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At least 127 records · Page 7

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DOE OSTI2019

Magnetron-Sputtered Ni-Cr and Ti-Si Layers to Protect Ti-46Al-8Nb (at.%) Substrates Against Gas Absorption

Ni-Cr and Ti-Si layers were deposited by magnetron sputtering on Ti-46Al-8Nb (at.%) substrates to suppress penetration of gases, which brings about undesirable changes in mechanical properties. Alloy samples with and without surface protection were subjected to interrupted oxidation at elevated temperature (700 and 800 °C) for up to 300 h. Selected mechanical properties as well as adhesion of surface layers were examined in the as-received and oxidized state. Analytical techniques used to characterize surfaces and cross sections of the samples included scanning electron microscopy and light microscopy, energy-dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy and x-ray diffraction. Both investigated layers were sufficiently adherent and effective in hindering gas absorption at 700 °C; however, only Ni-Cr showed promising properties for higher-temperature applications.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Grid-assisted magnetron sputtering deposition of nitrogen graded TiN thin films

Titanium Nitride (TiN) films were obtained using the grid-assisted magnetron sputtering deposition technique on Al substrates in two conditions: under constant and variable nitrogen concentration along the thin solid film thickness. The formation of a film with variable N concentration (herein referred as graded film) was confirmed using energy filtered transmission electron microscopy, X-ray photoelectron spectroscopy and grazing incidence X-ray diffraction. The TiN thin films microstructures were also analysed using scanning and transmission electron microscopies (SEM and TEM). Finally, the viability of synthesizing TiN thin films with variable N concentration is herein proposed as an alternative method for tailoring the properties of such functional coating materials.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Synthesis and characterization of dense Gd 2 Ti 2 O 7 pyrochlore thin films deposited using RF magnetron sputtering

Thin films of phase-pure pyrochlore Gd 2 Ti 2 O 7 have been synthesized by RF magnetron sputtering. The films were prepared from oxide targets in 50% O 2 /Ar atmosphere and deposited on 111 yttria-stabilized zirconia (YSZ) substrates at a temperature of 800 °C. The pyrochlore structure was confirmed via grazing angle X-ray diffraction and selected area electron diffraction (SAED). Transmission electron microscopy (TEM) analysis also showed that the films were dense and of uniform thickness with surface roughness of approximately 8 nm. The total conductivity measured with AC impedance spectroscopy was found to be independent of thickness and comparable in magnitude to that of bulk Gd 2 Ti 2 O 7 . Differences were observed in the Arrhenius behavior between the bulk and thin film samples and are attributed to varying states of order in the crystalline lattice compounded by different levels of background impurities.

36 MATERIALS SCIENCE↗

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 OSTI2016

Neutron reflectometry investigations of interfacial structures of Ti/TiN layers deposited by magnetron sputtering

We report that nanolayered metal-ceramic composite systems provide the possibility to produce new materials with exceptional strength, toughness, and radiation resistance not exhibited by their individual constituents. The unusual behaviors are frequently attributed to the high density of internal interfaces. Most layered structures studied to date contain sharp interfaces and the synthesis of more diffuse interfacial structures, where the interface is graded out of the interface plane, has not been deeply explored. Here we show how neutron reflectometry was used to study the structure of magnetron sputter deposited titanium and titanium nitride (Ti/TiN) layers as a function of deposition parameters: temperature, rate of N 2 flow or pressure, electrical bias applied to the sample, and orientation of the ion source relative to the sample. These different deposition and post-processing strategies resulted in profound changes in the structure of the interfacial region between the two components in Ti/TiN x bilayers. Finally, the results show that temperature and low step-wise N 2 flow rates, but not electrical bias, can form graded interfaces in a controlled manner.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Commissioning of a modulated pulse-power magnetron sputtering system for depositing niobium thin films

A modulated pulse-power magnetron sputtering system (MPPMS) was commissioned and used to deposit niobium on copper. MPPMS utilizes a modulated pulse train with high peak-to-average energy ratios, thereby increasing the energy density leading to the production of the energetic ions. The MPPMS modulator was designed and constructed based on large voltage/current IGBT modules, which can be externally modulated, produce bi-polar waveforms, and are readily available. A high voltage power supply provides moderate current to the IGBT module to create the precise pulse structure. The MPPMS system was used to deposit ~1 mm thick, niobium film on a copper substrate held at ~77 K to minimize Nb atom surface diffusion and maximize intrinsic film energy. Finally, the Nb film had an average grain size of ~8 nm.

42 ENGINEERING↗

DOE OSTI2017

Advanced, phase-locked, 100 kW, 1.3 GHz magnetron

Calabazas Creek Research, Inc., in collaboration with Fermilab and Communications & Power Industries, LLC, is developing a phase-locked, 100 kW peak, 10 kW average power magnetron-based RF system for driving accelerators. Here, phase locking will be achieved using an approach originating at Fermilab that includes control of both amplitude and phase on a fast time scale.

43 PARTICLE ACCELERATORS↗

DOE OSTI2023

Effect of substrate and growth method on vanadium dioxide thin films by RF magnetron sputtering: Vanadium metal oxidation vs reactive sputtering

Vanadium dioxide (VO 2 ) undergoes a metal–insulator phase transition at ~70 °C and has attracted substantial interest for potential applications in electronics, including those in neuromorphic computing. The vanadium–oxygen system has a rather complicated phase diagram, and controlling the stoichiometry and the phase of thin films of vanadium oxides is a well-known challenge. Here, we explore the novel combination of two methods of VO 2 thin film deposition using off-axis RF magnetron sputtering on (100)- and (111)-oriented yttria-stabilized zirconia (YSZ) substrates: reactive sputtering of vanadium in an oxygen environment and sputtering of vanadium metal followed by oxidation to VO 2 . Interestingly, the reactive sputtering process on both substrate orientations yields the metastable semiconducting VO 2 (B) phase, which is structurally stabilized by the YSZ surface. The metal sputtering and oxidation process on YSZ produces mainly the equilibrium monoclinic (or M1) phase of VO 2 that exhibits a metal–insulator transition. Using this method, we obtained thin films of (010)-textured polycrystalline VO 2 (M1) that show a metal–insulator transition with an on/off ratio larger than 1000.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Transition from retrograde to prograde drift instabilities in a magnetron microdischarge

Rotating plasma structures, or “spokes,” in magnetized discharges characterized by perpendicular electric and magnetic fields have been seen in a growing number of studies and are believed to be the result of gradient-driven drift instabilities. Under certain conditions, we have shown the spoke’s rotation to be opposite to the E B direction, i.e., retrograde in its expected direction. Recently, we have linked such counter-intuitive rotation to a local inversion of the electric field. Here, we give further experimental evidence for this inversion and attempt to provide an explanation for a relatively distinct transition seen between retrograde and positive (prograde) drift. In the experiments, a partially magnetized plasma forms inside a magnetron device of mm radius operated with argon. Discharge current–voltage measurements are acquired for a range of argon fill pressure and inter-electrode spacing. We find two branches of operation—a low current branch of negative resistance, coinciding with the retrograde spoke rotation, and a higher current branch of positive resistance, coincident with prograde spoke rotation. We postulate that at low discharge currents, high magnetic field confinement leads to a large density gradient, causing more electron transport to the anode than that demanded by the external circuit. At higher currents, anomalous axial electron transport (across the magnetic field lines) becomes dominant, eliminating the conditions for field inversion. Here, the current thresholds for the field inversion are found to be sensitive to the argon pressure and inter-electrode spacing.

42 ENGINEERING↗

DOE OSTI2023

Coherent fluctuations in a partially magnetized small magnetron discharge operating on molecular nitrogen

We report experimental data on rotating plasma disturbances in a quasi-steady direct-current magnetron discharge operating with molecular nitrogen at pressures of 27, 40, 67, and 133 Pa. Experiments with a segmented anode measuring the local current flow reveal up to 12 coherent structures (“spokes”) propagating in the +E×B and −E×B azimuthal directions. The current–voltage characteristics are studied and found to follow a negative resistance profile at the lower discharge currents. The existence of coherent structures and the number of spokes observed depend on the discharge current and operating pressure. Lower pressures are more favorable to the retrograde −E×B spoke rotation, which is observed in the 27, 40, and 67 Pa discharges. The results are interpreted with a gradient-driven drift wave model, and using the dispersion relation, we show that the propagation direction depends on the orientation of the local electric field within the plasma. Using an electron fluid model, we show how experimental conditions can lead to field reversals that generate −E×B spoke rotation in the lower pressure discharges.

Physics↗

DOE OSTI2026

Combinatorial deposition of Au–Bi alloys via high-rate magnetron sputtering

Gold–bismuth (Au–Bi) alloy films are promising candidate materials for inertial confinement fusion (ICF) hohlraums due to their high laser-to-x-ray conversion efficiency, particularly compared with Au, Ta–Au, and Bi hohlraums. However, the fabrication of uniform and dense Au–Bi alloy films remains a challenge. Here, we use a combination of Monte-Carlo modeling and experiments to demonstrate that the microstructure and properties of Au–Bi alloy films can be greatly improved when direct-current magnetron sputtering with high deposition rates of ⩾5 μm h -1 is used. Resultant films are ~90% of their maximum theoretical densities and have low O content of <1 at.%. Films with Bi content above 40 at. % exhibit high electrical resistivity >100μΩ cm, making them suitable for both magnetized and non-magnetized ICF schemes.

Materials science↗

DOE OSTI2017

Structural and compositional characterization of RF magnetron cosputtered lithium silicate films: From Li2Si2O5 to lithium-rich Li8SiO6

In this study, the structure and composition of lithium silicate thin films deposited by radio-frequency magnetron cosputtering are investigated. Five compositions ranging from Li2Si2O5 to Li8SiO6 were confirmed by inductively coupled plasma-optical emission spectroscopy, and structural analysis on the evolution of nonbridging oxygens in the thin films was conducted using Fourier transform infrared spectroscopy. It was found that nonbridging oxygens increased as the silicate network breaks apart with the increasing lithium content, which agrees with previous studies on lithium silicates. Thin film impurities were examined using x-ray photoelectron spectroscopy and time of flight secondary ion mass spectroscopy and traced back to target synthesis. This study utilizes a unique synthesis technique for lithium silicate thin films that can be used to model the lithium silicates formed on the surface of silicon anodes in lithium ion batteries and can bridge the understanding between this layer and the influence of silicates on ionic conductivity of the silicon interphase layer.

Coyle, Jaclyn↗

DOE OSTI2018

MAGNETRON SPUTTERING OF Nb3Sn FOR SRF CAVITIES

Nb3Sn is a potential candidate for surface material of SRF cavities since it can enable the cavity to operate at higher temperatures with high quality factor and at an increased accelerating gradient. Nb-Sn films were deposited using magnetron sputtering of individual Nb and Sn targets onto Nb and sapphire substrates. The as-deposited films were annealed at 1200 °C for 3 hours. The films were characterized for their structure by X-ray Diffraction (XRD), morphology by Field Emission Scanning Electron Microscopy (FESEM), and composition by Energy Dispersive X-ray Spectroscopy (EDS) and Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS). The surface resistivity was measured down to cryogenic temperature to determine the superconducting transition temperature and its width. The composition of the multilayered films was controlled by varying the thickness of the Nb and Sn layers. The films showed crystalline Nb3Sn phases with Tc up to 17.6 K.

Eremeev, G.↗

DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb-Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 µm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 ? 18 K. Here, we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

Shakel, M.S.↗

DOE OSTI2023

First Results From Nb3Sn Coatings of 2.6 GHz Nb SRF Cavities Using DC Cylindrical Magnetron Sputtering System

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb- Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 μm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 – 18 K. Here we present the commissioning experience, s ystem optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

Shakel, M. S.↗

DOE OSTI2022

Tantalum Suboxide Films with Tunable Composition and Electrical Resistivity Deposited by Reactive Magnetron Sputtering

Tantalum-based films with tailored composition, density, and electrical resistivity are of interest for next generation hohlraums for magnetized indirect-drive inertial confinement fusion. Here, we use reactive direct-current magnetron sputtering to deposit tantalum suboxide films with O content in the range of 46–71 at.%. In contrast to a common approach involving varying reactive gas contents, compositional control is achieved kinetically by changing the total chamber pressure and the deposition rate, while keeping the working gas mix of Ar-5%O2 constant. The resultant films are X-ray amorphous with electrical resistivity varying by over seven orders of magnitude. The dominant conduction mechanism changes from metallic to activated tunneling above ∼55 at.% of O, which is characterized by a sharp increase in resistivity and a decrease in the carrier density at low temperatures.

36 MATERIALS SCIENCE↗

DOE OSTI2019

High Strength and Deformation Mechanisms of A l0.3 CoCrFeNi High-Entropy Alloy Thin Films Fabricated by Magnetron Sputtering

Recently, high-entropy alloy thin films (HEATFs) with nanocrystalline structures and high hardness were developed by magnetron sputtering technique and have exciting potential to make small structure devices and precision instruments with sizes ranging from nanometers to micrometers. However, the strength and deformation mechanisms are still unclear. In this work, nanocrystalline Al0.3CoCrFeNi HEATFs with a thickness of ~4 μm were prepared. The microstructures of the thin films were comprehensively characterized, and the mechanical properties were systematically studied. It was found that the thin film was smooth, with a roughness of less than 5 nm. The chemical composition of the high entropy alloy thin film was homogeneous with a main single face-centered cubic (FCC) structure. Furthermore, it was observed that the hardness and the yield strength of the high-entropy alloy thin film was about three times that of the bulk samples, and the plastic deformation was inhomogeneous. Our results could provide an in-depth understanding of the mechanics and deformation mechanism for future design of nanocrystalline HEATFs with desired properties.

36 MATERIALS SCIENCE↗