FURTHER DEVELOPMENT OF LARGE-AREA MICRO-CHANNEL PLATES FOR A BROAD RANGE OF COMMERCIAL APPLICATIONS
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46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
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Titanium Disulfide Coated Carbon Nanotube Hybrid Electrodes Enable High Energy Density Symmetric Pseudocapacitors
While electrochemical supercapacitors often show high power density and long operation lifetimes, they are plagued by limited energy density. Pseudocapacitive materials, in contrast, operate by fast surface redox reactions and are shown to enhance energy storage of supercapacitors. Furthermore, several reported systems exhibit high capacitance but restricted electrochemical voltage windows, usually no more than 1 V in aqueous electrolytes. Here, it is demonstrated that vertically aligned carbon nanotubes (VACNTs) with uniformly coated, pseudocapacitive titanium disulfide (TiS 2 ) composite electrodes can extend the stable working range to over 3 V to achieve a high capacitance of 195 F g -1 in an Li-rich electrolyte. A symmetric cell demonstrates an energy density of 60.9 Wh kg -1 —the highest among symmetric pseudocapacitors using metal oxides, conducting polymers, 2D transition metal carbides (MXene), and other transition metal dichalcogenides. Nanostructures prepared by an atomic layer deposition/sulfurization process facilitate ion transportation and surface reactions to result in a high power density of 1250 W kg -1 with stable operation over 10 000 cycles. In conclusion, a flexible solid-state supercapacitor prepared by transferring the TiS 2 –VACNT composite film onto Kapton tape is demonstrated to power a 2.2 V light emitting diode (LED) for 1 min.
36 MATERIALS SCIENCE↗
Effective Corrosion-Resistant Single-Atom Alloy Catalyst on HfO 2 -Passivated BiVO 4 Photoanode for Durable (≈800 h) Solar Water Oxidation
Green hydrogen (H 2 ) production from solar water splitting necessitates photoelectrodes with superior photoelectrochemical (PEC) activity and durability. However, surface defects and photocorrosion instability—especially at high potentials—limit PEC performance and stability. Herein, the prototypical bismuth vanadate (BiVO 4 ) photoanode is used to demonstrate a holistic approach to improve photocurrent density and long-term stability. In this approach, high surface-area nanostructuring of BiVO 4 is combined with barium (Ba) doping with semi-crystalline hafnium oxide (HfO 2 ) surface passivation and single-atom nickel platinum (NiPt) catalysts. The introduction of Ba 2+ ions into BiVO 4 increases the concentration of conductive V 4+ ions or the ratio of V 4+ ions to oxygen vacancies, avoiding V 5+ dissolution during water oxidation. The semi-crystalline HfO 2 , which serves as a passivation layer, prevents BiVO 4 photocorrosion by suppressing harmful chemical reactions when holes are transferred to the electrolyte. The synergistic use of isolated single-atom and Ni-Pt coordination improves charge transfer at the photoanode/electrolyte interface, leading to enhanced PEC kinetics and stability. As a result, a photoelectrode is demonstrated with ≈6.5 mA cm -2 at 1.23 V versus a reversible hydrogen electrode (RHE) and continuous operation for 800 h with a negligible degradation rate. This work provides a promising approach to improve photoanodes for PEC H 2 production.
08 HYDROGEN↗
Large Area Picosecond Photodetector (LAPPD TM ) - Pilot production and development status
Here, we discuss performance results achieved for fully functional sealed Large Area Picosecond Photodetectors (LAPPD (TM)) in tests performed at Incom Inc., as well as independent test results reported by our early adopters. The LAPPD is a microchannel plate (MCP) based large area picosecond photodetector, capable of imaging with single-photon sensitivity at high spatial and temporal resolutions in a hermetic package. The LAPPD has an active area of 350 square centimeters in an all-glass hermetic package with a fused silica window and bottom plate and sidewalls made of borosilicate float glass. Signals are generated by a bi-alkali Na 2 KSb photocathode and amplified with a stacked chevron pair of MCPs produced by applying resistive and emissive atomic layer deposition coatings to glass capillary array (GCA) substrates. Signals are collected on RF stripline anodes applied to the bottom plates which exit the detector via pin-free hermetic seals under the side walls. LAPPD test and performance results for product produced and delivered to early adopter customers during the first half of 2018 are reviewed. These results include electron gains ≥ 7.5 x 10 6 @ 850/950 V (entry/exit MCP), low dark noise rates (22 Cts/s/cm 2 ), single photoelectron (PE) timing resolution of 64 picoseconds RMS, and single photoelectron spatial resolution along and across strips of 2.8 mm and 1.3 mm RMS respectively. Many of these devices also had very high QE photocathodes that were uniform over the full 195 mm x 195 mm window active area (LAPPD #15 QE% @ 365 nm Max/Avg/Min = 25.8/22.3 ± 3/15.7). An update is additionally provided of developments that enable capacitive signal coupling from the detector to application specific pads or stripline readout patterns deployed on printed circuit boards positioned beneath the file, outside of the vacuum package. We conclude with examples of how sensors offering picosecond timing, in diverse applications can bring transformative change to detector technology and applications in future experiments.
47 OTHER INSTRUMENTATION↗
Gamma and proton irradiation effects and thermal stability of electrical characteristics of metal-oxide-silicon capacitors with atomic layer deposited Al 2 O 3 dielectric
The radiation hardness and thermal stability of the electrical characteristics of atomic layer deposited Al 2 O 3 layers to be used as passivation films for silicon radiation detectors with slim edges are investigated. To directly measure the interface charge and to evaluate its change with the ionizing dose, metal-oxide-silicon (MOS) capacitors implementing differently processed Al 2 O 3 layers were fabricated on p-type silicon substrates. Qualitatively similar results are obtained for degradation of capacitance–voltage and current–voltage characteristics under gamma and proton irradiations up to equivalent doses of 30 Mrad and 21.07 Mrad, respectively. While similar negative charge densities are initially extracted for all non-irradiated capacitors, superior radiation hardness is obtained for MOS structures with alumina layers grown with H 2 O instead of O 3 as oxidant precursor. Competing effects between radiation-induced positive charge trapping and hydrogen release from the H 2 O-grown Al 2 O 3 layers may explain their higher radiation resistance. Finally, irradiated and non-irradiated MOS capacitors with differently processed Al 2 O 3 layers have been subjected to thermal treatments in air at temperatures ranging between 100 °C and 200 °C and the thermal stability of their electrical characteristics has been evaluated. Partial recovery of the gamma-induced degradation has been noticed for O 3 -grown MOS structures. Lastly, this can be explained by a trapped holes emission process, for which an activation energy of 1.38 ± 0.15 eV has been extracted.
24 POWER TRANSMISSION AND DISTRIBUTION↗
Effects of oxidant gas for atomic layer deposition on crystal structure and fatigue of ferroelectric Hf x Zr 1-x O 2 thin films
TiN/Hf x Zr 1-x O 2 (HZO)/TiN capacitors were prepared using two types of HZO films fabricated by atomic layer deposition using H 2 O or O 2 plasma as an oxidant gas, and post-deposition annealing at 400 °C was performed before the TiN top-electrode fabrication. The ferroelectric orthorhombic phase was dominantly formed for the O 2 plasma-based capacitor due to the strongly oxidizing source of O 2 plasma, resulted in higher remanent polarization (2P r = 20 µC/cm 2 ) than that (13 µC/cm 2 ) of the H 2 O-based capacitor. The fatigue properties for the O 2 plasma-based capacitor were improved by 14 % after 106 cycles compared to the H 2 O-based capacitor. This could be attributed to an oxygen-rich interface reaction layer (IRL) including TiO x between the HZO film and TiN bottom-electrode for the O 2 plasma-based capacitor. In conclusion, based on these results, superior 2P r and fatigue properties can be obtained using O 2 plasma-based HZO films.
36 MATERIALS SCIENCE↗
High thermal stability of La 2 O 3 and CeO 2 -stabilized tetragonal ZrO 2
Catalyst support materials of tetragonal ZrO 2 , stabilized by either La 2 O 3 (La 2 O 3 -ZrO 2 ) or CeO 2 (CeO 2 -ZrO 2 ), were synthesized under hydrothermal conditions at 200 °C with NH 4 OH or tetramethylammonium hydroxide as the mineralizer. From In Situ synchrotron powder X-ray diffraction and small-angle X-ray scattering measurements, the calcined La 2 O 3 -ZrO 2 and CeO 2 -ZrO 2 supports were nonporous nanocrystallites that exhibited rectangular shapes with thermal stability up to 1000 °C in air. These supports had an average size of ~10 nm and a surface area of 59-97 m 2 /g. The catalysts Pt/La 2 O 3 -ZrO 2 and Pt/CeO 2 -ZrO 2 were prepared by using atomic layer deposition with varying Pt loadings from 6.3-12.4 wt %. Mono-dispersed Pt nanoparticles of ~3 nm were obtained for these catalysts. As a result, the incorporation of La 2 O 3 and CeO 2 into the t-ZrO 2 structure did not affect the nature of the active sites for the Pt/ZrO 2 catalysts for the water-gas-shift (WGS) reaction.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Internal Photoemission Spectroscopy Measurements of Interfacial Energy Barriers in Operating TaN/Hf 0.5 Zr 0.5 O 2 /TaN Metal/Ferroelectric/Metal (MFM) Devices
The effect of the "waking" and subsequent "poling" operations on the electron barriers at both top and bottom electrode interfaces in operating ferroelectric hafnium zirconium oxide (Hf 0.5 Zr 0.5 O 2 , HZO) metal/ferroelectric/metal (MFM) devices are measured for the first time via internal photoemission (IPE) spectroscopy. Top and bottom (TaN/HZO and HZO/TaN) barriers for pristine devices were measured at 2.6 eV and 2.9 eV, respectively. The waking operation (10 kHz bipolar voltage cycling above the coercive field) increased the top barrier to 2.8 eV while leaving the bottom barrier essentially unchanged. Poling operations (application of a longer 10 msec unipolar pulse) were found to significantly decrease both top and bottom barriers. Here, the poling direction (polarity) had relatively little impact. The barrier for the top interface under positive (P↓) and negative poling (P↑) was 2.1 and 2.2 eV, respectively, while the bottom barrier was 2.3 eV for P↓ and 2.4 eV for P↑. All barrier heights remained unchanged after several months at room temperature. Potential physical mechanisms responsible for the changes observed under electrical operation are consistent with movement and/or creation of charged oxygen vacancy defects.
36 MATERIALS SCIENCE↗
Trimethylaluminum and Oxygen Atomic Layer Deposition on Hydroxyl-Free Cu(111)
Not Available
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Active Site and Electronic Structure Elucidation of Pt Nanoparticles Supported on Phase-Pure Molybdenum Carbide Nanotubes
Here, we recently showed that phase-pure molybdenum carbide nanotubes can be durable supports for platinum (Pt) nanoparticles in hydrogen evolution reaction (HER). In this paper we further characterize surface properties of the same Pt/β-Mo 2 C catalyst platform using carbon monoxide (CO)-Pt and CO-Mo 2 C bond strength of different Pt particle sizes in the <3 nm range. Results from diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and temporal analysis of products (TAP) revealed the existence of different active sites as Pt particle size increases. Correlation between the resultant catalyst activity and deposited Pt particle size was further investigated using water–gas-shift (WGS) as a probe reaction, suggesting that precise control of particle diameter and thickness is needed for optimized catalytic activity.
36 MATERIALS SCIENCE↗
Palladium-Coated Platinum Powders with Tunable, Nanostructured Surfaces for Applications in Catalysis
Simultaneous control of nanoscale surface morphology and composition remains a challenge in preparing bimetallic catalysts, particularly at the large scale required for industrial application and with high-surface-area substrates. Atomic layer electroless deposition (ALED) is a scalable approach to prepare surface-modified metal powders in which elements more noble than the surface hydrides of the substrate metal are deposited layer-by-layer in a surface-limited fashion. In this paper, we demonstrate that high-surface-area Pt powder is a viable substrate for controlled deposition of Pd adlayers using this technique, with the potential for large-scale preparation, for use in electrocatalytic and catalytic applications such as fuel cells and functionalization of petrochemical feedstocks. Two different growth mechanisms have been proposed based on bulk and surface Pd atomic fractions obtained from atomic absorption spectroscopy and X-ray photoelectron spectroscopy, respectively. Further, spectral simulations were performed to strengthen the proposed growth mechanisms, favoring conformal growth in initial deposition followed by island formation in subsequent cycles. Observation of multiple pathways suggests a means of controlling adlayer surface morphology of ALED materials, in which an initial cycle of deposition sets the fractional coverage and subsequent cycles tune adlayer thickness.
36 MATERIALS SCIENCE↗
“Intelligent” Pt Catalysts Studied on High-Surface-Area CaTiO 3 Films
CaTiO 3 -supported Pt is sometimes referred to as an “Intelligent” catalyst because Pt can reversibly leave or enter the perovskite lattice following high-temperature reduction or oxidation; however, slow egress-ingress kinetics associated with large perovskite crystallites make these systems impractical. In this study, thin films (~1 nm) of CaTiO 3 were deposited onto MgAl 2 O 4 and then examined as catalyst supports for Pt and Pd. While Pd/CaTiO 3 /MgAl 2 O 4 showed adsorption and CO-oxidation properties that were essentially the same as Pd/MgAl 2 O 4 , the Pt/CaTiO 3 /MgAl 2 O 4 catalyst exhibited evidence for strong support interactions. Pt/CaTiO 3 /MgAl 2 O 4 showed high activity for CO oxidation following reduction at 1073 K, even though CO adsorption was suppressed; but the catalysts were dramatically less active after oxidation at 1073 K and reduction at 773 K. Both Pt/CaTiO 3 /MgAl 2 O 4 and a catalyst formed by ex-solution of CaTi 0.95 Pt 0.05 O 3 exhibited very low rates for toluene hydrogenation in comparison to Pt/MgAl 2 O 4 . Scanning Transmission Electron Microscopy (STEM) and Energy Dispersive Spectroscopy (EDS) showed that the CaTiO 3 films uniformly covered the MgAl 2 O 4 surface after both reduction and oxidation at 1073 K. Pt particles on reduced Pt/CaTiO 3 /MgAl 2 O 4 exhibited an unusual rhombohedral shape and may be flat, a further indication of strong interactions between the metal and the support. Low Energy Ion Scattering (LEIS) indicated that high-temperature reduction caused a restructuring of the CaTiO 3 . Lastly, the implications of these results for understanding catalysts formed by ex-solution of metals from a perovskite lattice are discussed.
36 MATERIALS SCIENCE↗
Coherent X-ray Spectroscopy Elucidates Nanoscale Dynamics of Plasma-Enhanced Thin-Film Growth
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36 MATERIALS SCIENCE↗
Catalyst Design with Atomic Layer Deposition
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bio-inspired↗
Ligand Locking on Quantum Dot Surfaces via a Mild Reactive Surface Treatment
At the outermost surface of colloidal QDs are organic surface ligands which dynamically bind and release in solution to control the growth kinetics, control the size/shape of the crystals, passivate surface states, and provide colloidal stability through favorable interactions with the solvent. However, the dynamicity comes at the expense of the stability of the QD suspension. Here, we show that ligands can be permanently locked on the QD surface by a thin layer of an inert metal oxide which forms within the ligand shell, over the headgroup. By interrogating the surface chemistry with different spectroscopic methods, we prove the ligand locking on the QD surface. As a result, an exceptional stability of the coated QD inks is achieved in a wide concentration range, even in the presence of chemically competing surface ligands in solution. We anticipate that this critical breakthrough will benefit different areas related to colloidal QDs, spanning from single-particle studies to displays and solar cells and biological applications. Furthermore, the same chemistry could be easily translated to surface treatments of bulk materials and thin films.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Effect of thermal annealing and chemical treatments on secondary electron emission properties of atomic layer deposited MgO
This study reports on the secondary electron emission (SEE) performance of atomic layer deposited MgO films, with thicknesses in the range from 5 to 25 nm, for the application in the Timed Photon Counter. In this novel, photodetector MgO is utilized as a material for the fabrication of ultrathin transmission dynodes (tynodes). Two different types of PECVD silicon oxide films are applied on top of MgO, in order to protect it against etching steps in the fabrication of tynodes and also as a prevention against aging. Applicability of these two materials as capping films is evaluated in terms of achieved secondary electron yield (SEY) of MgO after their removal. Emission of secondary electrons is known to depend on numerous physical and chemical properties of the material, such as surface roughness and chemical composition. On that account, morphological and structural properties of modified MgO are determined by atomic force microscope and x-ray photoelectron spectrometer and linked to the changes in SEE behavior. The authors demonstrate that the application of a suitable capping layer followed by its removal provides an SEY of 6.6, as opposed to the value of 4.8 recorded from the as-deposited MgO film. Furthermore, in a following experiment, they showed that annealing of MgO films at high temperatures (up to 1100 °C) significantly improved the secondary electron emission, elevating the SEY to 7.2.
ALD↗