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DOE OSTI2020

In situ indentation and high cycle tapping deformation responses in a nanolaminate crystalline/amorphous metal composite

The incorporation of nanostructured and amorphous metals into modern applications is reliant on the understanding of deformation and failure modes in constrained conditions. To study this, a 105 nm crystalline Cu/160 nm amorphous Cu 45 Zr 55 (at.%) multilayer structure was fabricated with the two crystalline layers sputter deposited between the top-middle-bottom amorphous layers and prepared to electron transparency. The multilayer was then in situ indented either under a single load to a depth of ~ 100 nm (max load of ~ 100 μN) or held at 20 μN and then repeatedly indented with an additional 5 μN up to 20,000 cycles in a transmission electron microscope to compare the deformation responses in the nanolaminate. For the single indentation test, the multilayer showed serrated load-displacement behavior upon initial indentation inductive of shear banding. Additionally, at an indentation depth of ~ 32 nm, the multilayer exhibited perfect plastic behavior and no strain hardening. Both indented and fatigue-indented films revealed diffraction contrast changes with deformation. Subsequent Automated Crystal Orientation Mapping (ACOM) measurements confirmed and quantified global texture changes in the crystalline layers with specifically identified grains revealing rotation. Using a finite element model, the in-plane displacement vectors under the indent mapped conditions where ACOM determined grain rotation was observed, indicating the stress flow induced grain rotation. Furthermore, the single indented Cu layers also exhibited evidence of deformation induced grain growth, which was not evident in the fatigue-indented Cu based multilayer. Finally, the single indented multilayer retained a significant plastic crater in the upper most amorphous layer that directly contacted the indenter; a negligible crater impression in the same region was observed in the fatigued tested multilayer. These differences are explained by the different loading methods, applied load, and deformation mechanisms experienced in the multilayers.

36 MATERIALS SCIENCE↗

NASA NTRS1981

Soft X-ray imaging with a normal incidence mirror

By sputtering, it is possible to make multilayered structures (layered synthetic microstructures or LSMs) with individual layers as thin as a fraction of a nanometer. These techniques have been used to make a multilayered interference mirror to reflect carbon K X rays (at a wavelength of 4.48 nm) at normal incidence. The structure consists of 76 layers of tungsten of thickness 0.765 nm with layers of carbon (thickness 1.510 nm) interspersed, deposited on a 111 line type silicon wafer substrate. This LSM was formed into a concave mirror of radius approximately 1.1 m by bending the substrate, and used in an optical set-up to form images of grids illuminated by an X-ray source. The mirror was found to have a resolution of 5 lines/mm and an efficiency, integrated over the CK band, of between 4 and 8%.

Underwood, J. H.↗

NASA NTRS2017

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↗

NASA NTRS2006

Developing Multilayer Thin Film Strain Sensors With High Thermal Stability

A multilayer thin film strain sensor for large temperature range use is under development using a reactively-sputtered process. The sensor is capable of being fabricated in fine line widths utilizing the sacrificial-layer lift-off process that is used for micro-fabricated noble-metal sensors. Tantalum nitride films were optimized using reactive sputtering with an unbalanced magnetron source. A first approximation model of multilayer resistance and temperature coefficient of resistance was used to set the film thicknesses in the multilayer film sensor. Two multifunctional sensors were fabricated using multilayered films of tantalum nitride and palladium chromium, and tested for low temperature resistivity, TCR and strain response. The low temperature coefficient of resistance of the films will result in improved stability in thin film sensors for low to high temperature use.

Wrbanek, John D.↗

NASA NTRS2006

Highly Efficient Multilayer Thermoelectric Devices

Multilayer thermoelectric devices now at the prototype stage of development exhibit a combination of desirable characteristics, including high figures of merit and high performance/cost ratios. These devices are capable of producing temperature differences of the order of 50 K in operation at or near room temperature. A solvent-free batch process for mass production of these state-of-the-art thermoelectric devices has also been developed. Like prior thermoelectric devices, the present ones have commercial potential mainly by virtue of their utility as means of controlled cooling (and/or, in some cases, heating) of sensors, integrated circuits, and temperature-critical components of scientific instruments. The advantages of thermoelectric devices for such uses include no need for circulating working fluids through or within the devices, generation of little if any noise, and high reliability. The disadvantages of prior thermoelectric devices include high power consumption and relatively low coefficients of performance. The present development program was undertaken in the hope of reducing the magnitudes of the aforementioned disadvantages and, especially, obtaining higher figures of merit for operation at and near room temperature. Accomplishments of the program thus far include development of an algorithm to estimate the heat extracted by, and the maximum temperature drop produced by, a thermoelectric device; solution of the problem of exchange of heat between a thermoelectric cooler and a water-cooled copper block; retrofitting of a vacuum chamber for depositing materials by sputtering; design of masks; and fabrication of multilayer thermoelectric devices of two different designs, denoted I and II. For both the I and II designs, the thicknesses of layers are of the order of nanometers. In devices of design I, nonconsecutive semiconductor layers are electrically connected in series. Devices of design II contain superlattices comprising alternating electron-acceptor (p)-doped and electron-donor (n)-doped, nanometer- thick semiconductor layers.

Boufelfel, Ali↗

DOE OSTI2024

Low-temperature formation of Ti2AlN during post-deposition annealing of reactive multilayer systems

M n+1 AXn-phase Ti 2 AlN thin-films were synthesized using reactive sputtering-based methods involving the deposition of single-layer TiAlN, and Ti/AlN and TiN/TiAl multilayers of various modulation periods at ambient temperature and subsequent annealing at elevated temperatures. Ex situ and in situ x-ray diffraction measurements were used to characterize the Ti 2 AlN formation temperature and phase fraction. During annealing, Ti/AlN multilayers yielded Ti 2 AlN at a significantly lower in situ temperature of 650 °C compared to TiN/TiAl multilayers or single-layer TiAlN (750 °C). The results suggest a reactive multilayer mechanism whereby distinct Ti and AlN layers react readily to release exothermic energy resulting in lower phase transition temperatures compared to TiN and TiAl layers or mixed TiAlN. With a modulation period of 5 nm, however, Ti/AlN multilayers yielded Ti 2 AlN at a higher temperature of 750 °C, indicating a disruption of the reactive multilayer mechanism due to a higher fraction of low-enthalpy interfacial TiAlN within the film.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS1994

Sputter process investigation: Material and environment interaction processes investigation

The multilayer Ellipsometry program has been developed with which the thickness and the optical properties of top layer can be determined with the additional information obtained from other measurement such as the optical constant of the middle layer film. Once the proper parameters are input into the program, the multilayer Ellipsometry program which was developed by H. Kim and Dr. Fromhold gives the best possible set of the solutions for the top layer thickness or its optical index graphically on a PC screen. In this report the basic two layer Ellipsometry theory will be summarized briefly as well as the one layer case. All the code is written in Microsoft Quickbasic version 4.5 for IBM PC with a VGA color graphics monitor so that the measurement could be cross-checked out graphically on the screen.

Williams, John R.↗

DOE OSTI2024

Metal DiSulfide thin films synthesized by pulsed ion beam ablation: Self-assembled structures with improved mechanical properties in humid conditions

Thin films composed of transition metal dichalcogenides such as molybdenum disulfide (MoS 2 ) or tungsten disulfide (WS 2 ) are well known for their solid lubricating behavior in dry environments such as space, but deteriorate rapidly in environments where oxygen is present. There have been many attempts over recent decades to improve MoS 2 lubricating performance in humid environments by addition of metals such as titanium to the film. The additions have come in the form of co-sputtering with the MoS 2 , or formation of nano multilayer coatings. We have previously reported on the synthesis of MoS 2 films by high-power ion beam ablation [Prasad et al, Matls. Lett. 65 (2010) 4–6]. The resulting films are observed to contain spheres of pure Mo of 10–100 nm size evenly dispersed throughout the ~1 μm-thick film, a form of self-assembly not before seen in films produced by sputtering or by pulsed laser deposition (PLD). The remaining Mosingle bondS matrix was observed to crystalize in situ under frictional contact into MoS 2 with the basal planes orienting themselves in the direction of sliding underneath the wear surface. The present study concerns metal additions in the form of alternating layers with MoS 2 deposited in between from an ablation target. The addition of Ti resulted in the extension of good tribological performance to humid air conditions, but the path to good performance appears to be relatively narrow. The same distributed Mo spheres were present in the new film, and similar self-assembled morphologies when V was substituted for the Ti, and when multilayers were formed of WS 2 with Zr additions. Furthermore, it appears that addition of Ti resulted in improvements in mechanical film strength that contributed to the wear ability in humid conditions.

Intense ion beams↗

DOE OSTI2020

Study of a linear surface wave plasma source for tin removal in an extreme ultraviolet source

Tin deposition mitigation employs hydrogen radicals and ions, formed in a hydrogen plasma, to interact with tin to form tin hydride (SnH 4 ) in the gaseous state, which is then pumped away. Surface wave plasma (SWP) technology developed at Illinois generates hydrogen radicals and ions, resulting in tin etch rates that are high enough to keep extreme ultraviolet (EUV) lithographic tools clean. An advantage of an SWP antenna is the ability to generate a high density of hydrogen radicals and hydrogen ions directly at the desired etching location. In situ etching of tin enables high availability EUV tools by maintaining high reflectivity of the multilayer mirror of the collector. Additionally, the SWP is characterized with low ion energies and low electron temperature, such that the multilayer mirror does not suffer any damage from sputtering or implantation of hydrogen ions during operation. Here, experiments elucidating the fundamental processes of tin removal are conducted by varying pressure, power, surface temperature, and gas flow rate in order to observe the etch rate behavior. Our results have shown that the presence of hydrogen ions increases etch rates because ion bombardment weakens Sn–Sn bonds, which, in turn, allows for a higher rate of chemical etching by the radicals. The ion bombardment reduces the number of radicals needed to etch a single tin atom to the range of 10 2 –10 3 . The linear SWP antenna yields plasma densities on the order of 10 17 to 10 18 m -3 and radical densities on the order of 10 18 to 10 19 m -3 , allowing for greater utilization of ion etch enhancement. Etch rates of up to 200 nm/min have been achieved. The surface temperature of the samples is an important factor in the etching process such that the decrease in the surface temperature increases the etch rates and decreases the hydrogen desorption rates. In addition, a kinetic etch model is developed to explain the behavior of etch rates as a function of surface temperature. Furthermore, results from experiments performed in an Illinois NXE:3100 chamber will be discussed.

42 ENGINEERING↗

DOE OSTI2022

Strain-rate dependent deformation mechanisms in single-layered Cu, Mo, and multilayer Cu/Mo thin films

Here, strain-rate sensitivity and rate-dependent hardness, over a range of 10 -2 to 10 2 s -1 , of sputter-deposited single-layered Cu, Mo, and 5 nm Cu/ 5 nm Mo, and 100 nm Cu/ 100 nm Mo multilayer films with a total film thickness of 5 μm were measured using nanoindentation. The plastic zone underneath the nanoindents was characterized via cross-sectional transmission electron microscopy (XTEM). The multilayer films exhibited enhanced hardness but slightly reduced strain-rate sensitivity with decreasing layer thickness from 100 nm to 5 nm. Only the 5 nm Cu/ 5 nm Mo multilayer film exhibited shear bands underneath the nanoindents, and the size of the shear bands increased with increasing strain rate. In contrast, the 100 nm Cu/ 100 nm Mo multilayer film exhibited material pile-up around the indents and significant nanotwinning within Cu grains. The effect of strain rate and layer thickness on the hardness and strain rate sensitivity of the multilayer thin films is interpreted using a modified confined layer slip (CLS) model. The reduced rate sensitivity at 5 nm as compared to 100 nm correlates with abundant growth nanotwins in the Cu grains in 100 nm and formation of shear bands in 5 nm multilayers. In single layer films, a substructure with a high density of dislocations was observed consistent with the plastic strain gradient in the indent plastic zone. No evidence of deformation twins was noted in any of the samples.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Effects of diffusion barriers on reaction wave stability in Co/Al reactive multilayers

Bimetallic, reactive multilayers are uniformly structured materials composed of alternating sputter-deposited layers that may be ignited to produce self-propagating mixing and formation reactions. These nanolaminates are most commonly used as rapid-release heat sources. The specific chemical composition at each metal/metal interface determines the rate of mass transport in a mixing and formation reaction. The inclusion of engineered diffusion barriers at each interface will not only inhibit solid-state mixing but also may impede the self-propagating reactions by introducing instabilities to wavefront morphology. Here, this work examines the effect of adding diffusion barriers on the propagation of reaction waves in Co/Al multilayers. The Co/Al system has been shown to exhibit a reaction propagation instability that is dependent on the bilayer thickness, which allows for the occurrence of unstable modes in otherwise stable designs from the inclusion of diffusion barriers. Based on the known stability criteria in the Co/Al multilayer system, the way in which the inclusion of diffusion barriers changes a multilayer's heat of reaction, thermal conductivity, and material mixing mechanisms can be determined. These factors, in aggregate, lead to changes in the wavefront velocity and stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1988

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.↗

NASA NTRS1985

Molybdenum-silicon multilayer mirrors for the extreme ultraviolet

Multilayer structures of molybdenum and silicon have been synthesized by sputter deposition onto flat silicon single-crystal silicon substrates and spherically ground (0.5and 22.0-m radii) fused silica substrates; and the reflectivities for 170.4-A (72.8-eV), 160.1-A (77.4-eV), and 228-A (54.4-eV) light measured at near normal incidence. Observed peak values ranged from 26.2 to 78 percent, the highest reflectivities occurring closest to normal incidence. Energy resolutions were about 10 in all cases. Model calculations were performed using optical constants and experimentally determined multilayer structural parameters. In all cases the measured reflectivities were equal to or larger (by up to a factor of 2) than the calculated values, a result attributed to uncertainty in the optical constants used in the calculations. Experimental and calculated angular-peak positions and energy resolutions were in good agreement. The high reflectivities of these molybdenum-silicon structures will make possible application of traditional optics approaches in the EUV and support new developments including free-electron lasers.

Barbee, T. W., Jr.↗

DOE OSTI2020

Laser induced damage in coatings for cryogenic Yb:YAG active mirror amplifiers

We report results of a study of the laser induced damage threshold (LIDT) behavior of ion beam sputtered H f O 2 / S i O 2 multilayer coatings on Yb:YAG using 1-on-1 and N-on-1 test protocols. The tests were conducted at ambient, vacuum, and cryogenic conditions using 280 ps pulses at λ <#comment/> = 1030 n m . The 1-on-1 LIDT of antireflection (AR) stacks is found to be only slightly reduced under vacuum and cryogenic conditions, while that of high reflectivity (HR) stacks is insensitive to environmental conditions within the uncertainty of the measurements. Cryogenic N-on-1 tests show the LIDT of the HR coating is almost the same as in the 1-on-1 tests. Conversely, the cryogenic N-on-1 test of the AR coating shows damage at ∼ <#comment/> 13 J / c m 2 , a fluence lower than the 20.4 J / c m 2 of 1-on-1 tests. The AR damage behavior is found to be affected by imperfections at the Yb:YAG surface. These findings show that high surface quality is required to increase energy extraction from active mirror laser amplifiers.

Wang, Hanchen↗

DOE OSTI2022

High-throughput investigation of structural evolution upon solid-state in Cu–Cr–Co combinatorial multilayer thin-film

Cu-Cr-Co combinatorial multilayer thin-films were prepared by a high-throughput ion beam sputtering system. Based on the thickness ratio among the individual nanoscale monolayers (Cu, Cr, Co), the resulting stoichiometry covered the entire phase diagram. The chemical composition and structure of Cu-Cr-Co combinatorial chip upon solid-state reaction were studied by lab-based micro-X-ray fluorescence (mu-XRF) and high-throughput synchrotron X-ray diffraction (XRD), respectively. A composition-structure map for Cu-Cr-Co combinatorial chip was developed through automated data analysis employing hierarchical clustering techniques. The structural evolution of Cu-Cr-Co combinatorial chip as a function of heat-treatment temperature, time, and modulation period were studied systematically. Furthermore, the effect of the elemental distribution in-depth direction was investigated to gain more insights regarding phase transformation. This work provides an efficient method and new perspectives for the design and optimization of the composition and structure of high-performance thin-films.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Development and characterization of Nb3Sn/Al2O3 superconducting multilayers for particle accelerators

Abstract Superconducting radio-frequency (SRF) resonator cavities provide extremely high quality factors > 10 10 at 1–2 GHz and 2 K in large linear accelerators of high-energy particles. The maximum accelerating field of SRF cavities is limited by penetration of vortices into the superconductor. Present state-of-the-art Nb cavities can withstand up to 50 MV/m accelerating gradients and magnetic fields of 200–240 mT which destroy the low-dissipative Meissner state. Achieving higher accelerating gradients requires superconductors with higher thermodynamic critical fields, of which Nb 3 Sn has emerged as a leading material for the next generation accelerators. To overcome the problem of low vortex penetration field in Nb 3 Sn, it has been proposed to coat Nb cavities with thin film Nb 3 Sn multilayers with dielectric interlayers. Here, we report the growth and multi-technique characterization of stoichiometric Nb 3 Sn/Al 2 O 3 multilayers with good superconducting and RF properties. We developed an adsorption-controlled growth process by co-sputtering Nb and Sn at high temperatures with a high overpressure of Sn. The cross-sectional scanning electron transmission microscope images show no interdiffusion between Al 2 O 3 and Nb 3 Sn. Low-field RF measurements suggest that our multilayers have quality factor comparable with cavity-grade Nb at 4.2 K. These results provide a materials platform for the development and optimization of high-performance SIS multilayers which could overcome the intrinsic limits of the Nb cavity technology.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1967

High-temperature /1100 degrees F/ capacitors operate without supplement cooling

Multilayered capacitor with one-mil thick pyrolytic boron nitride and wrap around sputtered electrodes achieves parallel electrical interconnections in a stacked configuration of 3 to 9 wafers. These capacitors are compact, lightweight, and suitable for operation in high temperatures without supplemental cooling.

Stapleton, R. E.↗

DOE OSTI2022

Improving the laser performance of ion beam sputtered dielectric thin films through the suppression of nanoscale defects by employing a xenon sputtering gas

Laser damage-prone precursors in high index materials such as hafnia are believed to be the primary limiter in the performance of dielectric multilayer films to advance ultra-high power and energy laser applications. Removing or suppressing these precursors is the key to fabricating laser damage resistant thin films for the enabling technologies. Early work has revealed that nanobubbles formed by entrapped argon (Ar) working gas in ion beam sputtering (IBS) produced hafnia films are primarily responsible for the onset of laser damage upon exposure to UV, ns-laser pulses. In this study, we demonstrate that the UV ns-laser damage onset of IBS produced hafnia films can be improved to 3.1 +/- 0.2 J/cm 2 by substituting the conventional Ar working gas with xenon (Xe), a nearly 1 J/cm 2 increase from that of the Ar produced hafnia films. In addition to the suppression of the overall point-defect density of the hafnia films, the reduction of the Xe entrapment eliminates the nanobubbles and the generation of plasmas that initiates the laser damage. The defect suppression and its correlation to the increase in laser damage threshold is revealed by the combined analysis of Rutherford backscattering spectroscopy, electron paramagnetic resonance spectroscopy, transmission electron microscopy, and laser damage testing. Monte Carlo simulations suggest a much smaller entrapment of Xe gas by comparison to Ar, which is attributed to the significant difference in the energy of the reflected neutrals (3X) which are likely to be implanted. These results provide an effective process route with a fundamental understanding for producing high laser damage resistant dielectric films for high power and high energy laser applications.

36 MATERIALS SCIENCE↗