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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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White-light interferometry for early-stage metal oxide growth characterization

Oxidation of metals can provide a functional oxide film or an oxide layer that can lead to material degradation causing performance limiting concerns. Because of the technological and economic impacts of oxidation, understanding early-stage oxidation growth and its mechanisms is of high importance. Unfortunately, poor empirical data during early-stage oxidation has left our current understanding of oxidation incomplete and woefully inadequate. Measurement techniques previously used for oxidation kinetics characterization include microbalance, x-ray diffraction, Fourier-transform infrared spectroscopy, and spectroscopic ellipsometry. However, these techniques lack the necessary time-resolution or vertical resolution in addition to not providing any spatial data, which is essential to early-stage oxidation studies to understand both oxidation kinetics and mechanisms. Here, a novel rapid and surface-sensitive data collection technique that provides three-dimensional spatial data of a growing oxide layer with sub-nanometer thickness resolution using white-light interferometry has been developed. This technique will be the first technique capable of providing real-time spatial results of early-stage oxidation growth. The effectiveness of this characterization tool is shown by observing the early-stage oxidation kinetics and film cracking of uranium heated to 90 °C under 500 torr of pure O 2 . Initially a parabolic oxidation growth is observed. Once the oxide layer reaches ≈ 30 nm, the epitaxial stresses between the uranium substrate and oxide film layer causes localized cracking in addition to the observed transition of the parabolic growth rate to a linear growth rate. The results of the white-light interferometry are verified by glancing incidence x-ray diffraction.

47 OTHER INSTRUMENTATION↗

Topography restoration in white-light interferometry using an instrument transfer function evaluated with binary pseudo-random arrays

Accurate knowledge of the instrument transfer function (ITF) is vital for topography measurements using white-light interferometry (WLI). To this end, we derive a complete set of analytical expressions for the power spectral density (PSD) of a discretely sampled binary pseudo-random array (BPRA) as a theoretical benchmark. We then determine the ITF by comparing this theoretical PSD with the measured PSD of the BPRA. For the Zygo ZeGage Pro HR with a objective, the determined ITF closely matches the nominal modulation transfer function (MTF). Accordingly, we integrate the nominal MTF into Fourier-domain restoration filters and apply them to practical WLI topography data, yielding restored topographies that show improved agreement with atomic force microscopy measurements. Overall, our integrated BPRA-based ITF measurement and filtering methodology offers a robust yet practical means of characterizing WLI performance and enhancing the accuracy of surface measurements.

Hirose, Shigenobu [Japan Agency for Marine Earth S↗

White-light Interferometry using a Channeled Spectrum: II. Calibration Methods, Numerical and Experimental Results

In the companion paper, [Appl. Opt. 46, 5853 (2007)] a highly accurate white light interference model was developed from just a few key parameters characterized in terms of various moments of the source and instrument transmission function. We develop and implement the end-to-end process of calibrating these moment parameters together with the differential dispersion of the instrument and applying them to the algorithms developed in the companion paper. The calibration procedure developed herein is based on first obtaining the standard monochromatic parameters at the pixel level: wavenumber, phase, intensity, and visibility parameters via a nonlinear least-squares procedure that exploits the structure of the model. The pixel level parameters are then combined to obtain the required 'global' moment and dispersion parameters. The process is applied to both simulated scenarios of astrometric observations and to data from the microarcsecond metrology testbed (MAM), an interferometer testbed that has played a prominent role in the development of this technology.

phase correction↗

LLNL FY22 Aging and Lifetimes Exit Criteria (Milestone 8118, GC#5)

This report introduces a novel characterization tool that can rapidly collect in-situ time-dependent oxide thickness and hydride growth data together with spatial data using while-light interferometry. White-light interferometry is a non-destructive and non-contact optical surface profiling technique for materials characterization that offers excellent lateral and vertical resolution. A depleted uranium sample was used to assess the ability of white-light interferometry to provide quantitative corrosion reaction rates at metal surfaces for by hydriding and oxidation and compare this technique to existing characterization tools for capturing early-stage hydride and oxide growth kinetics.

36 MATERIALS SCIENCE↗

Early-stage uranium-hydrogen corrosion kinetics and mechanism

Research into the early-stage uranium-hydrogen degradation mechanism lacks unified interpretation and understanding due to inadequate temporal and spatial characterization resolution required to unify reaction observations. In this study, white-light interferometry was adapted to characterize the uranium-hydrogen reaction at a temperature of 50 °C and hydrogen pressure of 13.8 kPa. The uranium surface remained unchanged for 62 min during the hydride induction period before the first hydride blister appeared. This blister was monitored from induction through critical spallation and UH₃ powder release during rapid surface hydriding. The critical spallation dimensions measured for height, diameter, area, and perimeter of the first blister were 1.79 µm, 17.58 µm, 187.7 µm 2 and 59.79 µm. Hydriding growth kinetics were assessed by tracking the first hydride site over the reaction time. Analysis shows that the spall-front velocity of the hydride was changing at a rate of 0.91 µm/min which compares favorably with legacy Sievert’s experiments in literature. Total percentage of the surface area hydrided after 242 min was 42.7%, and post-characterization of the UH 3 powders shows both α-UH 3 and β-UH 3 . This work highlights the strength of characterizing the early-stage uranium-hydrogen reaction using white-light interferometry, but more importantly, unifying the understanding and mechanism of the uranium-hydrogen reaction kinetics.

Materials science↗

Sub-melt nanosecond pulsed-laser induced densification and strain-field relaxation in single-crystal diamond

Dislocations and polishing-induced defect networks in synthetic diamond introduce local strain fields and broaden Raman features, limiting performance in optical, thermal, and electronic applications. Laser annealing is emerging as a promising approach to repair surface and near-surface defects in diamond without entering the melt regime, yet surface densification, defect-state modification, and associated structural changes have not been well quantified. In this work, we show that sub-melt nanosecond pulsed-laser annealing (PLA) induces near-surface densification and defect-mediated strain relaxation in single-crystal Chemical Vapor Deposition (CVD) diamond. Single- and two-pulse PLA were applied, and structural evolution was quantified using co-registered ISO 25,178 white-light interferometry, depth-resolved Raman spectroscopy, and cross-sectional STEM with geometric phase analysis (GPA). Across a 5 × 6 grid (n = 30), responsive regions exhibit large reductions in local slope (Sdq 45–65%), developed area (Sdr 60–90%), height spread (Sp, Sz 30–65%), void volume (Vv 57–60%), and roughness amplitude (Sa, Sq 48–57%), consistent with densification of ∼4–6.5 nm. Raman profiling shows narrowing of the diamond line and improved spectral uniformity to depths of ∼2–3 μm. Given that the Raman probing depth significantly exceeds the densified layer thickness, this response is interpreted as consistent with long-range strain-field redistribution originating from the near-surface region. STEM-GPA strain maps further support this interpretation, showing smoother strain fields, suppressed hotspots, and redistribution of localized strain concentrations following PLA. These results are consistent with defect-mediated strain relaxation and densification-driven modification of the near-surface energy state. The approach provides a scalable pathway for improving near-surface structural quality in diamond relevant to electronic, photonic, and quantum applications.

Areal surface metrology (ISO 25,178)↗

Artificial linear brush abrasion of coatings for photovoltaic module first-surfaces

Natural soiling and the subsequent necessary cleaning of photovoltaic (PV) modules result in abrasion damage to the cover glass. The durability of the front glass has important economic consequences, including determining the use of anti-reflective and/or anti-soiling coatings as well as the method and frequency of operational maintenance (cleaning). Artificial linear brush abrasion using Nylon 6/12 bristles was therefore examined to explore the durability of representative PV first-surfaces, i.e., the surface of a module incident to direct solar radiation. Specimens examined include silane surface functionalized-, roughened (etched)-, porous silica-coated-, fluoropolymer-coated-, and ceramic (TiO 2 or ZrO 2 /SiO 2 /ZrO 2 /SiO 2 )-coated-glass, which are compared to monolithic-poly(methyl methacrylate) and -glass coupons. Characterization methods used in this study include: optical microscopy, ultraviolet–visible–near-infrared (UV-VIS-NIR) spectroscopy, sessile drop goniometry, white-light interferometry, atomic force microscopy (AFM), and depth-profiling X-ray photoelectron spectroscopy (XPS). The corresponding characteristics examined include: surface morphology, transmittance (i.e., optical performance), surface energy (water contact angle), surface roughness, scratch width and depth, and chemical composition, respectively. The study here was performed to determine coating failure modes; identify characterization methods that can detect nascent failures; compare the durability of popular contemporary coating materials; identify their corresponding damage characteristics; and compare slurry and dry-dust abrasion. This study will also aid in developing an abrasion standard for the PV industry.

14 SOLAR ENERGY↗

Advanced monolithic 2D multilayer Laue lens (MLL) optics for hard x-ray nanofocusing and nanotomography

We report on the development of a new generation of monolithic two-dimensional (2D) multilayer Laue lens (MLL) optics suitable for high-resolution hard x-ray nanoimaging. The 2D optics were assembled on microfabricated silicon templates with high orthogonality and lateral alignment precision, which were characterized using white-light interferometry and confirmed by x-ray measurements. The developed monolithic 2D MLL optics were successfully employed for hard x-ray nanofocusing and nanotomography experiments using the ptychography imaging modality, demonstrating sub-10 nm resolution in 2D and sample-limited ∼30 nm in three-dimensional while exhibiting excellent stability during extended measurements. The new 2D MLL templates with high alignment accuracy represent an important step forward in the development of 2D MLL optics toward direct nanoimaging experiments with sub-10 nm spatial resolution.

36 MATERIALS SCIENCE↗

Optical Fiber Strain Instrumentation for High Temperature Aerospace Structural Monitoring

The objective of the program is the development and laboratory demonstration of sensors based on silica optical fibers for measurement of high temperature strain for aerospace materials evaluations. A complete fiber strain sensor system based on white-light interferometry was designed and implemented. An experiment set-up was constructed to permit testing of strain measurement up to 850 C. The strain is created by bending an alumina cantilever beam to which is the fiber sensor is attached. The strain calibration is provided by the application of known beam deflections. To ensure the high temperature operation capability of the sensor, gold-coated single-mode fiber is used. Moreover, a new method of sensor surface attachment which permits accurate sensor gage length determination is also developed. Excellent results were obtained at temperatures up to 800-850 C.

Wang, A.↗

Artificial Linear Brush Abrasion of Coatings for Photovoltaic Module First Surfaces

Natural soiling and the subsequent requisite cleaning of photovoltaic (PV) modules result in abrasion damage to the cover glass. The durability of the front glass has important economic consequences, including determining the use of anti-reflective and/or anti-soiling coatings as well as the method and frequency of operational maintenance (cleaning). Artificial linear brush abrasion using Nylon 6/12 bristles was therefore examined to explore the durability of representative PV first-surfaces, i.e., the surface of a module incident to direct solar radiation. Specimens examined include silane surface functionalized-, roughened (etched)-, porous silica-coated-, fluoropolymer-coated-, and ceramic (TiO2 or ZrO2/SiO2/ZrO2/SiO2)-coated-glass, which are compared to monolithic-poly(methyl methacrylate) and -glass coupons. Characterization methods used in this study include: optical microscopy, ultraviolet-visible-near-infrared (UV-VIS-NIR) spectroscopy, sessile drop goniometry, white-light interferometry, atomic force microscopy (AFM), and depth-profiling X-ray photoelectron spectroscopy (XPS). The corresponding characteristics examined include: surface morphology, transmittance (i.e., optical performance), surface energy (water contact angle), surface roughness, scratch width and depth, and chemical composition, respectively. The study here was performed to determine coating failure modes; identify characterization methods that can detect nascent failures; compare the durability of popular contemporary coating materials; identify their corresponding damage characteristics; and compare slurry and dry-dust abrasion. This study will also aid in developing an abrasion standard for the PV industry.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Fiber optic sensors IV; Proceedings of the Third European Congress on Optics, The Hague, Netherlands, Mar. 13, 14, 1990

Recent advances in fiber-optic sensor (FOS) technology are examined in reviews and reports. Sections are devoted to components for FOSs, special fibers for FOSs, interferometry, FOS applications, and sensing principles and influence. Particular attention is given to solder glass sealing technology for FOS packaging, the design of optical-fiber current sensors, pressure and temperature effects on beat length in highly birefringent optical fibers, a pressure FOS based on vibrating-quartz-crystal technology, remote sensing of flammable gases using a fluoride-fiber evanescent probe, a displacement sensor with electronically scanned white-light interferometer, the use of multimode laser diodes in low-coherence coupled-cavity interferometry, electronic speckle interferometry compensated for environmentally induced phase noise, a dual-resolution noncontact vibration and displacement sensor based on a two-wavelength source, and fiber optics in composite materials.

Kersten, Ralf T.↗