Results for “Fused Silica” — Page 2

To fabricate optical components with surface layers compatible with high power laser applications that may operate as antireflective coatings, polarization rotators, or harness physical anisotropy for other uses, metasurfaces are becoming an appealing candidate. In this study, a large-beam (1.05 cm diameter) 351-nm laser-induced damage testing was done on an all-glass metasurface structure composed of cone-like features with a subwavelength spacing of adjacent features. These structures were fabricated on untreated fused silica glass and damage tested, as were structures that were fabricated on fused silica glass that experienced a preliminary etching process to remove the surface Beilby layer that is characteristic of polished fused silica. The laser-induced damage onset for structures on untreated fused silica glass was 19.3 J∙cm -2 , while the sample that saw an initial pretreatment etch exhibited an improved damage onset of 20.4 J∙cm -2 , only 6% short of the reference pretreated glass damage onset of 21.7 J∙cm -2 . For perspective, the National Ignition Facility (NIF) operational average fluence at this wavelength and pulse length is about 10 J/cm2. At a fluence of 25.5 J∙cm -2 , the reference (pretreated) fused silica initiated 5.2 damage sites per mm 2 , while the antireflective metasurface sample with a preliminary etching process treatment initiated 9.8 damage sites per mm 2 . In conclusion, these findings demonstrate that substrate-engraved metasurfaces are compatible with high energy and power laser applications, further broadening their application space.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Glass Additive and Subtractive Manufacturing of a Fiber Optic Rotary Encoder for Downhole Pressure Sensing

This article presents a fiber optic rotary encoder-based pressure sensor for downhole applications. The rotary encoder, which is composed of an encoding pad and an all-glass optical fiber sensing head, converts the rotation angles of a pressure transducer to digital codes. The optical fiber only serves as the telemetry channel to directly transmit the data in digital format such that the environmental temperature influence and the long-time drift are minimized. The glass additive and subtractive manufacturing (ASM) techniques are used to embed the multichannel optical fibers into a bulk-fused silica glass substrate. Because the fused silica glass shares a similar material property to the optical fiber (e.g., thermal expansion coefficient), the optical fiber sensing head is well sealed and fixed even at an elevated temperature. The picosecond laser blackening technique is used to fabricate the high reflectivity contrast encoding pad with high accuracy. Here, the proposed pressure sensor was manufactured and experimentally verified to have a signal-to-noise ratio (SNR) of 23 dB and a linear pressure response with a root-mean-square error (RMSE) of 0.37. During the 400-h 250 °C long-term stability test, there was no digital code variation. In addition, a mathematical model to study the relationships between the sensor’s performances and design parameters was established. According to the model, a 12-bit encoder (0.02% pressure sensitivity) can be achieved with a radius of 20 mm.

02 PETROLEUM↗

DOE OSTI2020

Solid Cherenkov detector for studying nucleosynthesis in inertial confinement fusion

Measuring gamma rays emitted from nuclear reactions gives insight into their nuclear structure. Notably, there are several nuclear reactions that produce gamma rays at ~1 MeV–3 MeV energies such as T( 4 He, γ) 7 Li, 4 He( 3 He, γ) 7 Be, and 12 C(p, γ) 13 N, which may solve questions lingering about big-bang nucleosynthesis and stellar nucleosynthesis. To observe 1 MeV–3 MeV gamma rays in an inertial confinement fusion system, a new style of the Cherenkov detector was developed using aerogel and fused silica as a Cherenkov medium. Utilizing the OMEGA laser facility, both aerogel and fused silica media were compared with the existing gas-medium Cherenkov detector to validate the concept. Furthermore, gamma ray measurements from high yield inertial confinement fusion implosions (deuterium–tritium and deuterium– 3 He) demonstrated that aerogel and fused silica were viable Cherenkov media, paving the way for a potential optimized detector to make these cross section measurements on OMEGA or the National Ignition Facility.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Probing the high-pressure densification of amorphous silica nanomaterials using SBA-15: An investigation into the paradoxical nature of the first sharp diffraction peak

The densification and X-ray scattering of mesoporous silica (SBA-15) were measured simultaneously under gigapascal (GPa) pressures. The results are compared to previous work on amorphous silica (aSiO 2 ) and demonstrate the feasibility of measuring the densification of aSiO 2 nanomaterials with small angle X-ray scattering (SAXS) in-situ in a diamond anvil cell. Compared to fused silica, the position of the SBA-15 first sharp diffraction peak (FSDP) is 7 times more sensitive to pressure and has a transition in its pressure dependance at a lower pressure (~2 GPa vs.~13 GPa). SBA-15 has two densification regimes, low-density amorphous and highdensity amorphous, which have equations of state comparable to low-density amorphous and high-density amorphous fused silica. Further, the transition between these two regimes occurs at a lower pressure than for fused silica (~1.5 GPa vs.~13 GPa). The results suggest that there is no direct relationship between the FSDP position and the aSiO 2 density during compression.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

A versatile and low-cost chip-to-world interface: enabling ICP-MS characterization of isotachophoretically separated lanthanides on a microfluidic device

Microfluidics offer novel and state-of-the-art pathways to process materials. Microfluidic systems drastically reduce timeframes and costs associated with traditional lab-scale efforts in the area of analytical sample preparations. The challenge arises in effectively connecting microfluidics to off-chip analysis tools to accurately characterize samples after treatment on-chip. Here, a fused silica microfluidic device (MFD) is connected to a fused-silica capillary in order to create a world-to-chip connection between the MFD and an inductively coupled plasma mass spectrometer (ICP-MS). Specifically, this is demonstrated by utilizing isotachophoresis (ITP) on a microfluidic chip to separate samples containing up to 14 lanthanides into elementally pure bands. The separated sample is successfully transferred across a 7 nL dead space at the microchip-capillary junction, such that separation resolution is maintained and even increased through the interface and into the ICP-MS, where the elemental composition of the separated sample is analysed. Lanthanide samples of varying composition are detected using ICP-MS, demonstrating this versatile and cost-effective approach that does not degrade the separation quality achieved on the MFD. This simple and inexpensive connection enables fast, low-cost sample preparation immediately prior to injection into an ICP-MS or other analytical instruments.

Lackey, Hope E.↗

DOE OSTI2022

Temperature-dependent spectral emittance of bauxite and silica particle beds

Bauxite and silica particles are candidate materials for solar thermal energy storage at high temperatures. The temperature-dependent emittance of packed beds with bauxite and silica particles was measured using a newly upgraded emissometer at wavelengths 2 μm ≤ λ ≤ 16 μm and temperatures up to ~730 K. The room-temperature emittance was obtained from the measured directional-hemispherical reflectance. A fused silica disc was used to test the emissometer by comparing the measured spectral emittance with the calculated emittance from a fitted Lorentz oscillator model. For the polycrystalline silica particles and the fused silica disc, the measured emittance increases with temperature in the mid-infrared region. The underlying mechanism is interpreted as the temperature-dependent damping coefficient in the Lorentz oscillator model. Two types of bauxite particles with different compositions and sizes were investigated. For λ > 10 μm, the measured emittance at elevated temperatures is higher than that at room temperature. In the region 2 μm < λ < 6 μm, the temperature dependence varies for different types of particles. The total emittance of bauxite particle beds was calculated by spectral integration using Planck’s distribution at the prescribed temperature. As a result, the calculated total emittance is between 0.89 and 0.96, but it does not change monotonically with temperature.

42 ENGINEERING↗

DOE OSTI2024

Spherical Indentation and Implementation of S 3 /P for yield stress determination of brittle materials

Here, a mathematically transparent and robust experimental method has been developed to estimate the yield stress of brittle materials through the analysis of depth-sensing spherical indentation. Employing Hertzian contact mechanics, an elastically invariant ratio based on the simple equation S 3 / P = 6RE r 2 , (where S and P are contact stiffness and indentation load, respectively) has been derived that enables more accurate and confident determination of the transition from elastic to inelastic deformation; a transition that the yield stress dictates and represents. Using two diamond spheres with radii of 3.2 and 8.6 μm, the indentation test method and analyses are applied to two vitreous silicates: Corning's HPFS 7980® fused silica and Vitro's Starphire® soda lime silicate. The estimated yield strengths are 8.15 GPa ± 2.5% for the fused silica and 6.1 GPa ± 3.3% for the soda-lime silicate, and both were independent of indenter radius. Verification of this new experimental method is demonstrated with an as-drawn titanium by showing equivalence of measured yield stress by its spherical indentation and that from uniaxial compression testing. This method will enable easier and more confident estimation of yield stress in brittle materials - a property that historically has been elusive to measure for these materials using common laboratory mechanical test methods.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Scalable waveplate for ultraviolet applications using laser-imprinted birefringence in silica

A method for fabrication of large-aperture waveplate suitable for operation in the near-ultraviolet spectral region is demonstrated. The waveplate was fabricated using femtosecond direct laser writing of bulk fused silica. This method enables the precise control of the induced birefringence, which is introduced via the generation of nanopores with geometrical features that are controlled by the laser processing parameters. The resulting structures also introduce a small loss of transmission that is on the order of 4% at 351 nm. The laser-induced–damage threshold in the nanosecond regime was found to approach that of the native fused-silica substrate, which makes it a suitable candidate for polarization control in laser fusion research applications.

Shevtsov, S. I. [Univ. of Southampton (United King↗