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At least 307 records · Page 17

Stress Compensating Multilayers

We present in-situ stress measurement results for single and multilayer thin-films deposited by magnetron sputtering. In particular, we report on the influence of the material interfaces on the ensuing stress in both the transient and steady-state regimes of film growth. This behavior is used to determine the appropriate thicknesses of the constituent layers that will result in a net tensile stress in multilayers composed of various material combinations. These multilayers can then be used to compensate the compressive integrated stress in single and multilayer EUV and x-ray optical coatings. The use of multilayers to compensate the integrated stress might be advantageous because, unlike single layers of chromium, the roughness is not expected to increase with the total thickness of the multilayer. In this paper, we demonstrate the technique for W/Si and Mo/Si multilayers and discuss its application to other material combinations.

Multilayer↗

Effect of Pre- and Post-Coat Processing on the Fatigue Life of Coated Disk Alloys

Increasing temperatures in aero gas turbines is resulting in oxidation and hot corrosion attack of turbine disks. Since disks are sensitive to low cycle fatigue (LCF), any environmental attack, and especially hot corrosion pitting, can seriously degrade the life of the disk. Application of metallic coatings is one means of protecting disk alloys from this environmental attack. However, since LCF is sensitive to surface conditions, pre- and post-coat processing can have a significant effect on the LCF life of coated bars. Various pre-and post-coating conditions were examined with a Ni-45wt. Cr coating applied by High-power impulse magnetron sputtering (HiPiMS) to a Ni-based disk alloy. Initial pre-coat surface conditions examined a grit blasted surface. Later pre-coat surface treatments involved wet blasting, two shot peening levels (8N-200 and 16N-200) and a highly polished surface. Post-coat treatments involved two shot peening levels (4N-100 and 16N-200) and a post-coat diffusion anneal in high purity Ar or a low PO2 environment to encourage chromia scale formation. Half of the coated and uncoated bars were LCF tested at 760C without further environmental exposure to evaluate the pre- and post-coat treatments. The second half of samples were either oxidized for 500 hours at 760C in air, hot corroded for 50 hours at 760C in air using a Na2SO4-MgSO4 salt, or subjected to both exposures. Results of the LCF testing and post-test characterization of the various coatings will be presented and future research directions discussed.

LCF Life↗

Supermirror Design for Hard X-Ray Telescopes On-Board Hitomi (ASTROH)

We designed depth-graded multilayers, so-called supermirrors, with platinum/carbon (Pt/C) layer pairs for the Hard X-Ray Telescope (HXT) that was on-board the sixth Japanese X-Ray Astronomy Satellite Hitomi (ASTRO-H). The HXT has multinested thin foil optics, and the grazing angles of the x-ray mirrors are 0.07 to 0.27 deg. Supermirrors for HXTs are designed to provide a broad energy response (up to 80 keV) for astronomical requests. Under practical boundary conditions, we establish a block method applying empirical rules to maximize the integrated reflectivity. We fabricated Pt/C supermirrors using a DC magnetron sputtering system. The reflectivity of the mirrors was measured in a synchrotron radiation facility, SPring-8. We describe the design method for the supermirrors and our results.

Tamura, Keisuke↗

Reflective Coatings for the Future X-Ray Mirror Substrates

We present the development of the reflective coating by magnetron sputtering deposition onto precisely-fabricated thin X-ray mirrors. Our goal is to remove distortion induced by the coating and then keep their surface pro les. We first addressed the uniform coating to minimize the distortion by introducing a mask to control the spatial distribution of the coating thickness. The uniformity was finally achieved within 1%. We next tried a platinum single-layer coating on a glass substrate with a dimension of 200 mm 125 mm. The distortion caused by the frontside coating with a thickness of 320 A was found to be at most 1 m, smaller than the previous results obtained from the non-uniform coating. We then carried out the platinum coating with the same amount of the thickness on the backside surface of the glass substrate. The surface pro le of the glass substrate was fully recovered, indicating that the residual stress was successfully balanced by the backside coating. Furthermore, we tried to an iridium single-layer coating with a thickness of 150 Aon the silicon mirrors. The frontside coating caused the degradation of the imaging quality by 7:5 arcsec in half-power width. However, the backside coating with the same amount of the thickness reduced this degradation to be 3:4 arcsec. Finally, an additional backside coating with a thickness of 100 A and the annealing to relax the residual stress were found to eliminate the distortion completely; the final degradation of the imaging quality was only 0:4 arcsec.

Mori, Hideyuki↗

LCF Life of As-Deposited and Annealed NiCr-Y Coatings for Oxidation and Hot Corrosion Protection of Disk Alloys

Increasing temperatures in aero gas turbines is resulting in oxidation and hot corrosion attack of turbine disks. Since disks are sensitive to low cycle fatigue (LCF), any environmental attack, and especially hot corrosion pitting, can seriously degrade the life of the disk. Application of metallic coatings is one means of protecting disk alloys from this environmental attack. However, the presence of a metallic coating can degrade the LCF life of a disk alloy. Therefore, coatings must be designed which are not only resistant to oxidation and corrosion attack, but do not significantly degrade the LCF life of the alloy.Three different NiCr-Y coating compositions (29, 35.5, 44 wt.% Cr, all with 0.1 wt.% Y) were applied at two thicknesses by Plasma Enhanced Magnetron Sputtering (PEMS) to two similar Ni-based disk alloys. One Ni-35.5Cr-0.1Y coating also received a thin ZrO2 overcoat. The coated samples were also given a short thermal anneal in a low PO2 environment to encourage bonding of the coating and substrate as well as initiating formation of a chromia scale. Without further environmental exposure, the LCF life of coated and uncoated samples was evaluated at 760°C in air. The LCF lifetime of all coated samples was less than that of uncoated samples. The LCF life scaled with the Cr content and the high-Cr, thin coating showed the highest LCF life. Pre and post-test characterization of the various coatings, including identification of crack initiation sites, will be presented and the effect of the coating on the LCF life discussed.

low cycle fatigue↗

LCF Life of NiCr-Y Coated Disk Alloys After Shot Peening, Oxidation and Hot Corrosion

In a prior companion study (Ref. 1), three different Ni-Cr coating compositions (29, 35.5, 45 wt% Cr) were applied at two thicknesses by Plasma Enhanced Magnetron Sputtering (PEMS) to two similar Ni-based disk alloys. One coating also received a thin ZrO2 overcoat. The low cycle fatigue (LCF) life of each coating was determined at 760 °C and was less than that of the uncoated specimens. In this followon effort, shot peening was examined as a means to improve the as-deposited coating morphology as well as impart a residual compressive stress in the near-surface region. After evaluating the effect of the shot peening on the LCF life, the effectiveness of the shot-peened coating in protecting the disk alloy from oxidation and hot corrosion attack was evaluated. This evaluation was accomplished by exposing coated and shot-peened specimens to 500 h of oxidation followed by 50 h of hot corrosion, both at 760 °C in air. These exposed specimens were then tested in fatigue and compared to similarly treated and exposed uncoated specimens. For all cases, shot peening improved the LCF life of the coated specimens. More specifically, the highest Cr coating showed the best LCF life of the coated specimens after shot peening, as well as after the environmental exposures. Characterization of the coatings after shot peening, oxidation, hot corrosion and LCF testing is presented and discussed.

James A Nesbitt↗

Improving Qubit Coherence Time Through Detailed Materials Analysis

This study investigates the defects, imperfections, and variations in Nb thin films deposited on sapphire substrates. Two samples, W114 and W118, were fabricated using DC Magnetron Sputtering and Electron Cyclotron Resonance (ECR), respectively. Each sample was analyzed at five distinct spots to compare elemental homogeneity and variations in oxide layers. Scanning Electron Microscopy (SEM) was employed to examine surface morphology, while Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) provided elemental and chemical state analyses. SEM revealed distinct structures in W114 and a uniform surface in W118. EDS showed higher aluminum signals in W118, indicating a thinner film in comparison to W114. XPS detected a higher Nb₂O₅ signal in W118, in comparison to W114, which can be attributed to the presence of a thicker Nb₂O₅ layer in W118. These findings highlight the critical role of precise material characterization in advancing quantum computing technologies.

Rosado Bonilla, Cristy M.↗

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↗

Optical and Electrical Properties of Reactively Sputtered TiN, ZrN, and HfN Thin Films

Thin films of titanium, zirconium, and hafnium nitride are prepared by DC magnetron reactive sputtering at room temperature on fused silica, optical glass, and silicon substrates. Deposition parameters are investigated in order to obtain stoichiometric films. The optical and electrical properties of the films as a function of nitrogen partial pressure are determined. The results show that an inverse correlation exists between the optical reflectance and the electrical resistivity of the films. Ellipsometer data for all three films show that their refractive index in the visible spectrum is decreased by increasing the film thickness while the extinction coefficient is unchanged. Thin films of TiN have the lowest room temperature resistivity relative to ZrN and HfN thin films.

Reactive↗

High-throughput synthesis and corrosion behavior of sputter-deposited nanocrystalline Al x (CoCrFeNi) 100-x combinatorial high-entropy alloys

High-entropy alloys (HEAs) are inherently complex and potentially span a vast composition space, making their research and discovery challenging. In the present study, high-throughput synthesis of an Al x (CoCrFeNi) 100-x combinatorial material library covering x = 4.5–40 atomic percent Al is achieved, using magnetron cosputtering. The effects of Al on the microstructure and corrosion behavior are investigated. With the increased amount of Al, crystal-structures of thin films transform from face-centered cubic (FCC) to body-centered cubic (BCC). Both the FCC and BCC thin films demonstrate a uniform elemental distribution. Corrosion characteristics of combinatorial samples immersed in the 3.5 wt% (wt%) NaCl solution are evaluated via electrochemical tests. Complementary X-ray photoelectron spectroscopy analysis reveals the compositional variation of passivated films formed on the sample surface after immersion. The results show that the Al x (CoCrFeNi) 100-x HEA thin films possess outstanding corrosion-resistant properties, but the resistance diminishes with the increasing Al content. The decreased corrosion resistance is revealed to be directly related to the constituents of passivated films.

36 MATERIALS SCIENCE↗

Fabrication of superconducting Nb 3 Sn film by Co-sputtering

High-efficiency SRF cavities are the key technology to construct cost-effective CW SRF accelerators. Improvements in the efficiency of SRF cavities are realized by using novel materials, such as niobium-tin. Advances in niobium-tin coatings on the inner surface of SRF cavities showed the potential for this material to increase the operating temperature of the SRF cavity to above 4 K, leading to significant reduction of the capital and operating cost of SRF accelerators. Among the techniques used to apply the niobium-tin coating to the surface of the SRF cavity is sputtering. Old Dominion University, Jefferson Lab, and Fermilab are collaborating on developing an optimized niobium-tin coating of the inside surface of niobium SRF cavities using a recently-developed cylindrical sputtering system. This research will result in optimized sputtering coating techniques leading to high efficiency SRF structures.

42 ENGINEERING↗

Antiferromagnetic Oxide Thin Films for Spintronic Applications

Antiferromagnetic oxides have recently gained much attention because of the possibility to manipulate electrically and optically the Néel vectors in these materials. Their ultrafast spin dynamics, long spin diffusion length and immunity to large magnetic fields make them attractive candidates for spintronic applications. Additionally, there have been many studies on spin wave and magnon transport in single crystals of these oxides. However, the successful applications of the antiferromagnetic oxides will require similar spin transport properties in thin films. In this work, we systematically show the sputtering deposition method for two uniaxial antiferromagnetic oxides, namely Cr2O3 and α-Fe2O3, on A-plane sapphire substrates, and identify the optimized deposition conditions for epitaxial films with low surface roughness. We also confirm the antiferromagnetic properties of the thin films. The deposition method developed in this article will be important for studying the magnon transport in these epitaxial antiferromagnetic thin films.

36 MATERIALS SCIENCE↗

The physical origin of heterogeneous solute clustering and nanoprecipitation at grain boundaries in ultrafine-grained immiscible alloys

Here, grain-boundary segregation effects on heterogeneous solute clustering and nanoprecipitation at low solute concentrations were investigated in sputter-deposited ultrafine-grained Ag-Cu alloy films. X-ray diffraction and scanning transmission electron microscopy revealed extended solubility of Cu in Ag matrix, accompanied by the formation of Cu-rich nanoprecipitates and solute clusters at grain boundaries and their junctions. Atomistic simulations further demonstrated that Cu solutes heterogeneously segregate to Ag GBs and form small clusters that grow into nuclei for Cu nanoprecipitates. These findings provide critical insights into the role of heterogeneous grain-boundary segregation in governing the phase separation pathways of immiscible nanocrystalline and ultrafine-grained alloys.

Heterogeneous segregation↗

TOF-SIMS analysis of decoherence sources in superconducting qubits

Superconducting qubits have emerged as a potentially foundational platform technology for addressing complex computational problems deemed intractable with classical computing. Despite recent advances enabling multiqubit designs that exhibit coherence lifetimes on the order of hundreds of μs, material quality and interfacial structures continue to curb device performance. Two-level system defects in the thin superconducting film and adjacent dielectric regions introduce stochastic noise and dissipate electromagnetic energy at the cryogenic operating temperatures. In this study, we utilize time-of-flight secondary ion mass spectrometry to understand the role specific fabrication procedures play in introducing such dissipation mechanisms in these complex systems. We interrogated Nb thin films and transmon qubit structures fabricated through slight modifications in the processing and vacuum conditions. We find that when the Nb film is sputtered onto the Si substrate, oxide and silicide regions are generated at various interfaces. We also observe that impurity species, such as niobium hydrides and carbides, are incorporated within the niobium layer during the subsequent lithographic patterning steps. The formation of these resistive compounds likely impacts the superconducting properties of the Nb thin film. Additionally, we observe the presence of halogen species distributed throughout the patterned thin films. We conclude by hypothesizing the source of such impurities in these structures in an effort to intelligently fabricate superconducting qubits and extend coherence times moving forward.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

X-ray photoelectron spectroscopy and rotating disk electrode measurements of smooth sputtered Fe-N-C films

Electrocatalysts for the oxygen reduction reaction (ORR) based on complexes of iron and nitrogen in a carbon matrix (Fe-N-C) are a promising alternative to platinum group metal (PGM) based catalysts in polymer electrolyte membrane (PEM) fuel cells. Further improvements of Fe-N-C catalysts would benefit from model thin film studies of activity and stability of catalytic sites, but synthesis of Fe-N-C model thin films is challenging. Here we report on synthesis and characterization of Fe-N-C thin films produced by co-sputtering iron and carbon in a reactive nitrogen atmosphere onto removable glassy carbon rotating disk electrode (RDE) tips. Scanning electron microscopy (SEM) measurements indicate that the Fe-N-C films deposited at high temperature are smoother than the films annealed at high temperature. Electrocatalytic activity measured on the thin Fe-N-C films is greater for both high-temperature samples than for the room-temperature sample. From the analysis of X-ray photoelectron spectroscopy (XPS) data, exposure of the films to high temperatures results in increased graphitization of the carbon with the Fe-N-C films, and increased relative amount of graphitic and hydrogenated nitrogen species. Overall the results of this study demonstrate the feasibility of a thin film model system approach for studying active sites in PGM-free catalysts.

14 SOLAR ENERGY↗

Structural characterization of highly alloyed (Al,Gd)N thin films

Highly alloyed (Al,Gd)N is of potential interest in a variety of applications, including neutron detection and in devices such as non-volatile memory. Gd has been shown to have very low equilibrium solubility in AlN at room temperature; however, non-equilibrium deposition techniques such as sputtering are able to deposit thin films, which incorporate large amounts of Gd. Here, we characterize a highly-alloyed (Al,Gd)N combinatorial thin film grown by RF sputtering on a GaN substrate, looking for any evidence of chemical or phase segregation or structural disorder in the films. Compositions with between 13% and 32% Gd (on a cation basis) were studied. No evidence was found for chemical or phase segregation in any studied composition. Higher degrees of Gd incorporation led to greater structural disorder in the film and a tendency toward amorphization; however, electron diffraction shows that the film does not become fully amorphous at any of the studied compositions, instead retaining textured local order even at 32% Gd. Electron energy loss spectra suggest that the material retains a locally wurtzite-like tetrahedral bonding environment at all studied compositions.

36 MATERIALS SCIENCE↗

Sputter deposition of ultrathick Bi coatings onto rotating substrates for inertial confinement fusion

Sputter-deposited Bi is a potential candidate material for the production of inertial confinement fusion (ICF) hohlraums, which are sphero-cylindrical canisters that serve as the housing for hydrogen-fuel-filled capsules in ICF implosions. The fabrication of hohlraums involves deposition onto rotating sphero-cylindrical substrates and, hence, requires an understanding of oblique angle deposition phenomena. Here, we systematically study the effect of dynamic substrate tilt on properties of Bi films deposited onto rotating planar substrates. Results show that film morphology, porosity, and electrical resistivity depend on substrate tilt. In comparison with films deposited onto substrates adhered to a stationary sample holder, films deposited on rotating substrates have more uniform microstructure with fewer void defects. Based on Monte Carlo simulations, these changes in film morphology and microstructure are attributed to averaging and geometric effects related to sample position and rotation. In conclusion, the fabrication of an ∼ 50-µm-thick Bi film on a rotating sphero-cylindrical mandrel demonstrates a significant step toward the production of Bi hohlraums.

Bismuth↗