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Iron redox analysis of silicate-based minerals and glasses using synchrotron X-ray absorption and laboratory X-ray emission spectroscopy
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Absorption and fluorescence of alexandrite and of titanium in sapphire and glass
The fluorescence and absorption data for titanium in crystalline sapphire and titanium doped into two silicate and one phosphate glass structures are analyzed. It is observed that the Ti-doped silicate glass sample exhibits no absorption related to the Ti(III) ion, the Ti-doped phosphate glass is deep blue, the absorption line width of the glass samples are a factor of two larger than that of sapphire, and the absorption peak for the Ti in the glass shifted about 100 nm to the red from the Ti:sapphire absorption peak. This shift reveals that the Ti(III) ion is sensitive to the crystalline environment and not to the glass environment. The photoluminescence spectra for Ti-doped sapphire and alexandrite are compared. It is detected that the Ti:sapphire exhibits a broader spectrum than that for alexandrite with a peak at 750 nm. The three zero phonon transitions of Ti:Al2O3 at liquid nitrogen temperatures are studied.
PRODUCTION OF GLASS-TO-METAL SEALS USING ADDITIVE MANUFACTURING TECHNIQUES
Glass-to-metal (GtM) seals are hermetic barriers between glass and metal components, often used in the electronic and vacuum industries. Creating the seals traditionally requires heating all the components to the glass melting temperature, where the glass will flow and bond to the metal. Due to the manufacturing constraints of the individual components and sealing conditions there are geometric and material restrictions. Additive manufacturing techniques were used to make GtM seals to reduce these restrictions. Hermetic, single pin seals were produced using printed metal shells, by selective laser melting (SLM), and digital light processing (DLP) printed glass preforms. Glass preforms were printed with photosensitive resin mixed with a silicate sealing glass powder in a 1:2 weight ratio. Thermal analysis, TGA/DSC, and screening experiments were used to determine an organic removal schedule. Video techniques determined a sintering schedule by producing a densification curve at different isothermal holds which were fit with a viscous sintering model. Single pin seals were also produced use a laser assisted manufacturing (LAM) process as an alternative to the conventional furnace sealing process. A Nd:YAG laser was focused on a solid glass preform, heating the glass to form the glass-metal bond. The sealing glass was doped with a transition metal oxide, Fe2O3 or CuO, to increase absorption of the laser wavelength. The interface of hermetic LAM seals were analyzed using electron microscopy, compared to conventional prepared seals, finding a reduction of interfacial morphologies.
Internal strain analysis of ceramics using scanning laser acoustic microscopy
Quantitative studies of material behavior characteristics are essential for predicting the functionality of a material under its operating conditions. A nonintrusive methodology for measuring the in situ strain of small dimeter (to 11 microns) ceramic fibers under uniaxial tensile loading and the local internal strains of ceramics and ceramic composites under flexural loading is introduced. The strain measurements and experimentally observed mechanical behavior are analyzed in terms of the microstructural development and fracture behavior of each test specimen evaluated. Measurement and analysis of Nicalon silicon carbide (SiC) fiber (15 microns diameter) indicate that the mean elastic modulus of the individual fiber is 185.3 GPa. Deviations observed in the experimentally determined elastic modulus values between specimens were attributed to microstructural variations which occur during processing. Corresponding variations in the fracture surface morphology were also observed. The observed local mechanical behavior of a lithium alumino-silicate (LAS) glass ceramic, a LAS/SiC monofilament composite, and a calcium alumino-silicate (CAS)/SiC fully reinforced composite exhibits nonlinearities and apparent hysteresis due to the subcritical mechanical loading. Local hysteresis in the LAS matrices coincided with the occurrence of multiple fracture initiation sites, localized microcracking, and secondary cracking. The observed microcracking phenomenon was attributed to stress relaxation of residual stresses developed during processing, and local interaction of the crack front with the microstructure. The relaxation strain and stress predicted on apparent mechanical hysteresis effects were defined and correlated with the magnitude of the measured fracture stress for each specimen studied. This quantitative correlation indicated a repeatable measure of the stress at which matrix microcracking occurred for stress relief of each material system. Stress relaxation occurred prior to the onset of steady state cracking conditions. The relaxation stress occurred at 18.5 percent of the fracture stress in LAS and 11.0 percent of the yield stress in CAS/SiC. The relaxation stress ratio was dependent upon the dominant fracture mode of the LAS/SiC specimens. Relaxation stress ratios greater than 0.30 were observed for specimens which fractured due to shear at the fiber matrix interface; specimens which fracture due to tensile cracking had relaxation stress ratios less than 0.30. The stress relaxation ratio appeared to be a specific characteristic of the glass ceramic material. The measured stress relaxation for LAS indicated a measure of the inherent residual stresses in the material due to processing and suggested localized toughening mechanisms for brittle material structures.
Elucidating the Atomic Structures of the Gel Layer Formed during Aluminoborosilicate Glass Dissolution: An Integrated Experimental and Simulation Study
The altered glasses produced during aqueous dissolution of silicate and borosilicate glasses are among the most complex structures to understand at the atomic level due to their amorphous nature, random porosity and various levels of hydration. In this study, we gained insights of the complex atomic structures of altered aluminoborosilicate glasses by combining a range of experimental and computational approaches. The altered glasses were prepared by dissolution of three glasses with varying level of alumina in acid for 7 days. A comprehensive set of experimental [elemental analysis, high-energy X-ray diffraction, 29 Si and 27 Al solid-state nuclear magnetic resonance (NMR), and O 1s X-ray photoelectron spectroscopy (XPS)] and modeling (molecular dynamics (MD) simulations using non-reactive and reactive force fields) were used to study the atomic structures of these altered glasses. Elemental analysis showed that most of the B in the pristine glasses was leached into the solution and was not contained in the altered glass. The 29 Si and 27 Al solid-state NMR spectra revealed that the altered glasses have more polymerized silicate network as compared to those in the pristine glasses due to the reformation of linkages among Si and Al oxygen polyhedral in the altered glasses. The bridging and non-bridging (or hydroxyl O) atoms in the altered glasses were also quantified from their O 1s XPS spectra. Atomic structure models of the altered glasses were constructed by using MD simulations using the reactive force field based on the compositional information obtained from experiments. Various pore structures were generated using the charge-scaling (CS) method by using different initial densities and CS temperatures; the best CS parameters of each alternated glass were then determined by comparing with the experimental structure factors obtained from high energy X-ray diffraction. Pore and the atomic structures and vibrational properties around these pore surfaces were analyzed. Furthermore, these results from this comprehensive study thus provides a realistic insight into the pore morphology, atomic structure, and vibrational properties of altered glasses.
Ceramic fiber-reinforced monoclinic celsian phase glass-ceramic matrix composite material
A hyridopolysilazane-derived ceramic fiber reinforced monoclinic celsian phase barium aluminum silicate glass-ceramic matrix composite material is prepared by ball-milling an aqueous slurry of BAS glass powder and fine monoclinic celsian seeds. The fibers improve the mechanical strength and fracture toughness and with the matrix provide superior dielectric properties.
An electromotive force series in a borosilicate glass-forming melt
An electromotive force series for redox couples was defined as a function of oxygen fugacity in a borosilicate melt at 1150 C. The resulting order of relative reduction potentials can be used to estimate the amounts of redox species in glass during processing. The electromotive force series in this melt is comparable to those in other silicate glass-forming melts and in aqueous systems but differs in detail because of interaction of the solvents with individual redox couples.
Looking through model medieval green glasses: From color to recipe
Abstract The colors of medieval stained glasses depend on their chemical composition. The redox interactions in glass between iron and copper and their influence on the color were investigated in two soda‐lime silicate model glasses. Both glasses have close iron and copper redox ratios and copper oxidizes iron when the iron content is smaller than the copper content. The redox speciation of iron and copper was determined using combining x‐ray and optical absorption spectroscopies in relation with the resulting color. The molar extinction coefficient of Cu 2+ was estimated from the combined analysis to be 32 mol/L/cm. The glass color change from green to blue‐green color is assigned to the decrease of the total iron content, confirming that ancient glassmakers could control the final color with the glass recipe. These results provide reference data for further spectroscopic investigations of medieval stained glasses. Comparison with ancient copper‐colored green glass compositions suggests that the higher ratio of copper to iron total contents was imposed by the more reducing melting conditions in medieval furnaces.
Scalable and Cost-Effective Roll-To-Roll Additive Manufacturing of Highly Durable and Thermal Insulating Silica-Carbon Aerogel (Final Report)
The research objective of this project is to demonstrate low cost silica aerogel insulation materials with high R-value and low installed price of R7.5/inch, and $0.94/ft2-inch, respectively, which can meet the cost and performance targets of the Department of Energy’s 2030 Building Technology Office Emerging Technologies program. The main tasks of this project include the following three topics: a) Low-cost silica gel precursor: Repeat silica sol gel chemical approach which is reproducible and scalable. Also explore suitability of water-glass on silica aerogel system to further control cost efficiency. In addition, our aim is to synthesize hollow silica using low-cost precursors. Sodium silicate (water glass) was chosen as our silica source because of its availability and low price compared to the other precursors; b) In situ ambient pressure-drying (APD) and surface modification: confirm and improve silica aerogel under cost-effective continuous ambient pressure-drying and investigate silica aerogel performance under time and temperature dependence; c) Roll-to-Roll (R2R) manufacturing with the targeted structure, thermal and mechanical characteristics: evaluate 3D printing with silica aerogel precursor to modify aerogel formation.
Multiscale Investigation of the Mechanisms Controlling the Corrosion of Borosilicate Glasses in Hyper-Alkaline Media
The overarching goal of the present multiscale investigation is to unearth the kinetics and mechanisms of corrosion of borosilicate glasses in hyper-alkaline (pH = 13) environments as a function of their chemical composition. Accordingly, a series of 3- to 6-component borosilicate glasses have been designed starting from Na 2 O–B 2 O 3 –SiO 2 ternary, wherein the compositional complexity has been added in a systematic tiered approach, finally resulting in the composition of the well-known international simple glass (ISG). Tetramethylammonium hydroxide (TMAH), one of the most widely used alkaline etchant in the glass and electronics industry, has been used as the corrosion media. A series of state-of-the-art characterization techniques including magic angle spinning nuclear magnetic resonance spectroscopy, X-ray photoelectron spectroscopy, inductively coupled plasma optical emission spectroscopy, elastic recoil detection analysis, and high-resolution transmission electron microscopy have been employed to unearth the compositional dependence of glass corrosion in hyper-alkaline environments. The glass compositions underwent congruent corrosion in the forward rate regime, whereas the controlling mechanism of corrosion in the residual rate regime depends on the presence/absence of Ca in the surrounding environment and can be explained on the basis of the dissolution–reprecipitation model. The dependence of corrosion kinetics and the chemistry of alteration products (in the residual rate regime) on the glass composition have been discussed. Here, the results presented in this contribution will ultimately supplement the scientific literature attempting to understand the fundamental science governing the aqueous corrosion of silicate-based glass chemistries and add to the growing database required to develop non-empirical predictive models for designing glasses with controlled dissolution rates.
Shock induced reaction in Chicxulub target materials (CaSO4 and SiO2) and their relation to extinctions
The global platinum element rich layer, the presence of shocked quartz grains (in some cases with stishovite), and the observation of a tektite-rich layer, precisely at the K-T boundary, are the three major arguments for the extinction bolide impact hypothesis of Alvarez et al. Tektites (spherules) from Beloc in Haiti and Mimbral in Mexico received particular interest because of their geological proximity to the Chicxulub impact structure, which is a leading candidate for at least one of the K-T impact craters. Although in most localities the original glass has weathered to clay minerals, some shock-induced glass is found in outcrops and drill cores which is used for Ar-38/Ar-39 dating. The glassy tektites were found to be chemically similar and coeval at 65.0 Ma with Chicxulub melt rock. Two kinds of K-T spherules were discovered: (1) a silic black glass; and (2) a yellow glass, enriched in Ca, Mg, and S. The high sulfur content of the glass and the abundance of anhydrite (CaSO4) in the carbonate-evaporite sequence observed in Drill Holes Y-1 and Y-2 at Chicxulub prompted studies of calcium sulfate devolatization. Further discussion of our experiments is presented.
Studies and testing of antireflective (AR) coatings for soda-lime glass
Processes for producing antireflection films on glass are concentrated in three areas: acid etching of glass, plasma etching of glass, and acid development of sodium silicate films on glass. The best transmission was achieved through the acid etching technique, while the most durable films were produced from development of sodium silicate films. Control of the acid etching technique is presently inadequate for production implementation. While films having excellent antireflective properties were fabricated by plasma etching techniques, all were water soluble.
High temperature crystal field spectra of transition metal-bearing minerals - Relevance to remote-sensed spectra of planetary surfaces
It is pointed out that transition metal ions in silicate minerals, glasses, and crystalline and amorphous oxyhydroxides and salts contribute to the visible-near infrared spectral profiles of planetary surfaces. Investigations are conducted to obtain spectral information which might be helpful in the interpretation of the remote-sensed spectra of planetary surfaces. A description is presented of the results of high temperature crystal field spectral measurements of a variety of heated minerals containing Cr(3+), Fe(3+), Fe(++), and Mn(++) ions in different coordination symmetries, taking into account a correlation of the temperature-induced variations with those previously observed for octahedrally coordinated Fe(++)-bearing silicates. The employed experimental methods are also discussed, giving attention to the preparation of the samples, the determination of the absorption spectra, electron microprobe analyses, and the curve fitting procedure.
Densification of non-radioactive porous siliceous particles loaded with cesium potassium copper hexacyanoferrate by spark plasma sintering
In the development of a conditioning process for cesium-bearing sorbents from the decontamination of aqueous waste streams, the treatment of a granular material composed of (Cs,K) 2 CuFe(CN) 6 loaded onto mesoporous silica particles has been investigated in an additive-free two-step conditioning process involving (i) calcination at 1000 °C to remove volatile species and (ii) densification by spark plasma sintering. A 92.0 % dense pellet was obtained after 10 min sintering at 850 °C under 100 MPa. Density and microstructural measurements indicate that densification is first driven by the viscous flow of a vitreous phase containing Cs, formed during calcination. Additionally, the density of the sample then increases further during sintering by grain boundary diffusion. However, a limited but non negligible part of cesium is lost during densification.
El Chichon volcanic ash in the stratosphere - Particle abundances and size distributions after the 1982 eruption
Volcanic ash particles collected from the stratosphere after the March/April, 1982 explosive eruption of El Chichon volcano, Mexico, were mostly 2-40 micron vesicular shards of silicic volcanic glass that varied in abundance, at 16.8-19.2 km altitude, from 200 per cu m (30-49 deg N lat.) in May to 1.3 per cu m (45-75 deg N) in October. At the minimum, the ash cloud covered latitudes 10-60 deg N in July and 10 deg S-75 deg N in October. In May and July, ash particles were mostly free, individual shards (and clusters of shards) but, by October, were intimately associated with liquid droplets (presumably, sulfuric acid). In May 1982, the total stratospheric burden of ash was at least 240 tons (2.2 x 10 to the 8th g) although the total ash injected into the stratosphere by the eruption was probably 480-8400 tons.
Whisker/Cone growth on the thermal control surfaces experiment no. S0069
An unusual surface 'growth' was found during scanning electron microscope (SEM) investigations of the Thermal Control Surface Experiment (TCSE) S0069 front thermal cover. This 'growth' is similar to the cone type whisker growth phenomena as studied by G. K. Wehner beginning in the 1960's. Extensive analysis has identified the most probable composition of the whiskers to be a silicate type glass. Sources of the growth material are outgassing products from the experiment and orbital atomic oxygen, which occurs naturally at the orbital altitudes of the LDEF mission in the form of neutral atomic oxygen. The highly ordered symmetry and directionality of the whiskers are attributed to the long term (5.8 year) stable flight orientation of the LDEF.
The History of Allan Hills 84001 Revised: Multiple Shock Events
The geologic history of Martian meteorite Allan Hills (ALH) 84001 is more complex than previously recognized, with evidence for four or five crater-forming impacts onto Mars. This history of repeated deformation and shock metamorphism appears to weaken some arguments that have been offered for and against the hypothesis of ancient Martian life in ALH 84001. Allan Hills 84001 formed originally from basaltic magma. Its first impact event (I1) is inferred from the deformation (D1) that produced the granular-textured bands ("crush zones") that transect the original igneous fabric. Deformation D1 is characterized by intense shear and may represent excavation or rebound flow of rock beneath a large impact crater. An intense thermal metamorphism followed D1 and may be related to it. The next impact (I2) produced fractures, (Fr2) in which carbonate "pancakes" were deposited and produced feldspathic glass from some of the igneous feldspars and silica. After I2, carbonate pancakes and globules were deposited in Fr2 fractures and replaced feldspathic glass and possibly crystalline silicates. Next, feldspars, feldspathic glass, and possibly some carbonates were mobilized and melted in the third impact (I3). Microfaulting, intense fracturing, and shear are also associated with 13. In the fourth impact (I4), the rock was fractured and deformed without significant heating, which permitted remnant magnetization directions to vary across fracture surfaces. Finally, ALH 84001 was ejected from Mars in event I5, which could be identical to I4. This history of multiple impacts is consistent with the photogeology of the Martian highlands and may help resolve some apparent contradictions among recent results on ALH 84001. For example, the submicron rounded magnetite grains in the carbonate globules could be contemporaneous with carbonate deposition, whereas the elongate magnetite grains, epitaxial on carbonates, could be ascribed to vapor-phase deposition during I3.