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New molecular precursors for low-temperature routes to new oxide materials. Final progress report

Description: In this grant period, the authors have explored the single-source precursor route to silicate materials containing various main group and transition metals. They have also explored the development of polymeric precursors to zinc silicate materials. In addition, they have begun to examine precursors for phosphate materials, based on the di(tert-butyl)phosphate ligand, {minus}O{sub 2}P(O{sup t}Bu){sub 2}. A primary focus of these studies is the development of molecular precursors to homogeneous, ultrapure metal silicates and phosphates. More recently, the authors have attempted to develop template-assisted network-forming reactions that could lead to micro- or mesoporous materials. Findings are summarized below for Zr and HF systems, Al systems, Cr systems, Cu systems, metal phosphate precursors, zinc silicate luminescent materials, and syntheses of inorganic materials using dendrimeric polymers as templates.
Date: October 1, 1997
Creator: Tilley, T.D.
Partner: UNT Libraries Government Documents Department

Calcium Silicates: Glass Content and Hydration Behavior

Description: Pure, MgO doped and B2C3 doped monocalcium, dicalcium, and tricalcium silicates were prepared with different glass contents. Characterization of the anhydrous materials was carried out using optical microscopy, infrared absorption spectroscopy, and X-ray powder diffraction. The hydration of these compounds was studied as a function of the glass contents. The hydration studies were conducted at 25°C. Water/solid ratios of 0.5, 1, 10, and 16 were used for the various experiments. The hydration behavior was monitored through calorimetry, conductometry, pH measurements, morphological developments by scanning electron microscopy, phase development by X-ray powder diffraction, and percent combined water by thermogravimetry. A highly sensitive ten cell pseudo-adiabatic microcalorimeter was designed and constructed for early hydration studies. Conductometry was found to be of great utility in monitoring the hydration of monocalcium silicate and the borate doped dicalcium silicates.
Date: August 1987
Creator: Zgambo, Thomas P. (Thomas Patrick)
Partner: UNT Libraries

The Constitution of the Silicates

Description: A report about silicates which form nine-tenths of the earth's crust and are therefore of fundamental importance to geological changes. The report discusses analyzing them by finding out where they came from and what they are comprised of.
Date: 1895
Creator: Clarke, Frank Wigglesworth
Partner: UNT Libraries Government Documents Department

A Cooperative Investigation of Precision and Accuracy in Chemical, Spectrochemical and Modal Analysis of Silicate Rocks

Description: From foreword: This bulletin is the second of the series "Contributions to Geochemistry" which was begun in 1946 with Bulletin 950, "Contributions to Geochemistry, 1942-45". This series is the successor to earlier ones, also published as U. S. Geological Survey Bulletins, "Report of work done in the Division of Chemistry and Physics" (1879-1893), "Contributions to chemistry and mineralogy from the laboratory of the United States Geological Survey" (1900), "Contributions to mineralogy from the United States Geological Survey" (1905), and "Mineralogical Notes" (1911-16).
Date: 1951
Creator: Fairbairn, H. W.
Partner: UNT Libraries Government Documents Department

Nebular mixing constrained by the Stardust samples

Description: Using X-ray microprobe analysis of samples from comet Wild 2 returned by the Stardust mission, we determine that the crystalline Fe-bearing silicate fraction in this Jupiter-family comet is greater than 0.5. Assuming this mixture is a composite of crystalline inner solar system material and amorphous cold molecular cloud material, we deduce that more than half of Wild 2 has been processed in the inner solar system. Several models exist that explain the presence of crystalline materials in comets. We explore some of these models in light of our results.
Date: March 22, 2010
Creator: OGLIORE, R. C.; WESTPHAL, A. J.; GAINSFORTH, Z.; BUTTERWORTH, A. L.; FAKRA, S. C. & Marcus, Matthew A.
Partner: UNT Libraries Government Documents Department

Molecular Dynamics Simulations of Hexadecane/Silicalite Interfaces

Description: The interface between liquid hexadecane and the (010) surface of silicalite was studied by molecular dynamics. The structure of molecules in the interracial region is influenced by the presence of pore mouths on the silicalite surface. For this surface, whose pores are the entrances to straight channels, the concentration profile for partially absorbed molecules is peaked around 10 monomers inside the zeolite. No preference to enter or exit the zeolite based on absorption length is observed except for very small or very large absorption lengths. We also found no preferential conformation of the unabsorbed tails for partially absorbed molecules.
Date: January 20, 1999
Creator: Grest, G.S. & Webb, E.B.
Partner: UNT Libraries Government Documents Department

Temperature-Viscosity Relations in the Ternary System CaO-Al₂O₃-SiO₂

Description: Technical paper issued by the Bureau of Mines over studies on the relations of temperature-viscosity. The "observations on the temperature-viscosity relations of silicates" (p. 5) are presented and discussed. This report includes tables, and illustrations.
Date: April 1918
Creator: Feild, Alexander L. & Royster, P. H.
Partner: UNT Libraries Government Documents Department


Description: We evaluated the usefulness of manufactured quartz/mullite blend (MQMB) ceramic powder in increasing the resistance to acid of sodium silicate-activated slag (SSAS) cementitious material for geothermal wells. A 15-day exposure to 90{sup o} CO{sub 2}-laden H{sub 2}SO{sub 4} revealed that the MQMB had high potential as an acid-resistant additive for SSAS cement. Two factors, the appropriate ratio of slag/MQMB and the autoclave temperature, contributed to better performance of MQMB-modified SSAS cement in abating its acid erosion. The most effective slag/MQMB ratio in minimizing the loss in weight by acid erosion was 70/30 by weight. For autoclave temperature, the loss in weight of 100 C autoclaved cement was a less than 2%, but at 300 C it was even lower. Before exposure to acid, the cement autoclaved at 100 C was essentially amorphous; increasing the temperature to 200 C led to the formation of crystalline analcime in the zeolitic mineral family during reactions between the mullite in MQMB and the Na from sodium silicate. In addition, at 300 C, crystal of calcium silicate hydrate (1) (CSH) was generated in reactions between the quartz in MQMB and the activated slag. These two crystalline phases (CSH and analcime) were responsible for densifying the autoclaved cement, conveying improved compressive strength and minimizing water permeability. The CSH was susceptible to reactions with H{sub 2}SO{sub 4}, forming two corrosion products, bassanite and ionized monosilicic acid. However, the uptake of ionized monosilicic acid by Mg dissociated from the activated slag resulted in the formation of lizardite as magnesium silicate hydrate. On the other hand, the analcime was barely susceptible to acid if at all. Thus, the excellent acid resistance of MQMB-modified SSAS cement was due to the combined phases of lizardite and analcime.
Date: June 1, 2006
Partner: UNT Libraries Government Documents Department

Iron (II) and Silicate Effects on Mineralization and Immobilzation of Actinides

Description: Abstract - The unique composition of the Yucca Mountain repository site, which contains large concentrations of silicate in an oxidative environment, has required extensive research into compound formation involving uranium and iron(II) under such conditions. The possibility of uranium leakage from within the containment vessels into the near-field ground water, as well as iron leaching from the vessel itself, necessitates study of the individual contributions of these elements for compound formation. By mimicking the known silicate concentration found in surrounding ground water and varying concentrations of both uranyl and iron(II), subsequent precipitation of uranyl silicate phases has shown evidence of iron(II) sorption to the available sites on the mineral surface. The mineralization seems to be driven by the formation of uranyl silicate, in contrast to iron(III)-control of precipitation in the oxidated system. Characterization of this system presented includes ICP-AES analysis as well as preliminary EDAX, XRD, and FT-IR
Date: January 1, 2006
Creator: Sullens, Tyler A.; Gong, Cynthia-May S. & Szerwinski, Kenneth R.
Partner: UNT Libraries Government Documents Department

Iron (II) sorption to mineral surfaces in uranyl and silicate rich media

Description: Abstract - The unique composition of the Yucca Mountain repository site, which contains large concentrations of silicate in an oxidative environment, has required extensive research into compound formation involving uranium and iron(II) under such conditions. The possibility of uranium leakage from within the containment vessels into the near-field ground water, as well as iron leaching from the vessel itself, necessitates study of the individual contributions of these elements for compound formation. By mimicking the known silicate concentration found in surrounding ground water and varying concentrations of both uranyl and iron(II), subsequent precipitation of uranyl silicate phases has shown evidence of iron(II) sorption to the available sites on the mineral surface. The mineralization seems to be driven by the formation of uranyl silicate, in contrast to iron(III)-control of precipitation in the oxidated system. We present characterization of this system using ICP-AES/MS, EDAX, XRD, and single-crystal X-ray diffraction.
Date: January 1, 2006
Creator: Sullens, Tyler A.; Gong, Cynthia-May S. & Czerwinski, Kenneth R.
Partner: UNT Libraries Government Documents Department

Mesoscale Molecular Dynamics of Geomaterials: the Glass Transition, Long-Range Structure of Amorphous Silicates and Relation between Structure, Dynamics and Properties of geomaterials at elevated Temperature and Pressure

Description: Objectives: Our aims were (1) Large particle-number Molecular Dynamics (MD) simulations of molten silicate and aluminosilicate geomaterials (e.g., CaAl{sub 2}Si{sub 2}O{sub 8}, MgSiO{sub 3}, Mg{sub 2}SiO{sub 4}) with emphasis on understanding the connection between atomic structure and properties at temperatures and pressures characteristic of Earth's mantle (2) Study of the transport properties and equations of state for silicate liquids based on the MD results (3) Development of geochemical models for the evolution of crustal magma bodies undergoing simultaneous assimilation, fractional crystallization, periodic recharge and periodic eruption and application to magmatic systems (4) Study of current-day rates of generation and eruption of magma on earth.
Date: July 31, 2006
Creator: Spera, Frank
Partner: UNT Libraries Government Documents Department

Materials properties of hafnium and zirconium silicates: Metal interdiffusion and dopant penetration studies.

Description: Hafnium and Zirconium based gate dielectrics are considered potential candidates to replace SiO2 or SiON as the gate dielectric in CMOS processing. Furthermore, the addition of nitrogen into this pseudo-binary alloy has been shown to improve their thermal stability, electrical properties, and reduce dopant penetration. Because CMOS processing requires high temperature anneals (up to 1050 °C), it is important to understand the diffusion properties of any metal associated with the gate dielectric in silicon at these temperatures. In addition, dopant penetration from the doped polysilicon gate into the Si channel at these temperatures must also be studied. Impurity outdiffusion (Hf, Zr) from the dielectric, or dopant (B, As, P) penetration through the dielectric into the channel region would likely result in deleterious effects upon the carrier mobility. In this dissertation extensive thermal stability studies of alternate gate dielectric candidates ZrSixOy and HfSixOy are presented. Dopant penetration studies from doped-polysilicon through HfSixOy and HfSixOyNz are also presented. Rutherford backscattering spectroscopy (RBS), heavy ion RBS (HI-RBS), x-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy (HR-TEM), and time of flight and dynamic secondary ion mass spectroscopy (ToF-SIMS, D-SIMS) methods were used to characterize these materials. The dopant diffusivity is calculated by modeling of the dopant profiles in the Si substrate. In this disseration is reported that Hf silicate films are more stable than Zr silicate films, from the metal interdiffusion point of view. On the other hand, dopant (B, As, and P) penetration is observed for HfSixOy films. However, the addition of nitrogen to the Hf - Si - O systems improves the dopant penetration properties of the resulting HfSixOyNz films.
Date: August 2002
Creator: Quevedo-Lopez, Manuel Angel
Partner: UNT Libraries

Results of Scoping Tests Examining the Effects of Gilsulate, Aluminum Silicate and Defoamers on the Operation of Conductivity Level Probes

Description: Scoping tests have been completed examining the effects of Gilsulate, sodium aluminum silicate, and some organic materials on the operation of tank level conductivity probes. This report documents the results of scoping studies completed to examine the effect of those materials on conductivity probes.
Date: February 17, 1999
Creator: Swingle, R.F.
Partner: UNT Libraries Government Documents Department

Sodium Aluminosilicate Formation in Tank 43H Simulants

Description: This work studied the formation of a sodium aluminosilicate, Na{sub 8}Al{sub 6}Si{sub 6}O{sub 24}(NO{sub 3}){sub 2?4}H{sub 2}O, at 40{degree} 110{degree} C in simulated waste solutions with varied amounts of silicon and aluminum. The data agree well with literature solubility data for sodalite, the analogous chloride salt. The following conclusions result from this work: (1) The study shows, by calculation and experiments, that evaporation of the September 1997 Tank 43H inventory will only form minor quantities of the aluminosilicate. (2) The data indicate that the rate of formation of the nitrate enclathrated sodalite solid at these temperatures falls within the residence time ({lt}; 4 h) of liquid in the evaporator. (3) The silicon in entrained Frit 200 transferred to the evaporator with the Tank 43H salt solution will quantitatively convert to the sodium aluminosilicate. One kilogram of Frit 200 produces 2.1 kg of the sodium aluminosilicate.
Date: November 1997
Creator: Wilmarth, W. R.; Walker, D. D. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Electrodeposition of Nickel and Nickel Alloy Coatings with Layered Silicates for Enhanced Corrosion Resistance and Mechanical Properties

Description: The new nickel/layered silicate nanocomposites were electrodeposited from different pHs to study the influence on the metal ions/layered silicate plating solution and on the properties of the deposited films. Nickel/layered silicate nanocomposites were fabricated from citrate bath atacidic pHs (1.6−3.0), from Watts’ type solution (pH ~4-5), and from citrate bath at basic pH (~9). Additionally, the new nickel/molybdenum/layered silicate nanocomposites were electrodeposited from citrate bath at pH 9.5. The silicate, montmorillonite (MMT), was exfoliated by stirring in aqueous solution over 24 hours. The plating solutions were analyzed for zeta potential, particle size, viscosity, and conductivity to investigate the effects of the composition at various pHs. The preferred crystalline orientation and the crystalline size of nickel, nickel/layered silicate, nickel/molybdenum, and nickel/molybdenum/layered silicate films were examined by X-ray diffraction. The microstructure of the coatings and the surface roughness was investigated by scanning electron microscopy and atomic force microscopy. Nickel/molybdenum/layered silicate nanocomposites containing low content of layered silicate (1.0 g/L) had increase 32 % hardness and 22 % Young’s modulus values over the pure nickel/molybdenum alloy films. The potentiodynamic polarization and electrochemical impedance measurements showed that the nickel/molybdenum/layered silicate nanocomposite layers have higher corrosion resistance in 3.5% NaCl compared to the pure alloy films. The corrosion current density of the nickel/molybdenum/layered silicate nanocomposite composed of 0.5 g/L MMT is 0.63 µA·cm-2 as compare to a nickel/molybdenum alloy which is 2.00 µA·cm-2.
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Date: August 2014
Creator: Tientong, Jeerapan
Partner: UNT Libraries

Carbon Dioxide Sequestration by Mechanochemical Carbonation of Mineral Silicates

Description: The University of Utah and the University of Idaho investigated the carbonation of silicate minerals by mechanochemical processing. This method uses intense grinding, and has the potential of being much less expensive than other methods of mineral sequestration. Tests were conducted in three types of grinding devices. In these tests, natural and synthetic silicate compounds were ground for varying times in the presence of gaseous CO{sub 2}. A significant change takes place in the lizardite variety of serpentine after 15 to 20 minutes of intense grinding in the presence of gaseous CO{sub 2}. The X-ray diffraction spectrum of lizardite thus treated was much different than that of the untreated mineral. This spectrum could not be identified as that of any natural or synthetic material. Laboratory analyses showed that small amounts of carbon are fixed by grinding lizardite, forsterite, and wollastonite (all naturally-occurring minerals), and synthetic magnesium silicate, in the presence of gaseous CO{sub 2}. It was thus concluded that further investigation was warranted, and a follow-up proposal was submitted to the Department of Energy under solicitation number.
Date: April 1, 2004
Creator: Nelson, Michael G.
Partner: UNT Libraries Government Documents Department

Thermodynamic properties of solid solutions at high temperatures

Description: The research carried out under this cortract was concerned with the determination of thermodynamic properties of inorganic matenials at high temperatures. Experimental methods were developed which permit accurate and reliable determination of activity-composition relations in solid solutions, and stabilities of end-member compounds. The data provide insight irto the general laws governing the behavior of materials in high-temperature envirorments. The phases selected for the experimental studies include onthosilicates, metasilicates, oxides of periclase structure, spinels, and titarates. It has been shown that directions of conjugation lines between coexisting solid-solution phases provide a powerful tool for determnining relative stabilities of endmember compounds and activity-composition relations of solid solutions. In general, oxide phases (including silicates and titanates) forming complete solid-solution series at high temperatures show less deviations from ideality in their activity- composition relations than do alloy systems. Deviations from ideality are particularly small for many solid solutions of relatively simple structures (e.g. oxides of peniclase structure), whereas those of greater structural complexities (e.g. spinels) show larger deviations from ideality. (auth)
Date: January 1, 1973
Creator: Muan, A.
Partner: UNT Libraries Government Documents Department


Description: Washed sodium-aluminosilicate (NAS) solids at initial concentrations of 3.55 and 5.4 g/L sorb or uptake virtually no cesium over 288 hours, nor do any NAS solids generated during that time. These concentrations of solids are believed to conservatively bound current and near-term operations. Hence, the NAS solids should not have affected measurements of the cesium during the mass transfer tests and there is minimal risk of accumulating cesium during routine operations (and hence posing a gamma radiation exposure risk in maintenance). With respect to actinide uptake, it appears that NAS solids sorb minimal quantities of uranium - up to 58 mg U per kg NAS solid. The behavior with plutonium is less well understood. Additional study may be needed for radioactive operations relative to plutonium or other fissile component sorption or trapping by the solids. We recommend this testing be incorporated in the planned tests using samples from Tank 25F and Tank 49H to extend the duration to bound expected inventory time for solution.
Date: July 31, 2007
Creator: Peters, T; Bill Wilmarth, B & Samuel Fink, S
Partner: UNT Libraries Government Documents Department

Fate of Uranium during Sodium Aluminosilicate Formation under Waste Tank Conditions

Description: Experiments have been conducted to examine the fate of uranium during the formation of sodium aluminosilicate (NAS) when wastes containing high aluminate concentrations are mixed with wastes of high silicate concentration. Testing was conducted at varying degrees of uranium saturation. Testing examined typical tank conditions, e.g., stagnant, slightly elevated temperature (50 C). The results showed that under sub-saturated conditions uranium is not removed from solution to any large extent in both simulant testing and actual tank waste testing. There are data supporting a small removal due to sorption of uranium on sites in the NAS. Above the solubility limit the data are clear that a reduction in uranium concentration occurs with the formation of aluminosilicate. This uranium precipitation is fairly rapid and ceases when uranium reaches its solubility limit. At the solubility limit, it appears that uranium is not affected, but further testing might be warranted. Lastly, analysis of the uranium speciation in a Tank 49H set of samples showed the uranium to be soluble. Analysis of the solution composition and subsequent use of the Hobb's uranium solubility model indicated a uranium solubility limit of 32 mg/L. The measured value of uranium in the Tank 49H matched the model prediction.
Date: June 22, 2005
Creator: Wilmarth, B
Partner: UNT Libraries Government Documents Department

Chemical Speciation of Sr, Am and Cm in high Level Waste: predictive modeling of phase partitioning during tank processing

Description: During this contract period, a number of papers were published. The papers prior to this report have been reported in earlier annual reports. This final report covers the 2005 & 2006 publications which have been published as well as the last few which have been submitted, but are still under review for acceptance for publication. The titles and abstracts of the papers are presented in section A, and the full published papers in Section B.
Date: December 20, 2006
Creator: Choppin, Gregory R.
Partner: UNT Libraries Government Documents Department


Description: Using the conventional well cements consisting of the calcium silicate hydrates (CaO-SiO{sub 2}-H{sub 2}O system) and calcium aluminum silicate hydrates (CaO-Al{sub 2}O{sub 3}-SiO{sub 2}-H{sub 2}O system) for the integrity of geothermal wells, the serious concern confronting the cementing industries was their poor performance in mechanically supporting the metallic well casing pipes and in mitigating the pipe's corrosion in very harsh geothermal reservoirs. These difficulties are particularly acute in two geological regions: One is the deep hot downhole area ({approx} 1700 m depth at temperatures of {approx} 320 C) that contains hyper saline water with high concentrations of CO{sub 2} (> 40,000 ppm) in conjunction with {approx} 100 ppm H{sub 2}S at a mild acid of pH {approx} 5.0; the other is the upper well region between the well's surface and {approx} 1000 m depth at temperatures up to 200 C. The specific environment of the latter region is characterized by highly concentrated H{sub 2}SO{sub 4} (pH < 1.5) brine containing at least 5000 ppm CO{sub 2}. When these conventional cements are emplaced in these harsh environments, their major shortcoming is their susceptibility to reactions with hot CO{sub 2} and H{sub 2}SO4, thereby causing their deterioration brought about by CO{sub 2}-catalyzed carbonation and acid-initiated erosion. Such degradation not only reduced rapidly the strength of cements, lowering the mechanical support of casing pipes, but also increased the extent of permeability of the brine through the cement layer, promoting the rate of the pipe's corrosion. Severely carbonated and acid eroded cements often impaired the integrity of a well in less than one year; in the worst cases, casings have collapsed within three months, leading to the need for costly and time-consuming repairs or redrilling operations. These were the reasons why the geothermal well drilling and cementing industries were concerned about using conventional well ...
Date: January 1, 2007
Creator: SUGAMA,T.
Partner: UNT Libraries Government Documents Department