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At least 595 records · Page 33
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Optimization of Extended-Surface PtNi Nanowire Oxygen Reduction Electrocatalysts Produced via Atomic Layer Deposition

Polymer electrolyte membrane fuel cells (PEMFCs) produce electricity with only heat and water as byproducts, but sluggish kinetics of the oxygen reduction reaction (ORR) at the cathode and durability limitations restrict widespread commercialization, motivating the development of advanced catalysts. In this research, extended-surface platinum nickel (PtNi) nanowires (NWs) synthesized using the scalable atomic layer deposition (ALD) technique are investigated with the goal of exploring the durability benefits of high-aspect-ratio electrocatalysts and the tunability of beneficial kinetic properties. The surface and bulk composition and the structure of the PtNi NWs were investigated as a function of a series of postsynthesis modifications. The results from a combination of electron microscopy and X-ray spectroscopy characterization techniques were correlated to electrochemical performance to gain a comprehensive understanding of the structure-property-performance relationships. The robust structure of the ALD-derived NWs enabled additional postsynthesis optimization steps, which were not possible with previous-generation materials synthesized via spontaneous galvanic displacement, resulting in a catalyst with beneficial properties for catalyst kinetics as well as improved durability. Our study demonstrates potential pathways toward further improving the performance of this class of materials through optimization of bulk and surface properties of the catalyst.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2022

Assessment of Protective Coatings for Metal-Supported Solid Oxide Electrolysis Cells

Green hydrogen is essential to achieving carbon neutrality, and solid oxide electrolysis cells can produce hydrogen using renewable power and waste heat. Insufficient long-term durability of solid oxide electrolysis cells has impeded their commercialization. Here, coatings in the porous stainless steel support of metal-supported solid oxide electrolysis cells (MS-SOECs) are used to dramatically improve their performance and durability. The long-term degradation rate of uncoated MS-SOECs is highly dependent on the current density, with the fastest degradation occurring at the highest current density tested, 0.5 A cm -2 . At this current density, coatings are quite effective. Three protective coatings, Co 3 O 4 deposited by atomic layer deposition (ALD), Co 3 O 4 deposited by electroplating deposition (ED), and CuMn 1.8 O 4 (CMO) deposited by electrophoretic deposition (EPD), are explored to enhance the performance of MS-SOECs with La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 -Sm 0.2 Ce 0.8 O 3 (LSCF-SDC) as the oxygen catalyst and SDC-Ni as the fuel catalyst. The initial average current density at 1.4 V is increased with coatings. It is 0.83 mA cm -2 for the ALD cells, 1.05 mA cm -2 for the ED cells, and 1.13 mA cm -2 for the EPD cells, compared to 0.65 mA cm -2 for the bare cells at 700 °C with 50% H 2 -50% H 2 O. The degradation rate over 1000 h of continuous operation is reduced from 36% to 26%, 27%, and 19% kh -1 with the three coatings, respectively. Furthermore, these improvements are ascribed to reduced Cr poisoning on the oxygen catalyst, which is one of the primary degradation modes for this type of MS-SOEC.

25 ENERGY STORAGE↗
DOE OSTI2020

Synthesis and Crystallization of Atomic Layer Deposition β-Eucryptite LiAlSiO 4 Thin-Film Solid Electrolytes

Atomic layer deposition (ALD) was used to control the stoichiometry of thin lithium aluminosilicate films, thereby enabling crystallization into the ion-conducting β-eucryptite LiAlSiO 4 phase. Here, the rapid thermal annealed ALD film developed a well-defined epitaxial relationship to the silicon substrate: β-LiAlSiO4 ($1\bar{21}0$)||Si (100) and β-LiAlSiO 4 ($10\bar{10}$)||Si (001). The extrapolated room temperature ionic conductivity was found to be 1.2 × 10 –7 S/cm in the [$1\bar{21}0$] direction. Because of the unique 1-D channel along the c axis of β-LiAlSiO 4 , the epitaxial thin film has the potential to facilitate ionic transport if oriented with the c axis normal to the electrode surface, making it a promising electrolyte material for three-dimensional lithium-ion microbatteries.

25 ENERGY STORAGE↗
DOE OSTI2022

Tunable Solid Acid Catalyst Thin Films Prepared by Atomic Layer Deposition

Solid acid catalysts, including zeolites and amorphous silica-aluminas (ASAs), are industrially important materials widely used in the fuel and petrochemical industries. The versatility of zeolites is due to the Brønsted acidity of the bridging hydroxyl and shape selectivity that can be tailored during and after synthesis. This is in contrast to amorphous silica-alumina, where tailoring acidity is a major challenge as the Brønsted acid structure in ASA is still debated. In both cases, however, the pore size and acidity cannot be tuned independently, and this is particularly limiting in the application of biomass conversion, where zeolite pores are too small for the molecules of interest. Herein, we present a method using atomic layer deposition (ALD) to prepare thin films of solid acid materials where the ratio of Brønsted to Lewis acid sites can be tuned precisely. This capability, combined with the sub-nm pore size control afforded by ALD yields a powerful and flexible method for synthesizing solid acid catalysts inside virtually any mesoporous host. We demonstrate the utility of these materials in two acid-catalyzed reactions relevant to biomass conversion: (1) Meerwein–Ponndorf–Verley–Oppenauer (MPVO) reaction and dehydration of fructose and (2) cascade reaction of glucose to 5-hydroxymethylfurfural. Finally, we propose a plausible structure for the Brønsted acid sites in our materials based on infrared spectroscopy and solid-state nuclear magnetic resonance measurements and density functional theory calculations and argue that this same structure might apply to conventional ASAs as well.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

The Influence of Structure and Processing on the Behavior of TiO 2 Protective Layers for Stabilization of n-Si/TiO 2 /Ni Photoanodes for Water Oxidation

Light absorbers with moderate band gaps (1–2 eV) are required for high-efficiency solar fuels devices, but most semiconducting photoanodes undergo photocorrosion or passivation in aqueous solution. Amorphous TiO 2 deposited by atomic-layer deposition (ALD) onto various n-type emiconductors (Si,GaAs, GaP, and CdTe) and coated with thin films or islands of Ni produces efficient, stable photoanodes for water oxidation, with the TiO 2 films protecting the underlying semiconductor from photocorrosion in pH = 14 KOH(aq). The links between the electronic properties of the TiO 2 in these electrodes and the structure and energetic defect states of the material are not yet well-elucidated. We show herein that TiO 2 films with a variety of crystal structures and mid-gap defect state distributions, deposited using both ALD and sputtering, form rectifying junctions with n-Si and are highly conductive towards photogenerated carriers in n-Si/TiO 2 /Ni photoanodes. Moreover, the photovoltage of these electrodes can be modified by annealing the TiO 2 in reducing or oxidizing environments. All of the polycrystalline TiO 2 films with compact grain boundaries investigated herein protected the n-Si photoanodes against photocorrosion in pH = 14 KOH(aq). Hence, in these devices conduction through the TiO 2 layer is neither specific to a particular amorphous or crystalline structure nor determined wholly by a particular extrinsic dopant impurity. The coupled structural and energetic properties of TiO 2 , and potentially other protective oxides, can therefore be controlled to yield optimized photoelectrode performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Atomic Layer Deposition of MnS: Phase Control and Electrochemical Applications

Manganese sulfide (MnS) thin films were synthesized via atomic layer deposition (ALD) using gaseous manganese bis(ethylcyclopentadienyl) and hydrogen sulfide as precursors. At deposition temperatures ≤150 °C phase-pure r-MnS thin films were deposited, while at temperatures >150 °C, a mixed phase, consisting of both r- and a-MnS resulted. In situ quartz crystal microbalance (QCM) studies validate the self-limiting behavior of both ALD half-reactions and, combined with quadrupole mass spectrometry (QMS) allow the derivation of a self-consistent reaction mechanism. Lastly, MnS thin films were deposited on copper foil and tested as a Li-ion battery anode. The MnS coin cells showed exceptional cycle stability and near-theoretical capacity.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Atomic-Scale Behavior of Radiation-Resistant ZnO under High-Energy Electron Bombardment

Understanding the atomic structure and defect characteristics of ZnO thin films is crucial for optimizing their electronic properties and performance in advanced applications. Here, we investigate the atomic structure and defect characteristics of atomic layer deposition (ALD)-grown ZnO thin films by using aberration-corrected scanning transmission electron microscopy (STEM). Atomic-resolution imaging identifies prevalent stacking faults, dipole disorder, and various grain boundary types, which are believed to influence the electronic properties of ZnO. Additionally, real-time electron beam exposure experiments demonstrate structural transformations, including crystal growth and surface rearrangements. These findings provide insights into the growth mechanisms of ALD ZnO under high-energy electron irradiation conditions, an important finding for the use of polycrystalline ZnO wide bandgap semiconductors in space-like conditions. In conclusion, our results underscore the capability of STEM in directly visualizing and quantifying atomic-scale defects and beam-induced transformations in radiation-resistant ZnO.

Defects↗
DOE OSTI2026

Mitigating electrochemical degradation in CsPbBr{sub 3} gamma detectors by organic and inorganic encapsulation.

CsPbBr3 perovskite semiconductors have emerged as a leading candidate for nextgeneration radiation detectors because of their exceptional charge transport properties, defect tolerance, and record-breaking sensitivity and energy resolution. Their long-term stability, however, is hindered by electrode-driven electrochemical decomposition, which is accelerated by moisture- and oxygen-assisted ion migration during operation. Here, we investigated organic and inorganic encapsulation strategies as both environmental barriers and means to suppress interfacial degradation pathways. Atomic layer deposition (ALD) of Al2O3 provided a conformal passivation layer that blocked environmental ingress, suppressed ionic diffusion, reduced leakage current, enhanced energy resolution and expanded the operational electric-field window beyond 5 kV∙cm1 . By contrast, organic encapsulants such as paraffin wax and polystyrene slowed moisture diffusion but did not suppress interfacial reactions, with wax extending stability to over 90 days. These results show that ALD-Al2O3 suppresses dominant interfacial degradation pathways, enabling stable, high-field operation and advancing the practical deployment of CsPbBr3 γ-ray detectors.

Unal, Mustafa↗
DOE OSTI2018

Interface engineering of colloidal CdSe quantum dots thin films as acid-stable photocathodes for solar-driven hydrogen evolution

Colloidal semiconductor quantum dots-based (CQD) photocathodes for solar-driven hydrogen evolution have attracted significant attention due to their tunable size, nanostructured morphology, crystalline orientation, and band-gap. Here, we report a thin film heterojunction photocathode composed of organic PEDOT:PSS as a hole transport layer, CdSe CQDs as a semiconductor light absorber, and conformal Pt layer deposited by atomic layer deposition (ALD) serving as both a passivation layer and cocatalyst for hydrogen evolution. In neutral aqueous solution, a PEDOT:PSS/CdSe/Pt heterogeneous photocathode with 200 cycles of ALD Pt produces a photocurrent density of -1.08 mA/cm 2 (AM1.5G, 100 mW/cm 2 ) at a potential of 0 V vs. RHE (j 0 ) in neutral aqueous solution, which is nearly 12 times that of the pristine CdSe photocathode. This composite photocathode shows an onset potential for water reduction at +0.46 V vs. RHE and long-term stability with negligible degradation. In acidic electrolyte (pH = 1), where the hydrogen evolution reaction is more favorable but stability is limited due to photocorrosion, a thicker Pt film (300 cycles) is shown to greatly improve the device stability and a j 0 of -2.14 mA/cm 2 is obtained with only 8.3% activity degradation after 6 h, compared to 80% degradation under the same conditions when the less conformal electrodeposition method is used to deposit the Pt layer. Electrochemical impedance spectroscopy and time-resolved photoluminescence results indicate that these enhancements stem from a lower bulk charge recombination rate, higher interfacial charge transfer rate, and faster reaction kinetics. In conclusion, we believe that these interface engineering strategies can be extended to other colloidal semiconductors to construct more efficient and stable heterogeneous photoelectrodes for solar fuel production.

42 ENGINEERING↗
DOE OSTI2019

Interfacial Engineering for High Efficiency Nanorod Array Structured Perovskite Solar Cells

TiO 2 nanorod (NR) array for perovskite solar cells (PSCs) has attached great importance due to superb power conversion efficiency (PCE) compared to traditional mesoporous TiO 2 film. A TiO 2 compact layer for the growth of TiO 2 NR array via spin-coating cannot meet the requirements for efficient NR based PSCs. Herein we have developed and demonstrated inserting an bifunctional extra-thin TiO 2 interlayer (5 nm) by atomic layer deposition (ALD) at the interface of FTO/TiO 2 compact layer to achieve an alleviated electron exchange and a reduced energetic barrier. Thus, an accelerated extraction of electrons from TiO 2 NR arrays via the compact layer to FTO substrate is ready for improving the PSC efficiency. The thickness of the spin-coated TiO 2 compact layer on the ALD-deposited TiO 2 layer is spontaneously optimized. Finally, an outstanding efficiency of 20.28% has been achieved from a champion PSC with negligible hysteresis and high reliability. To the best of our knowledge, this is the first time to demonstrate the superiority of TiO 2 -NR based PSCs withstanding in dry heat and thermal cycling tests. The results are of great importance for the preparation of efficient and durable PSCs for our real-world applications.

25 ENERGY STORAGE↗
DOE OSTI2021

4D Imaging of ZnO-Coated Nanoporous Al 2 O 3 Aerogels by Chemically Sensitive Ptychographic Tomography: Implications for Designer Catalysts

The 3D chemical structure (4D spectromicroscopy) of nanoporous Al 2 O 3 aerogels coated with ZnO by atomic layer deposition (ALD) was studied by multienergy scanning transmission X-ray microscopy. These materials are representative of a class of designer catalysts in which the nanoporous support is prepared separately from the active catalyst material, which is subsequently introduced by ALD, thereby allowing independent optimization of the morphology, chemistry, and spatial distribution of the support and catalyst. The samples studied were prepared by Ga ion and Xe plasma focused ion beam (FIB) milling as well as drop casting from water suspension. Zn L and Al K edge spectra of six samples with three different ZnO loadings were measured to investigate how loading and different sample preparation methods affect the 3D distribution of the ZnO and Al 2 O 3 . Scanning transmission X-ray microscopy (STXM) and ptychographic imaging at two energies each at the Zn L 3 and Al K edge were measured. The ptychography data were analyzed by using the SHARP reconstruction code to generate quantitative 2D chemical maps of the Al 2 O 3 and the ZnO. The STXM and ptychography maps were then measured at a sequence of tilt angles, covering up to 160° of rotation. The 3D structure of the ZnO and Al 2 O 3 was derived from the tilt series data by tomographic reconstruction using a compressed sensing algorithm. A twodimensional spatial resolution (half-period) of 6 nm, measured by Fourier ring correlation, and a 3D spatial resolution (half-period) of 9 nm, measured by Fourier shell correlation, were achieved when using the COSMIC beamline at the Advanced Light Source (ALS). The results show that for all of the ZnO loadings studied there is nonuniform coverage of the ZnO on the Al 2 O 3 aerogel framework. In addition, we found that both FIB methods create sample artifacts, although the distortion was less with Xe plasma than Ga ion FIB.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Chemical Passivation of Crystalline Si by Al 2 O 3 Deposited Using Atomic Layer Deposition: Implications for Solar Cells

The atomistic-level mechanism for the chemical passivation of the monocrystalline Si (c-Si) surface with thermally annealed Al 2 O 3 was studied using in situ infrared spectroscopy and photoconductance decay measurements. Al 2 O 3 was deposited on high-lifetime, float-zone c-Si substrates using atomic layer deposition (ALD) from trimethylaluminum (TMA), and H 2 O or O 3 . Surface-sensitive attenuated total reflection Fourier transform infrared spectroscopy was used to monitor the c-Si/Al 2 O 3 interface, as well as the bulk of the Al 2 O 3 film during the entire process. Our results show that some surface Si–H bonds are preserved after the ALD of Al 2 O 3 on H-terminated Si. During the annealing step at 400 °C, restructuring occurs at the c-Si/Al 2 O 3 interface to form interfacial SiO x . Isotope labeling was used to differentiate interfacial SiD bonds on the c-Si surface from H incorporated in Al 2 O 3 . Within the sensitivity of our infrared setup (~10 13 cm –2 ), we did not observe any net migration of atomic H or D from Al 2 O 3 to the c-Si/Al 2 O 3 interface. To isolate the effects of chemical and field-effect passivation of Al 2 O 3 thin films, we carried out surface passivation studies on c-Si/SiO 2 /Al 2 O 3 stacks. We also annealed these stacks in different atmospheres to test the influence of annealing atmospheres on the chemical passivation of c-Si by Al 2 O 3 and observed that O 2 -containing atmosphere led to the best surface chemical passivation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Structural Evolution of Molybdenum Disulfide Prepared by Atomic Layer Deposition for Realization of Large Scale Films in Microelectronic Applications

Molybdenum disulfide (MoS 2 ) films are attractive materials for electronic and optoelectronic devices, but the temperatures used in the chemical vapor deposition (CVD) of these materials are too high for device integration. Recently, a low-temperature atomic layer deposition (ALD) process was demonstrated for growth of MoS 2 films at 200 °C using MoF 6 and H 2 S. However, the as-deposited films were amorphous and required annealing to obtain the desired layered structure. The MoS 2 films were sulfur-deficient; however, after annealing the crystallinity improved. To study the structure of these films and the process by which they crystallize, we performed in this work X-ray absorption spectroscopy and high-energy X-ray scattering experiments on both as-deposited and annealed MoS 2 films. Analysis indicated that molybdenum atoms in the as-deposited films were well coordinated with sulfur but not well coordinated with other molybdenum atoms when compared to a crystalline reference. Further analysis revealed clusters of the sulfur-rich phase [Mo 3 S(S 6 ) 2 ] 2– , which decomposed after annealing in H 2 and H 2 S at 400 and 600 °C. When compared to the sulfur-deficient films reported previously for this ALD process, the sulfur-rich phase found here indicates that nucleation on the substrate plays an important role in the resulting film stoichiometry, which could be tuned to produce higher quality films for microelectronic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Dopamine-Mediated Polymer Coating Facilitates Area-Selective Atomic Layer Deposition

Area-selective atomic layer deposition (ALD) has the potential to significantly improve current fabrication approaches by introducing a bottom-up process in which robust and conformal thin films are selectively deposited onto patterned substrates. This bottom-up approach requires selective areas of the substrates to be masked to inhibit deposition. Spontaneous self-assembly and organization of a mask, incorporating adhesion and other functions, are particularly attractive for this role as they do not require a separate patterning step. In this work, we make use of the pH/light tunability of catechol adhesion to develop a catechol-functionalized polymer that exhibits tunable adhesion strengths on different materials based on their specific chemistry. Tunable selective deposition was shown between metal/metal oxide substrates by controlling the local pH. Moreover, by controlling the adhesion strength through UV light, the deposition of hafnium oxide (HfO 2 ) during ALD was successfully inhibited.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Metal Chalcogenide Nanofilms: Platforms for Mechanistic Studies of Electrocatalysis

The systematic development of improved electrocatalysts requires strategies for preparing candidate materials as well-defined thin-film electrodes that are amenable to straightforward characterization of reaction mechanism and catalyst specific activity. While numerous thin film preparation methods are established for transition metals and metal alloys, few strategies exist for transition metal chalcogenides, despite growing recognition of their role as potent electrocatalysts. Herein we show that electrochemical atomic layer deposition (E-ALD) is a powerful tool for accessing well-defined metal chalcogenide electrocatalysts, by synthesizing, for the first time, crystalline conformal films of Co 9 S 8 , a promising earth-abundant oxygen reduction catalyst, with tunable nanoscale thickness. The as-prepared nanofilms display relatively high activity for the oxygen reduction reaction and provide a robust platform for detailed mechanistic investigations. Initial mechanistic studies reveal that oxygen reduction on Co 9 S 8 nanofilms proceeds via rate-limiting one-electron transfer to O 2 with a specific activity of 20.6 μA cm –2 at 600 mV vs RHE. This study opens the door to the systematic application of E-ALD to investigate chalcogenide electrocatalysts across the transition series.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Suppressing Atmospheric Degradation of Sulfide-Based Solid Electrolytes via Ultrathin Metal Oxide Layers

Sulfide-based solid-state electrolytes (SSEs) are promising materials with superior Li-ion conductivity; however, their poor atmospheric stability limits commercial manufacturing at scale. Here, we investigate the impact of ultrathin metal oxide layers deposited via atomic layer deposition (ALD) on the stability of Li 6 PS 5 Cl (LPSCl). Al 2 O 3 layers grown directly on LPSCl particles significantly stabilize the surface chemistry and Li-ion transport properties relative to uncoated material upon exposure to both an ambient atmosphere (22% relative humidity, RH) and humidified O 2 (100% RH). Detailed investigations indicate that coatings impede the surface and bulk degradation kinetics of exposed materials, even for coatings as thin as ∼1 Å. Furthermore, this suggests that stabilization is due to more than just a physical barrier. Shifts in valence band edge positions of coated LPSCl indicate that ALD coatings alter the surface electronic structure and resulting oxidation tendency of underlying LPSCl, suggesting new avenues to improving the environmental stability of sulfide SSEs.

Atmospheric chemistry↗
DOE OSTI2025

Thermodynamics of MgO Atomic Layer Deposition Surface Reactions

The realities of atomic layer deposition (ALD) surface reactions often deviate from the simple ligand exchange frequently used to illustrate the technique. A detailed understanding of these reactions is necessary to develop greater surface synthetic control including chemical selectivity for patterning or to target defects. Here, the thermodynamics of surface reactions relevant to MgO ALD were investigated using pyroelectric calorimetry to measure the time-resolved heat generation. These reactions show exothermic heat generation of 0.12 mJ/cm 2 and 0.15 mJ/cm 2 for alternating Mg(CpEt) 2 and H 2 O reactions, respectively. The total reaction heat closely matches the standard reaction enthalpy for bulk MgO, supplemented with first-principles molecular calculations. First-principles models further reveal that while simple ligand exchange is favorable during surface reactions, the required increase in Mg-coordination number from two in the precursor to six in bulk MgO requires additional coverage-dependent surface reactions, which depend on the availability and stability of proximal surface hydroxyls.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Atomic Precision Processing of Two-Dimensional Materials for Next-Generation Microelectronics

The growth of the information era economy is driving the pursuit of advanced materials for microelectronics, spurred by exploration into “Beyond CMOS” and “More than Moore” paradigms. Atomically thin 2D materials, such as transition metal dichalcogenides (TMDCs), show great potential for next-generation microelectronics due to their properties and defect engineering capabilities. This perspective delves into atomic precision processing (APP) techniques like atomic layer deposition (ALD), epitaxy, atomic layer etching (ALE), and atomic precision advanced manufacturing (APAM) for the fabrication and modification of 2D materials, essential for future semiconductor devices. Additive APP methods like ALD and epitaxy provide precise control over composition, crystallinity, and thickness at the atomic scale, facilitating high-performance device integration. Subtractive APP techniques, such as ALE, focus on atomic-scale etching control for 2D material functionality and manufacturing. In APAM, modification techniques aim at atomic-scale defect control, offering tailored device functions and improved performance. Achieving optimal performance and energy efficiency in 2D material-based microelectronics requires a comprehensive approach encompassing fundamental understanding, process modeling, and high-throughput metrology. Finally, the outlook for APP in 2D materials is promising, with ongoing developments poised to impact manufacturing and fundamental materials science. Integration with advanced metrology and codesign frameworks will accelerate the realization of next-generation microelectronics enabled by 2D materials.

36 MATERIALS SCIENCE↗