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SiO2 glass has been irreversibly densified by pressures up to 250 kbar produced in a magnetic pinch apparatus. The threshold for significant densification was about 60 kbar. The recovered densities agree better with published shock wave results than with static results.
Optical examination of nine polished grain mounts of Luna-24 drill-core material (0.09-0.50 mm size) revealed melt inclusions in olivine crystals. Two inclusions consist of clear glass with exceptionally high Si, yet contain no visible daughter minerals and have had no reaction effects with the olivine walls. Their compositions (one has SiO2 93.8, Al2O3 1.51, FeO 2.32, MgO 1.61, CaO 0.06, Na2O less than 0.05, K2O 0.11, total 99.41%; the other is similar) are unique and quite unlike the high-Si high-K melt of granitic composition that is found as inclusions in late-stage minerals of these (and the Apollo) samples, from silicate liquid immiscibility. The host olivines are Fo73 and Fo51. The origin of the melt in the inclusions and the lack of reaction effects are perplexing unsolved problems.
The effects of retained bound hydroxyl groups on amorphous immiscibility behavior and on the kinetics of phase separation were studied in glasses containing from 10 to 19 percent sodium oxide preparaed by the gel process. Differences in behavior as functions of preliminary thermal treatment of the gel precursor and of melting conditions were studied, employing IR spectroscopy, SAXS and WAXD to monitor the variation in glass microstructure. Both the initial gel treatment and the OH concentration in the prepared glasses were found to affect the immiscibility temperatures, and the magnitude of the maximum temperature increase was also a function of the sodium oxide concentration. It is suggested that the variation in thermodynamic behavior may be caused by the structural arrangement attained by the OH groups during the gel condensation process, which in turn affects the extent of hydrogen bonding to nonbridging oxygen ions.
DTA and both isothermal and nonisothermal DSC techniques are presently used to investigate the crystallization kinetics of a 40 (mol) percent Li2O-60 percent SiO2 glass as a function of glass powder particle size, the use of either alumina or Pt as the crucible material, the use of N, O, or Ar atmospheres, and surface pretreatments of the glass powder with deionized water, HCl, or HF. Neither the furnace atmosphere nor the crucible material had a significant effect on activation energy, frequency factor, or Avrami exponent. Washings of the glass with the three different fluids decreased the crystallization temperature by 25 to 30 C.
For the first (low energy) calculation both the particle and crater parameters (from tests at AU/HIF) were known, For the second (high energy) calculation, only the particle parameters were known. In both cases the computed craters agreed with historical data of impact on glass. Additional tests at AU/HIF are expected to confirm the results of the second calculation and to validate the technique for use at higher velocities.
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During phenolic liner manufacture, resin-impregnated (pre-preg) bias tape of silica, glass, or carbon cloth is tape-wrapped, cured, machined, and then wiped with 1,1,1 tri-chloroethane (TCA) to remove contaminants that may have been introduced during machining and handling. Following the TCA wipe, the machined surface is given a resin wet-coat and over-wrapped with more prepreg and cured. A TCA replacement solvent for these wiping operations must effectively remove both surface contaminants, and sub-surface oils and greases while not compromising the integrity of this interface. Selection of a TCA replacement solvent for phenolic over-wrap interface cleaning began with sub-scale compatibility tests with cured phenolics. Additional compatibility tests included assessment of solvent retention in machined phenolic surfaces. Results from these tests showed that, while the candidate solvent did not degrade the cured phenolics, it was retained in higher concentrations than TCA in phenolic surfaces. This effect was most pronounced with glass and silica cloth phenolics with steep ply angles relative to the wiped surfaces.
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.
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.
Residual gases present in closed ampoules may affect different crystal growth processes. Their presence may affect techniques requiring low pressures and affect the crystal quality in different ways. For that reason a good understanding and control of formation of residual gases may be important for an optimum design and meaningful interpretation of crystal growth experiments. Our extensive experimental and theoretical study includes degassing of silica glass and generation of gases from various source materials. Different materials processing conditions, like outgassing under vacuum, annealing in hydrogen, resublimation, different material preparation procedures, multiple annealings, different processing times, and others were applied and their effect on the amount and composition of gas were analyzed. The experimental results were interpreted based on theoretical calculations on diffusion in silica glass and source materials and thermochemistry of the system. Procedures for a reduction of the amount of gas are also discussed.
Residual gases present in closed ampoules may affect different crystal growth processes. That seems to be particularly true under microgravity conditions where, due to weightlessness of the melt, the gases may lead to detached solidification and/or formation of voids and bubbles, as observed in the past. For that reason a good understanding and control of formation of residual gases is important for an optimum design and meaningful interpretation of crystal growth experiments. Our extensive experimental and theoretical studies of the subject, summarized in this paper, include degassing of silica glass and generation of gases from different source materials. Different materials processing conditions, like outgassing under vacuum, annealing in hydrogen, resublimation, different material preparation procedures, multiple annealings, different processing times, and others were applied and their effect on the amount and composition of gas were analyzed. The experimental results were interpreted based on theoretical calculations on diffusion in silica glass and source materials and thermochemistry of the system. Procedures for a reduction of the amount of gas are also discussed.
A dynamic fatigue study was performed on a Li2O-Al2O3-SiO2 glass-ceramic in order to assess its susceptibility to delayed failure. Fracture mechanics techniques were used to analyze the results for the purpose of making lifetime predictions for optical elements made from this material. The material has reasonably good resistance (N = 20) to stress corrosion in ambient conditions. Analysis also indicated the elements should survive applied stresses incurred during grinding and polishing operations.
The glass-ceramic (Zerodur, Schott Glaswerke, Mainz, Germany) contains 70% to 78% by weight crystalline phase of high-quartz structure with a mean crystal size of 50-55 nm. The vitreous phase has a positive thermal expansion coefficient which is practically balanced by the negative coefficient of the crystalline phase. This results in a material which can maintain longitudinal stability during thermal cycling. This was one of the reasons for its choice as the material for the grazing incidence mirrors for the Chandra X-Ray Facility. Brittle materials such as glass and glass-ceramics which exhibit slow crack growth and subsequent fast fracture to failure exhibit a time dependence in strength. The decrease in strength for a constant applied load is known as static fatigue. In many cases, environment plays a major role in the material lifetime. It has been shown for silicate glasses that crack velocity will increase as the amount of water vapor in the environment surface finish and rate of loading. A rough surface finish leads to a lower tensile strength than for an optically polished surface. The strength of glass is observed in general to increase with increasing load rate. This phenomena is known as dynamic fatigue. This was observed for Zerodur by Tucker and Gent and Tucker in previous dynamic fatigue studies, in which lifetimes were obtained. All of the above named factors need to be considered when glass is to be used in load bearing applications.
Bonding between silica glass reinforcement and plastic matrix of glass-reinforced plastic composite material
The reflectances of two low-expansion materials, a recrystallized glass ceramic and a high silica glass, have been measured at five angles of incidence from 15 to 85 deg in the wavelength region from 80 to 310 A and in some cases up to 1050 A. Optical constants are derived and silicon core-level transitions analyzed.
A 50 cm by 50 cm solar array panel test patch was investigated for spacecraft charging and arcing effects. Bombardment with monochromatic electron was carried out. Some objectives of the test were: (1) to estimate at what voltage of electron bombardment arcing would be probable; (2) to find whether the arc's energy would be tolerable or damagingly large; (3) to try and separate thermal and photoeffects; and, (4) to see whether materials used were such as to minimize arcing. Some conclusions were: In sunlight the tracking data relay satellite's solar panel which has ceria glass on the front and conductive paint on the backside is probably a good design for reducing charge-up. In a geomagnetic substorm simulated in testing there will be arcing at the interconnects during eclipse and transitions into and out of eclipse in testing especially in view of the very cold temperatures that will be reached by this lightweight array. Ceria-doped glass is preferred to fused silica glass for reducing charge build up. The Kapton bare patch should still be conductively painted. The differential voltages on the panel determine when arcing first begins, and the electron beam voltages vary depending upon whether the metallic structure is directly grounded or semifloating.
Physical properties investigation of silica glass systems with complex three-dimensional crystal structures and high moduli of elasticity
The TSC (Thermally Stable Composite) refers to a family of graphite reinforced glass matrix composite materials developed by UTOS. This fiber matrix combination exhibits low coefficients of thermal expansion (CTE), exceptional dimensional stability, high specific strength and stiffness, adequate fracture toughness, and space environment compatibility. The dimensional stability of a TSC mirror structure was experimentally characterized at the Steward Observatory. Preliminary results indicate that TSC is significantly more thermally stable than most current structural composite materials. In addition, the use of lower CTE glass matrix materials, such as 96 percent silica glass, have the potential for producing graphite/glass panels with expansion rates and stability comparable to that of fused silica.