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At least 91 records · Page 5

Broadband 920-nm mirror thin film damage competition

The 2023 Laser Damage conference thin-film damage competition was devoted to a survey on the state-of-the-art broadband near-IR multilayer dielectric (MLD) mirrors designed for ultra-short pulsed laser applications. The requirements for the coatings were a minimum reflection of 99.5% at 45-deg incidence angle for S-polarization from 830 nm to 1010 nm and group delay dispersion (GDD) < ± 50fs 2 . The participants were allowed to select the coating materials, coating design, and coating deposition method. Samples were damage tested at a single testing facility to enable direct comparison among the participants using a 25 ± 5 fs optical parametric chirped-pulse amplification (OPCPA) laser system operating at 5 Hz. The testing results from this set of 37 samples showed that dense coatings by ion-beam sputtering (IBS), magnetron sputtering (MS), and electron-beam ion assisted deposition (e-beam IAD) exhibited highest damage initiation onset (laser-induced damage threshold or LIDT) while e-beam coatings were low performers. In addition, multilayer coatings using tantala and/or hafnia as high index materials were top performers. Furthermore, this competition included for the first time the measurement of the damage growth onset (laser-induced damage growth threshold or LDGT). This latter performance metric plays an important role in establishing the safe operational conditions for larger aperture ultrashort pulsed lasers. Information pertaining to the morphology of the damage sites and their evolution under subsequent exposure to different laser fluences leading to damage growth is presented. Finally, not all coating samples in the survey met the GDD requirements stated above and associated measurements are discussed in the context of the present and past thin-film damage competitions focused on similar broadband near-IR MLD coatings.

23 broadband high reflectors↗

Metal-ion-controlled growth and nanoindentation response of 3D, bicontinuous Cu–Fe thin films

Bicontinuous, nanocomposite thin film morphologies depend largely on the deposition conditions applied during physical vapor deposition. With the introduction of high power impulse magnetron sputtering (HiPIMS), the range of potential morphologies achieved during deposition has been increased. In this work, we compare the deposition outcomes between traditional direct-current magnetron sputtering (DCMS) and HiPIMS for a thin film co deposit of Cu and Fe. Modular control of the columnarity, porosity and roughness was achieved by varying the Cu and Fe metal ion currents during deposition. The directionality of the nanostructured phase-separated morphology was also controlled as the ion current increased. At zero ion current for both Cu and Fe sputtered species during DCMS, the film exhibited lateral concentration modulations of Cu and Fe. The directionality of the Cu- and Fe-rich phases shifted to vertical concentration modulations at low ion currents of I Fe = 1A and I Cu = 0:1A and to lateral concentration modulations at relatively moderate ion currents of I Fe = 5A and I Cu = 2A: At high ion currents of I Fe = 18A and I Cu = 2A; a more randomized phase domain structure was observed on the nanoscale. This structural shift is rationalized using an interdiffusion model. Here, the role of different kinds of phase separated morphologies, achieved during DCMS deposition, on the mechanical properties has also been studied. Results indicated increase in hardness, indentation modulus and flow strength values with the increase in indentation strain rates. Bicontinuous Cu-Fe nanocomposites are found to be stronger than multilayer Cu-Fe samples.

36 MATERIALS SCIENCE↗

Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations

Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO 3 /BaTiO 3 multilayer illustrate implementation of this instrument.

47 OTHER INSTRUMENTATION↗

Redefining precision interferometry and spectroscopy with high-performance optical interference coatings

High-performance optical interference coatings have transformed precision interferometry and spectroscopy by enabling unparalleled control over light–matter interactions. This review explores recent innovations in ion-beam sputtered amorphous dielectric, as well as substrate-transferred crystalline coatings, and their impact on systems at the forefront of precision metrology. These state-of-the-art coating techniques generate multilayers with ultralow optical losses, yielding mirrors with exceptional reflectivity. Refinements in their noise performance push the ultimate limits of sensitivity, resolution, and stability in demanding laser-based metrology applications. These technologies underpin the most advanced timekeeping and spatial measurement tools, enabling high-finesse reference cavities for the world’s most precise optical atomic clocks and low-noise reflective test masses for km-baseline gravitational-wave detectors. Emerging hybrid designs combining these techniques expand access to the mid-infrared spectral region, enabling the first ultralow-optical-loss coatings in the 3000–5000 nm wavelength range for enhanced spectroscopy and trace-gas detection. We highlight how these technologies redefine coating performance metrics and set new benchmarks in quantum science, fundamental physics, and precision optical sensing.

Cole, Garrett D. [University of Arizona, Tucson, A↗

Nanoscale phase transition in impact indented Mo/Cu thin films

The study reveals a size effect in deformation mechanisms via unique structural transitions in sputter deposited fcc/bcc nanolayers under high strain rate impact nanoindentation as layer thickness is reduced from around 100-200 nm to around 5 nm. Here, the indented 5 nm Cu/5 nm Mo multilayer films characterized via cross-sectional scanning/transmission electron microscopy have revealed a phase transition in the 5 nm thick Mo layers from BCC to a coherent metastable FCC structure and fine deformation twins in the 5 nm Cu layers inside a shear band that is approximately 500 nm long and inclined to the layer interfaces. In contrast, thicker layers, 80 nm Cu/180 nm Mo, show different deformation behavior with uneven layer thickness reduction, shearing of Cu layers, and bending of the columnar Mo grains beneath the indentation without any sign of shear band and localized phase transformation.

36 MATERIALS SCIENCE↗

Reaction of amorphous Ni-W and Ni-N-W films with substrate silicon

Wiley et al. (1982) have studied sputtered amorphous films of Nb-Ni, Mo-Ni, Si-W, and Si-Mo. Kung et al. (1984) have found that amorphous Ni-Mo films as diffusion barriers between multilayer metallizations on silicon demonstrate good electrical and thermal stability. In the present investigation, the Ni-W system was selected because it is similar to the Ni-Mo system. However, W has a higher silicide formation temperature than Mo. Attention is given to aspects of sample preparation, sample characterization, the interaction between amorphous Ni-W films and Si, the crystallization of amorphous Ni(36)W(64) films on SiO2, amorphous Ni-N-W films, silicide formation and phase separation, and the crystallization of amorphous Ni(36)W(64) and Ni(30)N(21)W(49) layers.

Zhu, M. F.↗

Hard X-Ray and Wide Focusing Telescopes

Studies are being carried out to compare the performance of several different separation materials used in the replication process. This report presents the results obtained during the second year of a program which consists of replicating smooth, thin substrates, depositing multilayer coatings upon them, and evaluating their performance. Replication and multilayer coatings are both critically important to the development of focussing hard X-ray telescopes that function up to 100 keV. The activities of the current year include extending the comparison between sputtered amorphous carbon and evaporated gold to include sputtered as well as evaporated gold. The figure of merit being the smoothness of the replica which has a direct effect on the specular reflectivity. These results were obtained with epoxy replication, but they should be applicable to electroformed nickel, the process we expect to use for the ultimate replicated optics.

Gorenstein, Paul↗

Directed Growth of Carbon Nanotubes Across Gaps

An experiment has shown that when single-walled carbon nanotubes (SWNTs) are grown by chemical vapor deposition in the presence of an electric field of suitable strength, the nanotubes become aligned along the electric field. In an important class of contemplated applications, one would exploit this finding in fabricating nanotube transistors; one would grow SWNTs across gaps between electrodes that would serve, subsequently, as source and drain contacts during operation of the transistors. In preparation for the experiment, a multilayer catalyst comprising a 20-nmthick underlayer of iridium (platinum group), a 1-nm-thick middle layer of iron, and a 0.2-nm-thick outer layer of molybdenum was ion-beam sputtered onto a quartz substrate. A 25 micrometers-diameter iron wire was used as a shadow mask during the sputtering to create a 25 micrometers gap in the catalyst. Then electrical leads were connected to the catalyst areas separated by the gap so that these catalyst areas would also serve as electrodes. The substrate as thus prepared was placed in a growth chamber that consisted of a quartz tube of 1-in. (2.54-cm) diameter enclosed in a furnace. SWNTs of acceptably high quantity and quality were grown in 10 minutes with methane at atmospheric pressure flowing through the chamber at a rate of 1,000 standard cubic centimeters per minute at a temperature of 900 C. To prevent oxidation of the SWNTs, the chamber was purged with 99.999-percent pure argon before and after growth, and the chamber was cooled to less than 300 C before opening it to the atmosphere after growth. When no voltage was applied across the gap, the SWNTs grew in random directions extending out from the edges of the catalyst at the gap. When a potential of 10 V was applied between the catalyst/electrode areas to create an electric field across the gap, the SWNTs grew across the gap, as shown in the figure.

Delzeit, Lance↗

Origin and effect of film sub-stoichiometry on ultraviolet, ns-laser damage resistance of hafnia single layers

Understanding the origin of laser damage-prone precursors in high index materials such as hafnia holds the key to the development of laser damage-resistant multilayer dielectric coated optics for high power and energy laser systems. In this study, we investigate the source of sub-stoichiometry, a potent laser damage precursor, in hafnia films produced by an ion beam sputtering (IBS) deposition method and the effect of such defects on the film performance upon ns ultraviolet (UV) laser (8 ns, 355 nm) exposure. Chemical analysis of data obtained via Rutherford backscattering spectroscopy (RBS) suggests that hafnia films deposited at two different planetary locations from the same deposition run exhibit anisotropic and location-dependent stoichiometries. While the oxygen-to-hafnium ratio is at the stoichiometric value of 2 for the hafnia film at the edge location, the ratio is significantly deviated and is 1.7 for that deposited at the planetary center. The sub-stoichiometric hafnia films display a much lower 1-on-1 damage onset at 1.6 ± 0.2 J/cm 2 compared to 2.3 ± 0.2 J/cm 2 in a stoichiometric film. The low damage performance films also have an over three times higher damage density at fluences above initiation. Coupled with Monte Carlo simulations, we reveal that sub-stoichiometry is primarily attributed to preferential removal of oxygen during film deposition by the bombardment of energetic reflected argon neutrals. The resulting oxygen deficiencies create the sub-bandgap states which facilitate the strong laser energy coupling and reduce the resistance to laser-induced damage in the hafnia single layer films.

36 MATERIALS SCIENCE↗

Characterization of ZrO2 buffer layers for sequentially evaporated Y-Ba-CuO on Si and Al2O3 substrates

Thin film high temperature superconductors have the potential to change the microwave technology for space communications systems. For such applications it is desirable that the films be formed on substrates such as Al2O3 which have good microwave properties. The use of ZrO2 buffer layers between Y-Ba-Cu-O and the substrate has been investigated. These superconducting films have been formed by multilayer sequential electron beam evaporation of Cu, BaF2 and Y with subsequent annealing. The three layer sequence of Y/BaF2/Cu is repeated four times for a total of twelve layers. Such a multilayer film, approximately 1 micron thick, deposited directly on SrTiO3 and annealed at 900 C for 45 min produces a film with a superconducting onset of 93 K and critical temperature of 85 K. Auger electron spectroscopy in conjunction with argon ion sputtering was used to obtain the distribution of each element as a function of depth for an unannealed film, the annealed film on SrTiO3 and annealed films on ZrO2 buffer layers. The individual layers were apparent. After annealing, the bulk of the film on SrTiO3 is observed to be fairly uniform while films on the substrates with buffer layers are less uniform. The Y-Ba-Cu-O/ZrO2 interface is broad with a long Ba tail into the ZrO2, suggesting interaction between the film and the buffer layer. The underlying ZrO2/Si interface is sharper. The detailed Auger results are presented and compared with samples annealed at different temperatures and durations.

Valco, George J.↗

Thermal stability and diffusion characteristics of ultrathin amorphous carbon films grown on crystalline and nitrogenated silicon substrates by filtered cathodic vacuum arc deposition

Amorphous carbon (a-C) films are widely used as protective overcoats in many technology sectors, principally due to their excellent thermophysical properties and chemical inertness. The growth and thermal stability of sub-5-nm-thick a-C films synthesized by filtered cathodic vacuum arc on pure (crystalline) and nitrogenated (amorphous) silicon substrate surfaces were investigated in this study. Samples of a-C/Si and a-C/SiN x /Si stacks were thermally annealed for various durations and subsequently characterized by high-resolution transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). The TEM images confirmed the continuity and uniformity of the a-C films and the 5-nm-thick SiN x underlayer formed by silicon nitrogenation using radio-frequency sputtering. The EELS analysis of cross-sectional samples revealed the thermal stability of the a-C films and the efficacy of the SiNx underlayer to prevent carbon migration into the silicon substrate, even after prolonged heating. The obtained results provide insight into the important attributes of an underlayer in heated multilayered media for preventing elemental intermixing with the substrate, while preserving the structural stability of the a-C film at the stack surface. An important contribution of this investigation is the establishment of an experimental framework for accurately assessing the thermal stability and elemental diffusion in layered microstructures exposed to elevated temperatures.

42 ENGINEERING↗

Growth and micro structural studies on Yittria Stabilized Zirconia (YSZ) and Strontium Titanate (STO) buffer layers

Microstructure of Yittria Stabilized Zirconia (YSZ) and Strontium Titanate (STO) of radio frequency magnetron sputtered buffer layers was studied at various sputtering conditions on Si (100), Sapphire and LaAlO3 (100) substrates. The effect of substrate temperatures up to 800 C and sputtering gas pressures in the range of 50 mTorr. of growth conditions was studied. The buffer layers of YSZ and STO showed a strong tendency for columnar growth was observed above 15 mTorr sputtering gas pressure and at high substrate temperatures. Post annealing of these films in oxygen atmosphere reduced the oxygen deficiency and strain generated during growth of the films. Strong c-axis oriented superconducting YBa2Cu3O7-x (YBCO) thin films were obtained on these buffer layers using pulsed laser ablation technique. YBCO films deposited on multilayers of YSZ and STO were shown to have better superconducting properties.

Srinivas, S.↗

A Multilayered Thin Film Insulator for Harsh Environments

The status of work to develop a reliable high temperature dielectric thin film for use with thin film sensors is presented. The use of thin films to electrically insulate thin film sensors on engine components minimizes the intrusiveness of the sensor and allows a more accurate measurement of the environment. A variety of insulating films were investigated for preventing electrical shorting caused by insulator failure between the sensor and the component. By alternating layers of sputtered high temperature ceramics, a sequence of insulating layers was devised that prevents pinholes from forming completely through the insulator and maintains high electrical resistivity at high temperatures. The major technical challenge remaining is to optimize the fabrication of the insulator with respect to composition to achieve a reliable high temperature insulating film. Data from the testing of various potentially insulating thin film systems is presented and their application to thin film sensors is also discussed.

Wrbanek, John D.↗

Combinatorial Cu-Ni Alloy Thin-Film Catalysts for Layer Number Control in Chemical Vapor-Deposited Graphene

We synthesized a combinatorial library of CuxNi1−x alloy thin films via co-sputtering from Cu and Ni targets to catalyze graphene chemical vapor deposition. The alloy morphology, composition, and microstructure were characterized via scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), and X-ray diffraction (XRD), respectively. Subsequently, the CuxNi1−x alloy thin films were used to grow graphene in a CH4-Ar-H2 ambient at atmospheric pressure. The underlying rationale is to adjust the CuxNi1−x composition to control the graphene. Energy dispersive x-ray spectroscopy (EDS) analysis revealed that a continuous gradient of CuxNi1−x (25 at. % < x < 83 at.%) was initially achieved across the 100 mm diameter substrate (~0.9%/mm composition gradient). The XRD spectra confirmed a solid solution was realized and the face-centered cubic lattice parameter varied from ~3.52 to 3.58 A˙, consistent with the measured composition gradient, assuming Vegard’s law. Optical microscopy and Raman analysis of the graphene layers suggest single layer growth occurs with x > 69 at.%, bilayer growth dominates from 48 at.% < x < 69 at.%, and multilayer (≥3) growth occurs for x < 48 at.%, where x is the Cu concentration. Finally, a large area of bi-layer graphene was grown via a CuxNi1−x catalyst with optimized catalyst composition and growth temperature.

2D materials↗

Fracture resistance of hierarchical Cu–Mo nanocomposite thin films

We report the fracture behavior of high-temperature co-sputtered Cu/Mo nanocomposite thin films was investigated through in situ 3-point bend testing of pre-notched microbeams in SEM. The as-synthesized nanocomposites present hierarchical nano/microstructures composed of a matrix of phase-separated Cu–Mo with nanoscale ligaments dispersed with sub-micron scale Cu-rich islands containing Mo nano-precipitates. Results show a significant crack growth resistance in the hierarchical nanocomposite, several times higher than that measured in Cu/Mo nanoscale multilayers. Based on electron microscopy characterization, three mechanisms of crack growth resistance in the hierarchical structures are proposed: crack bridging by the Cu-rich layer, crack deflection via shear along the Cu/Mo interface, and multiple cracking. This work demonstrates an approach to increase toughness in high strength nanocomposites through interface micro-structure design.

36 MATERIALS SCIENCE↗

Understanding spectral dependance of laser-induced damage precursors in dielectric materials (Full report_23-ERD-006)

The performance of high-energy laser systems is constrained by laser-induced damage in dielectric coatings, particularly those containing hafnium oxide (HfO 2 ). While thresholds at fundamental Nd harmonics are well studied, the spectral dependence of damage initiation—especially under dual-wavelength irradiation—remains poorly characterized. This project provides the first systematic investigation of wavelength-dependent laser damage in hafnia coatings, focusing on nanoscale precursors such as craze lines, nanobubbles, stoichiometric variations, nodules, and controlled crystallization. Coatings were fabricated via ion beam sputtering and electron-beam deposition and characterized using spectrophotometry, ellipsometry, AFM, GI-XRD, RBS, PCI absorption, and fs/ns laser damage testing. Results show that craze lines, benign under infrared light, strongly initiate damage under UV due to wavelength-selective field intensification. Substituting xenon for argon suppresses nanobubbles and improves UV thresholds by up to 32%. Oxygen modulation reveals that fully oxidized films maximize UV resistance, though at the cost of porosity and stress in multilayers. HfO 2 –SiO 2 composites resist crystallization and defects while achieving ppm-level absorption and elevated thresholds, whereas full crystallization of HfO 2 enhances LIDT by reducing defects and improving thermal transport. Collectively, these findings link photon energy, defect states, and bandgap collapse, providing a predictive framework for wavelength-dependent laser damage. The outcomes directly inform the design of durable, multi-wavelength coatings for facilities such as NIF, MEC, HAPLS, and DPAL, advancing the readiness of next-generation optics.

36 MATERIALS SCIENCE↗

Multi-Dimensional Damage Detection for Surfaces and Structures

Current designs for inflatable or semi-rigidized structures for habitats and space applications use a multiple-layer construction, alternating thin layers with thicker, stronger layers, which produces a layered composite structure that is much better at resisting damage. Even though such composite structures or layered systems are robust, they can still be susceptible to penetration damage. The ability to detect damage to surfaces of inflatable or semi-rigid habitat structures is of great interest to NASA. Damage caused by impacts of foreign objects such as micrometeorites can rupture the shell of these structures, causing loss of critical hardware and/or the life of the crew. While not all impacts will have a catastrophic result, it will be very important to identify and locate areas of the exterior shell that have been damaged by impacts so that repairs (or other provisions) can be made to reduce the probability of shell wall rupture. This disclosure describes a system that will provide real-time data regarding the health of the inflatable shell or rigidized structures, and information related to the location and depth of impact damage. The innovation described here is a method of determining the size, location, and direction of damage in a multilayered structure. In the multi-dimensional damage detection system, layers of two-dimensional thin film detection layers are used to form a layered composite, with non-detection layers separating the detection layers. The non-detection layers may be either thicker or thinner than the detection layers. The thin-film damage detection layers are thin films of materials with a conductive grid or striped pattern. The conductive pattern may be applied by several methods, including printing, plating, sputtering, photolithography, and etching, and can include as many detection layers that are necessary for the structure construction or to afford the detection detail level required. The damage is detected using a detector or sensory system, which may include a time domain reflectometer, resistivity monitoring hardware, or other resistance-based systems. To begin, a layered composite consisting of thin-film damage detection layers separated by non-damage detection layers is fabricated. The damage detection layers are attached to a detector that provides details regarding the physical health of each detection layer individually. If damage occurs to any of the detection layers, a change in the electrical properties of the detection layers damaged occurs, and a response is generated. Real-time analysis of these responses will provide details regarding the depth, location, and size estimation of the damage. Multiple damages can be detected, and the extent (depth) of the damage can be used to generate prognostic information related to the expected lifetime of the layered composite system. The detection system can be fabricated very easily using off-the-shelf equipment, and the detection algorithms can be written and updated (as needed) to provide the level of detail needed based on the system being monitored. Connecting to the thin film detection layers is very easy as well. The truly unique feature of the system is its flexibility; the system can be designed to gather as much (or as little) information as the end user feels necessary. Individual detection layers can be turned on or off as necessary, and algorithms can be used to optimize performance. The system can be used to generate both diagnostic and prognostic information related to the health of layer composite structures, which will be essential if such systems are utilized for space exploration. The technology is also applicable to other in-situ health monitoring systems for structure integrity.

Williams, Martha↗

Soft x ray optics by pulsed laser deposition

A series of molybdenum thin film depositions by PLD (Pulsed Laser Deposition) have been carried out, seeking appropriate conditions for multilayer fabrication. Green (532 nm) and UV (355 nm) light pulses, in a wide range of fluences, were used. Relatively large fluences (in comparison with Si) are required to cause evaporation of molybdenum. The optical penetration depths and reflectivities for Mo at these two wavelengths are comparable, which means that results should be, and do appear to be similar for equal fluences. For all fluences above threshold used, a large number of incandescent particles is ejected by the target (either a standard Mo sputtering target or a Mo sheet were tried), together with the plasma plume. Most of these particles are clearly seen to bounce off the substrate. The films were observed with light microscopy using Nomarski and darkfield techniques. There is no evidence of large debris. Smooth films plus micron-sized droplets are usually seen. The concentration of these droplets embedded in the film appears not to vary strongly with the laser fluence employed. Additional characterization with SEM and XRD is under way.

Fernandez, Felix E.↗