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At least 19 records

Thin Film Synthesis of SrZn2P2 with SrI2 Post-Annealing for Enhanced Crystallinity and Optoelectronic Quality

Ternary Zintl phosphides are promising light-absorbing semiconductors for thin-film optoelectronic applications, but strategies for controlling their microstructure and optoelectronic quality remain underexplored. Here, we report the synthesis of phase-pure SrZn2P2 thin films using radio-frequency co-sputtering in a PH3 + Ar atmosphere and investigate the impact of post-growth processing on their structural and optical properties. Grazing-incidence X-ray scattering and Raman spectroscopy confirm the formation of crystalline SrZn2P2 films over a finite compositional window. Optical measurements reveal clear absorption near the direct-band-gap energy (~1.8 eV) and near-band-edge photoluminescence. Further, we have studied the effects of chemically compatible halide-assisted annealing. It is found that SrI2 treatments lead to pronounced grain growth and reduced diffraction peak broadening while preserving phase purity, in contrast to rapid thermal or forming-gas annealing. Notably, annealing with SrI2 at 450 degrees C significantly enhances both the intensity and spatial uniformity of the photoluminescence, thus connecting the observed microstructural consolidation with improved radiative recombination. Our study demonstrates that halide-assisted annealing provides an effective pathway for microstructural control in SrZn2P2 thin films and highlights a generalizable processing strategy for advancing Zintl phosphide semiconductors toward optoelectronic applications.

14 SOLAR ENERGY↗

Pre- and post-annealing of mechanical damage in silicon wafers

Basic properties of mechanical damage in silicon consisting of cracks and abrasion were studied using transmission electron microscopy. The crystallographic structure of mechanical damage was determined before and after high temperature annealing. The main findings include that stresses in silicon around crack tips are not plastically relieved at room temperature and that abrasion at room temperature introduces shear loops into the silicon. It was also found that cracks of micron size can be annealed out, specifically, if cleavage occurs on 111 planes. The healing products of such cracks are 60 deg and 90 deg dislocations. Submicron cracks transform into stacking faults during annealing. Likewise high concentrations of shear loops due abrasion were found to anneal into stacking faults. A one to one correlation between surface areas containing small cracks and stacking faults was made. Measurements of damage removal on silicon surfaces through chemical-mechanical etching techniques are presented. It is shown that silicon dioxide repolishes damaged silicon surfaces most effectively.

Schwottke, G. H.↗

A New Route Toward Atomically Flat and Defect-Free Ge/SiGe Planar Heterostructures

Germanium-based planar heterostructures are emerging as versatile platforms for realizing quantum devices. In particular, planar Ge/SiGe quantum wells (QWs) host hole states with exceptionally high mobility and strong, electrically tunable spin–orbit interactions, enabling full electrical control of quantum information. A key requirement for these systems is the growth of microscopic, defect-free, atomically flat Ge QW heterostructures on relaxed or reverse-graded SiGe buffer layers, as well as on commercial Ge substrates. While several physical deposition techniques have demonstrated high-quality planar Ge/SiGe QWs, a major challenge remains: minimizing defect density typically requires high growth temperatures, which are incompatible with standard CMOS process flows. Here, we present a convenient low-temperature process for realizing high-quality planar SiGe/Ge heterostructures using a combination of thermal and electron-beam evaporation. We systematically map the effects of ex-situ and in-situ substrate preparation protocols, growth temperature, and post-deposition annealing conditions, and correlate these parameters with surface roughness and defect density. We find that in-situ oxide desorption conditions and post-annealing parameters have the most pronounced impact on improving surface quality. Under optimized conditions, we achieve atomically smooth surfaces with root-mean-square roughness σrms​ ≤ 10 Å and negligible defect density. Interestingly, thermally evaporated Ge layers exhibit oriented triangular crystallites that elongate upon post-annealing in the presence of high Ge vapor pressure. These results demonstrate that this simple, low-temperature deposition approach is a viable and effective route for achieving high-quality Ge QW heterostructures, with strong potential for scalable quantum computing and sensing applications.

Tripathi, Malvika [Fermilab] (ORCID:00000001989251↗

A New Route Toward Atomically Flat and Defect-Free Ge/SiGe Planar Heterostructures

Germanium-based planar heterostructures are emerging as versatile platforms for realizing quantum devices. In particular, planar Ge/SiGe quantum wells (QWs) host hole states with exceptionally high mobility and strong, electrically tunable spin–orbit interactions, enabling full electrical control of quantum information. A key requirement for these systems is the growth of microscopic, defect-free, atomically flat Ge QW heterostructures on relaxed or reverse-graded SiGe buffer layers, as well as on commercial Ge substrates. While several physical deposition techniques have demonstrated high-quality planar Ge/SiGe QWs, a major challenge remains: minimizing defect density typically requires high growth temperatures, which are incompatible with standard CMOS process flows. Here, we present a convenient low-temperature process for realizing high-quality planar SiGe/Ge heterostructures using a combination of thermal and electron-beam evaporation. We systematically map the effects of ex-situ and in-situ substrate preparation protocols, growth temperature, and post-deposition annealing conditions, and correlate these parameters with surface roughness and defect density. We find that in-situ oxide desorption conditions and post-annealing parameters have the most pronounced impact on improving surface quality. Under optimized conditions, we achieve atomically smooth surfaces with root-mean-square roughness σrms​ ≤ 10 Å and negligible defect density. Interestingly, thermally evaporated Ge layers exhibit oriented triangular crystallites that elongate upon post-annealing in the presence of high Ge vapor pressure. These results demonstrate that this simple, low-temperature deposition approach is a viable and effective route for achieving high-quality Ge QW heterostructures, with strong potential for scalable quantum computing and sensing applications.

Tripathi, Malvika [Fermilab] (ORCID:00000001989251↗

Coherent-Precipitation-Stabilized Phase Formation in Over-Stoichiometric Rocksalt-Type Li Superionic Conductors

Rationalizing synthetic pathways is crucial for material design and property optimization, especially for polymorphic and metastable phases. Over-stoichiometric rocksalt (ORX) compounds, characterized by their face-sharing configurations, are a promising group of materials with unique properties; however, their development is significantly hindered by challenges in synthesizability. Here, taking the recently identified Li superionic conductor, over-stoichiometric rocksalt Li–In–Sn–O (o-LISO) material as a prototypical ORX compound, the mechanisms of phase formation are systematically investigated. It is revealed that the spinel-like phase with unconventional stoichiometry forms as coherent precipitate from the high-temperature-stabilized cation-disordered rocksalt phase upon fast cooling. This process prevents direct phase decomposition and kinetically locks the system in a metastable state with the desired face-sharing Li configurations. This insight enables us to enhance the ionic conductivity of o-LISO to be >1 mS cm -1 at room temperature through low-temperature post-annealing. This work offers insights into the synthesis of ORX materials and highlights important opportunities in this new class of materials.

36 MATERIALS SCIENCE↗

Long-term thermal stability and calibration of Type-II fiber Bragg grating array inscribed in radiation-hardened fibers

This paper investigates the long-term thermal stability of Type-II fiber Bragg grating (FBG) arrays, inscribed by femtosecond laser in radiation-hardened fiber, for potential applications as multiplexed sensors in high-temperature energy systems. The thermal stability of FBG sensors was assessed through 16 thermal cycles from room temperature (RT) to 750 ℃ about two months, involving 100 FBG sensors. The results show that the absolute temperature drift of FBG sensors can be reduced to less than 0.4 pm/day after 54 h thermal annealing process at a constant temperature of 800 ℃. As temperature sensors, the FBGs demonstrated stable performance, achieving a standard deviation (STD) of 1.8 pm (corresponding to a temperature resolution of 0.118 ℃) post-annealing. Repeated thermal cycles revealed a random drift of 2.3 pm in the FBG wavelength at RT. Polynomial fitting was explored as a calibration method to convert FBG wavelength shifts into absolute temperature measurements. By optimizing calibration temperature points (RT, 200 ℃, 400 ℃, and 750 ℃), the study shows that cubic polynomial calibration using four points yields an average R2 of 0.9997 and an RMSE of 3.58 ℃ across the entire temperature range (RT to 750 ℃). This approach represents an 11.53-fold improvement over empirical slope calibration and a 1.34-fold improvement over four-point piecewise fitting. The findings indicate that Type-II FBGs inscribed in radiation-hardened fibers can function as accurate temperature sensors, with performance on par with or exceeding that of thermocouples. With their multiplexing capability, robust signal transmission over long lead cables, and immunity to electromagnetic interference, FBG sensors offer a promising alternative to traditional electronic sensors for energy system monitoring.

Dominguez-Ontiveros, Elvis [ORNL] (ORCID:000000018↗

Additive manufacturing for electrocaloric terpolymer thin films

Current heating, venting, and air conditioning (HVAC) systems have drawbacks of high energy consumption, large CO 2 emissions, and low efficiency. Electrocaloric (EC) cycles present an eco-friendly alternative by converting thermal energy to electrical energy. Defect-free thin films with uniform thickness are required to achieve optimal EC performance. A scalable thin film fabrication process is essential for integrating EC cycles into HVAC systems. This study introduces EC thin films prepared by electrospray (ES) processing, a manufacturing method that deposits EC polymer layer by layer using high voltage. The resulting films show superior thickness control, smoother surfaces, and improved thermal and electrical properties compared with solution casting. In addition, post-annealing at 120°C enhances the thermal and EC performance, with films achieving a temperature change (ΔT) of 3.6°C at 100 MV/m when tested near room temperature. With the potential for future scalability, the ES method offers a promising approach for fabricating EC thin films.

36 MATERIALS SCIENCE↗

Characterization of n-Type Iodine-Doped and Indium-Doped CdTe/Cd-Se-Te Thin Films Fabricated by Close-Spaced Sublimation Epitaxy

In this study, n-type CdTe thin films, specifically iodine-doped CdTe (CdTe:I), indium-doped CdTe (CdTe:In), and indium-doped Cd-Se-Te (CST:In), were synthesized using close-spaced sublimation epitaxy (CSSE). Characterization techniques secondary ion mass spectrometry (SIMS), electron backscatter diffraction (EBSD), Hall-effect measurements, and time-resolved photoluminescence (TRPL) were employed to analyze the chemical, structural, and electronic properties of these materials. The results indicated epitaxial single crystal CSSE films grew on the single crystal substrates, with carrier density ranging from 10^14 - 10^16 cm -3 , and after post-annealing, the minority-carrier lifetimes reach near the radiative limit. Additionally, a preliminary exploration of homojunction structures with an n- type (CdTe:In /CST:In /CdTe:I) /CdTe:P /Cu /Mo configuration was performed. The best device performance was achieved with CdTe:I including CdS aiding in band alignment, resulting in a power conversion efficiency (..eta..) of 2.61% with open circuit voltage (Voc) of 850 mV, fill factor (FF) of 47.8%, and short-circuit current (Jsc) of 6.44 mA/cm 2 . The observed low Jsc and efficiency may be attributed to a buried junction and a poor interface, due to dopant interdiffusion. Consequently, further investigations focusing on interface optimization, diffusion blocking, and reduced recombination through passivation, are crucial to enhancing the efficiency of CSSE CdTe homojunction devices in the future.

cadmium compounds↗

Co-Sputtering of Nb3Sn into SRF Cavity Using Composite Target and Optimizing Surface Homogeneity

Nb₃Sn coating method for superconducting radiofrequency (SRF) cavity has been developed following co-sputtering of Nb-Sn composite target using a DC cylindrical sputter coater. Deposition parameters and annealing strategies were optimized for uniform Nb₃Sn coating. 1.5 m Nb-Sn film was deposited onto 2.6 GHz Nb SRF cavity and annealed at 600 C for 6 h, followed by 950 C for 1 h. Cryogenic RF testing confirmed Nb₃Sn formation with Tc = 17.8 K. A post-annealing light Sn recoating process improved the cavity s performance, achieving Q₀ = 8.5 10⁸ at 2.0 K.

Shakel, M. S. [Old Dominion U.]↗

Virtual Growth of SRF Materials

Niobium's native surface oxide affects SRF cavity and superconducting qubit performance, motivating interest in controlling its crystalline structure. We combine a literature-derived machine-learning analysis with temperature-dependent XRD to study crystalline ordering in Nb2O5. Random Forest models, trained on 74 processing conditions from 17 papers and validated by leave-one-group-out cross-validation, predicted broad crystallinity outcomes well (balanced accuracy 0.809), but struggled with specific polymorph identity (0.577). Annealing temperature was the dominant predictor across all targets; oxygen partial pressure showed negligible importance, reflecting narrow literature coverage rather than physical irrelevance. Temperature-dependent XRD on anodized and H2O2-treated Niobium showed structural evolution consistent with the machine learning predictions. Our model and overall approach provide a data-driven framework for identifying and optimizing conditions that promote crystallization in initially amorphous oxides. This framework can guide the selection of growth and post-annealing conditions for Nb surfaces by narrowing the experimental parameter space, thereby reducing trial-and-error efforts in developing oxide structures relevant to SRF applications.

Tilkin, Anthony [Fermilab]↗

Structure of molybdenum disulfide films sputtered on substrates at various temperatures

Molybdenum disulfide films 300 to 400 A thick were rf sputtered on aluminum and nickel surfaces at elevated, ambient, and liquid nitrogen temperatures. Electron transmission micrographs and electron diffraction patterns were taken to determine the structural growth. These transmission micrographs revealed that sputtered MoS2 films at ambient and elevated temperatures (320 and 150 C) formed an irregular network of ridges. The electron diffraction patterns of these films showed relatively sharp diffraction rings, indicating crystallinity. The transmission micrographs of sputtered films at liquid nitrogen temperatures revealed a continuous featureless film. The electron diffraction patterns showed broad, diffused rings indicating an amorphous film. The transmission micrographs of a post-annealed (425 C) MoS2 film sputtered at liquid-nitrogen temperature revealed the tendency for ridge formation. Electron diffraction patterns also showed increased sharpness of the diffraction rings. Friction tests showed that MoS2 films deposited at ambient and elevated temperatures exhibited good lubricating properties. The MoS2 films deposited at cryogenic temperatures had no lubricating characteristics.

Spalvins, T.↗

The effects of space radiation on thin films of YBa2Cu3O(sub 7-x)

This investigation had two objectives: (1) to determine the effects of space radiation on superconductor parameters that are most important in space applications; and (2) to determine whether this effect can be simulated with Co-60 gamma rays, the standard test method for space materials. Thin films of yttrium barium copper oxide (YBCO) were formed by coevaporation of Y, BaF2, and Cu and post-annealing in wet oxygen at 850 C for 3.5 h. The substrate used was (100) silicon with an evaporated zirconia buffer layer. The samples were characterized by four point probe electrical measurements as a function of temperature. The parameters measured were the zero resistance transition temperature (T sub c) and the room temperature resistance. The samples were then exposed to Co-60 gamma-rays in air and in pure nitrogen, and to 780 keV electrons, in air. The parameters were then remeasured. The results are summarized. The results indicate little or no degradation in the parameters measured for samples exposed up to 10 Mrads of gamma-rays in nitrogen. However, complete degradation of samples exposed to 10-Mrad in air was observed. This degradation is preliminarily attributed to the high level of ozone generated in the chamber by the gamma-ray interaction with air. It can be concluded that: (1) the electron component of space radiation does not degrade the critical temperature of the YBCO films described, at least for energies around 800 keV and doses similar to those received by surface materials on spacecraft in typical remote sensing missions; and (2) for qualifying this and other superconducting materials against the space-radiation threat the standard test method in the aerospace industry, namely, exposure to Co-60 gamma-rays in air, may require some further investigation. As a minimum, the sample must be either in vacuum or in positive nitrogen pressure.

Herschitz, R.↗

An experimental study of high Tc superconducting microstrip transmission lines at 35 GHz and the effect of film morphology

Microstrip transmission lines in the form of ring resonators were fabricated from a number of in-situ grown laser ablated films and post-annealed co-sputtered YBa2Cu3O(7-x) films. The properties of these resonators were measured at 35 GHz and the observed performance is examined in light of the critical temperature (Tc) and film thickness and also the film morphology which is different for the two deposition techniques. It is found that Tc is a major indicator of the film performance for each growth type with film thickness becoming important as it decreases towards 100 A. It is also found that the films with a mixed grain orientation (both a axis and c axis oriented grains) have poorer microwave properties as compared with the primarily c axis oriented material. This is probably due to the significant number of grain boundaries between the different crystallites, which may act as superconducting weak links and contribute to the surface resistance.

Chorey, C. M.↗

An experimental study of high Tc superconducting microstrip transmission lines at 35 GHz and the effect of film morphology

Microstrip transmission lines in the form of ring resonators were fabricated from a number of in-situ grown laser ablated films and post-annealed co-sputtered YBa2Cu3O(7-x) films. The properties of these resonators were measured at 35 GHz and the observed performance is examined in light of the critical temperature (Tc) and film thickness, and also the film morphology, which is different for the two deposition techniques. It is found that Tc is a major indicator of the film performance for each growth type, with film thickness becoming important as it decreases towards 1000 A. It is also found that the films with a mixed grain orientation (both a-axis and c-axis oriented grains) have poorer microwave properties as compared with the primarily c-axis oriented material. This is probably due to the significant number of grain boundaries between the different crystallites, which may act as superconducting weak links and contribute to the surface resistance.

Chorey, C. M.↗

The effects of space radiation on thin films of YBa2Cu3O(7-x)

This investigation had two objectives: (1) to determine the effects of space radiation on superconductor parameters that are most important in space applications; and (2) to determine whether this effect can be simulated with Co-60 gamma rays, the standard test method for space materials. Thin films of yttrium barium copper oxide (YBCO) were formed by coevaporation of Y, BaF2, and Cu and post-annealing in wet oxygen at 850 C for 3.5 h. The substrate used was (100) silicon with an evaporated zirconia buffer layer. The samples were characterized by four point probe electrical measurements as a function of temperature. The parameters measured were the zero resistance transition temperature T(sub c) and the room temperature resistance. The samples were then exposed to Co-60 gamma-rays in air and in pure nitrogen, and to 780 keV electrons, in air. The parameters were then remeasured. The results are summarized. The results indicate little or no degradation in the parameters measured for samples exposed up to 10 Mrads of gamma-rays in nitrogen. However, complete degradation is preliminarily attributed to the high level of ozone generated in the chamber by the gamma-ray interaction with air. It can be concluded that: (1) the electron component of space radiation does not degrade the critical temperature of the YBCO films described, at least for energies around 800 keV and doses similar to those received by surface materials on spacecraft in typical remote sensing missions; and (2) for qualifying this and other superconducting materials against the space-radiation threat the standard test method used in the aerospace industry, namely, exposure to Co-60 gamma-rays in air, may require some further investigation. As a minimum, the sample must be either in vacuum or in positive nitrogen pressure.

Herschitz, R.↗

Properties of large area ErBa2Cu3O(7-x) thin films deposited by ionized cluster beams

Ionized cluster beam (ICB) deposition is employed to produce ErBa2Cu3O(7-x) films on different substrates without post-annealing. Films with diameters of up to 70 mm are grown on SrTiO3 100 plane and exhibit Tc values of 84-87 K, Jc of about 10 exp 6 A/sq m at 77 K. These films are epitaxial with the c-axis perpendicular to the plane of the substrate surface, and they can be routinely produced by ICB with good Jc and Tc.

Levenson, L. L.↗

Current Status of Thin Film (Ba,Sr)TiO3 Tunable Microwave Components for RF Communications

The performance of proof-of-concept ferroelectric microwave devices has been moving steadily closer to the level needed for satellite and other rf communications applications. This paper will review recent progress at NASA Glenn in developing thin film Ba(x)Sr(1-x)TiO3 tunable micro-wave components for these applications. Phase shifters for phased array antennas, tunable filters and tunable oscillators employing microstrip and coupled microstrip configurations will be presented. Tunabilities, maximum dielectric constants, and phase shifter parameters will be discussed (e.g., coupled microstrip phase shifters with phase shift over 200 deg at 18 GHz and a figure of merit of 74.3 deg/dB). Issues of post-annealing, Mn-doping and Ba(x)Sr(1-x) TiO3 growth on sapphire and alumina substrates will be covered. The challenges of incorporating these devices into larger systems, such as yield, variability in phase shift and insertion loss, and protective coatings will also be addressed.

VanKeuls, F. W.↗

Investigation of Thermal Processing on the Properties of PS304: A Solid Lubricant Coating

The effect of thermal processing on PS304, a solid lubricant coating, was investigated. PS304 is a plasma sprayed solid lubricant consisting of 10% Ag and 10% BaF2 and CaF2 in a eutectic mixture for low and high temperature lubricity respectively. In addition, PS304 contains 20% Cr2O3 for increased hardness and 60% NiCr which acts as a binder. All percents are in terms of weight not volume. Previous research on thermal processing (NAG3-2245) of PS304 revealed that substrate affected both the pre- and post-anneal hardness of the plasma spray coating. The objective of this grant was to both quantify this effect and determine whether the root cause was an artifact of the substrate or an actual difference in hardness due to interaction between the substrate and the coating. In addition to clarifying past research developments new data was sought in terms of coating growth due to annealing.

Benoy, Patricia A.↗