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At least 325 records · Page 18
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Impact of Microstructure on MoS 2 Oxidation and Friction

In this work, we demonstrate the role of microstructure in the friction and oxidation behavior of the lamellar solid lubricant molybdenum disulfide (MoS 2 ). We report on systematic investigations of oxidation and friction for two MoS 2 films with distinctively different microstructures—amorphous and planar/highly-ordered—before and after exposure to atomic oxygen (AO) and high-temperature (250 °C) molecular oxygen. A combination of experimental tribology, molecular dynamics simulations, X-ray photoelectron spectroscopy (XPS), and high-sensitivity low-energy ion scattering (HS-LEIS) was used to reveal new insights about the links between structure and properties of these widely utilized low-friction materials. Initially, ordered MoS 2 films showed a surprising resistance to both atomic and molecular oxygens (even at elevated temperature), retaining characteristic low friction after exposure to extreme oxidative environments. Finally, XPS shows comparable oxidation of both coatings via AO; however, monolayer resolved compositional depth profiles from HS-LEIS reveal that the microstructure of the ordered coatings limits oxidation to the first atomic layer.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Variation of the Passive Film on Compositionally Concentrated Dual-Phase Al 0.3 Cr 0.5 Fe 2 Mn 0.25 Mo 0.15 Ni 1.5 Ti 0.3 and Implications for Corrosion

The passive film on a dual-phase Al 0.3 Cr 0.5 Fe 2 Mn 0.25 Mo 0.15 Ni 1.5 Ti 0.3 FCC + Heusler (L2 1 ) compositionally concentrated alloy formed during extended exposure to an applied potential in the passive range in dilute chloride solution was characterized. Each phase, with its own distinct composition of passivating elements, formed unique passive films separated by a heterophase interface. High-resolution, surface sensitive characterization enabled chemical analysis of the passive film formed over individual phases. The film formed over the L2 1 phase had a higher concentration of Al, Ni, and Ti, while the film formed over FCC phase was of similar thickness but contained comparatively higher Cr, Fe, and Mo concentrations, consistent with the differences in bulk microstructure composition. The passive film was continuous across phase boundaries and the distribution of passivating elements (Al, Cr, and Ti) indicated both phases were independently passivated. Spatially resolved analysis of the surface chemistry of the dual-phase CCA revealed that the cation with the highest composition in passive film formed on the FCC phase was Cr (52.4 at. pct) and for the L2 1 phase was Ti (53.1 at. pct) despite the bulk concentration of each element being below 20 at. pct in their respective phases. Al, Cr, and Ti were enriched in both phases within the passive film relative to their respective bulk compositions. In parallel studies, single-phase alloys with compositions representative of the FCC and L2 1 phases were synthesized to evaluate the corrosion behavior of each phase in isolation. The corrosion behavior of the dual-phase alloy showed passivity evidenced by a pitting potential of 0.615 V SCE in 0.01 M NaCl. The pitting potential and other electrochemical parameters suggested a combination of behaviors of both single-phase samples, suggesting that the global corrosion behavior may be represented by a composite theory applied to phases, their area fractions, and interphase length. However, the interphase in the dual-phase CCA was a local corrosion initiation site and may limit localized corrosion protectiveness. The alloy design implications for optimization of second phase structure and morphology are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Superconducting Thin Films for The Enhancement of Superconducting Radio Frequency Accelerator Cavities

Bulk niobium (Nb) superconducting radio frequency (SRF) cavities are currently the preferred method for acceleration of charged particles at accelerating facilities around the world. However, bulk Nb cavities have poor thermal conductance, impose material and design restrictions on other components of a particle accelerator, have low reproducibility and are approaching the fundamental material-dependent accelerating field limit of approximately 50MV/m. Since the SRF phenomena occurs at surfaces within a shallow depth of ~1 μm, a proposed solution to this problem has been to utilize thin film technology to deposit superconducting thin films on the interior of cavities to engineer the active SRF surface in order to achieve cavities with enhanced properties and performance. Two proposed thin film applications for SRF cavities are: 1) Nb thin films coated on bulk cavities made of suitable castable metals (such as copper or aluminum) and 2) multilayer films designed to increase the accelerating gradient and performance of SRF cavities. While Nb thin films on copper (Cu) cavities have been attempted in the past using DC magnetron sputtering (DCMS), such cavities have never performed at the bulk Nb level. However, new energetic condensation techniques for film deposition, such as High Power Impulse Magnetron Sputtering (HiPIMS), offer the opportunity to create suitably thick Nb films with improved density, microstructure and adhesion compared to traditional DCMS. Clearly use of such novel technique requires fundamental studies to assess surface evolution and growth modes during deposition and resulting microstructure and surface morphology and the correlation with RF superconducting properties. Here we present detailed structure-property correlative research studies done on Nb/Cu thin films and NbN- and NbTiN-based multilayers made using HiPIMS and DCMS, respectively. Experiment Numbers:

Burton, Matthew↗
DOE OSTI2020

Combinatorial Synthesis and High-Throughput Characterization of Microstructure and Phase Transformation in Ni–Ti–Cu–V Quaternary Thin-Film Library

Ni–Ti–based shape memory alloys (SMAs) have found widespread use in the last 70 years, but improving their functional stability remains a key quest for more robust and advanced applications. Named for their ability to retain their processed shape as a result of a reversible martensitic transformation, SMAs are highly sensitive to compositional variations. Alloying with ternary and quaternary elements to fine-tune the lattice parameters and the thermal hysteresis of an SMA, therefore, becomes a challenge in materials exploration. Combinatorial materials science allows streamlining of the synthesis process and data management from multiple characterization techniques. In this study, a composition spread of Ni–Ti–Cu–V thin-film library was synthesized by magnetron co-sputtering on a thermally oxidized Si wafer. Composition-dependent phase transformation temperature and microstructure were investigated and determined using high-throughput wavelength dispersive spectroscopy, synchrotron X-ray diffraction, and temperature-dependent resistance measurements. Of the 177 compositions in the materials library, 32 were observed to have shape memory effect, of which five had zero or near-zero thermal hysteresis. These compositions provide flexibility in the operating temperature regimes that they can be used in. A phase map for the quaternary system and correlations of functional properties are discussed with respect to the local microstructure and composition of the thin-film library.

42 ENGINEERING↗
DOE OSTI2022

Quality Control Metrics to Assess MoS2 Sputtered Films for Tribological Applications

Abstract Pure molybdenum disulfide (MoS 2 ) solid lubricant coatings could attain densities comparable to doped films (and the associated benefits to wear rate and environmental stability) through manipulation of the microstructure via deposition parameters. Unfortunately, pure films can exhibit highly variable microstructures and mechanical properties due to processes that are not controlled during deposition (i.e., batch-to-batch variation). This work focuses on developing a relationship between density, hardness, friction, and wear for pure sputtered MoS 2 coatings. Results show that dense films ( ρ = 4.5 g/cm 3 ) exhibit a 100 × lower wear rate compared to porous coatings ( ρ = 3.04–3.55 g/cm 3 ). The tribological performance of high density pure MoS 2 coatings is shown to surpass that of established composite coatings, achieving a wear rate 2 × ( k = 5.74 × 10 –8 mm 3 /Nm) lower than composite MoS 2 /Sb 2 O 3 /Au in inert environments.

Babuska, Tomas F.↗
DOE OSTI2020

Comparison of Orientation Mapping in SEM and TEM

In this work, multiple experimental configurations for performing nanoscale orientation mapping are compared to determine their fidelity to the true 3D microstructure of a sample. Transmission Kikuchi Diffraction (TKD) experiments in an SEM and nanobeam diffraction (NBD) experiments in a TEM were performed on thin electrodeposited hard Au films with two different microstructures. The Au samples either have a grain size that is >50 nm or <20 nm. The same regions of the samples were measured with TKD apparatuses at 30 kV in an SEM with detectors in the horizontal and vertical configurations and in the TEM at 300 kV. Under the proper conditions, we demonstrate all three configurations can produce data of equivalent quality.Each method has strengths and challenges associated with its application and representation of the true microstructure. The conditions needed to obtain high-quality data for each acquisition method and the challenges associated with each will be discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Investigation on microstructures and phase transition characteristics of titanium/yttrium co-doped vanadium oxide thin films

Highlights: • Conjugated interaction between Ti{sup 4+} and Y{sup 3+} ions has been observed in Ti/Y codoped VO{sub 2} films. • The conjugated interaction causes the appearance of VO{sub 2} (B), even complete amorphization in Ti/Y co-doped VO{sub 2} thin film. • Ti/Y co-doping restrains the SMT feature of VO{sub 2} films. - Abstract: Co-doping with two elements has recently attracted attention as a novel approach for tailoring the semiconductor-metal transition (SMT) characteristics of vanadium dioxide (VO{sub 2}). Here, we investigate the influence of titanium/yttrium (Ti/Y) co-doping on the microstructure and SMT characteristics of VO{sub 2} thin films. At low Y concentration, Ti/Y co-doped VO{sub 2} thin films exhibit a monoclinic structure similar to VO{sub 2} but characterized by a smaller grain size, whereas, the VO{sub 2}(B) phase appears as the Y concentration is increased. Interestingly, even a complete amorphization of the film is obtained for co-doped VO{sub 2} thin films. The strong dependence of the microstructure upon the co-doping level is ascribed to the conjugated influence from the simultaneous adjustment of VV chains and VO bonds due to the existence of Ti{sup 4+} and Y{sup 3+} ions in VO{sub 2} lattice, respectively. As a result, the SMT feature of VO{sub 2} thin films is strongly limited or even fully disappears.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Enhanced properties of tungsten films by high-power impulse magnetron sputtering

Tungsten films (750–1200 nm thick) deposited by high-power impulse magnetron sputtering (HiPIMS) under various sputtering gas pressure and substrate bias are investigated for their physical and microstructural characteristics. Compared to films deposited by the traditional direct current (DC) method with the same deposition configuration and similar parameters, HiPIMS materials exhibit higher hardness, a smoother surface, and better adhesion to a substrate. These excellent properties are attributed to the highly uniform grain structures developed during HiPIMS deposition, in contrast to the funnel shaped grains seen in DC sputtered films. Finally, combined with the in-situ stress measurements, we discuss the underlying mechanisms that lead to enhanced properties of HiPIMS tungsten films.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Understanding the deposition mechanism of pulsed laser deposited B-C films using dual-targets

Boron carbide thin films with stoichiometry (boron-carbon atomic ratio) range of 0.1 ∼ 8.9 were fabricated via pulsed laser deposition by using boron-carbon dual-targets. However, this experimental data on stoichiometry were smaller than the computer simulation values. The discrepancy was investigated by studies on composition and microstructure of the thin films and targets by scanning electron microscopy, excitation laser Raman spectroscopy, and X-ray photoelectron spectroscopy. The results indicate that the boron liquid droplets were formed by phase explosion after laser irradiation on boron sector. Part of the boron droplets would be lost via ejection in the direction of laser beam, which is tilted 45° to the surface of substrate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Features of Pulsed Laser Annealing of BC{sub 3} Films on a Sapphire Substrate

The morphology, chemical composition, microstructure, and electrical properties of BC{sub 3} thin films subjected to melting by a nanosecond laser pulse are investigated. The original films have been created by pulsed laser codeposition of B and C onto a sapphire substrate at 150 and 350°C. Morphological changes in the films depended on their initial structural state. However, a “frozen” structure of both films after irradiation corresponded to the B-saturated graphite-like phase, the local composition of which varied due to the formation of inclusions of amorphous boron carbide. Before and after irradiation, the films exhibited a slightly decreasing dependence of the surface resistance with increasing temperature from 4.2 to 330 K. After laser irradiation, the films resistance has decreased by a factor of ~2.6.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

The Role of Side Chains and Hydration on Mixed Charge Transport in n ‐Type Polymer Films

Abstract Introducing ethylene glycol (EG) side chains to a conjugated polymer backbone is a well‐established synthetic strategy for designing organic mixed ion‐electron conductors (OMIECs). However, the impact that film swelling has on mixed conduction properties has yet to be scoped, particularly for electron‐transporting (n‐type) OMIECs. Here, the authors investigate the effect of the length of branched EG chains on mixed charge transport ofn‐type OMIECs based on a naphthalene‐1,4,5,8‐tetracarboxylic‐diimide‐bithiophene backbone. Atomic force microscopy (AFM), grazing‐incidence wide‐angle X‐ray scattering (GIWAXS), and scanning tunneling microscopy (STM) are used to establish the similarities between the common‐backbone films in dry conditions. Electrochemical quartz crystal microbalance with dissipation monitoring (EQCM‐D) and in situ GIWAXS measurements reveal stark changes in film swelling properties and microstructure during electrochemical doping, depending on the side chain length. It is found that even in the loss of the crystallite content upon contact with the aqueous electrolyte, the films can effectively transport charges and that it is rather the high water content that harms the electronic interconnectivity within the OMIEC films. These results highlight the importance of controlling water uptake in the films to impede charge transport inn‐type electrochemical devices.

Chemistry↗
DOE OSTI2015

Structural modification of nanocrystalline diamond films via positive/negative bias enhanced nucleation and growth processes for improving their electron field emission properties

Electron field emission (EFE) properties of nanocrystalline diamond (NCD) films synthesized by the bias-enhanced growth (beg) process under different bias voltages were investigated. The induction of the nanographitic phases is presumed to be the prime factor in enhancing the EFE properties of negative biased NCD films. Transmission electron microscopic investigations reveal that a negative bias voltage of −300 V increases the rate of growth for NCD films with the size of the grains changing from nano to ultranano size. This effect also is accompanied by the induction of nanographitic filaments in the grain boundaries of the films. The turn-on field (E{sub 0}) for the EFE process then effectively gets reduced. The EFE process of the beg-NCD{sub −300V} films can be turned on at E{sub 0} = 3.86 V/μm, and the EFE current density achieved is 1.49 mA/cm{sup 2} at an applied field of 7.85 V/μm. On the other hand, though a positive-bias beg process (+200 V) results in the reduction of grain size, it does not induce sufficient nanographitic phases to lower the E{sub 0} value of the EFE process. Moreover, the optical emission spectroscopic investigation indicates that one of the primary causes that changes the granular structure of the NCD films is the increase in the proportion of C{sub 2} and CH species induced in the growing plasma. The polarity of the bias voltage is of less importance in the microstructural evolution of the films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

RF Results of Nb Coated SRF Accelerator Cavities via HiPIMS

Bulk Niobium (Nb) SRF (superconducting radio frequency) cavities are currently the preferred method for acceleration of charged particles at accelerator facilities around the world. However, bulk Nb cavities have poor thermal conductance and impose material and design restrictions on other components of a particle accelerator. Since the SRF phenomena occurs within a shallow depth of 40 nm (for Nb), a proposed solution to this problem has been to deposit a superconducting Nb thin film on the interior of a cavity made of a suitable alternative material such as copper or aluminum. While this approach has been attempted in the past using DC magnetron sputtering (DCMS), such cavities have never performed at the bulk Nb level. However, new energetic condensation techniques for film deposition offer the opportunity to create suitably thick Nb films with improved density, microstructure and adhesion compared to traditional DCMS. One such technique that has been developed somewhat recently is ?High Power Impulse Magnetron Sputtering? (HiPIMS). Here we report early results from various thin film coatings carried out on 1.3 GHz Cu cavities, a 1.5 GHz Nb cavity, and small Cu coupon samples coated at Jefferson Lab using HiPIMS.

Burton, Matthew Creed↗
DOE OSTI2018

Microstructural study and simulation of intrinsic two-way shape memory behavior of functionally graded Ni-rich/NiTiCu thin film

Highlights: • Ni-rich/Ti-rich bi-layer thin film was deposited on Si by using DC magnetron sputtering. • The bi-layer exhibits the gradient structure and mechanical properties through the thickness. • The bi-layer shows intrinsic two-way shape memory effect due to functionally graded structure. • The intrinsic two-way shape memory effect was confirmed by finite element simulation. - Abstract: In this research, the gradient structure and mechanical properties of an austenitic/martensitic (Ni{sub 50.8}Ti/Ni{sub 45}TiCu{sub 5} (at.%)) bi-layer thin film was investigated. The bi-layer was deposited on a Si substrate using DC magnetron sputtering. After crystallization of the film at 773 K for 60 min, the microstructure and mechanical properties of the bi-layer thin film were characterized using X-ray diffraction (XRD), transmission electron microscopy (STEM and HRTEM) and nanoindentation, respectively. The diffraction pattern illustrated that the crystallized bi-layer was combined of martensitic and austenitic layers while secondary ion mass spectroscopy (SIMS) and high resolution transmission electron microscopy analysis demonstrated the existence of a compositional gradient through the thickness and residual strain in the interface of the bi-layer, respectively. Furthermore, the compositional gradient in the bi-layer led to gradual variations in the structure, hardness and Young's modulus through the thickness of the bi-layer. The intrinsic two-way shape memory effect due to its functionally graded structure and the induced stress was confirmed by experimental test and finite element simulation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Enhanced thermal stability by introducing TiN diffusion barrier layer between W and SiC

The combination of W and SiC has many applications such as a hot cell of a thermionic energy converter, nuclear material, and high temperature microelectronics. In this study, a 2 µm thick TiN film is introduced as a diffusion barrier between SiC and W to avoid the inter-diffusion reaction at high temperature. Additionally, the effect of annealing temperature on the surface morphology and microstructure of the TiN film is studied to explore its high temperature stability. Then 500 nm W film is sputtered on the TiN film to characterize the inter-diffusion and stability of the W/TiN/SiC multilayer at 1100°C by XRD, Raman spectroscopy and cross-sectional EDS mapping techniques. The results indicate that the W/TiN/SiC multilayer is very stable even when heated at 1100°C for 25 hours.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics↗
DOE OSTI2019

Effects of Silicon Content on the Microstructures and Mechanical Properties of (AlCrTiZrV)-Si x -N High-Entropy Alloy Films

A series of (AlCrTiZrV)-Si x -N films with different silicon contents were deposited on monocrystalline silicon substrates by direct-current (DC) magnetron sputtering. The films were characterized by the X-ray diffractometry (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and nano-indentation techniques. The effects of the silicon content on the microstructures and mechanical properties of the films were investigated. The experimental results show that the (AlCrTiZrV)N films grow in columnar grains and present a (200) preferential growth orientation. The addition of the silicon element leads to the disappearance of the (200) peak, and the grain refinement of the (AlCrTiZrV)-Si x -N films. Meanwhile, the reticular amorphous phase is formed, thus developing the nanocomposite structure with the nanocrystalline structures encapsulated by the amorphous phase. With the increase of the silicon content, the mechanical properties first increase and then decrease. The maximal hardness and modulus of the film reach 34.3 GPa and 301.5 GPa, respectively, with the silicon content (x) of 8% (volume percent). The strengthening effect of the (AlCrTiZrV)-S ix -N film can be mainly attributed to the formation of the nanocomposite structure.

(AlCrTiZrV)-Six-N films↗
NASA NTRS1999

Characterization of (Ba(0.5)Sr(0.5)) TiO3 Thin Films for Ku-Band Phase Shifters

The microstructural properties of (Ba(0.5)Sr(0.5)TiO3) (BSTO) thin films (300, 700, and 1400 nm thick) deposited on LaAlO3 (LAO) substrates were characterized using high-resolution x-ray diffractometry. Film crystallinity was the parameter that most directly influenced tunability, and we observed that a) the crystalline quality was highest in the thinnest film and progressively degraded with increasing film thickness; and b) strain at the film/substrate interface was completely relieved via dislocation formation. Paraelectric films such as BSTO offer an attractive means of incorporating low-cost phase shifter circuitry into beam-steerable reflectarray antennas.

Mueller, Carl H.↗