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The technology of broad-beam ion sources is reviewed from the viewpoint of the sputtering-deposition user. This review includes a short description of the development of discharge chambers, accelerator systems, and cathodes; the present alternatives for these components and the expected future improvements.
Critical currents in sputtered Chevrel-phase lead molybdenum sulfide have been measured at several temperatures as a function of applied magnetic field up to 19 T. A critical current density of approximately 50 million A/sq m was obtained at 15 T and 1.8 K, and the effective upper critical field was estimated to be 30 T. The pinning force at low fields was found to be dependent on the amount of free lead.
Report reviews advances in tribological uses of RF-sputtered and ion-plated films of solid film lubricants (laminar solids, soft metals, organic polymers) and wear-resistant refractory compounds.
Thermal barrier coatings of yttria stabilized zirconia and zirconia-ceria mixtures were deposited by RF reactive sputtering. Coatings were 1-2 mils thick, and were deposited on copper cylinders intended to simulate the inner wall of a regeneratively cooled thrust chamber. Coating stoichiometry and adherence were investigated as functions of deposition parameters. Modest deposition rates (approximately 0.15 mil/hr) and subambient sustrate temperatures (-80 C) resulted in nearly stoichiometric coatings which remained adherent through thermal cycles between -196 and 400 C. Coatings deposited at higher rates or substrates temperatures exhibited greater oxygen deficiences, while coatings deposited at lower temperatures were not adherent. Substrate bias resulted in structural changes in the coating and high krypton contents; no clear effect on stoichiometry was observed.
The friction and wear properties of several refractory silicides, borides, and carbide coatings were examined. The coatings were applied to type 440C steel surfaces by radio-frequency sputtering. The friction and wear properties of the coatings were found to be related to stoichiometry and impurity content of the bulk coating as well as the degree of interfacial adherence between coating and substrate. Bulk coating stoichiometry could to large extent be controlled by the application of a negative bias voltage during deposition. Adherence was promoted by the formation of an oxidized layer at the interface. Deliberate preoxidizing of the 440C produced enhanced adherence for many compounds which is related to the formation of a mixed oxide transition region.
The study searches for interface treatment that would increase the adhesion of TiC coating to nickel- and titanium-base alloys. Rene 41 (19 wt percent Cr, 11 wt percent Mo, 3 wt percent Ti, balance Ni) and Ti-6Al-4V (6 wt percent Al, 4 wt percent V, balance Ti) are considered. Adhesion of the coatings is evaluated in pin-and disk friction tests. The coatings and interface regions are examined by X-ray photoelectron spectroscopy. Results suggest that sputtered refractory compound coatings adhere best when a mixed compound of coating and substrate metals is formed in the interfacial region. The most effective type of refractory compound interface appears to depend on both substrate and coating material. A combination of metallic interlayer deposition and mixed compound interface formation may be more effective for some substrate coating combinations than either alone.
An electron bombardment argon ion source was used to sputter deposit 17 different metal and metal oxide films ranging in thickness from 1 to 8 micrometers on H-13 steel substrates. The film adherence to the substrate surface was measured using a tensile test apparatus. Comparisons in bond strength were made between ion beam, ion plating, and RF deposited films. A protective coating to prevent heat checking in H-13 steel dies used for aluminum die casting was studied. The results of exposing the coated substrates to temperatures up to 700 degrees are presented.
This investigation determined whether selected ion beam sputtered coatings on H-13 die steel would have the potential of improving the thermal fatigue behavior of the steel used as a die in aluminum die casting. The coatings were selected to test candidate insulators and metals capable of providing protection of the die surface. The studies indicate that 1 micrometer thick W and Pt coatings reduced the thermal fatigue more than any other coating tested and are candidates to be used on a die surface to increase die life.
Sputtered coatings of Mo, W, Pt, Ag, Au, Co, Cr, Ni, Ag + Cu, Mo + Pt, Si3N4, A1N, Cr3C2, Ta5Si3, and ZrO2 were applied to a 2-inch-square, 7-inch-long thermal fatigue test specimen which was then internally water cooled and alternately immersed in molten aluminum and cooled in air. After 15,000 cycles the thermal fatigue cracks at the specimen corners were measured. Results indicate that a significant improvement in thermal fatigue resistance was obtained with platinum, molybdenum, and tungsten coatings. Metallographic examination indicates that the improvement in thermal fatigue resistance resulted from protection of the surface of the die steel from oxidation. The high yield strength and ductility of molybdenum and tungsten contributed to the better thermal fatigue resistance.
An electron bombardment argon ion source sputter deposited 17 metals and metal oxides on H-13 steel. The films ranged 1 to 8 micrometers in thickness and their adherence was generally greater than the capacity of the measuring device; adherence quality depended on proper precleaning of the substrate before deposition. N2 or air was introduced for correct stoichiometry in metallic compounds. Au, Ag, MgO, and Ta5Si3 films 8 microns thick have bond strength equal to 1 micron coatings; the bond strength of pure metallic films up to 5 microns thick was greater than the epoxy to film bond (8000 psi). The results of exposures of coated material to temperatures up to 700 C are presented.
Friction and wear tests were conducted on optimized sputtered Cr2O3 and Cr2O3 with metallic binder coatings. The coatings were applied on the bearing surface of journal foil air bearings and were tested against chrome-carbide-coated journal surfaces. The objective of the study was to develop a coating system which would withstand 9000 start-stops and high-speed rubs (maximum acceleration, 100 gs) in temperatures ranging from room temperature to 650 C. The Cr2O3 coating completed the test sequence and the coating consisting of Cr2O3 with metallic binders completed 3000 start-stops. The coefficient of friction of the coatings at 650 C was found to be about half that at room temperature. It was concluded, therefore, that the coatings should perform much better in a high temperature environment alone. The decrease in friction at high temperature is attributed to oxidation and interactions of the coatings and substrates at the interface temperature.
Three experimental research designs investigating candidate materials and processes involved in protective die surface coating procedures by sputter deposition, using ion beam technologies, are discussed. Various pre-test results show that none of the coatings remained completely intact for 15,000 test cycles. The longest lifetime was observed for coatings such as tungsten, platinum, and molybdenum which reduced thermal fatigue, but exhibited oxidation and suppressed crack initiation only as long as the coating did not fracture. Final test results confirmed earlier findings and coatings with Pt and W proved to be the candidate materials to be used on a die surface to increase die life. In the W-coated specimens, which remained intact on the surface after thermal fatigue testing, no oxidation was found under the coating, although a few cracks formed on the surface where the coating broke down. Further research is planned.
Reliable gold contacts are deposited on niobium by combination of RF sputtering and photolithography. Process results in structures having gold only where desired for electrical contact. Contacts are stable under repeated cycling from room temperature to 4.2 K and show room-temperature contact resistance as much as 40 percent below indium contacts made by thermalcompression bonding.
The theory put forward by Clayton (1977) for the formation of the Ca-Al-rich inclusions within C3 meteorites is extended to an evolutionary history in a three-phase interstellar medium. Widespread supersonic turbulence in the hot interstellar medium is maintained by supernova shock waves, giving rise to heavy sputtering of the refractory dust. Subsequent reaccumulation with varying dust/gas ratios or varying particle sizes produces isotopically fractionated Ca-Al-rich accumulates. It is thought that the Ca-Al-rich inclusions themselves are formed by the following sequence in the solar system: (1) cold accumulation of larger-than-average Ca-Al-rich particles containing supernova condensate cores into macroscopic (approximately 1 cm) Ca-Al-rich agglomerates, probably by sedimentation; and (2) fusion of the supernova condensates into macroscopic minerals by exothermic chemical reactions that begin when the accumulate has been warmed, thereby releasing energy from the unequilibrated forms accumulated from the interstellar medium.
The plasma or ion-assisted coating techniques such as sputtering and ion plating are discussed in view of wear and corrosion protection. The basic processes and the unique features of the technique are discussed in regard to the synthesis and development of high reliability wear and corrosion resistant films. The ions of the plasma which transfer energy, momentum, and charge to the substrate and the growing films can be beneficially used. As a result, coating adherence and cohesion is improved. Favorable morphological growth such as high density and porosity-free films can be developed, and residual stresses can be reduced.
Considerable effort is being devoted to the development of overlay coatings for protecting critical components such as turbine blades against high-temperature oxidation, corrosion, and erosion damage in service. The most commercially advanced methods for depositing coatings are electron-beam evaporation and plasma spraying. Sputter-ion plating (SIP) offers a potentially cheaper and simpler alternative method for depositing overlays. Experimental work on SIP of Co-Cr-Al-Y and Ni-Cr-Al-Ti alloy coatings is described. Results are presented of metallographic assessment of these coatings, and of the results obtained from high-velocity testing using a gas-turbine simulator rig.
Amorphous, 'diamond-like' carbon films have been deposited on Si substrates, using ion-beam sputtering. The interfacial properties are studied using capacitance and conductance measurements. Data are analyzed using existing theories for interfacial electrical properties. The density of electronic states at the interface, along with corresponding time constants are determined.
The centricular catheter comprises a multiplicity of inlet microtubules. Each microtubule has both a large opening at its inlet end and a multiplicity of microscopic openings along its lateral surfaces. The microtubules are perforated by an ion beam sputter etch technique. The holes are etched in each microtubule by directing an ion beam through an electro formed mesh mask producing perforations having diameters ranging from about 14 microns to about 150 microns. This structure assures a reliable means for shunting cerebrospinal fluid from the cerebral ventricles to selected areas of the body.