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At least 145 records · Page 8

Liquid crystal light valve structures

An improved photosensor film and liquid crystal light valves embodying said film is provided. The photosensor film and liquid crystal light valve is characterized by a significant lower image retention time while maintaining acceptable photosensitivity. The photosensor film is produced by sputter depositing CdS onto an ITO substrate in an atmosphere of argon/H2S gas while maintaining the substrate at a temperature in the range of about 130 C to about 200 C and while introducing nitrogen gas into the system to the extent of not more than about 1% of plasma mixture. Following sputter deposition of the CdS, the film is annealed in an inert gas at temperatures ranging from about 300 C to about 425 C.

Koda, N. J.↗

Development of sputter coatings for the gravity probe B gyroscope housings

Cu/Ti coatings have been applied by sputter deposition to fused quartz housings to serve as the electrodes and lands of electrostatically supported gyroscopes. Niobium-coated fused quartz gyro rotors have been successfully suspended and spun up in those housings. The Cu/Ti bilayer coating and alternative multilayer coatings (Cu/Mo, Mo/Cu/Ti and Mo/Cu/Mo) with 2-micron thickness produced by sputter deposition on flat, fused quartz substrates have been examined with scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and four-point resistivity measurement techniques. The multilayer coatings with a molybdenum bonding layer appear to produce smoother surfaces than those with a titanium bonding layer. All multilayer coatings survived thermal cycling to 77 K without adhesion failure.

Zhou, P.↗

Improved Performance of Cu(InGa)(SeS) 2 PV Modules Using the Reaction of Metal Precursors. Final Report

This project “Improved Performance of Cu(InGa)(SeS) 2 PV Modules using the Reaction of Metal Precursors” was a partnership led by the Institute of Energy Conversion (IEC) at the University of Delaware with Columbia University and the Molecular Foundry at the Lawrence Berkeley National Laboratory. The aim was to develop pathways to improve Cu(InGa)(SeS) 2 (CIGSS) thin film photovoltaic modules using processes compatible with low manufacturing cost. The CIGSS approach investigated was a two-step process including deposition of metal precursor films following by reaction in hydride gases utilizing IEC’s novel reactor. The process was similar to that under commercial development by the project’s industry partner Stion. When Stion went out of business mid-project the focus changed to a rapid thermal process considered more commercially viable. Approaches to improve the performance of solar cells using the reacted films focused on two material innovations. First, the overall Ga content was increased to increase the operating voltage, which is desirable for scale-up to commercial modules. Second, the processing and performance advantages arising from Ag alloying were investigated. Advanced characterization guided process and material development including control of relative composition gradients. Research on the formation of Cu-Ga-In metal precursors utilized sputtering deposition which is normally used in commercial applications. The work resulted in processes for deposition of precursor stacks with increased relative Ga content and effects of deposition parameters on morphology and phase composition were established. It was shown that the metal precursor films have comparable phase composition and morphology so subsequent reaction follows from the same starting point. The addition of Ag to the metal precursors gave more uniform morphology and improved adhesion of reacted films which enable higher reaction temperature for faster processing. A novel outcome was the discovery of a previously undocumented material phase in sputter-deposited and evaporated Ag-Cu-In-Ga thin films. Hydride gas reaction processes including time-temperature-concentration profiles were developed for different precursor compositions. This enables control of composition profiles to engineer through-film gradients for solar cell optimization with characterization and simulations used to correlate measured film composition profiles to measurements of devices. In particular, the gradient of sulfur at the front of the CIGSS film was found to be critical. The simulations guided process development leading to improved reproducibility of devices improved performance with higher Ga content and higher voltage. With Ag-alloyed precursors, the reaction pathways leading were determined. A significant finding was that Ag-alloying increases the reaction rate to completely convert precursor films to the final chalcopyrite which could enable reduced reaction time to benefit manufacturability. To maintain potential commercial viability, the process under investigation was refocused to a rapid thermal process that could potentially be incorporated into an in-line process for manufacturing. Precursors with different composition were capped with an extra selenium layer and reacted in hydrogen sulfide 5-15 minutes, compared to typically 2 hours in the previous multi-step batch process. Critical RTP parameters were identified to control the reaction. Further optimization would be needed for high efficiency solar cells but pathways to high quality devices with further optimization and improved heating uniformity were developed. The project also developed new optoelectronic characterization approaches with a focus on development and application of spatial- and time-resolved photoluminescence and a custom mapping photoluminescence microscope built. It was shown how critical electronic transport properties strongly depend on the chemical composition of the material and that a wide range of samples show inhomogeneity on a length scale larger than the grains in the films. Additionally, two-photon excitation capability was developed to distinguish bulk vs surface losses. The project advances the state-of-the -art for precursor reaction processes in several ways that could impact manufacturing. This includes validation of approaches to increase voltage and establishment of model-guided control to form optimal composition profiles. The application of process control approaches with knowledge of phase formation and reaction pathways can be critically valuable in designing a large-scale process.

14 SOLAR ENERGY↗

Mirrors for High Resolution X-Ray Optics---Figure Preserving IR/PT Coating

Coating stress of 10 - 20 nm of Ir is sufficiently high to distort the figure of arc-second thin lightweight mirrors. For iridium: --Stress sigma ~ 4 GPa for 15 nm film implies 60 Nm integrated stress-- Need less than 3 N/m (or stress less than 200 MPa) for sub-arcsecond optics. Basic Approaches for Mitigation. A. Annealing the film-- Glass can be heat up to 400 C without distortion. Silicon is even more resistant.-- It was found that recovery is limited by residual thermal stress from taking the mirror down from high T. B. Coating bi-layer films with compressive stress with tensile stress. C. Front-and-back coating with magnetron sputtering or atomic layer deposition-- Sputtering involve spanning of substrates. Geometric difference in setup (convexness/concaveness of curved mirrors) does not permit precise front-and-back matching-- Atomic layer deposition can provide a uniform deposition front and back simultaneously.

MIRRORS FOR HIGH RESOLUTION X-RAY OPTICS↗

Polarity Effects of Substrate Surface in Epitaxial ZnO Film Growth

Epitaxial ZnO films were grown on the two polar surfaces (0-face and Zn-face) of (0001) ZnO single crystal substrates using off-axis magnetron sputtering deposition. As a comparison, films are also deposited on the (000 I) Al203 substrates. It is found that the two polar surfaces have different photoluminescence (PL) spectrum, surface structure and morphology, which are strongly inference the epitaxial film growth. The morphology and structure of epitaxial films on the ZnO substrates are different from the film on the Al203 substrates. An interesting result shows that high temperature annealing of ZnO single crystals will improve the surface structure on the O-face surface rather than the opposite Surface. The measurements of PL, low-angle incident x-ray diffraction, and atomic force microscopy of ZnO films indicate that the O-terminated surface is better for ZnO epitaxial film growth using reactive sputtering deposition.

Zhu, Shen↗

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↗

Exploring the First High-Entropy Thin Film Libraries: Composition Spread-Controlled Crystalline Structure

Thin films of two types of high-entropy oxides (HEOs) have been deposited on 76.2 mm Si wafers using combinatorial sputter deposition. In one type of the oxides, (MgZnMnCoNi)O x , all the metals have a stable divalent oxidation state and similar cationic radii. In the second type of oxides, (CrFeMnCoNi)O x , the metals are more diverse in the atomic radius and valence state, and have good solubility in their sub-binary and ternary oxide systems. Therefore, the resulting HEO thin films were characterized using several high-throughput analytical techniques. The microstructure, composition, and electrical conductivity obtained on defined grid maps were obtained for the first time across large compositional ranges. The crystalline structure of the films was observed as a function of the metallic elements in the composition spreads, that is, the Mn and Zn in (MgZnMnCoNi)O x and Mn and Ni in (CrFeMnCoNi)O x . The (MgZnMnCoNi)O x sample was observed to form two-phase structures, except single spinel structure was found in (MgZnMnCoNi)O x over a range of Mn > 12 at. % and Zn < 44 at. %, while (CrFeMnCoNi)O x was always observed to form two-phase structures. Composition-controlled crystalline structure is not only experimentally demonstrated but also supported by density function theory calculation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diamondlike carbon protective coatings for IR materials

Diamondlike carbon (DLC) films have the potential to protect optical windows in applications where it is important to maintain the integrity of the specular transmittance of these films on ZnS and ZnSe infrared transmitting windows. The films must be adherent and durable such that they protect the windows from rain and particle erosion as well as chemical attack. In order to optimize the performance of these films, 0.1 micro m thick diamondlike carbon films were deposited on fused silica and silicon wafers, using three different methods of ion beam deposition. One method was sputter deposition from a carbon target using an 8 cm ion source. The merits of hydrogen addition were experimentally evaluated in conjunction with this method. The second method used a 30 cm hollow cathode ion source with hydrocarbon/Argon gases to deposit diamondlike carbon films from the primary beam at 90 to 250 eV. The third method used a dual beam system employing a hydrocarbon/Argon 30 cm ion source and an 8 cm ion source. Films were evaluated for adherence, intrinsic stress, infrared transmittance between 2.5 and 50 micro m, and protection from particle erosion. An erosion test using a sandblaster was used to give quantitative values of the protection afforded to the fused silica by the diamondlike carbon films. The fused silica surfaces protected by diamondlike carbon films were exposed to 100 micro m diameter SiO particles at 60 mi/hr (26.8/sec) in the sandblaster.

Mirtich, M. J.↗

Oxidation-resistant reflective surfaces for solar dynamic power generation in near Earth orbit

Reflective surfaces for space station power generation systems are required to withstand the atomic oxygen-dominated environment of near Earth orbit. Thin films of platinum and rhodium, which are corrosion resistant reflective metals, have been deposited by ion beam sputter deposition onto various substrate materials. Solar reflectances were then measured as a function of time of exposure to a RF-generated air plasma. Similarly, various protective coating materials, including MgF2, SiO2, Al2O3, and Si3N4, were deposited onto silver-coated substrates and then exposed to the plasma. Analysis of the films both before and after exposure by both ESCA and Auger spectroscopy was also performed. The results indicate that Pt and Rh do not suffer any loss in reflectance over the duration of the tests. Also, each of the coating materials survived the plasma environment. The ESCA and Auger analyses are discussed as well.

Gulino, D. A.↗

Oxidation-resistant reflective surfaces for solar dynamic power generation in near earth orbit

Reflective surfaces for Space Station power generation systems are required to withstand the atomic oxygen-dominated environment of near earth orbit. Thin films of platinum and rhodium, which are corrosion resistant reflective metals, have been deposited by ion beam sputter deposition onto various substrate materials. Solar reflectances were then measured as a function of time of exposure to a RF-generated air plasma.

Gulino, Daniel A.↗

Deposition of ultrathick heavy-metal alloys on rotating substrates by high-power impulse magnetron sputtering: Target erosion effects

Sputter deposition of ultrathick (≈20μm) Au–Ta alloy coatings on sphero-cylindrical substrates is key for the fabrication of hohlraums for magnetically assisted inertial confinement fusion. In this work, we study the deposition of AuTa 4 alloy coatings onto rotating substrates. We use high-power impulse magnetron sputtering (HiPIMS) in a constant peak target voltage mode. Results show that the target erosion state has a strong impact on the dominant crystallographic phase, microstructure, surface morphology, and electrical resistivity of AuTa 4 films. This is due to effects of changes in the confining magnetic field with target erosion on the HiPIMS discharge characteristics and the sputter source output. We quantify these effects via plasma diagnostics and discuss the optimization of HiPIMS deposition of ultrathick films for cases when target erosion effects dominate film properties.

36 MATERIALS SCIENCE↗

Fabrication of Freestanding Metallic Ni-Mo-W Microcantilever Beams With High Dimensional Stability

Recent studies have elucidated a promising balance of physical and mechanical properties of sputter deposited nickel-molybdenum-tungsten (Ni-Mo-W) films that have a unique nanotwinned microstructure and promising potential for use in high temperature microelectromechanical systems (MEMS). Here, the current study was undertaken to establish the feasibility of making nanotwinned Ni-Mo-W microcantilevers with standard micro- fabrication processing, to assess their dimensional stability, and to demonstrate the possibility of using nanotwinned Ni-Mo-W in metal MEMS devices. Deposition of Ni-Mo-W films in commercial sputtering chambers revealed a wide processing window for the formation of the requisite nanotwinned microstructure. Conventional photolithography and etchants were employed to shape blanket Ni-Mo-W films into freestanding microcantilever beams. Monitoring microcantilever deflections via interferometry provided a direct measure of residual stresses and overall dimensional stability. Heat treatments of 200° C and 400° C were used to mimic wafer bonding temperatures. At 400°C, microcantilevers exhibited modest stress relaxation, yielding beam deflection profiles on the nanometer scale and portending dimensional stability and control for future metal MEMS devices.

36 MATERIALS SCIENCE↗

Sputtering: A vacuum deposition method for coating material

The sputtering process is described in terms of its features: versatility, momentum transfer, configuration of target, precise controls and the relatively slow deposition rate. Sputtered films are evaluated in terms of adherence, coherence, and internal stresses. The strong adherence is attributed to the high kinetic energies of the sputtered material, sputter etched (cleaned) surface, and the submicroscopic particle size. An illustration is a sputtered solid film lubricant such as MoS2. Friction tests were conducted on a thin, 2000 A deg thick MoS2 film. These films are very dense and without observable pinholes, and the particle to particle cohesion is strong. Tolerances (film thickness) can be controlled to a millionth of a centimeter. Very adherent films of sputtered Teflon can be deposited in a single operation on any type of material (metal, glass, paper) and on any geometrical configuration with a dense adherent film.

Spalvins, T.↗

Commissioning of a two-target DC cylindrical magnetron sputter coater for depositing Nb 3 Sn film on Nb superconducting radiofrequency cavities

A DC cylindrical magnetron sputter coater was commissioned and used to coat Nb 2.6 GHz superconducting radiofrequency (SRF) cavity with Nb 3 Sn. The sputter coater has two identical cylindrical magnetrons that can move, with a controlled speed, along the axis of the SRF cavity to coat the inside surface of the cavity. The design of the sputter coater is discussed, along with its performance. Initially, a sample holder that allows coating on flat substrates at positions similar to the equator and beam tubes of a 2.6 GHz SRF cavity was used to test conditions for fabricating Nb 3 Sn layers. Multilayers of Nb and Sn were sequentially sputtered on flat Nb and sapphire substrates mounted on the equivalent positions of the cavity's beam tubes and the equator using the two identical cylindrical magnetrons. Then, the Nb/Sn multilayers were annealed at 950 °C for 3 h. Here, the ~1.2 μm thick Nb 3 Sn film did not show any other Nb–Sn compounds and had a superconducting transition temperature of 17.61–17.76 K. The 2.6 GHz SRF cavity was coated using similar conditions as flat samples. Cryogenic RF testing of the Nb 3 Sn-coated cavity demonstrated a quality factor of 3.2 × 10 8 at an accelerating gradient of 5 MV/m at 4.4 K.

43 PARTICLE ACCELERATORS↗

Masking Technique for Ion-Beam Sputter Etching

Improved process for fabrication of integrated circuits developed. Technique utilizes simultaneous ion-beam sputter etching and carbon sputter deposition in conjunction with carbon sputter mask or organic mask decomposed to produce carbon-rich sputter-mask surface. Sputter etching process replenishes sputter mask with carbon to prevent premature mask loss.

Banks, B. A.↗

Solutions for discharge chamber sputtering and anode deposit spalling in small mercury ion thrusters

Proposed solutions to the problems of sputter erosion and sputtered material spalling in the discharge chamber of small mercury ion thrusters are presented. The accelerated life test evaluated three such proposed solutions: (1) the use of tantalum as a single low sputter yield material for the exposed surfaces of the discharge chamber components subject to sputtering, (2) the use of a severely roughened anode surface to improve the adhesion of the sputter-deposited coating, and (3) the use of a wire cloth anode surface in order to limit the size of any coating flakes which might spall from it. Because of the promising results obtained in the accelerated life test with anode surfaces roughened by grit-blasting, experiments were carried out to optimize the grit-blasting procedure. The experimental results and an optimal grit-blasting procedure are presented.

Power, J. L.↗

Simultaneous ion sputter polishing and deposition

Results of experiments to study ion beam sputter polishing in conjunction with simultaneous deposition as a mean of polishing copper surfaces are presented. Two types of simultaneous ion sputter polishing and deposition were used in these experiments. The first type utilized sputter polishing simultaneous with vapor deposition, and the second type utilized sputter polishing simultaneous with sputter deposition. The etch and deposition rates of both techniques were studied, as well as the surface morphology and surface roughness.

Rutledge, S.↗

High-throughput multimodal exploration of a nanocrystalline Cu-Ag library

Sputter-deposited, nanocrystalline Cu-Ag thin films produced across a broad compositional and deposition-parameter space were evaluated to unravel the process-structure-property relationships important for creating hard, conductive electrical contacts and coatings. Combinatorial deposition involving pulsed direct current magnetron sputtering of elemental targets enabled swift examination of nearly the full range of alloy compositions and a relevant portion of deposition atomistics. Several high-throughput characterization modalities were employed to evaluate the chemistry, structure, and properties of the films. The resultant hardness, modulus, film density, crystal texture, and resistivity were analyzed in terms of key deposition characteristics (incident atom kinetic energy and incidence angle) predicted by binary-collision, kinematic Monte Carlo simulations. The study revealed improved hardness, parabolic resistivity dependence on composition, and compositional and process dependencies of film tarnishing. The results are discussed in the context of variations in microstructure and film density. Transmission electron microscopy and X-ray diffraction demonstrate several forms of compositional variation including solute segregation to grain boundaries as well as periodic, intragranular compositional modulations. Annealing of a Cu-rich alloy film exhibiting grain boundary segregation showed that this as-deposited, compositional variation is not stable above 100 °C. Finally, the Cu-Ag system is shown to have potential for hard, conductive, tarnish-resistant and room temperature-stable nanocrystalline thin films across the composition space.

36 MATERIALS SCIENCE↗