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DOE OSTI2019

A High-Speed Z-Axis MEMS STM Nanopositioner

Scanning tunneling microscope (STM) is a powerful and versatile tool, not only capable of obtaining topographic information at atomic levels from a conductive surface, but also suited for patterning, manipulation and other applications, all with unprecedented precision. A typical STM’s operation relies on the quantum tunneling phenomenon. Providing a few angstroms of tip-sample separation, and a bias voltage between the two, a tunneling current (TC) is established. The tunneling current is logarithmically proportional to the tip sample separation . During imaging, a three degree of freedom (DOF) piezotube is employed to scan the tip over the surface, while a PI controller drives the Z axis in order to maintain the tunneling current at the set value. Therefore, an image of the sample surface can be constructed using the Z axis controller output, along with the corresponding X, and Y coordinates from the piezotube. Despite its well-established use in high precision applications, the achievable scan speed of the conventional STM has remained limited since its advent. One of the main reasons limiting the achievable scan speed is the relatively low operation bandwidth of the bulky piezotube Z-axis positioner, which is typically less than 1 kHz in conventional systems . This limitation correspondingly hinders the ability of the Z-axis controller to rapidly respond to the changes in the topography during the scan. To address this limitation, we design, build and characterize a high-bandwidth, 1-DOF nanopositioner with an electrostatic parallel plate actuation mechanism and a conductive tip, to replace the Z axis of the currently available STM piezotubes (Figure 1). The device is microfabricated using an SOI wafer with two device layers, where the top-most layer is designated for the tunneling current sensing, and contains the conductive tip realized by FIB induced deposition. The bottom device layer, on the other hand, comprises the actuation mechanism along with the shuttle and mechanical flexures, that provides 2-µm displacement range in one direction, comparable to a typical STM piezoelectric tube scanner. Importantly, the nanopositioner is structurally designed to have a -3dB bandwidth of 15.6 kHz, increasing the STM positioners’ Z axis bandwidth more than an order of magnitude as experimentally shown in Figure 2. Using this system we were able to demonstrate that tunneling current can be successfully established on an HOPG sample in air and successfully maintained for over two minutes (Figures 3-4).

FIB↗

DOE OSTI2016

Understanding the formation and growth of Ag nanoparticles on silver chromate induced by electron irradiation in electron microscope: A combined experimental and theoretical study

Ag{sub 2}CrO{sub 4} microcrystals were synthesized using the co-precipitation method. These microcrystals were characterized through X-ray diffraction (XRD) with Rietveld analysis, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), micro-Raman (MR). XRD patterns and Rietveld refinement data showed that the material exhibits an orthorhombic structure without any deleterious phases. FE-SEM and TEM micrographs revealed the morphology and the growth of Ag nanoparticles on Ag{sub 2}CrO{sub 4} microcrystals during electron beam irradiation. These events were directly monitored in real-time. Their optical properties were investigated using ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy that allowed the calculation of the optical band gap energy. Theoretical analyses based on the density functional theory level indicate that the incorporation of electrons is responsible for structural modifications and formation of defects on the [AgO{sub 6}] and [AgO{sub 4}] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag{sub 2}CrO{sub 4} orthorhombic structure. Display Omitted - Highlights: • The Ag{sub 2}CrO{sub 4} microcrystals indicate an orthorhombic structure. • The formation of Ag{sup 0} promotes Ag-nanoparticle growth on the surface of the Ag{sub 2}CrO{sub 4}. • Electron irradiation of the material induces the formation of Ag vacancies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Effect of pattern transfer process on roughness of block copolymer patterns from directed self-assembly

Block copolymer-directed self-assembly (DSA) remains promising for improving pattern quality and reducing the stochastic variations that challenge high numerical aperture extreme ultraviolet lithography. Equally critical is refining pattern transfer methods for accurately transferring the rectified DSA features to the underlying substrate. We compare two atomic layer deposition (ALD)-based techniques: sequential infiltration synthesis (SIS) and dry liftoff, applied to polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) DSA patterns. Both methods utilize aluminum oxide hard masks, with one synthesized through infiltration into the PMMA domains and the other through conformal ALD coating. High-resolution scanning electron micrographs were analyzed to measure line edge, width, and placement roughness for both the line (PMMA) and space (PS) features. Although both methods yielded similar overall 3σ rms roughness, they differed significantly in the frequency-dependent power spectral density (PSD) profiles. SIS reduced line placement roughness at length scales associated with the polymer pitch, but increased space width roughness at low frequencies, whereas dry liftoff mimicked the frequency content of the original guiding pattern. This study underscores the importance of PSD evaluation in selecting optimal pattern transfer strategies for specific applications.

Block copolymers↗

DOE OSTI2025

Autonomous Multistate Nanoencoding Using Combinatorial Ferroelectric Closure Domains in BiFeO 3

Recent advances in ferroic materials have identified topological defects as promising candidates for enabling additional functionalities in future electronic systems. The generation of stable and customizable polar topologies is needed to achieve multistates that enable beyond-binary device architectures. Here, in this study, we show how to autonomously pattern on-demand highly tunable striped closure domains in pristine rhombohedral-phase BiFeO 3 thin films through precise scanning of a biased atomic force microscopy tip along carefully designed paths. By employing this strategy, we generate and manipulate closed-loop structures with high spatial resolution in an automated manner, allowing the creation of highly tunable and intricate topological domain structures that exhibit distinct polarization configurations without the need for electrode deposition or complex heterostructure growth. As a proof-of-concept for ferroelectric beyond-binary memory devices, we use such topological domains as multistates, engineering an alphabet and automating the symbolic writing/reading process using autonomous microscopy. The resulting information density is compared with that of current commercially available memory devices, demonstrating the potential of ferroelectric topological domains for multistate information storage applications.

BiFeO3↗

DOE OSTI2016

Guiding, bending, and splitting of coupled defect surface modes in a surface-wave photonic crystal

We experimentally demonstrate a type of waveguiding mechanism for coupled surface-wave defect modes in a surface-wave photonic crystal. Unlike conventional spoof surface plasmon waveguides, waveguiding of coupled surface-wave defect modes is achieved through weak coupling between tightly localized defect cavities in an otherwise gapped surface-wave photonic crystal, as a classical wave analogue of tight-binding electronic wavefunctions in solid state lattices. Wave patterns associated with the high transmission of coupled defect surface modes are directly mapped with a near-field microwave scanning probe for various structures including a straight waveguide, a sharp corner, and a T-shaped splitter. These results may find use in the design of integrated surface-wave devices with suppressed crosstalk.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2016

Direct imaging of coexisting ordered and frustrated sublattices in artificial ferromagnetic quasicrystals

Here, we have used scanning electron microscopy with polarization analysis and photoemission electron microscopy to image the two-dimensional magnetization of permalloy films patterned into Penrose P2 tilings (P2T). The interplay of exchange interactions in asymmetrically coordinated vertices and short-range dipole interactions among connected film segments stabilize magnetically ordered, spatially distinct sublattices that coexist with frustrated sublattices at room temperature. Numerical simulations that include long-range dipole interactions between sublattices agree with images of as-grown P2T samples and predict a magnetically ordered ground state for a two-dimensional quasicrystal lattice of classical Ising spins.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this paper, we describe a detailed procedure for acquiring and processing x-ray microfluorescence (μXRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al 2 O 3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g. , one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Structure, Morphology, Cation Distribution and Magnetic Properties of Cr{sup 3+}-Substituted CoFe{sub 2}O{sub 4} Nanoparticles

The present investigations deal with the effect of trivalent chromium ions (Cr{sup 3+}) on structural and magnetic properties of nanocrystalline cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles. The samples of CoCr{sub x}Fe{sub 2−x}O{sub 4} (where x = 0.0 to 1.0 in step of 0.2) were successfully synthesized by citric acid-assisted sol-gel auto combustion method. Further, the prepared samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (IR) and pulsed field hysteresis loop technique for structural, morphological and magnetic properties analysis, respectively. XRD patterns showed the formation of single-phase cubic spinel structure with broad Bragg’s peak for all the samples. The value of lattice parameter was found to be decreased with chromium substitution x. Cation distribution studies revealed that Co{sup 2+} and Fe{sup 3+} occupied both A and B sites, whereas Cr{sup 3+} ions occupied only B site. SEM analysis of the prepared samples confirmed the nanocrystalline nature of the material. The two absorption bands belonging to spinel structure were observed in IR spectra. Saturation magnetization (M{sub S}), remanence magnetization (M{sub r}) and coercivity (H{sub C}) was found to be decreased with increase in chromium substitution x.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2020

Tilted fluctuation electron microscopy

Fluctuation electron microscopy (FEM) is a scanning nanodiffraction-based method that offers a unique approach to characterizing nanometer-scale medium-range order (MRO) in disordered materials. In addition to determining the degree of MRO, careful analysis of scanning nanodiffraction data can also be used to determine strain in thin film amorphous samples. We applied FEM to characterize the strain and MRO of magnetron sputtered amorphous tantalum (a-Ta) thin films over a range of tilt angles from 0° to 45° in order to measure any deviations between the in-plane and out-of-plane strain and MRO. We validate our approach using electron diffraction simulations of FEM experiments for a-Ta. We measure anisotropic strain in the simulated a-Ta diffraction patterns and find that the experimental a-Ta is isotropically strained within the accuracy of our method. Our approach provides a workflow for acquiring tilted scanning nanodiffraction data, determining the relative strain and ordering as a function of in- A nd out-of-plane directions, and removing any artifacts induced in FEM data due to strain. We also describe some limitations of the tilted FEM method when applied to thin films with very low strains.

36 MATERIALS SCIENCE↗

DOE OSTI2018

FeCo Nanorods Preparation Using New Chemical Synthesis

The as-prepared and annealed iron/cobalt (FeCo) magnetic nanoparticles (NPs) were obtained using a simple method by iron chloride hexahydrate (FeCl{sub 3}.6H{sub 2}O) and cobalt chloride hexahydrate (CoCl{sub 3}.6H{sub 2}O) as precursors and sodium borohydride (NaBH{sub 4}) agent. The samples were characterized by high-resolution transmission electron microscopy (HRTEM), field effect scanning electron microscopy (FESEM), x-ray diffraction (XRD), electron-dispersive spectroscopy (EDS), and Fourier transform infrared spectroscopy (FTIR). The XRD patterns of FeCo samples showed the body center cubic (bcc) structure with a lattice constant of 2.70 Å. The SEM images showed that the particle size of the as-prepared sample was around 15 nm and the annealed sample was around 35 nm in diameter at 500 {sup ∘}C. It was found that by increasing annealing temperature, the size of the FeCo NPs increased to 60 nm at 1100 {sup ∘}C. TEM studies showed the rod-like particles for annealed sample. The sharp peaks in FTIR spectrum determined the element of FeCo NPs. EDS shows peaks of iron and cobalt with impurities in prepared samples. The result of magnetic measurements showed a good coercive field and saturation magnetization around 1158 Oe and 22 emu g{sup − 1}, respectively.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Structural, thermal and electrical characterizations of multiwalled carbon nanotubes and polyaniline composite

The undoped and doped composite of MWNTs (Multiwalled Carbon Nanotubes) with PANI (/Polyaniline) was prepared by chemical oxidative polymerization. The MWNTs/PANI composites have been characterized by using various techniques like Thermogravometric Analysis (TGA), Fourier transform infrared (FT-IR) spectrometer and Field emission scanning electron microscope (FE-SEM) and conductivity measurement by using two probe method. TGA results has shown that thermal stability followed the pattern undoped MWNTs/PANI composite < doped MWNTs/PANI composite. FE-SEM micrographs demonstrated the morphological changes on the surface of MWNTs as a result of composite formation. Fourier transformed infrared (FT-IR) spectra ascertained the formation of the composite. Study of electrical characteristics demonstrated that the doped MWNTs/PANI composite (1.2 × 10{sup 1} Scm{sup −1}) have better conductivity than the undoped MWNTs/PANI composite (10{sup −4} Scm{sup −1}). These CNTs based polymeric composites are of great importance in developing new nano-scale devices for future chemical, mechanical and electronic applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2015

A clip-based protocol for breast boost radiotherapy provides clear target visualisation and demonstrates significant volume reduction over time

The clinical target volume (CTV) for early stage breast cancer is difficult to clearly identify on planning computed tomography (CT) scans. Surgical clips inserted around the tumour bed should help to identify the CTV, particularly if the seroma has been reabsorbed, and enable tracking of CTV changes over time. A surgical clip-based CTV delineation protocol was introduced. CTV visibility and its post-operative shrinkage pattern were assessed. The subjects were 27 early stage breast cancer patients receiving post-operative radiotherapy alone and 15 receiving post-operative chemotherapy followed by radiotherapy. The radiotherapy alone (RT/alone) group received a CT scan at median 25 days post-operatively (CT1rt) and another at 40 Gy, median 68 days (CT2rt). The chemotherapy/RT group (chemo/RT) received a CT scan at median 18 days post-operatively (CT1ch), a planning CT scan at median 126 days (CT2ch), and another at 40 Gy (CT3ch). There was no significant difference (P = 0.08) between the initial mean CTV for each cohort. The RT/alone cohort showed significant CTV volume reduction of 38.4% (P = 0.01) at 40 Gy. The Chemo/RT cohort had significantly reduced volumes between CT1ch: median 54 cm{sup 3} (4–118) and CT2ch: median 16 cm{sup 3}, (2–99), (P = 0.01), but no significant volume reduction thereafter. Surgical clips enable localisation of the post-surgical seroma for radiotherapy targeting. Most seroma shrinkage occurs early, enabling CT treatment planning to take place at 7 weeks, which is within the 9 weeks recommended to limit disease recurrence.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2015

Deposition of Pd–Ag thin film membranes on ceramic supports for hydrogen purification/separation

Highlights: • Thin film Pd–Ag membranes have been produced for hydrogen selectivity. • Magnetron sputtering yields Pd–Ag compact films for atomic H diffusion. • The thin film Pd–Ag membranes yielded a selectivity of α (H{sub 2}/N{sub 2}) = 10. - Abstract: Pd–Ag based membranes supported on porous α-Al{sub 2}O{sub 3} (doped with yttria-stabilized zirconia) were studied for hydrogen selective separation. Magnetron sputtering technique was employed for the synthesis of thin film membranes. The hydrogen permeation flux is affected by the membrane columnar structure, which is formed during deposition. From scanning electron microscopy analysis, it was observed that different sputtering deposition pressures lead to distinct columnar structure growth. X-ray diffraction patterns provided evidence of a Pd–Ag solid solution with an average crystallite domain size of 21 nm, whose preferential growth can be altered by the deposition pressure. The gas-permeation results have shown that the Pd–Ag membrane supported on porous α-Al{sub 2}O{sub 3} is selective toward H{sub 2}. For optimized membrane synthesis conditions, the permeance toward N{sub 2} is 0.076 × 10{sup −6} mol m{sup −2} s{sup −1} Pa{sup −1} at room temperature, whereas for a pressure difference of 300 kPa the H{sub 2}-flux is of the order of ca. 0.21 mol m{sup −2} s{sup −1}, which corresponds to a permeance of 0.71 × 10{sup −6} mol m{sup −2} s{sup −1} Pa{sup −1}, yielding a selectivity of α (H{sub 2}/N{sub 2}) = 10. These findings suggest that the membrane has a reasonable capacity to selectively permeate this gas.

36 MATERIALS SCIENCE↗

DOE OSTI2015

SU-C-210-03: Impact of Breathing Irregularities On Gated Treatments

Purpose: To evaluate the effect of breathing irregularities on target location in gated treatments using amplitude and phase gating. Methods: 111 breathing patterns acquired using RPM system were categorized based on period and amplitude STD as regular (STD period ≤ 0.5 s, STD amplitude ≤ 1.5 mm), medium (0.5 s < STD period ≤ 1 s, 1.5 mm < STD amplitude ≤ 3 mm) and irregular (STD period > 1 s, STD amplitude > 3 mm). One pattern representative of the average defined population was selected per category and corresponding target motion reproduced using Quasar Respiratory Motion Phantom. Phantom in motion underwent 4D-CT scan with phase reconstruction. Gated window was defined at end of exhale and DRRs reconstructed in treatment planning at 40% (beam on) and 60% phase (beam off). Target location uncertainty was assessed by comparing gated kV triggered images continuously acquired at beam on/off on a True Beam 2.0 with corresponding DRRs. Results: Average target uncertainty with amplitude gating was in [0.4 – 1.9] mm range for the different scenarios with maximum STD of 1.2 mm for the irregular pattern. Average target uncertainty with phase gating was [1.1 – 2.2] mm for regular and medium patterns, while it increased to [3.6 – 9.6] mm for the irregular pattern. Live gated motion was stable with amplitude gating, while increasing with phase gating for the irregular pattern. Treatment duration range was [68 – 160] s with amplitude and [70 – 74] s with phase gating. Conclusion: Breathing irregularities were found to affect gated treatments only when using phase gating. For regular and medium patterns no significant difference was found between the two gating strategies. Amplitude gating ensured stable gated motion within the different patterns, thus reducing intra-fraction target location variability for the irregular pattern and resulting in longer treatment duration.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Epitaxial growth of monolayer PdTe 2 and patterned PtTe 2 by direct tellurization of Pd and Pt surfaces

Two-dimensional (2D) palladium ditelluride (PdTe 2 ) and platinum ditelluride (PtTe 2 ) are two Dirac semimetals, which have fascinating quantum properties such as superconductivity, magnetism and topological order and show the promising applications in future nanoelectronics and optoelectronics. However, the synthesis of PdTe 2 and PtTe 2 monolayers (MLs) is hindered by a strong interlayer coupling and orbital hybridization. Here, in this study, we demonstrate an efficient synthesis of PdTe 2 and PtTe 2 MLs Large-area and high quality MLs of PdTe 2 and patterned PtTe 2 were epitaxially grown on the Pd(111) and Pt(111) surfaces by direct telurization in ultra-high vacuum. This was confirmed by x-ray photoelectron spectroscopy, low energy electron diffraction and scanning tunnelling microscopy. PdTe 2 ML demonstrated high thermal stability showing no decomposition sign after annealing at 470 °C. A well-ordered (2 × 2) PtTe 2 structure with Kagome lattice was observed on Te/Pt(111) surface following annealing at 200 °C in UHV, where the (2 × 2) pattern was formed by Te atom vacancies. PtTe 2 multilayer film was prepared as well, and it demonstrated the excitation of the Dirac plasmons as measured by high-resolution electron energy loss spectroscopy. The direct tellurization offers the simple and reliable protocol for the preparation of the ML of PdTe 2 and patterned PtTe 2 , and this opens new opportunities for quantum phenomena research and for practical optoelectronics applications.

2D materials↗

DOE OSTI2020

Phase‐Dependent Band Gap Engineering in Alloys of Metal‐Semiconductor Transition Metal Dichalcogenides

Abstract Bandgap engineering plays a critical role in optimizing the electrical, optical and (photo)‐electrochemical applications of semiconductors. Alloying has been a historically successful way of tuning bandgaps by making solid solutions of two isovalent semiconductors. In this work, a novel form of bandgap engineering involving alloying non‐isovalent cations in a 2D transition metal dichalcogenide (TMDC) is presented. By alloying semiconducting MoSe 2 with metallic NbSe 2 , two structural phases of Mo 0.5 Nb 0.5 Se 2 , the 1T and 2H phases, are produced each with emergent electronic structure. At room temperature, it is observed that the 1T and 2H phases are semiconducting and metallic, respectively. For the 1T structure, scanning tunneling microscopy/spectroscopy (STM/STS) is used to measure band gaps in the range of 0.42–0.58 at 77 K. Electron diffraction patterns of the 1T structure obtained at room temperature show the presence of a nearly commensurate charge density wave (NCCDW) phase with periodic lattice distortions that result in an uncommon 4 × 4 supercell, rotated approximately 4° from the lattice. Density‐functional‐theory calculations confirm that local distortions, such as those in a NCCDW, can open up a band gap in 1T ‐Mo 0.5 Nb 0.5 Se 2 , but not in the 2H phase. This work expands the boundaries of alloy‐based bandgap engineering by introducing a novel technique that facilitates CDW phases through alloying.

Wang, Shuxi↗

DOE OSTI2017

The effect of grain orientation on nanoindentation behavior of model austenitic alloy Fe-20Cr-25Ni

Instrumented nanoindentation was used in this paper to investigate the hardness, elastic modulus, and creep behavior of an austenitic Fe-20Cr-25Ni model alloy at room temperature, with the indented grain orientation being the variant. The samples indented close to the {111} surfaces exhibited the highest hardness and modulus. However, nanoindentation creep tests showed the greatest tendency for creep in the {111} indented samples, compared with the samples indented close to the {001} and {101} surfaces. Scanning electron microscopy and cross-sectional transmission electron microscopy revealed slip bands and dislocations in all samples. The slip band patterns on the indented surfaces were influenced by the grain orientations. Deformation twinning was observed only under the {001} indented surfaces. Finally, microstructural analysis and molecular dynamics modeling correlated the anisotropic nanoindentation-creep behavior with the different dislocation substructures formed during indentation, which resulted from the dislocation reactions of certain active slip systems that are determined by the indented grain orientations.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Real-time microstructure imaging by Laue microdiffraction: A sample application in laser 3D printed Ni-based superalloys

Synchrotron-based Laue microdiffraction has been widely applied to characterize the local crystal structure, orientation, and defects of inhomogeneous polycrystalline solids by raster scanning them under a micro/nano focused polychromatic X-ray probe. In a typical experiment, a large number of Laue diffraction patterns are collected, requiring novel data reduction and analysis approaches, especially for researchers who do not have access to fast parallel computing capabilities. In this article, a novel approach is developed by plotting the distributions of the average recorded intensity and the average filtered intensity of the Laue patterns. Visualization of the characteristic microstructural features is realized in real time during data collection. As an example, this method is applied to image key features such as microcracks, carbides, heat affected zone, and dendrites in a laser assisted 3D printed Ni-based superalloy, at a speed much faster than data collection. Such analytical approach remains valid for a wide range of crystalline solids, and therefore extends the application range of the Laue microdiffraction technique to problems where real-time decision-making during experiment is crucial (for instance time-resolved non-reversible experiments).

36 MATERIALS SCIENCE↗