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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Theoretical Analysis of Experimental Data of Sodium Diffusion in Oxidized Molybdenum Thin Films

In this work, the diffusion process of sodium (Na) in molybdenum (Mo) thin films while it was deposited on soda lime glass (SLG) was studied. A small amount of oxygen was present in the chamber while the direct-current (DC) magnetron sputtering was used for the deposition. The substrate temperatures were varied to observe its effect. Such molybdenum films, with or without oxidations, are often used in thin film solar cells, either as back contact or as hole transport layers. Secondary ion mass spectrometry (SIMS) was used to quantify the concentration of the species. A grain diffusion mechanistic model incorporating the effect of grain and grain boundary geometrical shape and size was developed. The model was used to provide an in-depth theoretical analysis of the sodium diffusion in molybdenum thin films that lead to the measured SIMS data. It was observed that not only diffusion coefficients should be considered when analyzing diffusion processes in thin films but also the ratio of grain boundary size to grain size. Both depend on substrate temperature and directly affect the amount of diffused species in the film. The data were analyzed under the light of the film growth speed versus diffusion front speed, the effect of oxygen content, and the effect of substrate temperature on the overall diffusion process. The temperature inversely affects the ratio of grain boundary size and grain size and directly affects the diffusion coefficient, which leads to a preferable temperature at which the highest amount of alkali can be found in the film.

36 MATERIALS SCIENCE↗
NASA NTRS2016

Electron-Beam Deposition of Superconducting Molybdenum Thin Films for the Development of Mo/Au TES X-Ray Microcalorimeter

We are exploring the properties of electron-beam evaporated molybdenum thin films on silicon nitride coated silicon wafers at substrate temperatures between room temperature and 650 C. The temperature dependence of film stress, transition temperature, and electrical properties are presented. X-ray diffraction measurements are performed to gain information on molybdenum crystallite size and growth. Results show the dominant influence of the crystallite size on the intrinsic properties of our films. Wafer-scale uniformity, wafer yield, and optimal thermal bias regime for TES fabrication are discussed.

Microcalorimeter↗
DOE OSTI2022

Structural, Optical and Mechanical Properties of Nanocrystalline Molybdenum Thin Films Deposited under Variable Substrate Temperature

Molybdenum (Mo), which is one among the refractory metals, is a promising material with a wide variety of technological applications in microelectronics, optoelectronics, and energy conversion and storage. However, understanding the structure–property correlation and optimization at the nanoscale dimension is quite important to meet the requirements of the emerging nanoelectronics and nanophotonics. In this context, we focused our efforts to derive a comprehensive understanding of the nanoscale structure, phase, and electronic properties of nanocrystalline Mo films with variable microstructure and grain size. Molybdenum films were deposited under varying temperature (25–500 °C), which resulted in Mo films with variable grain size of 9–22 nm. The grazing incidence X-ray diffraction analyses indicate the (110) preferred growth behavior the Mo films, though there is a marked decrease in hardness and elastic modulus values. In particular, there is a sizable difference in maximum and minimum elastic modulus values; the elastic modulus decreased from ~460 to 260–280 GPa with increasing substrate temperature from 25–500 °C. The plasticity index and wear resistance index values show a dramatic change with substrate temperature and grain size. Additionally, the optical properties of the nanocrystalline Mo films evaluated by spectroscopic ellipsometry indicate a marked dependence on the growth temperature and grain size. This dependence on grain size variation was particularly notable for the refractive index where Mo films with lower grain size fell in a range between ~2.75–3.75 across the measured wavelength as opposed to the range of 1.5–2.5 for samples deposited at temperatures of 400–500 °C, where the grain size is relatively higher. The conductive atomic force microscopy (AFM) studies indicate a direct correlation with grain size variation and grain versus grain boundary conduction; the trend noted was improved electrical conductivity of the Mo films in correlation with increasing grain size. The combined ellipsometry and conductive AFM studies allowed us to optimize the structure–property correlation in nanocrystalline Mo films for application in electronics and optoelectronics.

36 MATERIALS SCIENCE↗
NASA NTRS1989

Thin film molybdenum silicide as potential temperature sensors for turbine engines

Temperature measurements of Mo-Si-based thin-film resistance thermometers were studied. Annealing in an argon ambient at a temperature above 1000 C for at least 1 h is required to form the stable tetragonal MoSi2 phase. With a crack-free 2-micron-thick AlN barrier layer on top, a sensor was tested up to 1200 C. The resistivity vs temperature characteristic shows the room temperature resistivity and temperature coefficient of resistivity (TCR) of the sensor to be approximately 350 microohm and 0.01195 K, respectively. No film adhesion problems were observed for at least four testing cycles.

Ho, C. H.↗
DOE OSTI2019

Impact of Water Ingress on Molybdenum Thin Films and Its Effect on Cu(In,Ga)Se 2 Solar Cells

Solar cell degradation can occur through many pathways and at the different stages of the fabrication process, notably because of the water condensation. In the case of Cu(In,Ga)Se 2 (CIGS) solar cells, the impact of water ingress on Mo back contact can be substantial for not only the film itself but also the device performance and reliability. Microstructural modification, change in film morphology, loss in reflectance, and increased resistivity because of the moisture ingress were observed via X-ray diffraction, transmission electron microscopy, spectroscopic ellipsometry, and four-point probe measurements, respectively. Secondary ion mass spectrometry measurements revealed drastic changes in the alkali (Na, K) profiles in both the CIGS and Mo layers, likely because of the modification of their diffusion coefficient through Mo. This, in turn, negatively impacts the solar cell efficiency by decreasing both fill factor and open-circuit voltage. Additional experiments, modifying the substrate and utilizing a NaF postdeposition treatment, highlight the mechanisms of degradation as being due to both a modification of the Mo/CIGS interface and the lack of alkali diffusion after water ingress.

14 SOLAR ENERGY↗
DOE OSTI2026

Plasma-Enhanced Atomic Layer Deposition Synthesis of Nanolayered Molybdenum Diselenide (MoSe 2 ) Thin Films for Nanoelectronics

Nanolayered molybdenum diselenide (MoSe 2 ) thin films were synthesized by plasma-enhanced atomic layer deposition (PE-ALD) using molybdenum pentachloride (MoCl 5 ) and diethyldiselenide (C 4 H 10 Se 2 ) precursors. Scanning and transmission electron microscopy revealed horizontally stacked nanolayers near the substrate and vertically oriented nanosheets at the surface of the film. X-ray diffraction confirmed the (002), (100), and (110) reflections of crystalline MoSe 2 , while X-ray photoelectron spectroscopy showed relative atomic concentrations of 33.5% Mo and 66.5% Se, consistent with stoichiometric MoSe 2 . Raman spectra exhibited characteristic E 1g , A 1g , and E$^1_{2g}$ vibrational modes. Field-effect transistors incorporating PE-ALD-grown MoSe 2 as the channel material displayed p-type behavior, demonstrating the potential of nanolayered MoSe 2 for nanoelectronic applications. This work demonstrates the feasibility of low-temperature, stoichiometric growth of nanolayered MoSe 2 by PE-ALD and its direct integration into transistor architectures.

36 MATERIALS SCIENCE↗
NASA NTRS1994

Soft x ray optics by pulsed laser deposition

A series of molybdenum thin film depositions by PLD (Pulsed Laser Deposition) have been carried out, seeking appropriate conditions for multilayer fabrication. Green (532 nm) and UV (355 nm) light pulses, in a wide range of fluences, were used. Relatively large fluences (in comparison with Si) are required to cause evaporation of molybdenum. The optical penetration depths and reflectivities for Mo at these two wavelengths are comparable, which means that results should be, and do appear to be similar for equal fluences. For all fluences above threshold used, a large number of incandescent particles is ejected by the target (either a standard Mo sputtering target or a Mo sheet were tried), together with the plasma plume. Most of these particles are clearly seen to bounce off the substrate. The films were observed with light microscopy using Nomarski and darkfield techniques. There is no evidence of large debris. Smooth films plus micron-sized droplets are usually seen. The concentration of these droplets embedded in the film appears not to vary strongly with the laser fluence employed. Additional characterization with SEM and XRD is under way.

Fernandez, Felix E.↗
NASA NTRS1987

Alkali metal thermoelectric converter (AMTEC) electrode lifetime studies

Experimental studies are being conducted at JPL to identify long life, high area power density electrodes for AMTEC. Power versus time measurements are being made in a demountable electrode test cell and, for longer term experiments, a self-contained recirculating cell. The experimental apparatus and procedures are described in detail. The results show that thin film molybdenum electrodes can be designed to produce power near 0.5 W/sq cm for over two hundred hours. Also, platinum/tungsten electrodes exhibit power densities that are stable near 0.5 W/sq cm. If the performance of these electrodes is verified for longer periods (thousands of hours), then practical AMTEC systems will be possible.

Bankston, C. Perry↗
NASA NTRS1987

Alkali metal thermoelectric conversion (AMTEC) technology status review

AMTEC operating principles, technical problems, and recent electrode research results are briefly reviewed. The mechanisms responsible for the degradation of thin-film molybdenum electrodes are discussed, and four alternate high-power electrode compositions and morphologies are identified. Separate self-contained recirculating AMTEC cells have demonstrated 19-percent efficiency, 10,000 hr at high temperature, and multicell operation including series connection. Results of systems studies in the 0.5-100 kWe range indicate that AMTEC performance and operating characteristics make it a strong candidate for future space applications.

Bankston, C. P.↗
DOE OSTI2021

Modulating the optoelectronic properties of hybrid Mo-thiolate thin films

In this study, hybrid MoS 2 -based molybdenum thiolate thin films with selected organic motifs are grown using molecular layer deposition (MLD), allowing for tunable optoelectronic film properties. The thin films are deposited at 170°C using the metal precursor molybdenum hexacarbonyl and one of the three organic precursors: 1,2-ethanedithiol, 1,4-butanedithiol, and 1,4-benzenedithiol. The resulting Mo-ethanethiolate, Mo-butanethiolate, and Mo-benzenethiolate films show saturating growth with a growth per cycle of 1.2, 1.0, and 1.5 Å/cycle, respectively. Fourier transform infrared spectroscopy, x-ray photoelectron spectroscopy, Raman spectroscopy, x-ray absorption spectroscopy, and x-ray diffraction are used to characterize the as-deposited films. Results show that by changing the organic precursor, the film composition as well as the optical and electronic properties can be tuned. The Mo-thiolate films grown with benzenedithiol exhibit the lowest resistivity, which at 12 mΩ cm is ~400 times more conductive than Mo-thiolates grown with aliphatic organic linkers. All three backbone chemistries of the Mo-thiolates show an optical bandgap between 2.3 and 2.4 eV and mild photoconductivity response. The MLD of these Mo-thiolate films demonstrates the synthesis of transition metal-organosulfur thin films with tunable properties.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Growth of nanostructured molybdenum disulfide (MoS 2 ) thin films on a nanohole-patterned substrate using plasma-enhanced atomic layer deposition (ALD)

Nanostructured molybdenum disulfide (MoS 2 ) thin films were grown on a nanohole-patterned silicon substrate using plasma-enhanced atomic layer deposition. A nanoscale hole-patterned silicon substrate was fabricated for the growth of MoS 2 film using the self-assembly-based nanofabrication method. The nanoscale holes can significantly increase the surface area of the substrate while the formation and growth of nanostructures normally start at the surface of the substrate. Hydrogen sulfide (H 2 S) gas was used as the S source in the growth of molybdenum disulfide (MoS 2 ) while molybdenum (V) chloride (MoCl 5 ) powder was used as the Mo source. The MoS 2 film had a stoichiometric ratio of 1 (Mo) to 2 (S), and had peaks of E 1 2g and A 1g , which represent the in-plane and out-plane vibration modes of the Mo–S bond, respectively. It was found that the MoS 2 film grown in the nanoscale hole, especially at the wall of the hole, has more hexagonal-like structures due to the effects of nanoscale space confinement and the nanoscale interface although the film shows an amorphous structure. Post-growth high-temperature annealing ranging from 800 to 900 °C produced local crystalline structures in the film, which are compatible with those reported by other researchers.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS1976

Physical properties of thin-film field emission cathodes with molybdenum cones

Field emission cathodes fabricated using thin-film techniques and electron beam microlithography are described, together with effects obtained by varying the fabrication parameters. The emission originates from the tip of molybdenum cones that are about 1.5 micron tall with a tip radius around 500 A. Such cathodes have been produced in closely packed arrays containing 100 and 5000 cones as well as singly. Maximum currents in the range 50-150 microamp per cone can be drawn. Life tests with the 100-cone arrays drawing 2 mA total emission (or 3 A per sq cm) have proceeded in excess of 7000 hr with about a 10% drop in emission current. Studies are presented of the emission characteristics and current fluctuation phenomena. It is tentatively concluded that the emission arises from only one or a few atomic sites on the cone tips.

Spindt, C. A.↗
DOE OSTI2022

Study of synergistic effects and compositional dependence of hydrogen evolution reaction on MoxNiy alloy thin films in alkaline media

In this paper hydrogen evolution reaction (HER) on the molybdenum-nickel thin films has been studied. The Mo x Ni y thin films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). A change in the crystal structure of the samples prepared at different temperatures was observed. The structure of the samples prepared at 25 °C are bcc or amorphous. The structure of alloys sputtered at 800 °C changed to fcc. Tafel plots were constructed for each Mo x Ni y alloy sample. The mechanism of HER was determined from Tafel slope analysis. Values of charge transfer resistance were also determined by impedance spectroscopy. The compositional dependence of activity and the stability of Mo x Ni y thin films in 1 M NaOH were determined by cycling and chronoamperometry. Our results demonstrate that Mo x Ni y thin films prepared at 800 °C show significantly improved activity compared to pure Mo and Ni metals. On the other hand, Mo x Ni y thin films sputtered at 25°C do not show increased activity in comparison to pure Ni metal. Furthermore, this points to a synergistic effect between fcc Mo and fcc Ni in thin films sputtered at elevated temperatures. Mo 63 Ni 67 thin films alloy prepared at 800 °C shows the best values of catalytic activity for HER from all investigated compositions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Large-field magnetoresistance of nanometer scale nickel films grown on molybdenum disulfide

The magnetoresistance of thin nickel films grown on molybdenum disulfide was measured in perpendicular magnetic fields as high as 90 kOe. Films with thicknesses of 20 nm provided continuous surfaces for measurement. The magnetoresistance was found to be linear with respect to the applied magnetic field with no sign of saturation. There was also no evidence of hysteresis or temperature dependence between 100 to 300 K. STM measurement showed the deposited Ni forms a continuous film of extremely small nanoclusters. However, the field dependence of magnetoresistance was found to be significantly larger than bulk Ni, which is in turn larger than Ni with nanoscale grains. We expect the unusual magnetoresistance behavior to arise from some property of the Ni-MoS 2 interface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Sputter-Deposited Mo Thin Films: Multimodal Characterization of Structure, Surface Morphology, Density, Residual Stress, Electrical Resistivity, and Mechanical Response

Multimodal datasets of materials are rich sources of information which can be leveraged for expedited discovery of process–structure–property relationships and for designing materials with targeted structures and/or properties. For this data descriptor article, we provide a multimodal dataset of magnetron sputter-deposited molybdenum (Mo) thin films, which are used in a variety of industries including high temperature coatings, photovoltaics, and microelectronics. In this dataset we explored a process space consisting of 27 unique combinations of sputter power and Ar deposition pressure. Here, the phase, structure, surface morphology, and composition of the Mo thin films were characterized by x-ray diffraction, scanning electron microscopy, atomic force microscopy, and Rutherford backscattering spectrometry. Physical properties—namely, thickness, film stress and sheet resistance—were also measured to provide additional film characteristics and behaviors. Additionally, nanoindentation was utilized to obtain mechanical load-displacement data. The entire dataset consists of 2072 measurements including scalar values (e.g., film stress values), 2D linescans (e.g., x-ray diffractograms), and 3D imagery (e.g., atomic force microscopy images). An additional 1889 quantities, including film hardness, modulus, electrical resistivity, density, and surface roughness, were derived from the experimental datasets using traditional methods. Minimal analysis and discussion of the results are provided in this data descriptor article to limit the authors’ preconceived interpretations of the data. Overall, the data modalities are consistent with previous reports of refractory metal thin films, ensuring that a high-quality dataset was generated. The entirety of this data is committed to a public repository in the Materials Data Facility.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Atomic layer deposition of MoO x thin films using Mo( i PrCp) 2 H 2 and O 3

Here, this work studied the growth of molybdenum oxide thin films with thermal atomic layer deposition (ALD) using Mo(iPrCp)2H2 and O3 as precursors. Growth parameters were determined by varying growth temperature and precursor dose times. ALD growth was exhibited in a temperature range of 100–200 °C. The growth per cycle ranged from 1.3 to 1.7 Å/cycle with a standard uniformity parameter of <5%. Attempts to grow films using H2O as an oxygen source showed no significant growth. Film properties were measured using spectroscopic ellipsometry, x-ray reflectivity, x-ray diffraction, x-ray photoelectron spectroscopy, and infrared spectroscopy.

36 MATERIALS SCIENCE↗