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NASA NTRS1981

Ion beam microtexturing of surfaces

Some recent work in surface microtecturing by ion beam sputtering is described. The texturing is accomplished by deposition of an impurity onto a substrate while simultaneously bombarding it with an ion beam. A summary of the theory regarding surface diffusion of impurities and the initiation of cone formation is provided. A detailed experimental study of the time-development of individual sputter cones is described. A quasi-liquid coating was observed that apparently reduces the sputter rate of the body of a cone compared to the bulk material. Experimental measurements of surface diffusion activation energies are presented for a variety of substrate-seed combinations and range from about 0.3 eV to 1.2 eV. Observations of apparent crystal structure in sputter cones are discussed. Measurements of the critical temperature for cone formation are also given along with a correlation of critical temperature with substrate sputter rate.

Robinson, R. S.↗

NASA NTRS1983

A two-stage mechanism for escape of Na and K from Io

A two-stage process is presented to identify Io as the source of Na and K ions in the Io plasma torus. The Voyager I IRIS experiment recorded an SO2 abundance of 0.2 cm atm in the Io subsolar region, and further calculations determined that the S(+) and O(+) would have sufficient energy to penetrate the Io atmosphere and produce sputtering of surface atoms at a rate of 800 million/sq cm per sec. If K, Na, and S are present on the surface in cosmic proportions, then an evenly applied sputter distribution would produce the same abundances of sputtered Na and K as observed in the Na and K clouds around Io. Sputtered into the atmosphere, the ions undergo thermal Jean's escape and attain velocities of at least 2.6 km/sec. The sputtering ions are a factor of two greater on the Jupiter side than on the solar side, in agreement with asymmetries measured by the Voyager.

Summers, M. E.↗

NASA NTRS1984

Method for sequentially processing a multi-level interconnect circuit in a vacuum chamber

An apparatus is disclosed which includes a vacuum system having a vacuum chamber in which wafers are processed on rotating turntables. The vacuum chamber is provided with an RF sputtering system and a dc magnetron sputtering system. A gas inlet introduces various gases to the vacuum chamber and creates various gas plasma during the sputtering steps. The rotating turntables insure that the respective wafers are present under the sputtering guns for an average amount of time such that consistency in sputtering and deposition is achieved. By continuous and sequential processing of the wafers in a common vacuum chamber without removal, the adverse affects of exposure to atmospheric conditions are eliminated providing higher quality circuit contacts and functional device.

Routh, D. E.↗

NASA NTRS1985

Rapid evaluation of ion thruster lifetime using optical emission spectroscopy

A major life-limiting phenomenon of electric thrusters is the sputter erosion of discharge chamber components. Thrusters for space propulsion are required to operate for extended periods of time, usually in excess of 10,000 hr. Lengthy and very costly life-tests in high-vacuum facilities have been required in the past to determine the erosion rates of thruster components. Alternative methods for determining erosion rates which can be performed in relatively short periods of time at considerably lower costs are studied. An attempt to relate optical emission intensity from an ion bombarded surface (screen grid) to the sputtering rate of that surface is made. The model used a kinetic steady-state (KSS) approach, balancing the rates of population and depopulation of ten low-lying excited states of the sputtered molybdenum atom (MoI) with those of the ground state to relate the spectral intensities of the various transitions of the MoI to the population densities. Once this is accomplished, the population density can be related to the sputting rate of the target. Radiative and collisional modes of excitation and decay are considered. Since actual data has not been published for MoI excitation rate and decay constants, semiempirical equations are used. The calculated sputtering rate and intensity is compared to the measured intensity and sputtering rates of the 8 and 30 cm ion thrusters.

Rock, B. A.↗

NASA NTRS1986

Interactions of planetary magnetospheres with icy satellite surfaces

When natural satellites and ring particles are embedded within magnetospheric plasmas, the charged particles interact with the surfaces of these solid bodies. These interactions have important implications for the surface, the atmosphere of the parent body, and the magnetosphere as a whole. Significant erosion of the surface by sputtering, as well as redeposition of sputter ejecta, can occur over geologic time. The surface can also be chemically modified. Sputter ejecta can make important contributions to the atmosphere; sputtering provides a lower limit to the atmospheric column density even for arbitrarily cold satellite surfaces. Sputter ejecta escaping from the parent body can form extensive neutral clouds within the magnetosphere. Ionization and dissociation within these neutral clouds can be dominant sources of low-energy plasma. The importance of these processes is discussed for the satellites and magnetospheres of Jupiter, Saturn and Uranus.

Cheng, A. F.↗

NASA NTRS1991

High temperature static strain gage development

Final results are presented from a program to develop a thin film static strain gage for use on the blades and vanes of running, test stand gas turbine engines with goals of an 3 x 3 mm gage area and total errors of less than 10 pct. of + or - 2,000 microstrain after 50 hrs at 1250 K. Pd containing 13 Wt. pct. Cr was previously identified as a new strain sensor alloy that appeared to be potentially usable to 1250 K. Subsequently, it was discovered, in contrast with its behavior in bulk, that Pd-13Cr suffered from oxidation attack when prepared as a 4.5 micron thick thin film. Continuing problems with electrical leakage to the substrate and the inability of sputtered alumina overcoats to prevent oxidation led to the discovery that sputtered alumina contains appreciable amounts of entrapped argon. After the argon has been exsolved by heating to elevated temperatures, the alumina films undergo a linear shrinkage of about 2 pct. resulting in formation of cracks. These problems can be largely overcome by sputtering the alumina with the substrate heated to 870 K. With 2 micron thick hot sputtered alumina insulation and overcoat films, total 50 hr drifts of about 100 microstrain (2 tests) and about 500 microstrain (1 test) were observed at 1000 and 1100 K, respectively. Results of tests on complete strain gage systems on constant moment bend bars with Pd temperature compensation grids revealed that oxidation of the Pd grid was a major problem even when the grid was overcoated with a hot or cold sputtered alumina overcoat.

Hulse, C. O.↗

NASA NTRS1993

Solar wind-induced secondary ions and their relation to lunar surface composition

Based on previous laboratory experiments simulating solar wind sputtering of lunar surface materials, it appears that solar wind ions sputter secondary ions in sufficient numbers to be measured from low-altitude lunar orbit. Solar wind protons are hundreds of times less efficient than those used in standard secondary ion mass spectrometry; nevertheless secondary ions of Na, Mg, Al, Si, K, Ca, Mn, Ti and Fe were observed sputtered from sample simulants of mare and highland soils. These secondary ion fluxes depend both on concentration in the soil and on probability of ionization; yields of easily ionized elements such as K and Na are relatively much greater than those for the more electronegative elements and compounds. The principal geochemical indicator elements Na, Mg, Al, Si, K, Ca, Ti, Mn and Fe are nevertheless detectable. However, it has not been shown that the observed secondary ions vary strictly one-to-one with their concentrations in the geochemically distinct soil simulants used here. While we have a first order understanding of secondary ion sputtering, it is not clear that the observed ion yields can be linked with great accuracy to the simulant's composition. The simulants were analyzed by electron microprobe to establish their detailed composition. The observed secondary ion fluxes can then be compared with the microprobe results. For example Ti(+) fluxes from the three simulants correspond to the true composition with accuracies of better than 10 percent for the high-Ti basalt, and about 20 percent for the low-Ti simulant. The highlands simulant produced a statistically insignificant Ti(+) count rate. Here we discuss the results of further SIMS experiments using the ASU/Center for Solid State Science facility. With careful isolation and preparation of samples, we avoid the problems of the previous experiments. In particular, we will make use of ground-up sample to mimic the sputtering behavior of regolith, and will avoid charging by placing the soil on a conducting indium substrate. We report the results of a blind test of the SIMS technique using a sample of unknown composition.

Elphic, R. C.↗

NASA NTRS1999

Titanium Optics for Ion Thrusters

Ion thruster total impulse capability is limited, in part, by accelerator grid sputter erosion. A development effort was initiated to identify a material with a lower accelerator grid volumetric sputter erosion rate than molybdenum, but that could utilize the present NSTAR thruster grid design and fabrication techniques to keep development costs low, and perform as well as molybdenum optics. After comparing the sputter erosion rates of several atomic materials to that of molybdenum at accelerator voltages, titanium was found to offer a 45% reduction in volumetric erosion rates. To ensure that screen grid sputter erosion rates are not higher at discharge chamber potentials, titanium and molybdenum sputter erosion rates were measured at these potentials. Preliminary results showed only a slightly higher volumetric erosion rate for titanium, so that screen grid erosion is insignificant. A number of material, thermal, and mechanical properties were also examined to identify any fabrication, launch environment, and thruster operation issues. Several titanium grid sets were successfully fabricated. A titanium grid set was mounted onto an NSTAR 30 cm engineering model ion thruster and tested to determine optics performance. The titanium optics operated successfully over the entire NSTAR power range of 0.5 to 2.3 kW. Differences in impingement-limited perveances and electron backstreaming limits were found to be due to a larger cold gap for the titanium optics. Discharge losses for titanium grids were lower than those for molybdenum, likely due to a slightly larger titanium screen grid open area fraction. Radial distributions of beam current density with titanium optics were very similar to those with molybdenum optics at all power levels. Temporal electron backstreaming limit measurements showed that titanium optics achieved thermal equilibrium faster than molybdenum optics.

Soulas, George C.↗

NASA NTRS2004

Post-Test Analysis of the Deep Space One Spare Flight Thruster Ion Optics

The Deep Space 1 (DSl) spare flight thruster (FT2) was operated for 30,352 hours during the extended life test (ELT). The test was performed to validate the service life of the thruster, study known and identify unknown life limiting modes. Several of the known life limiting modes involve the ion optics system. These include loss of structural integrity for either the screen grid or accelerator grid due to sputter erosion from energetic ions striking the grid, sputter erosion enlargement of the accelerator grid apertures to the point where the accelerator grid power supply can no longer prevent electron backstreaming, unclearable shorting between the grids causes by flakes of sputtered material, and rouge hole formation due to flakes of material defocusing the ion beam. Grid gap decrease, which increases the probability of electron backstreaming and of arcing between the grids, was identified as an additional life limiting mechanism after the test. A combination of accelerator grid aperture enlargement and grid gap decrease resulted in the inability to prevent electron backstreaming at full power at 26,000 hours of the ELT. Through pits had eroded through the accelerator grid webbing and grooves had penetrated through 45% of the grid thickness in the center of the grid. The upstream surface of the screen grid eroded in a chamfered pattern around the holes in the central portion of the grid. Sputter deposited material, from the accelerator grid, adhered to the downstream surface of the screen grid and did not spall to form flakes. Although a small amount of sputter deposited material protruded into the screen grid apertures, no rouge holes were found after the ELT.

NASA Solar electric propulsion Technology Applicat↗

NASA NTRS2010

Radiation Chemistry in Ammonia-Water Ices

We studied the effects of 100 keV proton irradiation on films of ammonia-water mixtures between 20 and 120 K. Irradiation destroys ammonia, leading to the formation and trapping of H2, N2 NO, and N2O, the formation of cavities containing radiolytic gases, and ejection of molecules by sputtering. Using infrared spectroscopy, we show that at all temperatures the destruction of ammonia is substantial, but at higher temperatures (120 K), it is nearly complete (approximately 97% destroyed) after a fluence of 10(exp 16) ions per square centimeter. Using mass spectroscopy and microbalance gravimetry, we measure the sputtering yield of our sample and the main components of the sputtered flux. We find that the sputtering yield depends on fluence. At low temperatures, the yield is very low initially and increases quadratically with fluence, while at 120 K the yield is constant and higher initially. The increase in the sputtering yield with fluence is explained by the formation and trapping of the ammonia decay products, N2 and H2 which are seen to be ejected from the ice at all temperatures.

Loeffler, M. J.↗

NASA NTRS2011

The Effect on the Lunar Exosphere of a Coroual Mass Ejection Passage

Solar wind bombardment onto exposed surfaces in the solar system produces an energetic component to the exospheres about those bodies. The solar wind energy and composition are highly dependent on the origin of the plasma. Using the measured composition of the slow wind, fast wind, solar energetic particle (SEP) population, and coronal mass ejection (CME), broken down into their various components, we have estimated the total sputter yield for each type of solar wind. We show that the heavy ion component, especially the He++ and 0+7 can greatly enhance the total sputter yield during times when the heavy ion population is enhanced. Folding in the flux, we compute the source rate for several species during different types of solar wind. Finally, we use a Monte Carlo model developed to simulate the time-dependent evolution of the lunar exosphere to study the sputtering component of the exosphere under the influence of a CME passage. We simulate the background exosphere of Na, K, Ca, and Mg. Simulations indicate that sputtering increases the mass of those constituents in the exosphere a few to a few tens times the background values. The escalation of atmospheric density occurs within an hour of onset The decrease in atmospheric density after the CME passage is also rapid, although takes longer than the increase, Sputtered neutral particles have a high probability of escaping the moon,by both Jeans escape and photo ionization. Density and spatial distribution of the exosphere can be tested with the LADEE mission.

Killen, R. M.↗

DOE OSTI2017

On the SIMS Ionization Probability of Organic Molecules

The prospect of improved secondary ion yields for secondary ion mass spectrometry (SIMS) experiments drives innovation of new primary ion sources, instrumentation, and post-ionization techniques. The largest factor affecting secondary ion efficiency is believed to be the poor ionization probability (α{sup +}) of sputtered material, a value rarely measured directly, but estimated to be in some cases as low as 10{sup −5}. Our lab has developed a method for the direct determination of α{sup +} in a SIMS experiment using laser post-ionization (LPI) to detect neutral molecular species in the sputtered plume for an organic compound. Here, we apply this method to coronene (C{sub 24}H{sub 12}), a polyaromatic hydrocarbon that exhibits strong molecular signal during gas-phase photoionization. A two-dimensional spatial distribution of sputtered neutral molecules is measured and presented. It is shown that the ionization probability of molecular coronene desorbed from a clean film under bombardment with 40 keV C{sub 60} cluster projectiles is of the order of 10{sup −3}, with some remaining uncertainty arising from laser-induced fragmentation and possible differences in the emission velocity distributions of neutral and ionized molecules. In general, this work establishes a method to estimate the ionization efficiency of molecular species sputtered during a single bombardment event. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Evaluation of hydrogen evolution reaction activity of molybdenum nitride thin films on their nitrogen content

We report preparation and electrochemical properties of molybdenum nitride Mo x N (x from 1 to 2) and Mo thin films prepared by the magnetron sputtering. We adjusted amount of nitrogen during reactive sputtering, to achieve different ratios of Mo:N in the films.We could prepare well-defined and extremely smooth films. We determined hydrogen evolution reaction (HER) activity and other kinetics parameters such as Tafel slopes and exchange current densities. Corrosion stability at anodic potentials was also evaluated from onset potentials of dissolution of prepared films. We found that Mo x N thin film HER activity dependence on nitrogen content in the film exhibits volcano-like diagram. From XRD measurements we identified several phases present in the films from pure Mo to β-Mo 2 N and δ-MoN. We find that β-Mo 2 N phase has the highest HER activity. Stability of studied nitrides at anodic potentials increases with increasing content of nitrogen. Mo films sputtered at high substrate temperatures exhibit higher HER activity than Mo x N systems. Furthermore, with increasing substrate temperature during sputtering, HER activity of pure Mo thin films increases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

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↗

DOE OSTI2018

New Resonance Ionization Mass Spectrometry Scheme for Improved Uranium Analysis

Resonance ionization mass spectrometry (RIMS) combines tunable laser spectroscopy with mass spectrometry to provide here a high-efficiency means of analyzing solid materials. We previously showed a very high useful yield of 24% for analysis of uranium using three lasers to excite and ionize atoms sputtered from metallic uranium and uranium dioxide. A new resonance ionization scheme using only two lasers achieves a higher useful yield of 38% by accessing both the ground electronic state and a low-lying electronic state of atomic uranium that is significantly populated by sputtering. The major loss channel in analyzing uranium dioxide is the formation of UOx molecules during sputtering. Prebombardment of the surface with 3 keV noble gas ions prior to analysis reduces the surface and results in a sputtered flux with a greatly enhanced proportion of atomic U. This method of surface reduction results in uranium useful yields as high as 6.6% for uranium dioxide analysis, compared to 2% from previous work.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2019

Low-loss single-photon NbN microwave resonators on Si

We present coplanar waveguide (CPW) microwave resonators with exceptionally low loss produced from NbN sputtered on Si. The NbN films are deposited with a modest RF substrate bias during reactive DC magnetron sputtering at a substrate temperature of 250 °C and can achieve a critical temperature as high as 15 K depending on the N2 flow rate. We measure the internal quality factors (Qi) of two such resonators at high-powers near saturation and report high-power quality factors in excess of 1.2 × 106 at 200 mK and 3.5 × 105 at 2 K. We also measure the temperature-dependent frequency shift at high power levels and the quality factor at single-photon power levels. From these measurements, we find a low-power (average photon number less than one) Qi value of 4.2 × 105 at 200 mK, which is consistent with a system limited by two-level-system loss.

Carter, Faustin W. (ORCID:0000000212363517)↗

DOE OSTI2018

Thin-film X-ray filters on microstructured substrates and their thermophysical properties

It is shown that structured substrates having micron- or submicron-sized through holes and coated with an ultrathin organic film can be used for the fabrication of thin-film X-ray filters via direct growth of functional layers on a substrate by sputter deposition, without additional complex processing steps. An optimised process is considered for the fabrication of X-ray filters on support structures in the form of electroplated fine nickel grids and on track-etched polymer membranes with micron- and submicron-diameter through pores. ‘Optimisation’ is here taken to mean matching the sputter deposition conditions with the properties of substrates so as to avoid overheating. The filters in question are intended for both imaging and single-channel detectors operating in the soft X-ray and vacuum UV spectral regions, at wavelengths from 10 to 60 nm. Thermal calculations are presented for the heating of ultrathin layers of organic films and thin-film support substrates during the sputter deposition of aluminium or other functional materials. The paper discusses approaches for cooling thin-film composites during the sputter deposition process and the service of the filters in experiments and gives a brief overview of the works that utilised filters produced by the described technique on microstructured substrates, including orbital solar X-ray research in the framework of the CORONAS programme and laboratory laser plasma experiments. (invited paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2022

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↗