 1 micrometer in an attempt to remove the surface layer of trapped solar-wind gases, thereby allowing detection of the more deeply implanted solar-flare ions in the remaining trapped gases. A tendency found for the Ne-20/Ne-22 ratios in the etched ilmenite to reflect the solar-wind ratio measured in the solar-wind composition experiment foils may represent a cancellation of mass-fractionation effects. The Ne-20/Ne-22 ratio in the saturated layer is lowered with respect to the solar wind by preferential diffusive loss, but is raised again in the gas diffusing inward by the same preferential mobilization of Ne-20 relative to Ne-22. Attention is also given to the significance of the findings in the case of argon, krypton, and xenon.

Leich, D. A.↗

Solar, planetary, and other inert gases in two sieve fractions of a disaggregated Allende sample - A study by stepwise heating extraction

Inert gases released by stepwise heating of unaltered, strongly magnetic, and weakly magnetic samples from the 0-64 micron and the 105-250 micron fractions of a disaggregated and sieved sample of the Allende meteorite reveal the occurrence of both solar and planetary neon. The origin of the solar neon is thought to be implantation of solar wind ions. The origin of the planetary neon remains unresolved. Heavy isotope enriched components of krypton and xenon have been detected and there are some indications that a light krypton component may also be present. Other than a larger concentration of Xe-129 in the weakly magnetic samples, the signatures of the magnetic separates are isotopically very similar.

Palma, R. L.↗

Continued Investigations of the Accretion History of Extraterrestrial Matter over Geologic Time

This grant supported our ongoing project to characterize the accretion rate of interplanetary dust particles (IDPs) to Earth over geologic time using He-3 as a tracer. IDPs are derived from collisions in the asteroid belt and from disaggregation of active comets. Owing to their small size (few to few hundred micrometers diameter) these particles spiral into the sun under Poynting-Robertson drag typically in less than a few tens of kyrs. Thus IDPs must be continually resupplied to the zodiacal cloud, and because the processes of IDP production are likely to be sporadic, time variation in the IDP accretion rate to Earth is likely to be time-varying. For example, major asteroidal collisions and comet showers should greatly enhance the IDP accretion rate. Our ultimate objective (still ongoing) is to document this time variance so as to better understand the history of the solar system, the source of IDPs accreting to Earth, and the details of the mechanism by which particles are captured by Earth. To document variations in IDP accretion rate through time we use He-3 as a tracer. This isotope is in extremely low abundance in terrestrial matter, but IDPs have very high concentrations of He-3 from implantation of solar wind ions. By measuring He-3 in seafloor sediments, we can estimate the IDP accretion rate for at least the last few hundred Myrs. Under an earlier NASA grant we identified the existence of a large increase in He-3 flux in the Late Eocene (35 Myr ago), coincident with the two largest impact craters of the Cenozoic Era. The simplest interpretation of this observation is the occurrence of a shower of long period comets at that time, simultaneously increasing the impact cratering probability and accretion rate of IDPs to Earth (Farley et al., 1998). Comet showers produced by stellar perturbation of the Oort cloud should be fairly common in the geologic record, so this is not an unreasonable interpretation of our observations.

Farley, Kenneth↗