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At least 829 records · Page 46

Effect of fabrication processes on BaTiO 3 capacitor properties

There is an increasing desire to utilize complex functional electronic materials such as ferroelectrics in next-generation microelectronics. As new materials are considered or introduced in this capacity, an understanding of how we can process these materials into those devices must be developed. Here, the effect of different fabrication processes on the ferroelectric and related properties of prototypical metal oxide (SrRuO 3 )/ferroelectric (BaTiO 3 )/metal oxide (SrRuO 3 ) heterostructures is explored. Two different types of etching processes are studied, namely, wet etching of the top SrRuO 3 using a NaIO 4 solution and dry etching using an Ar + -ion beam (i.e., ion milling). Polarization-electric-field hysteresis loops for capacitors produced using both methods are compared. For the ion-milling process, it is found that the Ar + beam can introduce defects into the SrRuO 3 /BaTiO 3 /SrRuO 3 devices and that the milling depth strongly influences the defect level and can induce a voltage imprint on the function. Realizing that such processing approaches may be necessary, work is performed to ameliorate the imprint of the hysteresis loops via ex situ “healing” of the process-induced defects by annealing the ferroelectric material in a barium-and-oxygen-rich environment via a chemical-vapor-deposition-style process. This work provides a pathway for the nanoscale fabrication of these candidate materials for next-generation memory and logic applications.

36 MATERIALS SCIENCE↗

Repair of a mirror coating on a large optic for high laser damage applications using ion milling and over-coating methods

Here, when an optical coating is damaged, deposited incorrectly, or is otherwise unsuitable, the conventional method to restore the optic often entails repolishing the optic surface, which can incur a large cost and long lead time. We propose three alternative options to repolishing, including (i) burying the unsuitable coating under another optical coating, (ii) using ion milling to etch the unsuitable coating completely from the optic surface and then recoating the optic, and (iii) using ion milling to etch through a number of unsuitable layers, leaving the rest of the coating intact, and then recoating the layers that were etched. Repairs were made on test optics with dielectric mirror coatings according to the above three options. The mirror coatings to be repaired were quarter wave stacks of HfO 2 and SiO 2 layers for high reflection at 1054 nm at 45 deg incidence in P-polarization. One of the coating layers was purposely deposited incorrectly as Hf metal instead of HfO2 to evaluate the ability of each repair method to restore the coating’s high laser-induced damage threshold (LIDT) of 64.0 J/cm 2 . The repaired coating with the highest resistance to laser-induced damage was achieved using repair method (ii) with an LIDT of 49.0 to 61.0 J/cm 2 .

36 MATERIALS SCIENCE↗

Fabrication of a terahertz quantum-cascade laser with a double metal waveguide based on multilayer GaAs/AlGaAs heterostructures

The Postgrowth processing of GaAs/AlGaAs multilayer heterostructures for terahertz quantumcascade lasers (QCLs) are studied. This procedure includes the thermocompression bonding of In–Au multilayer heterostructures with a doped n{sup +}-GaAs substrate, mechanical grinding, and selective wet etching of the substrate, and dry etching of QCL ridge mesastripes through a Ti/Au metallization mask 50 and 100 μm wide. Reactive-ion-etching modes with an inductively coupled plasma source in a BCl{sub 3}/Ar gas mixture are selected to obtain vertical walls of the QCL ridge mesastripes with minimum Ti/Au mask sputtering.

36 MATERIALS SCIENCE↗

Investigation of Bearing Axial Cracking: Benchtop and Full-Scale Test Results

The most common failure mode in wind turbine gearboxes is axial cracking in intermediate and high-speed-stage bearings, also commonly called white-etching cracks (WECs). Although these types of cracks have been reported for over a decade, the conditions leading to WECs, the process by which this failure culminates, and the reasons for their apparent prevalence in wind turbine gearboxes are all highly debated. This paper summarizes the state of a multipronged research effort to examine the causes of WECs in wind turbine gearbox bearings. Recent efforts have recreated WECs on a benchtop test rig in highly loaded sliding conditions, wherein it was found that the formation of a dark etching microstructure precedes the formation of a crack, and a crack precedes the formation of white-etching microstructure. A cumulative frictional sliding energy criterion has been postulated to predict the presence of WECs. Bearing loads have also been measured and predicted in steady state and transient drivetrain operations in dynamometer testing. In addition, both loads and sliding at full scale will be measured in planned uptower drivetrain testing. If the cumulative frictional sliding energy is the dominant mechanism that causes WECs, understanding the amount of frictional sliding energy that wind turbine bearings are subjected to in typical operations is the next step in the investigation. If highly loaded sliding conditions are found uptower, similar to the examined benchtop levels, appropriate mitigation solutions can be examined, ranging from new bearing coatings and improved lubricants to changes in gearbox designs and turbine operations.

17 WIND ENERGY↗

Rethinking surface reactions in nanoscale dry processes toward atomic precision and beyond: a physics and chemistry perspective

In this review, we discuss the progress of emerging dry processes with atomic precision. Researchers in the field of plasma processing and surface science have addressed the increasingly challenging demands of material selectivity by utilization of synergistic enhancement of etching or deposition. The discussion encompasses major challenges in the plasma science and technology community. Here, the focus of the review is advances in atomic layer etching and area-selective deposition with activation or deactivation, especially in terms of materials scaling and variety. Control of high-aspect-ratio feature fabrication in semiconductor manufacturing and etched shapes of interior features at the nanoscale are needed. Issues related to profile distortion have received much attention. State-of-the-art techniques used in semiconductor manufacturing are reviewed and future challenges are outlined.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Compact Submillimeter-Wave Receivers Made with Semiconductor Nano-Fabrication Technologies

Advanced semiconductor nanofabrication techniques are utilized to design, fabricate and demonstrate a super-compact, low-mass (<10 grams) submillimeter-wave heterodyne front-end. RF elements such as waveguides and channels are fabricated in a silicon wafer substrate using deep-reactive ion etching (DRIE). Etched patterns with sidewalls angles controlled with 1 deg precision are reported, while maintaining a surface roughness of better than 20 nm rms for the etched structures. This approach is being developed to build compact 2-D imaging arrays in the THz frequency range.

Silicon micromachining↗

Black-silicon as a Wideband Infrared Absorber for the Space Instruments: Fabrication, Modeling, and Characterization

The uniform black silicon (BSI) cryogenically etched has been demonstrated as a superior absorber in par with other ultra-absorbers such as carbon nano tubes in the visible and near-infrared spectrum. In this work, we discuss the fabrication, modeling, and characterization of the BSI aiming at the 2.5-5 microns range. We investigated a series of cryogenic parameters such as temperature, pressure, oxygen flowrate, power, and etching duration and fabricated a series of uniformly etched wafers. Additionally, we established at hree-dimensional mathematical model of a unit cell and manipulated the silicon needle geometry and shape. Our preliminary fabrication results show silicon needles of 8 micron height have five orders of magnitude specular reflectance in the infrared region. The modeling efforts how longer pillar heights could be better absorbers as the wavelength increases.

Wideband absorber↗

Advancing Core Safety of Gen IV and Gen IV + Reactors by Encompassing High-Temperature Resistant Materials - 18673

The paper focuses on the development of materials for Gen IV/IV+ reactor core. It discusses the advancement of materials studied and their application in different components of the reactor core and other auxiliary components which will help in the development of future generation reactors. The paper summarizes the material study showing the characteristic behavior of different materials (coated with FeB and FeB{sub 2}), towards irradiation at near high temperatures and high energy neutron flux condition. The project includes different materials which are coated on the boundaries with varied thickness of FeB and FeB{sub 2}. The samples included Carbon steel, Stainless steel 310, Stainless steel 316, Inconel 718. All above-mentioned samples were received by Prof. J. Szpunar, through an industry with coatings of FeB and FeB{sub 2} with varied thickness along with a bare sample of each material. The samples were irradiated at the University of Saskatchewan reactor, with fast neutron flux of 1.1x10{sup 11} n.cm{sup -2}.sec{sup -1}. I worked on all the samples but the paper particularly focuses on, two carbon steel samples results, received so far. The methodology for the project been followed for all the samples is as follow: 1. Received samples were first polished. 2. Vickers Hardness Test. 3. Mirror polished. 4. Etched with the appropriate etchant for the material. 5. Microscopic study of the etched surface. 6. SEM imaging. 7. Sent for irradiation. 8. The same set of material testing done after irradiation, with an EBSD run on the boundary and main surface. The two Carbon Steel samples (sample 21 and 19) analyzed, were irradiated for 14 hrs. Sample 21 was a bare sample and sample 19 had a coating of FeB, FeB{sub 2} with a ∼0.0010'' thickness. The methodology was followed for material testing before and after the irradiation. The advantage of FeB and FeB{sub 2} coatings are: 1. Higher hardness - 10 times (FeB-1775 and FeB{sub 2}-1450), 2. High-stress capacity, 3. Lower abrasion, 4. Low corrosion. Through the test results obtained before and after the irradiation, I was able to get a view of coating damage at the boundaries of sample 19. The bare sample don't show any difference after irradiation but the coated sample do show cracks in the FeB layer. Which can be seen in the SEM images of sample 19. The hardness results are promising, as hardness didn't change significantly. The hardness test was done on the substrate as the coating was significantly narrow to perform the test. Though the hardness test on coatings was performed by the possessor company which show hardness higher by a factor of 10 when compared to uncoated surfaces. The XRD results, reveal irradiation effect on the crystal lattice, making it deformed, which though is usual during irradiation. The overall analysis along with EBSD done on the two samples are favorable and promising. Though it still needs to be cleared out, whether the cracks on the coating were due to irradiation or due to etching after the samples were irradiated.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

A Reactive Inkjet Printing Process for Fabricating Biodegradable Conductive Zinc Structures

A novel reactive inkjet printing (RIJ) process for fabricating environmentally benign, conductive zinc structures on biodegradable substrates is reported. A precursor consisting of oxidized zinc microparticles is formulated into a viscous ink for high‐resolution, high‐repeatability screen printing. A single RIJ process is performed to selectively dispense an acid‐based oxide etching agent onto the screen‐printed zinc ink to significantly improve its electrical conductivity, up to 4 × 10 4 S m −1 . The RIJ process enables precise control of the amount of deposited etching agent, allowing control of conductivity and avoiding damage caused by excessive acid exposure. The RIJ process deposits the etching agent selectively on the screen‐printed, water‐soluble zinc patterns, thus preserving the print fidelity by avoiding ink smearing that can occur when using a blanket treatment such as submersion. A printed biodegradable antenna with a minimum feature size of 500 μm for use with a batteryless radio frequency identification (RFID) chip is fabricated as demonstration. Due to the higher ink conductivity and improved pattern fidelity, the antenna fabricated by the RIJ process shows a ≈2.2× increase in reading distance compared with a similar antenna that is screen printed and activated using a drop‐casting process.

Sui, Yongkun↗

Birefringent Glass‐Engraved Quasi‐Linear Nanograting Metasurface Based on Self‐Organizing Process for Large Aperture High Power Laser Applications

All-glass metasurface “nanograting” structures that exhibit birefringence in the formed layer are reported. The key enabler of this work is ion beam processing at an angle sufficiently off-normal incidence, inducing self-assembly of a deposited metal layer into quasi-linear metallic features that can function as an etching mask. As a result, a fused silica metasurface, monolithic to the underlying substrate, is demonstrated at 375 nm wavelength to exhibit a phase delay angle of 30° between the principal axes. The capability of an angled etch mask replenishment process is also demonstrated for achieving deeper etch depth and for increasing the grating period, another first – to the best of the knowledge. This is the first display of a technology capable of fabricating glass-engraved near-linear grating structure with a feature-to-feature period as small as 118.6 nm. Furthermore, this technology has the potential to generate grating-like structures with periods as small as 12.4 nm, as demonstrated here with reactive ion beam processing assisted mask assembly. Furthermore, these structures are shown to have reflectivity < 0.4% across the wavelength band 350 nm – 1000 nm. Such a technology can enable laser-durable grating structures for the deep-UV and even down to soft X-ray wavelengths.

Ray, Nathan J. [Lawrence Livermore National Labora↗

Copper Tantalate by a Sodium-Driven Flux-Mediated Synthesis for Photoelectrochemical CO 2 Reduction

Copper-tantalate, Cu 2 Ta 4 O 11 (CTO), shows significant promise as an efficient photocathode for multi-carbon compounds (C 2+ ) production through photoelectrochemical (PEC) CO 2 reduction, owing to its suitable energy bands and catalytic surface. However, synthesizing CTO poses a significant challenge due to its metastable nature and thermal instability. In this study, this challenge is addressed by employing a flux-mediated synthesis technique using a sodium-based flux to create sodium-doped CTO (Na-CTO) thin films, providing enhanced nucleation and stabilization for the CTO phase. To evaluate the PEC performance and catalytic properties of the films, copper(II) oxide (CuO) at the Na-CTO surface is selectively etched. The etched Na-CTO shows a lower dark current, with decreased contribution from photocorrosion, unlike the non-etched Na-CTO which has remaining CuO on the surface. Furthermore, Na-CTO exhibits 7.3-fold ethylene selectivity over hydrogen, thus highlighting its promising potential as a photocathode for C 2+ production through PEC CO 2 reduction.

copper tantalate↗

Simulation and design of a compact GaAs based tunable dual-wavelength diode laser system

We present our design of a compact, integrated and tunable dual-wavelength diode laser system emitting around 785 nm, which is of interest for several applications like Raman spectroscopy and the generation of THz radiation. To achieve a more compact device compared to previous GaAs based designs two etch depths are realized, leading to shallowly etched ridge waveguides in regions were optical gain is applied and deeply etched waveguides used to enable compact integrated waveguide components. The device parameters are optimized using a numerically efficient simulation tool for passive waveguides. Subsequently, the entire laser system is further analyzed applying a sophisticated traveling-wave equation based model for active devices giving access to internal intensity and carrier density distributions. It is shown that active laser simulations are crucial to deduce critical and performance limiting design aspects not accessible via an all-passive simulation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Operando STM study of the interaction of imidazolium-based ionic liquid with graphite

Understanding interactions at the interfaces of carbon with ionic liquids (ILs) is crucially beneficial for the diagnostics and performance improvement of electrochemical devices containing carbon as active materials or conductive additives in electrodes and ILs as solvents or additives in electrolytes. The interfacial interactions of three typical imidazolium-based ILs, 1-alkyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (AMImTFSI) ILs having ethyl (C 2 ), butyl (C 4 ) and octyl (C 8 ) chains in their cations, with highly oriented pyrolytic graphite (HOPG) were studied in-situ by electrochemical scanning tunneling microscopy (EC-STM). The etching of HOPG surface and the exfoliation of graphite/graphene flakes as well as cation intercalation were observed at the HOPG/C 2 MImTFSI interface. The etching also takes place in C 4 MImTFSI at -1.5 V vs Pt but only at step edges with a much slower rate, whereas C 8 MIm + cations adsorbs strongly on the HOPG surface under similar conditions with no observable etching or intercalation. Finally, the EC-STM observations can be explained by the increase in van der Waals interaction between the cations and the graphite surface with increasing length of alkyl chains.

25 ENERGY STORAGE↗

Growth, structure, defects and polarized absorption spectral properties of Er:Yb:YCa{sub 4}O(BO{sub 3}){sub 3} crystals

YCa{sub 4}O(BO{sub 3}){sub 3} (YCOB) crystals co-doped with 3 at% Er{sup 3+} and 20 at% Yb{sup 3+} were successfully grown by the Czochralski method. X-ray powder diffraction (XRPD) results show that the as-grown Er:Yb:YCOB crystal belongs to the monoclinic system with space group Cm. And the lattice parameters are a=8.076(8) Å, b=16.023(7) Å, c=3.528(4) Å and β=101.15(4)°. Crystal defects were revealed by chemical etching experiments. The density of etch pits, attributed to dislocations and observed on (010) planes, was found to be not uniform along the crystal diameter. The detailed polarized absorption spectra were measured. The polarized absorption cross sections at 977 nm are 1.01×10{sup −20}, 1.22×10{sup −20} and 1.05×10{sup −20} cm{sup 2} for E//X, E//Y and E//Z, respectively. And the polarized absorption cross sections at 1538 nm is about 1.86×10{sup −20} cm{sup 2} for both E//X and E//Z, but for E//Y the result is 1.03×10{sup −20} cm{sup 2}, which is much smaller. The relationship between the crystal structure and absorption spectra was discussed. - Graphical abstract: The as-grown bulk Er:Yb:YCOB crystal (the long axis is along the b-axis) and LeBail fit to the XRPD pattern of Er:Yb:YCOB (top) compared to the diffraction pattern of YCOB from the JCPDS data bank (bottom). Reflection markers indicate the calculated reflection positions. The middle trace gives the difference between observed and calculated intensity. Reflection indices corresponding to the strongest diffraction peaks are marked on the experimental pattern. - Highlights: • Er:Yb:YCOB crystal with a new composition was grown. • XRPD and FT-IR showed a certain degree of deformation in the crystal structure. • Detailed polarized absorption cross sections at 977 nm and 1538 nm were calculated. • Crystal defects were clearly revealed by chemical etching experiments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Polymer microfilters with nanostructured surfaces for the culture of circulating cancer cells

There is a critical need to improve the accuracy of drug screening and testing through the development of in vitro culture systems that more effectively mimic the in vivo environment. Surface topographical features on the nanoscale level, in short nanotopography, effect the cell growth patterns, and hence affect cell function in culture. We report the preliminary results on the fabrication, and subsequent cellular growth, of nanoscale surface topography on polymer microfilters using cell lines as a precursor to circulating tumor cells (CTCs). To create various nanoscale features on the microfilter surface, we used reactive ion etching (RIE) with and without an etching mask. An anodized aluminum oxide (AAO) membrane fabricated directly on the polymer surface served as an etching mask. Polymer filters with a variety of modified surfaces were used to compare the effects on the culture of cancer cell lines in blank culture wells, with untreated microfilters or with RIE-treated microfilters. We then report the differences of cell shape, phenotype and growth patterns of bladder and glioblastoma cancer cell lines after isolation on the various types of material modifications. Our data suggest that RIE modified polymer filters can isolate model cell lines while retaining ell viability, and that the RIE filter modification allows T24 monolayering cells to proliferate as a structured cluster. Copyright 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Makarova, Olga V.↗

Short communication: Assessment of the dislocation density using X-ray topography in Al single crystals annealed for long times near the melting temperature

Earlier work by the authors determined the dislocation density as a function of time in aluminum single crystals annealed near the melting temperature using etch-pits. It was found that the dislocation density is stable and unchanged even with annealing times up to one year for statically annealed Al single crystals with an initially low dislocation density. As several investigators have suggested that etch-pits are not reliable compared to transmission electron microscopy in assessing the dislocation density, the current study utilized x-ray topography at a synchrotron for dislocation density measurements. This work, then, is a short paper complementing the authors earlier work by using a new, reliable, but rarely utilized non-destructive technique to measure the dislocation density. The results confirm the trend of the earlier study using etch-pits by the authors.

36 MATERIALS SCIENCE↗

Growth and Stability of Titanium Dioxide Nanoclusters on Graphene/Ru(0001)

Titanium dioxide/graphene composites have recently been demonstrated to improve the photocatalytic activity of TiO2 in visible light. To better understand the interactions of TiO2 with graphene we have investigated the growth of TiO2 nanoclusters on single-layer graphene/Ru(0001) using scanning tunneling microscopy (STM) and Auger electron spectroscopy (AES). Deposition of Ti in the O2 background at 300 K resulted in the formation of nanoclusters nucleating on intrinsic defects in the graphene (Gr) layer. The saturation nanocluster density decreased as the substrate temperature was increased from 300 to 650 K, while deposition at 700 K resulted in the significant etching of the Gr layer. We have also prepared nanoclusters with Ti2O3 stoichiometry using lower O2 pressures at 650 K. Thermal stability of the TiO2 nanoclusters prepared at 300 K was evaluated with AES and STM. No change in oxidation state for the TiO2 nanoclusters or etching of the Gr layer was observed up to ~900 K. Annealing studies characterized using STM revealed that cluster ripening proceeds via a Smoluchowski mechanism below 800 K and that Ostwald ripening dominates above 800 K. At even higher temperatures, the nanoclusters undergo reduction to TiOx (x ≈ 1 - 1.5) which is accompanied by oxidation and etching of the Gr. Our studies demonstrate that highly thermally stable TiOx nanoclusters of controlled composition and morphology can be prepared on Gr supports.

Auger electron spectroscopy↗

Layer-by-Layer Thinning of PdSe 2 Flakes via Plasma Induced Oxidation and Sublimation

Controlled O2/Ar plasma exposure and subsequent low temperature inert atmosphere annealing of chemical vapor deposition (CVD) grown PdSe2 flakes etch PdSe2 layer-by-layer in an atomic layer etching-like (ALE) process. X-ray photoelectron spectroscopy (XPS) shows that exposure to a remote inductively coupled plasma (ICP) oxygen plasma oxidizes the top layer of the PdSe2 to form PdO2 and SeO2. After an in situ annealing, XPS shows no trace of PdO2 or SeO2, suggesting the byproducts are volatile at low temperature. Atomic force microscopy of PdSe2 exposed to various O2 + Ar plasmas (O2 = 25–100%) demonstrates a clear trend between the oxygen concentration and the number of layers etched per cycle. PdSe2 field effect transistors (FETs) were characterized at various stages of two ALE-like cycles, and the electrical properties are correlated to the oxidation and byproduct desorption and layer reduction.

Hoffmann, Anna↗