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Interfacial Microstructure Formed by Reactive Metal Penetration of Al into Mullite

Description: Microstructure in the reaction interface between molten Al and dense mullite have been studied by transmission electron microscopy to provide insight into mechanisms for forming ceramic-metal composites by reactive metal penetration. The reactions, which have the overall stoichiometry, 3Al#iz01~ + (8+ x)A1 + 13 AlzO~ + xA1 + 6Si, were carried out at temperatures of 900, 1100, and 1200oC for 5 minutes and 60 minutes, and 1400oC for 15 minutes. Observed phases generally were those given in the above reaction, although their proportions and interracial rnicrostructures differed strongly with reaction temperature. After reaction at 900oC, a thin Al layer separated unreacted mullite from the cx-AlzO~ and Al reaction products. No Si phase was found near the reaction front. After 5 minutes at 1100"C, the nxtction front contained Si, ct-A120~, and an aluminum oxide phase with a high concentration of Si. After 60 minutes at 11O(YC many of the cx-A120g particles were needle-shaped with a preferred orientation. After reaction at 1200oC, the reaction front contained a high density of Si particles that formed a continuous layer over many of the mullite grains. The sample reacted at 140VC for 15 minutes had a dense ct-A120J reaction layer less than 2~m thick. Some isolated Si particles were present between the a-AlzO~ layer and the unreacted mullite. Using previously measured reaction kinetics data, the observed temperature dependence of the interracial microstructure have been modeled as three sequential steps, each one of which is rate-limiting in a different temperature range.
Date: April 27, 1999
Creator: Du, T.B.; Ewsuk, K.G.; Fahrenholtz, W.G.; Loehman, R.E. & Lu, P.
Partner: UNT Libraries Government Documents Department

Advanced hot-gas filter development

Description: Coal is the most abundant fossil-fuel resource in the United States. `Clean coal` technologies, such as pressurized fluidized-bed combustion (PFBC) and integrated gasification combined-cycle (IGCC), require a hot gas filter to remove the corrosive and erosive coal ash entrained in the combustion gas stream. These hot gas filters, or candle filters, must be cost-effective while able to withstand the effects of corrosion, elevated temperature, thermal shock, and temperature transients. Ash loadings may range from 500 to 10,000 ppm by weight, and may contain particles as fine as 0.008 mils. The operating environment for the hot gas filter can range in pressure from 10 to 20 atm, in temperatures from 700 to 1750{degrees}F, and can be oxidizing or reducing. In addition, the process gases may contain volatile chloride, sulfur, and alkali species. Field testing of various commercially available, porous, ceramic filter matrices has demonstrated a loss of up to 50 percent of as-manufactured strength after 1,000 to 2,000 hours of exposure to these operating conditions, although full-scale elements have remained intact during normal process operations. Ultramet, a small business specializing in advanced materials R&D, has developed a new class of hot gas filter materials that offers lower back-pressure, higher permeability, longer life, and high filtration efficiency in the PFBC and IGCC environments. Subscale Ultrafoam Duplex Filter elements have undergone accelerated corrosion testing at temperatures of up to 2370{degrees}F (at Ultramet), and have been subjected to over 2,800 hours of exposure to hot PFBC gases (in the Westinghouse Advanced Particulate Filtration System at Brilliant, OH) without any loss in strength in either case. The Ultrafoam Duplex Filter matrix demonstrated 100 percent particle- capture efficiency of coal ash, and had an initial pressure drop of 0.1 to 0.6 in-wc/fpm. The Ultrafoam Duplex Filter is composed of a chemical vapor deposition (CVD), silicon carbide ...
Date: December 31, 1997
Creator: Stankiewicz, E.P.; Sherman, A.J. & Zinn, A.A.
Partner: UNT Libraries Government Documents Department

Functionally Graded Alumina/Mullite Coatings for Protection of Silicon Carbide Ceramic Components from Corrosion

Description: During the six months of this reporting period, we accomplished the following: Preparatory work was done on the development of the feed supply system (for mixtures of AlCl{sub 3}, SiCl{sub 4}, H{sub 2} and CO{sub 2}) and effluent treatment section for the CVD system we plan to employ for coating preparation. A comprehensive literature survey of past work done on the chemical vapor deposition of silica, alumina and aluminosilicates (mullite) was carried out, and work was initiated on the study of thermochemical equilibrium in the Al/Si/Cl/C/O/H system so as to identify the boundaries of the region of the space of operating parameters and conditions where preparation of functionally graded mullite/ alumina coatings through CVD from metal chloride, CO{sub 2}, and H{sub 2} is feasible. Since the alumina/mullite films that are proposed to be developed can also be applied to carbon matrix composites provided that a layer that bridges the gap that exists between the thermal expansion coefficient of carbon and that of mullite is employed, experiments were conducted on the preparation of compositionally graded carbon/silicon carbide coatings. Deposition from mixtures of ethylene and methyltrichlorosilane or tetrachlorosilane (silicon tetrachloride) in hydrogen was used for the preparation of SiC/C coatings, and our experiments focused on the study of the occurrence of multiple steady states in the deposition process and the effects of the type of chlorosilane on the deposition rate and the deposit composition and their variation along the length of the reactor. The results showed that when operation is carried out outside the multiplicity region, codeposition of SiC and C from ethylene and chlorosilanes is a feasible route for preparation of SiC/C graded coatings.
Date: April 1, 1997
Creator: Sotirchos, S. V.
Partner: UNT Libraries Government Documents Department

FUNCTIONALY GRADED ALUMINA/MULLITE COATINGS FOR PROTECTION OF SILICON CARBIDE CERAMIC COMPONENTS FROM CORROSION

Description: The main objective of this research project is the formulation of processes that can be used to prepare compositionally graded alumina/mullite coatings for protection from corrosion of silicon carbide components (monolithic or composite) used or proposed to be used in coal utilization systems (e.g., combustion chamber liners, heat exchanger tubes, particulate removal filters, and turbine components) and other energy-related applications. Mullite will be employed as the inner (base) layer and the composition of the film will be continuously changed to a layer of pure alumina, which will function as the actual protective coating of the component. Chemical vapor deposition reactions of silica, alumina, and aluminosilicates (mullite) through hydrolysis of aluminum and silicon chlorides in the presence of CO2 and H2 will be employed to deposit compositionally graded films of mullite and alumina. Our studies will include the kinetic investigation of the silica, alumina, and aluminosilicate deposition processes, characterization of the composition, microstructure, surface morphology, and mechanical behavior of the prepared films, and modeling of the various deposition processes. During this six-month reporting period, the experimental work on the investigation of the deposition of alumina, silica, and aluminosilicates from mixtures of methyltrichlorosilane (MTS), aluminum trichloride, carbon dioxide, and hydrogen was continued. Experiments were also conducted on the deposition processes of the simple oxides, alumina and silica, from mixtures containing only one chloride (AlCl3 and MTS, respectively). Deposition rate data were obtained in a relatively broad range of operating conditions: temperatures in the range 800-1000 o C, 100 Torr pressure, 0.006-0.015 AlCl3 feed mole fraction, 0.011- 0.027 CH3SiCl3 feed mole fraction, and 0.004-0.07 CO2 feed mole fraction, and various positions along the axis of the deposition reactor. Since the effect of temperature had been examined in detail in the previous reporting period, our efforts were mainly concentrated on the investigation of the ...
Date: October 1, 1998
Creator: SOTIRCHOS, PROF. STRATIS V.
Partner: UNT Libraries Government Documents Department

Rheology Control of Highly Concentrated Mullite Suspensions with Polyelectrolyte for Robocasting

Description: Highly concentrated, aqueous mullite slurries were characterized and stabilized at solids concentrations as high as 60 vol% using less than 2 vol% of an organic polyelectrolyte dispersant. The maximum slurry concentration (60 vol%) is within 3 vol% of the maximum consolidated density of the slurry. The slurries were subsequently cast into parts by a solid freeform fabrication technique termed robocasting and characterized. Sedimentation analysis and viscometry provided the means of slurry characterization, while knowledge of polyelectrolyte and interparticle forces was used to interpret the sedimentation and viscometry data. Through proper control of slurry conditions, pseudoplastic mullite slurries were fabricated for use in the robocasting process. The slurries were robocast at 52 vol% solids and subsequently yielded a green density of 55 vol%. Fired densities of the robocasted slurries were high, with mullite >96% dense at 1,650 C.
Date: June 12, 2000
Creator: STUECKER,JOHN N.; CESARANO III,JOSEPH & HIRSCHFELD,DEIDRE A.
Partner: UNT Libraries Government Documents Department

Plasma synthesis of high temperature ceramic films

Description: Thin films of alumina, chromia, mullite, yttria and zirconia have been synthesized using a plasma-based method called metal plasma immersion ion implantation and deposition (Mepiiid)--a highly versatile plasma deposition technique with ion energy control. Monolithic films (a single ceramic component) and multilayer films (individual layers of different ceramic materials) were formed. The films were characterized for their composition and structure in a number of different ways, and the high temperature performance of the films was explored, particularly for their ability to maintain their integrity and adhesion when subjected to repetitive high temperature thermal cycling up 1100 C. We found that the films retain their adhesion and quality without any apparent degradation with time, even after a large number of cycles; (the tests were extended out to a total of 40 cycles each of 24 hours duration). After repetitive high temperature thermal cycling, the film-substrate adhesion was greater than {approx}70 Mpa, the instrumental limit of measurement, and the interface toughness was approximately 0.8 MPa m{sup 1/2}.
Date: November 1, 1998
Creator: Brown, I.G. & Monteiro, O.R.
Partner: UNT Libraries Government Documents Department

Reaction mechanisms and microstructures of ceramic-metal composites made by reactive metal penetration

Description: Ceramic-metal composites can be made by reactive penetration of molten metals into dense ceramic performs. The metal penetration is driven by a large negative Gibbs energy for reaction, which is different from the more common physical infiltration of porous media. Reactions involving Al can be written generally as (x+2)Al + (3/y)MO{sub y} {yields} Al{sub 2}O{sub 3} + M{sub 3/y}Al{sub x}, where MO{sub y} is an oxide that is wet by molten Al. In low Po{sub 2} atmospheres and at temperature above about 900{degrees}c, molten Al reduces mullite to produce Al{sub 2}O{sub 3} + M{sub 3/y}Al{sub x}, where MO is an oxide that is wet by molten Al. In low Po{sub 2} atmospheres and at temperatures above about 900{degrees}C, molten al reduces mullite to produce Al{sub 2}O{sub 3} and Si. The Al/mullite reaction has a {Delta}G{sub r}{degrees} (1200K) of -1014 kJ/mol and, if the mullite is fully dense, the theoretical volume change on reaction is less than 1%. A microstructure of mutually-interpenetrating metal and ceramic phases generally is obtained. Penetration rate increases with increasing reaction temperature from 900 to 1150{degrees}C, and the reaction layer thickness increases linearly with time. Reaction rate is a maximum at 1150{degrees}C; above that temperature the reaction slows and stops after a relatively short period of linear growth. At 1300{degrees}C and above, no reaction layer is detected by optical microscopy. Observations of the reaction front by TEM show only al and Al{sub 2}O{sub 3} after reaction at 900{degrees}C, but Si is present in increasing amounts as the reaction temperature increases to 1100{degrees}C and above. The kinetic and microstructural data suggest that the deviation from linear growth kinetics at higher reaction temperatures and longer times is due to Si build-up and saturation at the reaction front. The activation energy for short reaction times at 900 to 1150{degrees}C varies ...
Date: December 31, 1996
Creator: Fahrenholtz, W.F.; Ewsuk, K.G. & Loehman, R.E.
Partner: UNT Libraries Government Documents Department

Compressive Creep and Thermophysical Performance of Mullite Refractories

Description: Compressive creep testing of ten commercially available mullite refractories was performed at 1300-1450 C and at static stresses between 0.2-0.6 MPa. These refractories were examined because they are used in borosilicate glass furnace crowns and superstructures along with in sidewall applications. Additionally, despite their high cost ({approx}$500/ft{sup 3}) they are cheaper than other refractories such as chrome alumina ({approx}$3000/ft{sup 3}) or fusion-cast alumina ({approx}900/ft{sup 3}) which are used as replacements for traditional silica refractories in harsh oxy-fuel environments. The corrosion resistances of these ten materials were also evaluated. In addition, measurements were made that tracked their dimensional stability, phase content, microstructure, and composition as a function of temperature and time. The techniques used for these characterizations and their respective analyses are described. An intent of this study was to provide objective and factual results whose interpretations were left to the reader.
Date: April 1, 2002
Creator: Hemrick, JG
Partner: UNT Libraries Government Documents Department

Energy and environmental research emphasizing low-rank coal: Task 6.2. Joining of advanced structural materials

Description: Silicon carbide (SiC) is considered an attractive material for structural applications in fossil energy systems because of its corrosion and wear resistance, high thermoconductivity, and high temperature strength. These same properties make it difficult to sinter or join SiC. Conventional sintering techniques require applying pressure and heating to temperatures near 2000{degree}C, or the use of binders with lower melting temperatures, or pressureless sintering with the aid of carbon and boron to near full density about 2100{degree}C. The sintering temperature can be reduced to 1850{degree}--2000{degree}C if SiC is sintered with the addition of small quantities of Al{sub 2}O{sub 3} and Al{sub 2}O{sub 3} {plus} Y{sub 2}O{sub 3}. In addition, reaction sintering has been used by mixing Si and C with SiC powder and heating the mixture to 1400{degree}C to cause the Si and C to react and form SiC, which bonds the aggregate together. Work proposed for this year was to center on determining gas compositions that could be used to increase the sinterability of oxide binders and on using the binder and gas combinations to join bars of SiC, alumina, and mullite (3Al{sub 2}O{center_dot}2SiO{sub 2}). During the course of the year the focus was shifted to SiC joining alone, because it was felt that alumina and mullite are too prone to thermal shock for use in structural applications in fossil energy systems. Because of a thermal expansion mismatch between alumina and SiC, only SiC and mullite were investigated as joining aides for SiC. Therefore, the objectives of this work evolved into examining the sintering phenomena of SiC and mullite-derived binders at and below 1500{degree}C in various atmospheres and determining which conditions are suitable to form strong joints in monolithic SiC structures to be used at temperatures of 1000{degree}--1400{degree}C.
Date: March 1, 1995
Creator: Nowok, J.W. & Hurley, J.P.
Partner: UNT Libraries Government Documents Department

The development of chemically vapor deposited mullite coatings for the corrosion protection of SiC

Description: Crystalline mullite coatings have been chemically vapor deposited onto SiC substrates to enhance the corrosion and oxidation resistance of the substrate. Current research has been divided into three distinct areas: (1) Development of the deposition processing conditions for increased control over coating`s growth rate, microstructure, and morphology; (2) Analysis of the coating`s crystal structure and stability; (3) The corrosion resistance of the CVD mullite coating on SiC.
Date: May 1, 1998
Creator: Auger, M.; Hou, P.; Sengupta, A.; Basu, S. & Sarin, V.
Partner: UNT Libraries Government Documents Department

TEM characterization of Al/Al{sub 2}O{sub 3} composite fabricated by reactive metal infiltration

Description: The microstructure of Al/{alpha}-Al{sub 2}0{sub 3} composites made by infiltrating Al into dense mullite preforms has been characterized using transmission electron microscopy. Observations revealed that the formation of the Al/Al{sub 2}0{sub 3} composites involves three stages. Initially, Al infiltrates into a dense mullite preform through grain boundary diffusion, and reacts with mullite at grain boundaries to form a partial reaction zone. Then, a complete reaction takes place in the reaction region between the partial reaction zone and the full reaction zone to convert the dense mullite preform to a composite of {alpha}-Al{sub 2}0{sub 3} (matrix) and an Al-Si phase (thin channels). Finally, the reduced Si from the reaction diffuses out of the Al/Al{sub 2}0{sub 3} composite through the metal channels, whereas Al from the molten Al pool is continuously drawn to the reaction region until the mullite preform is consumed or the sample is removed from the molten Al pool. Based on the observed microstructure, infiltration mechanisms have been discussed, and a growth model of the composites is proposed in which the process involves repeated nucleation of Al{sub 2}0{sub 3} grains and grain growth.
Date: December 31, 1994
Creator: Gao, Y.; Jia, J.; Loehman, R.E. & Ewsuk, K.G.
Partner: UNT Libraries Government Documents Department

Interfacial Microstructure Formed by Reactive Metal Penetration of Al into Mullite

Description: Microstructures in the reaction interface between molten Al and dense mullite have been studied by transmission electron microscopy to provide insight into mechanisms for forming ceramic-metal composites by reactive metal penetration. The reactions, which have the overall stoichiometry, 3Al{sub 6}Si{sub 2}O{sub 13} + (8 + x)Al {r_arrow} 13Al{sub 2}O{sub 3} + xAl + 6Si, were carried out at temperatures of 900, 1100, and 1200 C for 5 minutes and 60 minutes, and 1400 C for 15 minutes. Observed phases generally were those given in the above reaction, although their proportions and interfacial microstructure differed strongly with reaction temperature. After reaction at 900 C, a thin Al layer separated unreacted mullite from the {alpha}-Al{sub 2}O{sub 3} and Al reaction products. No Si phase was found near the reaction front. After 5 minutes at 1100 C, the reaction front contained Si, {alpha}-Al{sub 2}O{sub 3}, and an aluminum oxide phase with a high concentration of Si. After 60 minutes at 1100 C many of the {alpha}-Al{sub 2}O{sub 3} particles were needle-shaped with a preferred orientation. After reaction at 1200 C, the reaction front contained a high density of Si particles that formed a continuous layer over many of the mullite grains. The sample reacted at 1400 C for 15 minutes had a dense {alpha}-Al{sub 2}O{sub 3} reaction layer less than 2 {micro}m thick. Some isolated Si particles were present between the {alpha}-Al{sub 2}O{sub 3} layer and the unreacted mullite. Using previously measured reaction kinetics data the observed temperature dependence of the interfacial microstructure have been modeled as three sequential steps, each one of which is rate-limiting in a different temperature range.
Date: March 3, 1999
Creator: Du, T.B.; Ewsuk, K.G.; Fahrenholtz, W.G.; Loehman, R.E. & Lu, P.
Partner: UNT Libraries Government Documents Department

Topical report to Morgantown Energy Technology Center for the interfacial coatings for ceramic-matrix composites

Description: This report summarizes the task conducted to examine various activities on interface development for ceramic-matrix composites (CMCs) intended for high-temperature applications. While several articles have been published on the subject of CMC interfaces, the purpose of this report is to describe the various ongoing efforts on interface concepts, material selection, and issues related to processing methods employed for developing interface coatings. The most exciting and new development in the field is the discovery of monazite as a potential interface material for mullite- and alumina-based composites. Monazite offers two critical properties to the CMC system; a weakly bonded layer due to its non-wetting behavior and chemical compatibility with both alumina and mullite up to very high temperatures (> 1,600 C). A description of the Department of Energy-related activities and some thoughts on processing issues, interface testing, and effects of processing on fiber strength are given.
Date: January 9, 1997
Partner: UNT Libraries Government Documents Department

Development of CVD Mullite Coatings for SiC Fibers

Description: A process for depositing CVD mullite coatings on SiC fibers for enhanced oxidation and corrosion, and/or act as an interfacial protective barrier has been developed. Process optimization via systematic investigation of system parameters yielded uniform crystalline mullite coatings on SiC fibers. Structural characterization has allowed for tailoring of coating structure and therefore properties. High temperature oxidation/corrosion testing of the optimized coatings has shown that the coatings remain adherent and protective for extended periods. However, preliminary tests of coated fibers showed considerable degradation in tensile strength.
Date: March 15, 2000
Creator: Sarin, V. K. & Varadarajan, S.
Partner: UNT Libraries Government Documents Department

AQUEOUS BIPHASE EXTRACTION FOR PROCESSING OF FINE COAL

Description: Ever-stringent environmental constraints dictate that future coal cleaning technologies be compatible with micron-size particles. This research program seeks to develop an advanced coal cleaning technology uniquely suited to micron-size particles, i.e., aqueous biphase extraction. The partitioning behavior of fly ash in the PEG-2000 Na{sub 2}SO{sub 4}/H{sub 2}O system was studied and the solid in each fraction was characterized by CHN analysis (carbon content), X-ray diffraction (XRD; crystal component), and inductively coupled plasma spectrophotometry (ICP; elemental composition in the ash). In the pH range from 2 to 5, the particles separated into two different layers, i.e., the polymer-rich (top) and salt-rich (bottom) layers. However, above pH 5, the particles in the polymer-rich phase split into two zones. The percent carbon content of the solids in the upper zone ({approximately}80 wt%) was higher than that in the parent sample (63.2 wt%), while the lower zone in the polymer-rich phase had the same percent ash content as the original sample. The particles in the salt-rich phase were mainly composed of ash (with < 4 wt% carbon content). However, when the solid concentration in the whole system increased from 1 wt% to 2 wt%, this 3-fraction phenomenon only occurred above pH 10. XRD results showed that the main crystal components in the ash included quartz, hematite, and mullite. The ICP results showed that Si, Al, and Fe were the major elements in the fly ash, with minor elements of Na, K, Ca, Mg, and Ba. The composition of the ash in the lower zone of the polymer-rich phase remained almost the same as that in the parent fly ash. The largest amount of product ({approximately}60% yield) with the highest carbon content ({approximately}80 wt% C) was obtained in the range pH 6-9. Based on the experimental results obtained, a flowsheet is proposed for the beneficiation ...
Date: June 2, 2000
Creator: Osseo-Asare, K.
Partner: UNT Libraries Government Documents Department

Corrosion protection of SiC-based ceramics with CVDMullite coatings

Description: Silicon carbide ceramics are the leading candidate materials for use as heat exchangers in advanced combined cycle power plants because of their unique combination of high temperature strength, high thermal conductivity, excellent thermal shock resistance, and good high temperature stability and oxidation resistance. Ceramic coatings are being considered for diesel engine cylinder liners, piston caps, valve faces and seats, piston rings, and for turbine components such as combustors, blades, stators, seals, and bearings. Under such conditions ceramics are better suited to high temperature environments than metals. For the first time, adherent crystalline mullite coatings have been chemically vapor deposited onto SiC substrates to enhance its corrosion/oxidation resistance. Thermodynamic and kinetic considerations have been utilized to produce mullite coatings with a variety of growth rates, compositions, and morphologies. The flexibility of processing can be exploited to produce coated ceramics with properties tailored to specific applications and varied corrosive environments. These corrosive environments include thermal, Na{sub 2}SO{sub 4}, O{sub 2} and coal slag.
Date: May 1, 1997
Creator: Sarin, V. & Auger, M.
Partner: UNT Libraries Government Documents Department

Alumina composites for oxide/oxide fibrous monoliths

Description: Most work on ceramic fibrous monoliths (FMs) has focused on the Si{sub 3}N{sub 4}/BN system. In an effort to develop oxidation-resistant FMs, several oxide systems have recently been examined. Zirconia-toughened alumina and alumina/mullite appear to be good candidates for the cell phase of FMs. These composites offer higher strength and toughness than pure alumina and good high-temperature stability. By combining these oxides, possibly with a weaker high-temperature oxide as the cell-boundary phase, it should be possible to product a strong, resilient FM that exhibits graceful failure. Several material combinations have been examined. Results on FM fabrication and microstructural development are presented.
Date: March 1, 2000
Creator: Cruse, T. A.; Polzin, B. J.; Picciolo, J. J.; Singh, D.; Tsaliagos, R. N. & Goretta, K. C.
Partner: UNT Libraries Government Documents Department

Development of sol-gel derived coating for NICALON{sup TM}/SiC composites

Description: Mullite and aluminum titanate precursor polymeric sols were developed for applying as coatings on Nicalon{trademark} fabrics and tows. A Nicalon{trademark}/SiC composite with a mullite interface was fabricated. The mullite precursor interface coatings were applied by a vacuum infiltration method and the SiC matrix was deposited by a forced flow chemical vapor infiltration process. Thin, uniform mullite interface coatings were obtained. However, the Nicalon{trademark}/SiC composite exhibited brittle fracture. Mullite and alumina-titania coatings were applied on Nicalon{trademark} tows and the effect of heat treatment at 1000{degrees}C in air is discussed.
Date: May 1, 1996
Creator: Shanmugham, S.; Liaw, P.K.; Stinton, D.P.; Besmann, T.M.; More, K.L.; Bleier, A. et al.
Partner: UNT Libraries Government Documents Department

Controlled densification of mullite for composite applications.

Description: As part of an effort to fabricate oxide-based fibrous monolithic ceramics, sintering of mullite has been examined. The effects of Y{sub 2}O{sub 3} additions on sinterability of sol-gel-derived mullite and on the resulting microstructure were evaluated over a range of compositions, sintering times, and temperatures. Electron microscopy, X-ray diffraction, differential thermal analysis, and density measurements indicated that the Y{sub 2}O{sub 3} additions promoted densification through formation of a Y-Si-Al-O liquid phase. This phase tended to solidify as a glass during normal processing, but could be crystallized by a two-step annealing process at 1300 and 1200 C. The four-point flexural strengths of mullite and mullite-5 Wt.% Y{sub 2}O{sub 3} were also examined.
Date: May 19, 1999
Creator: Cruse, T. A.
Partner: UNT Libraries Government Documents Department

EFFECT OF QUARTZ/MULLITE BLEND CERAMIC ADDITIVE ON IMPROVING RESISTANCE TO ACID OF SODIUM SILICATE-ACTIVATED SLAG CEMENT. CELCIUS BRINE.

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
Creator: SUGAMA, T.; BROTHERS, L.E. & VAN DE PUTTE, T.R.
Partner: UNT Libraries Government Documents Department

SODIUM POLYPHOSPHATE-MODIFIED CLASS C/CLASS F FLY ASH BLEND CEMENTS FOR GEOTHERMAL WELLS.

Description: The authors investigated the usefulness of the coal combustion by-products, Class C fly ash (C) and Class F fly ash (F), in developing cost-effective acid-resistant phosphate-based cements for geothermal wells. In the temperature range of 20-100 C, sodium polyphosphate (NaP) as the acidic cement-forming solution preferentially reacted with calcium sulfate and lime in the C as the base solid reactant through the exothermic acid-base reaction route, rather than with the tricalcium aluminate in C. This reaction led to the formation of hydroxyapatite (HOAp). In contrast, there was no acid-base reaction between the F as the acidic solid reactant and NaP. After autoclaving the cements at 250 C, a well-crystallized HOAp phase was formed in the NaP-modified C cement that was responsible for densifying the cement's structure, thereby conferring low water permeability and good compressive strength on the cement. however, the HOAp was susceptible to hot CO{sub 2}-laden H{sub 2}SO{sub 4} solution (pH 1.1), allowing some acid erosion of the cement. On the other hand, the mullite in F hydrothermally reacted with the Na from NaP to form the analcime phase. Although this phase played a pivotal role in abating acid erosion, its generation created an undesirable porous structure in the cement. They demonstrated that blending fly ash with a C/F ratio of 70/30 resulted in the most suitable properties for acid-resistant phosphate-based cement systems.
Date: February 1, 2006
Creator: SUGAMA, T.; BROTHERS, L.E. & KASPEREIT, D.
Partner: UNT Libraries Government Documents Department

Particulate hot gas stream cleanup technical issues. Quarterly report, October 1995--December 1995

Description: This is the fifth quarterly report describing the activities performed under Contract No. DE-AC21-94MC31160. Task 1 of this contract concerns analyses of HGCU ashes and descriptions of filter performance that are designed to address the problems with filter operation linked to the characteristics of the collected ash. Task 2 of this contract includes characterization of new and used filter elements. Some of the problems observed at the Tidd and Karhula PFBC facilities include excessive filtering pressure drop, the formation of large, tenacious ash deposits within the filter vessel, and bent or broken candle filter elements. These problems have been attributed to ash characteristics, durability of the ceramic filter elements, and specific limitations of the filter design. In addition to these problems related to the characteristics of PFBC ashes, our laboratory characterizations of gasifier and carbonizer ashes have shown that these ashes also have characteristics that might negatively affect filtration. Problems with the durability of the filter elements are being addressed by the development and evaluation of elements constructed from alternative ceramic materials.
Date: March 1, 1996
Partner: UNT Libraries Government Documents Department

Ceramic-metal composite formation by reactive metal penetration

Description: Ceramic-metal composites can be made to near-net-shape by reactive penetration of dense ceramic preforms by molten metals. Reactive metal penetration is driven by a strongly negative Gibbs energy for reaction. For Al, the general form of the reaction is (x+2) Al + (3/y) MO[sub y] yields Al[sub 2]O[sub 3] + M[sub 3/y]Al[sub x], where MO[sub y] is an oxide that is wet by molten Al. In low PO[sub 2] atmospheres and at temperatures above about 900 degrees C, molten Al reduces mullite to produce Al[sub 2]O[sub 3] and Si. The Al/mullite reaction has a delta G[sub r] degree(927 degrees C) of -338 per mole of mullite and, for fully dense mullite, the theoretical volume change on reaction is less than 1%. Experiments with commercial mullite containing a silicate grain boundary phase average less than 2% volume change on reaction. In the Al/mullite system, reactive metal penetration produces a fine-grained alumina skeleton with an interspersed metal phase. With > or =15 vol.% excess aluminum, mutually interpenetrating ceramic-metal composites are produced. Properties measurements show that ceramic-metal composites produced by reactive metal penetration of mullite by Al have a Young`s modulus and hardness similar to that of Al[sub 2]O[sub 3], with improved fracture toughness. Other compositions also are candidates for in- situ reaction synthesis, but they exhibit differences in reaction kinetics, most probably due to different wetting behavior.
Date: November 1, 1996
Creator: Loehman, R.E.; Ewsuk, K.G.; Fahrenholtz, W.G. & Lakshman, B.B.
Partner: UNT Libraries Government Documents Department

Conversion of coal wastes into waste-cleaning materials. Quarterly progress report, July 1, 1995--September 30, 1995

Description: In the last three months we studied the phase composition of the fly ash in order to better understand the important parameters in the zeolite formation process using fly ash. In addition, since the zeolites exist in powder form, for practical applications, some ways of binding them into a piece of material is necessary. For that purpose, we began exploring ways of forming porous materials using fly ash. It was found that mixing fly ash, phosphoric acid, and calcium oxide can generate a porous material with good integrity. Meanwhile, the research on forming mesoporous materials from fly ash continued. Some results on the formation of double lamellar phase was found during the study.
Date: December 31, 1995
Creator: Shih, Wei-Heng
Partner: UNT Libraries Government Documents Department