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At least 883 records · Page 49

Infrared nanospectroscopy characterization of metal oxide photoresists

Implementation of extreme ultraviolet (EUV) lithography in high-volume semiconductor manufacturing requires a reliable and scalable EUV resist platform. A mechanistic understanding of the pros and cons of different EUV resist materials is critically important. However, most material characterization methods with nanometer resolution use an x-ray photon or electron beam as the probe, which often cause damage to the photoresist film during measurement. Here, we illustrated the use of non-destructive infrared nanospectroscopy [or nano-Fourier-Transform infrared spectroscopy (nano-FTIR)] to obtain spatially resolved composition information in patterned photoresist films. Further, clear evidence of exposure-induced chemical modification was observed at a spatial resolution down to 40 nm, well below the diffraction limit of infrared light. With improvements, such a nano-FTIR technique with nanoscale spatial resolution, chemical sensitivity, and minimal radiation damage can be a promising candidate for the fundamental study of material properties relevant to EUV lithography.

36 MATERIALS SCIENCE↗

A submillimeter tripler using a quasi-waveguide structure

A new type of frequency multiplier structure is being developed which is suitable for application at frequencies above 1 THz. This structure preserves some of the properties of waveguide for mode control, yet is not truly single mode. The device resembles a sectoral horn, with a varactor diode mounted near the throat. Input and output coupling are through the same aperture, requiring a quasi-optical diplexer. Initial tests are directed at building a tripler at 500 GHz, for comparison with waveguide structures. The diplexer is a blazed diffraction grating with appropriate focusing optics. Model studies show that the impedance match to a varactor should be good, and initial tests of the beam patterns of the prototype indicate that optical coupling efficiency should be very high. The structure also has the potential for use as a fundamental mixer, or as a third harmonic mixer.

Erickson, Neal R.↗

Revolving-Pinhole Calibrator

Revolving-pinhole calibrator used to calibrate instrument called "Forward Scattering Spectrometer Probe" (FSSP). This instrument measures light scattered from water droplets in icing clouds. Scattering patterns used to determine sizes and distribution of sizes of droplets in connection with safety-oriented studies of icing on aircraft. Pinhole serves as diffraction standard for measuring small particles and drops.

Hovenac, Edward A.↗

Patterned OLEDs: effect of substrate corrugation pitch and height

Abstract An ongoing OLED challenge is cost-effective enhancement of light extraction, i.e., increasing the external quantum efficiency ( EQE ∼20% in conventional devices). OLEDs on corrugated substrates often show enhanced EQE s providing insight into light emission processes. In particular, patterned plastic substrates directly imprinted easily at room temperature and amenable to low-cost R2R production are ideal for studying/optimizing various structures, further elucidating the extraction process. We show new semi-quantitative data of the effect of the pitch ( a ) and height/depth ( h ) of plastic substrate patterns on the OLEDs’ stack and EQE , focusing on new designs, interestingly, some showing surprisingly enhanced EQE s that were neither reported nor discussed before. These includ e : ( i ) shallow ( h < 200 nm) convex polycarbonate with a ∼ 750 versus ∼400 nm, where the h gradually decreases as the OLED stack is built and ( ii ) concave PET/CAB with large a (∼2.8 and ∼7.8 μ m), where the EQE enhancement of conformal OLEDs may be due largely to scattering. EQE s of green, blue, and white phosphorescent OLEDs were measured. OLEDs on substrates with narrow a ∼ 400 nm and low h < 200 nm s h owed no enhancement, resembling flat devices. In contrast, OLEDs on substrates with comparable or smaller h , but larger a ∼ 750 nm show signific a nt EQE enhancement despite h reduction across the stack. Green OLEDs with a ∼ 750 nm and h ∼ 160 to ∼180 nm, showed EQE s ∼30%, reaching ∼58% with substrate mode extraction. Surprisingly, fully conformal OLEDs on a PET/CAB substrate with a ∼ 7.8 μ m showed blue a nd white EQE s reaching ∼33%, without substrate mode extraction. The enhancing patterns increase the OLEDs’ EQE by reducing surface plasmon excitation and internal waveguiding. The experimental results for OLEDs on substrates with a < 2 μ m are supported by scattering matrix simulations that assume conformal stacks, incorporating diffraction for internal losses reduction. EQE enhancement not predicted by simulations may be due additionally to scattering mostly for substrates with a signific a ntly larger than the emitting wavelength.

42 ENGINEERING↗

A technique for designing active control systems for astronomical telescope mirrors

This paper considers the problem of designing a control system to achieve and maintain the required surface accuracy of the primary mirror of a large space telescope. Control over the mirror surface is obtained through the application of a corrective force distribution by actuators located on the rear surface of the mirror. The design procedure is an extension of a model control technique developed for distributed parameter plants with known eigenfunctions to include plants whose eigenfunctions must be approximated by numerical techniques. Instructions are given for constructing the mathematical model of the system, and a design procedure is developed for use with. typical numerical data in selecting the number and location of the actuators. Examples of actuator patterns and their effect on various errors are given.

Active optics↗

Tracing Phase Transformation and Lattice Evolution in a TRIP Sheet Steel under High-Temperature Annealing by Real-Time In Situ Neutron Diffraction

Real-time in situ neutron diffraction was used to characterize the crystal structure evolution in a transformation-induced plasticity (TRIP) sheet steel during annealing up to 1000 °C and then cooling to 60 °C. Based on the results of full-pattern Rietveld refinement, critical temperature regions were determined in which the transformations of retained austenite to ferrite and ferrite to high-temperature austenite during heating and the transformation of austenite to ferrite during cooling occurred, respectively. The phase-specific lattice variation with temperature was further analyzed to comprehensively understand the role of carbon diffusion in accordance with phase transformation, which also shed light on the determination of internal stress in retained austenite. These results prove the technique of real-time in situ neutron diffraction as a powerful tool for heat treatment design of novel metallic materials.

Yu, Dunji [ORNL] (ORCID:0000000189467851)↗

TPSAS-NF1676L-31770-DND

HREBSD (high resolution electron backscatter diffraction) is a scanning electron microscope based diffraction technique that measures stress, elastic strain and dislocation density in crystalline materials with a spatial resolution on the order of tens of nanometers. This information represents a glut of quantitative data that may be directly incorporated in microscale crystal plasticity models. However, concerns over the accuracy of HREBSD make integration of microscopy data with material models problematic. This presentation addresses a number of issue concerning the accuracy of HREBSD, including pattern center error, cross-correlation error and random noise. Additionally, a computational framework is presented that allows for rapid, non-deterministic calibration of material models. Finally, several tests cases are presented where HREBSD is cross-validated with other diffraction techniques: X-ray diffraction, electron channeling contrast imaging and transmission electron microscopy. The accuracy of HREBSD, when incorporating these new techniques, is sufficient to measure local stress to below 10 MPa and to detect individual dislocations.

Timothy J Ruggles↗

Evolution of Microstructure, Residual Stress, and Tensile Properties of Additively Manufactured Stainless Steel Under Heat Treatments

This study investigated the microstructure, residual stress and tensile properties of the directed energy deposited stainless steel 316L (SS316L) under thermal annealing. Microstructure characterization shows the as-printed sample has laser-generated patterns where dendritic structure is observed at the edge of the patterns and cellular structure dominates the interior region. Here, the thermal annealing at 983 and 1093°C effectively removes the dendritic/cellular structures. Synchrotron X-ray diffraction reveals that the as-fabricated SS316L exhibits compressive residual stress of -197.4 MPa. The stress is greatly relieved to -53.8 MPa after annealing at 1093°C. The room temperature tensile testing indicates that the yield strength and ultimate tensile strength drop from 378 and 502 MPa in the as-printed sample to 258 and 446 MPa in the annealed samples (1093°C), respectively. Our study provides insights into the relationship between microstructure, residual stress, and tensile properties of laser additive manufactured SS316L.

36 MATERIALS SCIENCE↗

Calculating Effects of Reflector-Antenna Distortions

Mathematical numerical model accurately predicts effects of systematic distortions on radiation pattern of reflector antenna. Techniques for predicting radiation patterns developed previously for reflectors with perfect surfaces and surfaces with random deviations from perfection. New model treats reflectors distorted by thermal, gravitational, and dynamic effects. Diffraction analysis of reflector antenna depends on interpolation of surface description for farfield radiation integral. Local interpolation scheme uses bicubic or higher order polynomial approximation of surface to express desired surface point in terms of nearby known surface points.

Rahmat-Samii, Y.↗

Estimation of Supraglacial Dust and Debris Geochemical Composition via Satellite Reflectance and Emissivity

We demonstrate spectral estimation of supraglacial dust, debris, ash and tephra geochemical composition from glaciers and ice fields in Iceland, Nepal, New Zealand and Switzerland. Surface glacier material was collected and analyzed via X-ray fluorescence spectroscopy (XRF) and X-ray diffraction (XRD) for geochemical composition and mineralogy. In situ data was used as ground truth for comparison with satellite derived geochemical results. Supraglacial debris spectral response patterns and emissivity-derived silica weight percent are presented. Qualitative spectral response patterns agreed well with XRF elemental abundances. Quantitative emissivity estimates of supraglacial SiO2 in continental areas were 67% (Switzerland) and 68% (Nepal), while volcanic supraglacial SiO2 averages were 58% (Iceland) and 56% (New Zealand), yielding general agreement. Ablation season supraglacial temperature variation due to differing dust and debris type and coverage was also investigated, with surface debris temperatures ranging from 5.9 to 26.6 C in the study regions. Applications of the supraglacial geochemical reflective and emissive characterization methods include glacier areal extent mapping, debris source identification, glacier kinematics and glacier energy balance considerations.

Casey, Kimberly Ann↗

Surface coating by mechanofusion modulates bulk charging pathways and battery performance of Ni-rich layered cathodes

Ni-rich layered oxides as high-capacity battery cathodes suffer from degradation at high voltages. Here, we utilize a dry surface modification method, mechanofusion (MF), to achieve enhanced battery stability. The simplicity, high yield, and flexibility make it cost-effective and highly attractive for processing at the industrial scale. The underlying mechanisms responsible for performance improvement are unveiled by a systematic study combining multiple probes, e.g., 3D nano-tomography, spectroscopic imaging, in situ synchrotron diffraction, and finite element analysis (FEA). MF affects the bulk crystallography by introducing partially disordered structure, microstrain, and local lattice variation. Furthermore, the crack initiation and propagation pattern during delithiation are regulated and the overall mechanical fracture is reduced after such surface coating. We validate that MF can alter the bulk charging pathways. Such a synergic effect between surface modification and bulk charge distribution is fundamentally important for designing next-generation battery cathode materials.

25 ENERGY STORAGE↗

Acousto-optic spectrometer for radio astronomy

Recent developments in acousto-optic techniques and in photodetector arrays have made feasible a new type of RF spectrometer, offering the advantages of wide bandwidth, high resolution, large number of channels in compact, lightweight, energy efficient, and relatively low cost systems. Such a system employs an acousto-optic diffraction cell which serves the key role of converting RF signals to ultrasonic traveling-waves modulating the optical index of the cell. The cell is illuminated across its aperture by a monochromatic laser beam. A fraction of the light is diffracted by the acoustic waves. A focusing lens follows the cell and essentially performs a Fourier transform of the RF signal into a far-field intensity pattern. CSIRO in Australia and the Tokyo Astronomical Observatory in Japan have taken the lead in using acousto-optic techniques in astronomical applications. The first practical device was successfully made at CSIRO for obtaining dynamical spectrographs of solar radio emission.

Chin, G.↗

Unified aeroacoustics analysis for high speed turboprop aerodynamics and noise. Volume 2: Development of theory for wing shielding

A unified theory for aerodynamics and noise of advanced turboprops is presented. The theory and a computer code developed for evaluation at the shielding benefits that might be expected by an aircraft wing in a wing-mounted propeller installation are presented. Several computed directivity patterns are presented to demonstrate the theory. Recently with the advent of the concept of using the wing of an aircraft for noise shielding, the case of diffraction by a surface in a flow has been given attention. The present analysis is based on the case of diffraction of no flow. By combining a Galilean and a Lorentz transform, the wave equation with a mean flow can be reduced to the ordinary equation. Allowance is also made in the analysis for the case of a swept wing. The same combination of Galilean and Lorentz transforms lead to a problem with no flow but a different sweep. The solution procedures for the cases of leading and trailing edges are basically the same. Two normalizations of the solution are given by the computer program. FORTRAN computer programs are presented with detailed documentation. The output from these programs compares favorably with the results of other investigators.

Amiet, R. K.↗

Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

Source record↗

Measurement of shock roughness due to phase plate speckle imprinting relevant for x-ray diffraction experiments on 3rd and 4th generation light sources

Laser-shock compression experiments at 3rd and 4th generation light sources generally employ phase plates, which are inserted into the beamline to achieve a repeatable intensity distribution at the focal plane. Here, the laser intensity profile is characterized by a high-contrast, high-frequency laser speckle. Without sufficient smoothing, these laser non-uniformities can translate to a significant pressure distribution within the sample layer and can affect data interpretation in x-ray diffraction experiments. Here, we use a combination of one- and two-dimensional velocity interferometry to directly measure the extent to which spatial frequencies within the laser focal spot intensity pattern are smoothed out during propagation within the laser plasma and a polyimide ablator. We find that the use of thicker polyimide layers results in spatially smoother shock fronts, with the greatest degree of smoothing associated with the highest spatial frequencies. Focal spots with the smallest initial speckle separation produce the most rapid smoothing. Laser systems that employ smoothing by spectral dispersion techniques to rapidly modulate the focal plane intensity distribution are shown to be the most effective ones in producing a spatially smooth shock front. We show that a simple transport model combined with the known polyimide Hugoniot adequately describes the extent of shock smoothness as a function of polyimide thickness. Finally, our results provide a description of spatial structure smoothing across a shock front, which can be used to design targets on x-ray free electron laser facilities.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Salt-Mediated Coarsening in Conversion-Reaction-Synthesized Nanoporous Metals and Nanocomposites Resolved through In Situ Synchrotron Diffraction Studies

High-energy synchrotron X-rays were used to probe the structural and microstructural evolution in Fe, Co, and Cu nanoporous metals (NPMs) and metal/salt nanocomposites (NCs) produced by recently developed conversion reaction synthesis (CRS) methods. Microstructure analysis of as-synthesized samples via whole pattern fitting showed that the NPMs exhibit domain sizes that increase as Co < Fe < Cu, with both Fe and Co having crystallite sizes below 3.0 nm. The as-synthesized metal/salt NCs had similar metal sizes, and additionally, the salt in the composite had unusually large lattice microstrain whose origin is attributed to chemical substitution of metal ions into the salt (e.g., Li $1–3x$ Fe $x$ Cl for Fe 3+ ). When thermal annealing is used to modify crystallite size, pore collapse often occurs in NPMs but NCs can be effectively tuned without this problem. While the NC coarsening occurs slowly at low temperatures, it was found that there is a drastic acceleration of the reaction rate at a specific onset temperature that results in the crystallite size increasing by an order of magnitude in about a minute. Curiously, there was no evidence in the diffraction data for salt melting at this onset temperature. However, there was a sharp reduction in the salt chemical lattice strain at the onset temperature, indicating that rapid metal coarsening is facilitated by the salt. Importantly, this behavior indicates an unexpectedly coupled reaction mechanism by which the metal ions needed for grain growth are supplied by the salt in a rate-limiting fashion.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Synthesis, structure, linear and nonlinear optical properties of noncentrosymmetric quaternary diamond-like semiconductors, Cu 2 ZnGeSe 4 (CZGSe) and the novel Cu 4 ZnGe 2 Se 7

In this work, two quaternary diamond-like semiconductors (DLSs) in the Cu-Zn-Ge-Se system, the known Cu 2 ZnGeSe 4 (also referred to as CZGSe) and the new Cu 4 ZnGe 2 Se 7 , are compared in terms of their crystal structures, electronic structures and physicochemical properties. Both compounds were prepared by high-temperature, solid-state synthesis at 800 degrees C. Single crystal X-ray diffraction was used to determine the structure of Cu 4 ZnGe 2 Se 7 . The structures of both Cu 2 ZnGeSe 4 and Cu 4 ZnGe 2 Se 7 can be considered as derivatives of cubic diamond. Cu 4 ZnGe 2 Se 7 , with a reduced symmetry due to the cation ordering pattern, adopts the Cu 4 NiSi 2 S 7 structure type, with space group C2. The corner-sharing tetrahedra in Cu 4 ZnGe 2 Se 7 are slightly distorted because the charge for some of the S 2 - anions is not compensated by the first-nearest-neighbor cations. Rietveld refinements using synchrotron X-ray powder diffraction data were used to assess the phase purity of the samples and confirm the bulk structural behavior. Diffuse reflectance UV/Vis/NIR spectroscopy shows that Cu 2 ZnGeSe 4 and Cu 4 ZnGe 2 Se 7 have direct optical bandgaps of 1.38 and 0.91 eV, respectively. Electronic structure calculations implementing density functional theory confirm the direct bandgap for Cu 4 ZnGe 2 Se 7 , with a calculated value of 0.62 eV. Both compounds are air stable, thermally stable up to relatively high temperatures, undergo phase transitions and have wide windows of optical clarity. The Kurtz-Perry powder technique was used to determine the second harmonic generation (SHG) responses using a commercial AgGaSe 2 standard. While Cu 4 ZnGe 2 Se 7 displays a weak SHG response, Cu 2 ZnGeSe 4 exhibits a response that is greater than several benchmark materials, with a large SHG coefficient, χ (2) , of 43 ± 6 pm/V at λ = 2900 nm.

36 MATERIALS SCIENCE↗

A large interlaboratory electron diffraction study of monolayer graphene

Standardisation of data collection and analysis is essential to enable commercialisation of 2D materials in a wide range of technologies. Selected area electron diffraction (SAED) in the transmission electron microscope (TEM) is one of the key methods for distinguishing monolayer from bilayer and few-layer graphene by comparing the 1st and 2nd order diffraction spot intensities. Yet there are many factors that can affect the reliability of data collection and interpretation, causing the measurement of monolayer samples to deviate from the literature boundary condition of $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1 for monolayer graphene (1LG). Here we present the results of a large interlaboratory SAED comparison study, where 15 international laboratories measured and analysed nominally identical samples of chemical vapour deposited graphene. Large variations were observed in the measured ratios of diffraction spot intensities, with the largest variance associated with poor quality SAED data resulting from inadequate specimen handling and storage. To inform the reliable determination of monolayer thickness from SAED patterns we provide a description of best practice for specimen handling, TEM operation, data collection and analysis. This work was undertaken within VAMAS Technical Working Area 41: Graphene and related 2D materials—Project 9, the results of which have been directly incorporated into ISO/TS 21356–2 for the characterisation of graphene sheets. We find that when this methodology is followed, 1LG can be distinguished from bilayer or thicker material with high confidence where analysis of a single SAED pattern gives $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1.2, even in the absence of precise specimen tilting.

2D materials↗