High Power 650 MHz Magnetron RF Power Source
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Kroc, Thomas K.↗
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Precision Ion Energy and Flux Control For In-Situ Magnetron Deposition and Etching For Plasma-Assisted Material Synthesis At The Atomic Scale
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70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Single-beam ion source enhanced growth of transparent conductive thin films
A single-beam ion source was developed and used in combination with magnetron sputtering to modulate the film microstructure. The ion source emits a single beam of ions that interact with the deposited film and simultaneously enhances the magnetron discharge. The magnetron voltage can be adjusted over a wide range, from approximately 240 to 130 V, as the voltage of the ion source varies from 0 to 150 V, while the magnetron current increases accordingly. The low-voltage high-current magnetron discharge enables a 'soft sputtering mode', which is beneficial for thin-film growth. Indium tin oxide (ITO) thin films were deposited at room temperature using a combined single-beam ion source and magnetron sputtering. Furthermore, the ion beam resulted in the formation of polycrystalline ITO thin films with significantly reduced resistivity and surface roughness. Single-beam ion-source-enhanced magnetron sputtering has many potential applications in which low-temperature growth of thin films is required, such as coatings for organic solar cells.
36 MATERIALS SCIENCE↗
Optimization of sputtering NiOx films for perovskite solar cell applications
Highlights: • NiO{sub x} HTLs were fabricated by three kinds of magnetron sputtering techniques. • Chemical composition, lattice strain and energy levels of NiO{sub x} films were studied and compared. • PSCs based on sputtered NiO{sub x} HTL achieved highest PCE of 16.3% with negligible hysteresis. • Compared with PEDOT:PSS HTL, PSCs based on NiO{sub x} HTL exhibited enhanced stability in air. - Abstract: In this work, we systematically investigated the properties of three kinds of NiO{sub x} films prepared by magnetron sputtering either NiO or Ni target under direct current (DC) or radio frequency (RF) power without any preheating. Those NiO{sub x} films were found to be different in composition ratios, lattice strain and energy levels, thus showing different optical and carrier transport properties. By RF power source, sputtering Ni target in pure O{sub 2} atmosphere led to NiO{sub x} film with relatively good crystallization and surface properties compared with other two types of NiO{sub x} films. These NiO{sub x} films were further introduced into CH{sub 3}NH{sub 3}PbI{sub 3} based planar p-i-n heterojunction perovskite solar cells (PSCs) as the hole transport layers (HTL). It is revealed that PSCs based on NiO{sub x} HTL prepared by sputtering Ni target in pure O{sub 2} atmosphere achieved a highest power conversion efficiency of 16.3% with negligible hysteresis. Compared with devices with PEDOT:PSS HTL, PSCs based on magnetron sputtered NiO{sub x} HTL presented substantially improved stability in air. The results provide theoretical and experimental guidance on selecting NiO{sub x} HTLs fabricated by magnetron sputtering techniques.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Stability of Brillouin flow in the presence of slow-wave structure
Including a slow-wave structure (SWS) on the anode in the conventional, planar, and inverted magnetron, we systematically study the linear stability of Brillouin flow, which is the prevalent flow in crossed-field devices. The analytic treatment is fully relativistic and fully electromagnetic, and it incorporates the equilibrium density profile, flow profile, and electric field and magnetic field profiles in the linear stability analysis. Using parameters similar to the University of Michigan's recirculating planar magnetron, the numerical data show that the resonant interaction of the vacuum circuit mode and the corresponding smooth-bore diocotron-like mode is the dominant cause for instability. This resonant interaction is far more important than the intrinsic negative (positive) mass property of electrons in the inverted (conventional) magnetron geometry. It is absent in either the smooth-bore magnetron or under the electrostatic assumption, one or both of which was almost always adopted in prior analytical formulation. This resonant interaction severely restricts the wavenumber for instability to the narrow range in which the cold tube frequency of the SWS is within a few percent of the corresponding smooth bore diocotron-like mode in the Brillouin flow.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
"CHON" particles: The interstellar component of cometary dust
Interstellar dust is characterized by strong absorption in the ultraviolet and the mid-IR. Current models of interstellar dust are based on three chemically distinct components: a form of carbon (usually graphite), a silicate, and a blend of polycyclic aromatic hydrocarbons or other carbonaceous material. Previous work using effective medium theories to understand the optical properties of cometary dust suggested that an amalgam of materials could reproduce the observed interstellar and cometary dust features. Recently, Lawler and Brownlee (1992) re-analyzed the PIA and PUMA-1 data sets from the Giotto flyby of P/Halley and discovered that the so-called "CHON" particles were actually composed of a blend of carbon-bearing and silicon-bearing materials. Based on effective medium theories, the absorption spectrum of such a material would display the spectral features of each of the components - strong UV absorption from the carbonaceous component and strong absorption in the IR from the silicate component. To test this idea, vapor-deposited samples were created using two different deposition techniques: sputtering with an argon RF magnetron and deposition from an argon plasma torch. Two different compositions were tested: a blend of graphite and silica in a 7:1 ratio and an amalgam of materials whose approximate composition matches the "CHON"-silicate abundances for the uncompressed PIA data set of Lawler and Brownlee: graphite, iron oxide, magnesium oxide, ammonium sulfate, calcium carbonate, and silica in mass ratios of 6:4.3:4:2.2:1:9. The samples were finely ground and pressed into 2" diameter disks using a 40 ton press. In all, four different experiments were performed: one with each of the compositions (C:SiO and "CHON") in both the RF magnetron and the plasma torch chambers. The RF magnetron created a uniform dark thin film on the substrate surface, and the plasma torch created a coating of small (<100 micron) diameter grey particles. The spectra of all four samples show a strong, broad absorption feature at around 220 nm as well as a strong but narrower absorption peak near 10 microns. The RF magnetron sputtered samples showed some sub-structure in the UV, and the peak of the absorption was shifted toward longer wavelengths. The UV absorption in the plasma torch deposited samples have no sub-structure, and the peak absorption is very near 220 nm. Strong absorption near 9 microns is seen in the spectra from both sample preparation techniques, and is consistent with the IR spectra of some terrestrial silicates. Other features, particularly at 6.2 and 8.6 microns, are seen in the interstellar medium. A strong feature near 2 microns is due to absorbed water in the sample. Based on the results of these experiments, there is evidence that a material with a composition similar to that detected in "CHON" particles in the coma of P/Halley have a spectral signature which reproduces the main absorption features of interstellar dust. This suggests that the "CHON" particles could be the interstellar component of cometary dust.
Lien, David J.↗
Microstructural and nanomechanical studies of PVD Cr coatings on SiC for LWR fuel cladding applications
The microstructure and nanomechanical properties of pure Cr coatings deposited on SiC with various physical vapor deposition (PVD) methods have been investigated for the mitigation of hydrothermal corrosion of SiC-SiC f (SiC fiber-reinforced SiC matrix) composite fuel cladding in light water reactors (LWR). Cr coatings (4–7 μm thick) were deposited on unbiased SiC substrates using six variants of magnetron sputtering processes: (i) standard (S-DCMS), (ii) pulsed (P-DCMS), (iii) ion-assisted (I-DCMS), and (iv) pulsed ion-assisted direct current magnetron sputtering (PI-DCMS), (v) high-power impulse magnetron sputtering (HiPIMS), and (vi) bipolar HiPIMS (B-HiPIMS). Microstructural characterization and nanoindentation testing were used to evaluate effects of deposition technique on coating microstructure and nanomechanical properties. The application of positive reverse pulses to the sputter target induced coarsening of the columnar grain structure, while ion bombardment of substrates during deposition promoted densification of the coating microstructure. Both effects are exemplified in B-HiPIMS deposition, resulting in a high-density microstructure with compressive residual stress. Material pile-up around nano-indents and plastic work during nanoindentation were analyzed to understand deformation behavior of the coatings. Finally, the results suggest the B-HiPIMS process to be among the promising methods for the deposition of Cr coatings on SiC-SiC f for LWR cladding application.
36 MATERIALS SCIENCE↗
Co-sputter deposition of Nb₃Sn layer into SRF cavity using Nb-Sn composite target
Nb₃Sn, with its superior superconducting critical temperature (Tc ~18.3 K) and superheating field (Hsh ~400 mT), is considered a promising material for superconducting radiofrequency (SRF) cavities, offering enhanced cryogenic performance compared to bulk niobium cavities. A Nb₃Sn coating technique has been developed for Nb SRF cavities using co-sputtering of Nb-Sn composite target in a DC cylindrical magnetron sputtering system. The composite target configuration and discharge conditions for co-sputtering were optimized to deposit Nb-Sn films on flat Nb substrates, followed by annealing to form Nb₃Sn. Multiple strategies have been explored to improve the surface homogeneity of the Nb₃Sn coating, including optimizing a two-step annealing process, annealing in Sn vapor, and a light Sn recoating process. A 1.5 µm Nb-Sn co-sputtered film was deposited on the interior of a 2.6 GHz Nb SRF cavity and annealed at 600 °C for 6 h, followed by 950 °C for 1 h. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, confirming the formation of Nb₃Sn. Then, the annealed cavity underwent a light recoating treatment and attained a quality factor (Q0) of 8.5E+08 at 2.0 K.
Accelerator Physics↗
Friction and Wear Properties of Selected Solid Lubricating Films
To evaluate commercially developed solid film lubricants for aerospace bearing applications, we investigated the friction and wear behavior of bonded molybdenum disulfide (MoS2), magnetron-sputtered MoS2 and ion-plated silver films in sliding contact with 6-mm-diameter American Iron and Steel Institute (AISI) 440 C stainless steel balls. Unidirectional sliding friction experiments were conducted with a load of 5.9 N (600 g), a mean Herizian contact pressure of 0.79 GPa maximum 1.19 GPa), and a sliding velocity of 0.2 m/s at room temperature in three environments: ultrahigh vacuum (7x10 (exp -7Pa)), humid air (approx. 20 percent humidity), and dry nitrogen (less than 1 percent humidity). The resultant films were characterized by scanning electron microscopy, energy-dispersive x-ray spectroscopy, and surface profilometry. Marked differences in friction and wear resulted front the environmental conditions and the film materials. The main criteria for judging the performance were coefficient of friction and wear rate, which had to be less than 0.3 and on the order of 10 (exp -6mm exp 3/Nm or less), respectively. The bonded MoS2 and magnetron-sputtered MoS2 films met the criteria in all three environments. Also, the wear rates of the counterpart AISI 440 C stainless steel balls met that criterion in all three environments. The ion-plated silver films met the criteria only in ultrahigh vacuum. In ultrahigh vacuum the bonded MoS2 films were superior. In humid air the bonded MoS2 films had higher coefficient of friction and shorter wear life than did the magnetron-sputtered MoS2 films. The ion-plated silver films had a high coefficient of friction in humid air but relatively low coefficients of friction in the nonoxidative environments. Adhesion and plastic deformation played important roles in all three environments. All sliding involved adhesive transfer of materials.
Miyoshi, Kazuhisa↗
Solid Lubrication Fundamentals and Applications
This chapter focuses attention on the friction and wear properties of selected solid lubricating films to aid users in choosing the best lubricant, deposition conditions, and operational variables. For simplicity, discussion of the tribological properties of concern is separated into two parts. The first part of the chapter discusses the different solid lubricating films selected for study including commercially developed solid film lubricants: (1) bonded molybdenum disulfide (MoS2), (2) magnetron-sputtered MoS2, (3) ion-plated silver, (4) ion-plated lead, (5) magnetron-sputtered diamondlike carbon (MS DLC), and (6) plasma-assisted, chemical-vapor-deposited diamondlike carbon (PACVD DEC) films. Marked differences in the friction and wear properties of the different films resulted from the different environmental conditions (ultrahigh vacuum, humid air, and dry nitrogen) and the solid film lubricant materials. The second part of the chapter discusses the physical and chemical characteristics, friction behavior, and endurance life of the magnetron-sputtered MoS2 films. The role of interface species and the effects of applied load, film thickness, oxygen pressure, environment, and temperature on the friction and wear properties are considered.
Miyoshi, Kazuhisa↗
Evaluation of Selected Solid Lubricating Films
An investigation was conducted to examine the friction and wear properties of bonded molybdenum disulfide (MoS2), magnetron-sputtered MoS2, ion-plated silver, ion-plated lead, magnetron-sputtered diamondlike carbon (MS DLC), and plasma-assisted, chemical-vapor-deposited DLC (PACVD DLC) films in sliding contact with 6-mm-diameter AISI 440C stainless steel balls. Unidirectional ball-on-disk sliding friction experiments were conducted with a load of 5.9 N and a sliding velocity of 0.2 m/s at room temperature in three environments: ultrahigh vacuum (vacuum pressure, 7 x 10(exp -7) Pa), humid air (relative humidity, approx. 20 percent), and dry nitrogen (relative humidity, less than 1 percent). The main criteria for judging the performance of the solid lubricating films were coefficient of friction and wear rate, which had to be less than 0.3 and on the order of 10(exp -6) cubic mm/N(dot)m or less, respectively. The bonded MoS2 and magnetron-sputtered MoS2 films met the criteria in all three environments. The ion-plated lead and silver films met the criteria only in ultrahigh vacuum but failed in humid air and in dry nitrogen. The MS DLC and PACVD DLC films met the requirements in humid air and dry nitrogen but failed in ultrahigh vacuum.
Miyoshi, Kazuhisa↗
Durability Evaluation of Selected Solid Lubricating Films
An investigation was conducted to examine the coefficients of friction, wear rates, and durability of bonded molybdenum disulfide (MoS2), magnetron-sputtered MoS2, ion-plated silver, ion-plated lead, magnetron-sputtered diamondlike carbon (MS DLC), and plasma-assisted, chemical-vapor-deposited DLC (PACVD DLC) films in sliding contact with 6-mm-diameter AISI 440C stainless steel balls. Unidirectional ball-on-disk sliding friction experiments were conducted with a load of 5.9 N and a sliding velocity of 0.2 m/s at room temperature in three environments: ultrahigh vacuum (vacuum pressure, 7 x 10(exp -7) Pa), humid air (relative humidity, approx. 20 percent), and dry nitrogen (relative humidity, less than 1 percent). The main criteria for judging the performance of the solid lubricating films were coefficient of friction and wear rate, which had to be less than 0.3 and on the order of 10(exp -6) cu mm/N.m or less, respectively. The bonded MoS2 and magnetron-sputtered MoS2 films met the criteria in all three environments. The ion-plated lead and silver films met the criteria only in ultrahigh vacuum but failed in humid air and in dry nitrogen. The MS DLC and PACVD DLC films met the requirements in humid air and dry nitrogen but failed in ultrahigh vacuum.
Miyoshi, Kazuhisa↗
Wear Behavior of Low-Cost, Lightweight TiC/Ti-6Al-4V Composite Under Fretting: Effectiveness of Solid-Film Lubricant Counterparts
The wear behavior of low-cost, lightweight 10-wt% TiC-particulate-reinforced Ti-6Al-4V matrix composite (TiC/Ti- 6Al-4V) was examined under fretting at 296, 423, and 523 K in air. Bare 10-wt% TiC/Ti-6Al-4V hemispherical pins were used in contact with dispersed multiwalled carbon nanotubes (MWNTs), magnetron-sputtered diamondlike carbon/chromium (DLC/Cr), magnetron-sputtered graphite-like carbon/chromium (GLC/Cr), and magnetron-sputtered molybdenum disulphide/titanium (MoS2/Ti) deposited on Ti-6Al-4V, Ti-48Al-2Cr-2Nb, and nickel-based superalloy 718. When TiC/Ti-6Al-4V was brought into contact with bare Ti-6Al-4V, bare Ti-48Al-2Cr-2Nb, and bare nickel-based superalloy 718, strong adhesion, severe galling, and severe wear occurred. However, when TiC/Ti-6Al-4V was brought into contact with MWNT, DLC/Cr, GLC/Cr, and MoS2/Ti coatings, no galling occurred in the contact, and relatively minor wear was observed regardless of the coating. All the solid-film lubricants were effective from 296 to 523 K, but the effectiveness of the MWNT, DLC/Cr, GLC/Cr, and MoS2/Ti coatings decreased as temperature increased.
Miyoshi, Kazuhisa↗
Igniters for Liquid Oxygen/Liquid Methane Technology Development
As part of NASA's technology development of liquid methane / liquid oxygen engines for future exploration missions, two different igniters were recently studied at NASA Marshall Space Flight Center. The first igniter tested was an impinging injection, spark-initiated torch igniter, and the second was a microwave-generated plasma igniter. The purpose of the ignition tests was to define the ignition limits under vacuum conditions and characterize the transient start-up performance as a function of propellant mixture ratio (MR), mass flow rates, inlet temperatures, and pre-ignition chamber pressure. In addition, for the impinging igniter two different spark plugs were tested, and for the microwave igniter the magnetron filament warm-up time and the magnetron input power were both varied. The results gathered from these tests indicated that the impinging igniter is capable of operating over an MR range of 2 - 27, with methane and oxygen inlet temperatures as low as -161 F and -233 F, respectively. The microwave igniter was tested over an MR range of 2 - 9, with methane and oxygen inlet temperatures as low as -90 F and -200 F, respectively. The microwave igniter achieved ignition over this range, although an upper ignition limit was determined for the oxidizer mass flow rate. In general, the torch exhaust temperatures for the microwave igniter were not as high as those attained with the impinging igniter. The microwave igniter, however, was hot-fired 17 times and was still operational, whereas the impinging igniter spark plugs experienced thermal shock and erosion over nine hot-fire tests. It was concluded that for the microwave igniter better mixing of the propellants might be required in order to both raise the torch exhaust temperature and decrease the required magnetron input power, and for the impinging igniter the spark plug position within the igniter chamber should be varied in future tests to identify a more optimal location. All of the igniter tests were supported by the Propulsion & Cryogenics Advanced Development project, which is part of NASA's Exploration Technology Development Program.
Osborne, Robin J.↗
Synthesis of metal chloride films: Influence of growth conditions on crystallinity
This paper presents the first deposition of metal chlorides by RF magnetron sputtering. By integrating the sputter chamber with an Ar-filled glovebox, films of hygroscopic chlorides can be synthesized and studied. The structure, composition, and morphology of FeCl 3 and FeCl 2 films were investigated as a function of deposition rate. In FeCl 3 films, the deposition rate has a large impact on the crystallinity of as-deposited films regardless of the substrate used. At high deposition rates, 24 Å/s, FeCl 3 films are crystalline with a preferred orientation along the 003-plane, while at low deposition rates, 0.5 Å/s, no crystalline peaks are observed for FeCl 3 . In FeCl 2 , the highest deposition rate achieved in this study was 0.2 Å/s which yields films with no crystalline peaks; therefore, Raman spectroscopy was used to confirm the presence of FeCl 2 . Here, the deposition of iron chlorides by RF magnetron sputtering opens the way for the study of thin film metal halides to understand their growth, magnetic and electronic properties, and understand ion transport through their layered structures.
36 MATERIALS SCIENCE↗
Surface Modification of C17200 Copper-Beryllium Alloy by Plasma Nitriding of Cu-Ti Gradient Film
In the present work, a copper-titanium film of gradient composition was firstly fabricated by the dual magnetron sputtering through power control and plasma nitriding of the film was then conducted to modify C17200 Cu alloy. The results showed that the prepared gradient Cu-Ti film by magnetron sputtering was amorphous. After plasma nitriding at 650 °C, crystalline Cu-Ti intermetallics appeared in the multi-phase coating, including CuTi{sub 2}, Cu{sub 3}Ti, Cu{sub 3}Ti{sub 2} and CuTi. Moreover, even though the plasma nitriding duration of the gradient Cu-Ti film was only 0.5 h, the mechanical properties of the modified Cu surface were obviously improved, with the surface hardness enhanced to be 417 HV{sub 0.01}, the wear rate to be 0.32 × 10{sup −14} m{sup 3}/Nm and the friction coefficient to be 0.075 at the load of 10 N, which are all more excellent than the C17200 Cu alloy. In addition, the wear mechanism also changed from adhesion wear for C17200 Cu substrate to abrasive wear for the modified surface.
36 MATERIALS SCIENCE↗
Cyclotron Phase-Coherent Ion Spatial Dispersion in a Non-Quadratic Trapping Potential is Responsible for FT-ICR MS at the Cyclotron Frequency
Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) at the cyclotron frequency instead of the reduced cyclotron frequency has been experimentally demonstrated using narrow aperture detection electrode (NADEL) ICR cells. Here, based on the results of SIMION simulations, we provide the initial mechanistic insights into the cyclotron frequency regime generation in FT-ICR MS. The reason for cyclotron frequency regime is found to be a new type of a collective motion of ions with a certain dispersion in the initial characteristics, such as pre-excitation ion velocities, in a highly non-quadratic trapping potential as realized in NADEL ICR cells. During ion detection, ions of the same m/z move in phase for cyclotron ion motion but out of phase for magnetron (drift) ion motion destroying signals at the fundamental and high order harmonics that comprise reduced cyclotron frequency components. After an initial magnetron motion period, ion clouds distribute into a novel type of structures – ion slabs, elliptical cylinders, or star-like structures. These structures rotate at the Larmor (half-cyclotron) frequency on a plane orthogonal to the magnetic field, inducing signals at the true cyclotron frequency on each of the narrow aperture detection electrodes. To eliminate the reduced cyclotron frequency peak upon dipolar ion detection, a number of slabs or elliptical cylinders organizing a star-like configuration are formed. In a NADEL ICR cell with quadrupolar ion detection, a single slab or an elliptical cylinder is sufficient to minimize the intensity of the reduced cyclotron frequency components, particularly the second harmonic. .
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
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↗