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Experimental Methodology for Determining Optimum Process Parameters for Production of Hydrous Metal Oxides by Internal Gelation

Description: The objective of this report is to describe a simple but very useful experimental methodology that was used to determine optimum process parameters for preparing several hydrous metal-oxide gel spheres by the internal gelation process. The method is inexpensive and very effective in collection of key gel-forming data that are needed to prepare the hydrous metal-oxide microspheres of the best quality for a number of elements.
Date: October 28, 2005
Creator: Collins, J.L.
Partner: UNT Libraries Government Documents Department

Electrostriction in Field-Structured Composites: Basis for a Fast Artificial Muscle?

Description: The electrostriction of composites consisting of dielectric particles embedded in a gel or elastomer is discussed. It is shown that when these particles are organized by a uniaxial field before gelation, the resulting field-structured composites are expected to exhibit enhanced electrostriction in a uniform field applied along the same axis as the structuring field. The associated stresses might be large enough to form the basis of a polymer-based fast artificial muscle.
Date: January 27, 1999
Creator: Anderson, R.A. & Martin, J.E.
Partner: UNT Libraries Government Documents Department

Development of an Improved Permeability Modification Simulator

Description: This report describes the development of an improved permeability modification simulator performed jointly by BDM Petroleum Technologies and Schlumberger Dowell under a cooperative research and development agreement (CRADA) with the US Department of Energy. The improved simulator was developed by modifying NIPER's PC-GEL permeability modification simulator to include a radial model, a thermal energy equation, a wellbore simulator, and a fully implicit time-stepping option. The temperature-dependent gelation kinetics of a delayed gel system (DGS) is also included in the simulator.
Date: March 9, 1999
Creator: Gao, H.W. & Elphnick, J.
Partner: UNT Libraries Government Documents Department

Elastic properties of silica aerogels from a new rapid supercritical extraction process

Description: Silica aerogels were produced by a new process from Tetramethoxysilane (TMOS) with ammonia as base catalyst. the process involves pouring the liquid sol in a stainless steel mold and immediately heating it to supercritical conditions. Gelation and aging occurs during heating and reaction rates are high die to high average temperatures. the gel fills the container completely, which enables relatively fast venting of the supercritical fluid by providing a constraint for swelling and failure of the gel monolith. The whole process can be completed in 6 h or less. Longitudinal and shear moduli were measured in the dried aerogels by ultrasonic velocity measurements both as a function of chemical composition of the original sol and of position in the aerogel. It was found that the sound velocity exhibits marked maxima on the surface of the cylindrical specimens and specifically close to the ends, where the fluid left during venting. Specimens with high catalyst concentration and high water:TMOS ratio exhibited higher average moduli.
Date: August 11, 1997
Creator: Gross, J.; Coronado, P.R.; Hair, L.M. & Hrubesh, L.W.
Partner: UNT Libraries Government Documents Department

In-situ property measurements on laser-drawn strands of SL 5170 epoxy and SL 5149 acrylate

Description: Material behavior plays a significant role in the mechanics leading to internal stresses and, potentially, to distortion (curling) of parts as they are built by stereolithography processes that utilize photocuring resins. A study is underway to generate material properties that can be used to develop phenomenological material models of epoxy and acrylate resins. Strand tests are performed in situ in a 3D System`s SLA-250 machine; strands are drawn by either single or multiple exposures of the resin to a laser beam. Linear shrinkage, cross-sectional areas, cure shrinkage forces and stress-strain data are presented. Also, the curl in cantilever beam specimens, built with different draw patterns, are compared.
Date: August 1, 1995
Creator: Guess, T.R. & Chambers, R.S.
Partner: UNT Libraries Government Documents Department

Structural Formation Studies of UV-Catalyzed Gels and Aerogels byLight Scattering

Description: The skeletal structure of aerogel is determined before, during, and after the gel is formed. Supercritical drying of aerogel largely preserves the pore structure that is determined near the time of gelation. To better understand these gel formation mechanisms we carried out measurements of the time evolution of light scattering in a series of gels prepared without conventional acid or base catalysis. Instead, ultraviolet light was used to catalyze the formation of silica gels made from the hydrolysis of tetraethylorthosilicate and partly prehydrolyzed tetraethylorthosilicate in ethanol. Time evolution of light scattering provides information regarding the rate and geometrical nature of the assembly of the primary silica particles formed in the sol. UV-catalyzed gels show volumetric growth typical of acid-catalyzed gels, except when UV exposure is discontinued at the gel point, where gels then show linear chain formation typical of base-catalyzed gels. Long term UV exposure leads to coarsening of the pore network, a decrease in the clarity of the aerogel, and an increase in the surface area of the aerogel. Additionally, UV exposure up to the gel point leads to increased crystallinity in the final aerogel.
Date: April 1, 1998
Creator: Hunt, Arlon J. & Ayers, Michael R.
Partner: UNT Libraries Government Documents Department

Permeability Modification Using a Reactive Alkaline-Soluble Biopolymer

Description: Polymer injection has been used in reservoirs to alleviate contrasting permeability zones. Current technology relies on the use of cross-linking agents to initiate gelation. The use of biological polymers are advantageous in that they can block high permeability areas, are environmentally friendly, and have potential to form reversible gels without the use of hazardous cross-linkers. Recent efforts at the Idaho National Engineering and Environmental Laboratory (INEEL) have produced a reactive alkaline-soluble biopolymer from Agrobacterium sp. ATCC no. 31749 that gels upon decreasing the pH of the polymeric solution. The focus of this study was to determine the impact an alkaline-soluble biopolymer can have on sandstone permeability. Permeability modification was investigated by injecting solubilized biopolymer into Berea sandstone cores and defining the contribution of pH, salt, temperature, and Schuricht crude oil on biopolymer gelation. The biopolymer was soluble in KOH at a pH greater than 11.4 and gelled when the pH dropped below 10.8. The Berea sandstone core buffered the biopolymer solution, decreasing the pH sufficiently to form a gel, which subsequently decreased the permeability. The effluent pH of the control cores injected with 0.01 {und M} KOH (pH 12.0) and 0.10{und M} KOH (pH 13.0) decreased to 10.6 and 12.7, respectively. The permeability of the sandstone core injected with biopolymer was decreased to greater than 95% of the original permeability at 25 C in the presence of 2% NaCl, and Schuricht crude oil; however, the permeability increased when the temperature of the core was increased to 60 C. Residual resistance factors as high as 792 were seen in Berea cores treated with biopolymer. The buffering capacity of sandstone has been demonstrated to reduce the pH of a biopolymer solution sufficiently to cause the polymer to form a stable in-situ gel. This finding could potentially lead to alternate technology for permeability ...
Date: October 1, 2003
Creator: Fox, Snadra L.; Xie, X.; Schaller, K. D.; Robertson, E. P. & Bala, G. A.
Partner: UNT Libraries Government Documents Department

Determination of Ideal Broth Formulations Needed to Prepare Hydrous Aluminum Oxide Microspheres via the Internal Gelation Process

Description: A simple test-tube methodology was used to determine optimum process parameters for preparing hydrous aluminum oxide microspheres by the internal gelation process. Broth formulations of aluminum, hexamethylenetetramine, and urea were found that can be used to prepare hydrous aluminum oxide gel spheres in the temperature range of 60-90 C. A few gel-forming runs were made in which microspheres were prepared with some of these formulations in order to equate the test-tube gelation times with actual gelation times. These preparations confirmed that the test-tube methodology is reliable for determining the ideal broths.
Date: February 1, 2009
Creator: Collins, Jack Lee & Pye, S. L.
Partner: UNT Libraries Government Documents Department

Determination of Ideal Broth Formulations Needed to Prepare Hydrous Cerium Oxide Microspheres via the Internal Gelation Process

Description: A simple test tube methodology was used to determine optimum process parameters for preparing hydrous cerium oxide microspheres via the internal gelation process.1 Broth formulations of cerium ammonium nitrate [(NH4)2Ce(NO3)6], hexamethylenetetramine, and urea were found that can be used to prepare hydrous cerium oxide gel spheres in the temperature range of 60 to 90 C. A few gel-forming runs were made in which microspheres were prepared with some of these formulations to be able to equate the test-tube gelation times to actual gelation times. These preparations confirmed that the test-tube methodology is reliable for determining the ideal broth formulations.
Date: February 1, 2009
Creator: Collins, Jack Lee & Chi, Anthony
Partner: UNT Libraries Government Documents Department

Determination of Ideal Broth Formulations Needed to Prepare Hydrous Hafnium Oxide Microspheres via the Internal Gelation Process

Description: A simple test-tube methodology was used to determine optimum process parameters for preparing hydrous hafnium oxide microspheres by the internal gelation process. Broth formulations of hafnyl chloride [HfOCl{sub 2}], hexamethylenetetramine, and urea were found that can be used to prepare hydrous hafnium oxide gel spheres in the temperature range of 70-90 C. A few gel-forming runs were made in which microspheres were prepared with some of these formulations in order to equate the test-tube gelation times with actual gelation times. These preparations confirmed that the test-tube methodology is reliable for determining the ideal broths.
Date: February 1, 2009
Creator: Collins, Jack Lee; Hunt, Rodney Dale & Simmerman, S. G.
Partner: UNT Libraries Government Documents Department

Structural Modification of Sol-Gel Materials through Retro Diels-Alder Reaction

Description: Hydrolysis and condensation of organically bridged bis-triethoxysilanes, (EtO){sub 3}Si-R-Si(OEt){sub 3}, results in the formation of three dimensional organic/inorganic hybrid networks (Equation 1). Properties of these materials, including porosity, are dependent on the nature of the bridging group, R. Flexible groups (akylene-spacers longer than five carbons in length) polymerize under acidic conditions to give non-porous materials. Rigid groups (such as arylene-, alkynylene-, or alkenylene) form non-porous, microporous, and macroporous gels. In many cases the pore size distributions are quite narrow. One of the motivations for preparing hybrid organic-inorganic materials is to extend the range of properties available with sol-gel systems by incorporating organic groups into the inorganic network. For example, organically modified silica gels arc either prepared by co-polymerizing an organoalkoxysilane with a silica precursor or surface silylating the inorganic gel. This can serve to increase hydrophobicity or to introduce some reactive organic functionality. However, the type and orientation of these organic functionalities is difficult to control. Furthermore, many organoalkoxysilanes can act to inhibitor even prevent gelation, limiting the final density of organic functionalities. We have devised a new route for preparing highly functionalized pores in hybrid materials using bridging groups that are thermally converted into the desired functionalities after the gel has been obtained. In this paper, we present the preparation and characterization of bridged polysilsesquioxanes with Diels-Alder adducts as the bridging groups from the sol-gel polymerization of monomers 2 and 4. The bridging groups are constructed such that the retro Diela-Alder reaction releases the dienes and leaves the dienophiles as integral parts of the network polymers. In the rigid architecture of a xerogel, this loss of organic functionality should liberate sufficient space to modify the overall porosity. Furthermore, the new porosity will be functionalized with the dienophilic olefin bridging group. We also demonstrate that by changing the type of ...
Date: December 8, 1999
Creator: SHALTOUT,RAAFAT M.; LOY,DOUGLAS A.; MCCLAIN,MARK D.; PRABAKAR,SHESHASAYANA; GREAVES,JOHN & SHEA,KENNETH J.
Partner: UNT Libraries Government Documents Department

The Physics of Evaporation-Induced Assembly of Sol-Gel Materials

Description: Remarkable materials ordered at the nanoscale emerge when a sol-gel solution becomes co-organized with a surfactant. At sufficiently high concentration, the surfactant forms crystalline or liquid-crystalline arrays of micelles in the presence of the sol-gel, and as gelation proceeds the arrays become locked into the gel. Recent experiments demonstrate that the degree of order in the resulting mesoporous ceramic phase can be enhanced and controlled by continuous dip coating in which the solution, initially dilute, evolves through the critical micelle concentration by steady-state evaporation. The long-range order and microstructural orientation in these films suggest that the propagation of a critical-micelle-concentration transition front, with large physico-chemical gradients, promotes oriented self assembly of surfactant aggregates. This steep-gradient view is supported by results from unsteady evaporation of aerosols of similar solutions, in which internally well-ordered but complex particles are formed.
Date: July 24, 2000
Creator: Hurd, Alan J. & Steinberg, Lev
Partner: UNT Libraries Government Documents Department

Sol-gel processing of energetic materials

Description: As part of a new materials effort, we are exploring the use of sol- gel chemistry to manufacture energetic materials. Traditional manufacturing of energetic materials involves processing of granular solids. One application is the production of detonators where powders of energetic material and a binder are typically mixed and compacted at high pressure to make pellets. Performance properties are strongly dependent on particle size distribution, surface area of its constituents, homogeneity of the mix, and void volume. The goal is to produce detonators with fast energy release rate the are insensitive to unintended initiation. In this paper, we report results of our early work in this field of research, including the preparation of detonators from xerogel molding powders and aerogels, comparing the material properties with present state-of-the-art technology.
Date: August 18, 1997
Creator: Tillotson, T.M.; Hrubesh, L.H.; Fox, G.L.; Simpson, R.L.; Lee, R.W.; Swansiger, R.W. et al.
Partner: UNT Libraries Government Documents Department

A Mechanistic Investigation of Gelation. The Sol-Gel Polymerization of Bridged Silsesquioxane Monomers

Description: The study of a homologous series of silsesquioxane monomers has uncovered striking discontinuities in gelation behavior. An investigation of the chemistry during the early stages of the polymerization has provided a molecular basis for these observations. Monomers containing from one to four carbon atoms exhibit a pronounced tendency to undergo inter or intramolecular cyclization. The cyclic intermediates have been characterized by {sup 29}Si NMR, chemical ionization mass spectrometry and isolation from the reaction solution. These carbosiloxanes are local thermodynamic sinks that produce kinetic bottlenecks in the production of high molecular weight silsesquioxanes. The formation of cyclics results in slowing down or in some cases completely shutting down gelation. An additional finding is that the cyclic structures are incorporated intact into the final xerogel. Since cyclization alters the structure of the building block that eventually makes up the xerogel network, it is expected that this will contribute importantly to the bulk properties of the xerogel as well.
Date: July 14, 2000
Creator: SHEA,KENNETH J. & LOY,DOUGLAS A.
Partner: UNT Libraries Government Documents Department

Interaction of polymer with clays.

Description: Normally synthetic well defined monodisperse discotic laponite clays are known to form a gel phase at mass concentrations as low as a few percent in distilled water. Hydrosoluble polymer polyethylene oxide was added to this intriguing clay system, it was observed that it either prevents gelation or slows it down extremely depending on the polymer weight, concentration or the laponite concentration. Small Angle Neutron scattering (SANS) was used to study these systems because only by isotopic labelling can the structure of the adsorbed polymer layers be determined. The contrast variation technique is specifically used to determine separately the different partial structure factors of the clay and polymer. In this way the signal of the adsorbed chains is separated from the signal of the free chains.
Date: July 2, 1999
Creator: Auvray, L. & Lal, J.
Partner: UNT Libraries Government Documents Department

Gelcasting superalloy powders

Description: Gelcasting is a process for forming inorganic powders into complex shapes. It was originally developed for ceramic powders. A slurry of powder and a monomer solution is poured in to mold and polymerized in-situ to form gelled parts. Typically, only 2-4 wt % Polymer is used. The process has both aqueous and nonaqueous versions. Gelcasting is a generic process and has been used to produce ceramic parts from over a dozen different ceramic compositions ranging from alumina-based refractories to high-performance silicon nitride. Recently, gelcasting has been applied to forming superalloy powders into complex shapes. This application has posed several challenges not previously encountered in ceramics. In particular, problems were caused by the larger particle size and the higher density of the particles. Additional problems were encountered with binder removal. How these problems were overcome will be described.
Date: December 31, 1995
Creator: Janney, M.A.
Partner: UNT Libraries Government Documents Department

Investigation of the Peroxovanadate Sol-Gel Process and Characterization of the Gels

Description: In general, the peroxovanadate solution sol-gel process can be thought of as consisting of two parts: (1) the decomposition of the peroxo species and (2) cation hydrolysis leading to gelation. By controlling the synthesis conditions, both layered and amorphous compounds can be created. However, the type of water coordination observed in these gels was found to be identical no matter what the long-range order. The current work clarified many of the discrepancies found in the literature and offered much new valuable information. Highlights include the types of vanadium environments present at various stages of hydration, the role of adsorbed water, oxygen exchange from adsorbed water into the gel sites, and the ability to create metastable VMoO solid solution phases. These results could have a variety of impacts on future catalysis research.
Date: December 2001
Creator: Fontenot, Craig Joseph
Partner: UNT Libraries Government Documents Department

Application of NMR Spectroscopy and Multidimensional Imaging to the Gelcasting Process and in-situ Real-Time Monitoring of Cross-Linking Polyacrylamide Gels

Description: In the gelcasting process, a slurry of ceramic powder in a solution of organic monomers is cast in a mold. The process is different from injection molding in that it separates mold-filling from setting during conversion of the ceramic slurry to a formed green part. In this work, NMR spectroscopy and imaging have been conducted for in-situ monitoring of the gelation process and for mapping the polymerization. ¹H nuclear magnetic resonance spectra have been obtained during polymerization of a premix of soluble reactive methacrylamide (monomer) and N, N'-methylene bisacrylamide (cross-linking molecules). The premix was polymerized by adding ammonium persulfate (initiator) and tetramethyl-ethylene-diamine (accelerator) to form long-chain, cross-linked polymers. The time-varying spin-lattice relaxation times T₁ during polymerization have been studied at 25 and 35 C, and the variation of spectra and T₁ with respect to extent of polymerization has been determined. To verify homogeneous polymerization, multidimensional NMR imaging was utilized for in-situ monitoring of the process. The intensities from the images are modeled and the correspondence shows a direct extraction of T₁ data from the images.
Date: April 1995
Creator: Ahuja, S.; Dieckman, S. L.; Gopalsami, Nachappa; Raptis, A. C. & Omatete, Oritsegbemi O.
Partner: UNT Libraries Government Documents Department

Low density, microcellular, dopable, agar/gelatin foams for pulsed power experiments

Description: Low-density, microcellular foams prepared from the natural polymers agar and gelatin have been developed for pulsed-power physics experiments. Numerous experiments were supported with foams having densities at or below 10 mg/cm{sup 3}. For some of the experiments, the agar/gelatin foam was uniformly doped with metallic elements using soluble salts. Depending on the method of preparation, cell sizes were typically below 10 microns and for one process were below 1.0 micron.
Date: April 1997
Creator: McNamara, W. F. & Aubert, J. H.
Partner: UNT Libraries Government Documents Department

Improving reservoir conformance using gelled polymer systems. Final report, September 25, 1992--July 31, 1996

Description: The objectives of the research program were to (1) identify and develop polymer systems which have potential to improve reservoir conformance of fluid displacement processes, (2) determine the performance of these systems in bulk and in porous media, and (3) develop methods to predict their performance in field applications. The research focused on four types of gel systems--KUSP1 systems that contain an aqueous polysaccharide designated KUSP1, phenolic-aldehyde systems composed of resorcinol and formaldehyde, colloidal-dispersion systems composed of polyacrylamide and aluminum citrate, and a chromium-based system where polyacrylamide is crosslinked by chromium(III). Gelation behavior of the resorcinol-formaldehyde systems and the KUSP1-borate system was examined. Size distributions of aggregates that form in the polyacrylamide-aluminum colloidal-dispersion gel system were determined. Permeabilities to brine of several rock materials were significantly reduced by gel treatments using the KUSP1 polymer-ester (monoethyl phthalate) system, the KUSP1 polymer-boric acid system, and the sulfomethylated resorcinol-formaldehyde system were also shown to significantly reduce the permeability to supercritical carbon dioxide. A mathematical model was developed to simulate the behavior of a chromium redox-polyacrylamide gel system that is injected through a wellbore into a multi-layer reservoir in which crossflow between layers is allowed. The model describes gelation kinetics and filtration of pre-gel aggregates in the reservoir. Studies using the model demonstrated the effect filtration of gel aggregates has on the placement of gel systems in layered reservoirs.
Date: June 1, 1997
Creator: Green, D.W.; Willhite, G.P.; Buller, C.; McCool, S.; Vossoughi, S. & Michnick, M.
Partner: UNT Libraries Government Documents Department

Molecular engineering with bridged polysilsesquioxanes

Description: Bridged polysilsesquioxanes are a class of hybrid organic-inorganic materials that permit molecular engineering of bulk properties including porosity. Prepared by sol-gel polymerization of monomers with two or more trialkoxysilyl groups, the materials are highly cross-linked amorphous polymers that are readily obtained as gels. The bridging configuration of the hydrocarbon group insures that network polymers are readily formed and that the organic functionality is homogeneously distributed throughout the polymeric scaffolding at the molecular level. This permits the bulk properties, including surface area, pore size, and dielectric constant to be engineered through the selection of the bridging organic group. Numerous bridging groups have been incorporated. This presentation will focus on the effects that the length, flexibility, and substitution geometry of the hydrocarbon bridging groups have on the properties of the resulting bridged polysilsesquioxanes. Details of the preparation, characterization, and some structure property relationships of these bridged polysilsesquioxanes will be given.
Date: May 9, 2000
Creator: LOY,DOUGLAS A. & SHEA,KENNETH J.
Partner: UNT Libraries Government Documents Department

Transparent monolithic metal ion containing nanophase aerogels

Description: The formation of monolithic and transparent transition metal containing aerogels has been achieved through cooperative interactions of high molecular weight functionalized carbohydrates and silica precursors, which strongly influence the kinetics of gelation. After initial gelation, subsequent modification of the ligating character of the system, coordination of the group VIII metal ions, and supercritical extraction afford the aerogels. The structures at the nanophase level have been probed by photon and electron transmission and neutron scattering techniques to help elucidate the basis for structural integrity together with the small entity sizes that permit transparency in the visible range. They also help with understanding the chemical reactivities of the metal-containing sites in these very high surface area materials. These results are discussed in connection with new reaction studies.
Date: December 1, 1999
Creator: Risen, W. M., Jr.; Hu, X.; Ji, S. & Littrell, K.
Partner: UNT Libraries Government Documents Department