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Sample records for mullite

  1. Mullite Whiskers and Mullite-whisker Felt

    NASA Technical Reports Server (NTRS)

    Talmy, Inna G.; Haught, Deborah A.

    1993-01-01

    The Naval Surface Warfare Center has developed processes for the preparation of mullite (3(Al2O3)(dot)2(SiO2)) whiskers and mullite-whisker felt. Three patents on the technology were issued in 1990. The processes are based on chemical reactions between AlF3, Al2O3, and SiO2. The felt is formed in-situ during the processing of shaped powdered precursors. It consists of randomly oriented whiskers which are mutually intergrown forming a rigid structure. The microstructure and properties of the felt and size of the whiskers can be modified by varying the amount of Al2O3 in the starting mixture. Loose mullite whiskers can be used as a reinforcement for polymer-, metal-, and ceramic-matrix composites. The felt can be used as preforms for fabricating composite materials as well as for thermal insulation and high temperature, chemically stable filters for liquids (melts) and gases.

  2. Metal-mullite reactions

    SciTech Connect

    Loehman, R.E.; Tomsia, A.P.

    1993-11-01

    Mullite was reacted with pure Al and with Ti or Zr dissolved in Ag-Cu eutectic alloys at 1100 C in Ar. Analysis of the Ti and Zr-containing specimens showed reaction zones with compositions of Ti{sub 50}Cu{sub 3O}O{sub 20} and ZrO{sub 2}, respectively. The Al-mullite specimen showed much more extensive penetration into the ceramic and a more diffuse reaction zone than the other two systems. Al{sub 2}O{sub 3} and Si were the main reaction products for Al-mullite reaction.

  3. Production of mullite fibers

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S. (Inventor); Sparks, J. Scott (Inventor)

    1991-01-01

    Disclosed here is a process for making mullite fibers wherein a hydrolizable silicon compound and an aluminum compound in the form of a difunctional aluminum chelate are hydrolized to form sols using water and an alcohol with a catalytic amount of hydrochloric acid. The sols are mixed in a molar ratio of aluminum to silicon of 3 to 1 and, under polycondensation conditions, a fibrous gel is formed. From this gel the mullite fibers can be produced.

  4. Directionally solidified mullite fibers

    SciTech Connect

    Sayir, A.; Farmer, S.C.

    1995-10-01

    Directionally solidified fibers with nominal mullite compositions of 3Al{sub 2}O{sub 3} {center_dot} 2SiO{sub 2} were grown by the laser heated float zone (LHFZ) method at NASA Lewis. High resolution digital images from an optical microscope evidence the formation of a liquid-liquid miscibility gap during crystal growth. Experimental evidence shows that the formation of mullite in aluminosilicate melts is in fact preceded by liquid immiscibility. The average fiber tensile strength is 1.15 GPa at room temperature. The mullite fibers retained 80% of their room temperature tensile strength at 1,450 C. SEM analysis revealed that the fibers were strongly faceted and that the facets act as critical flaws. Examined in TEM, these mullite single crystals are free of dislocations, low angle boundaries and voids. Single crystal mullite showed a high degree of oxygen vacancy ordering. Regardless of the starting composition, the degree of order observed in polycrystalline fibers was lower than that observed in the mullite single crystals.

  5. Boron incorporation into mullite

    NASA Astrophysics Data System (ADS)

    Griesser, K. J.; Beran, A.; Voll, D.; Schneider, H.

    2008-03-01

    Boron-doped mullites were synthesized using aluminium nitrate-nonahydrate, tetraethoxysilane and boric acid in a sol gel process with subsequent annealing at 950 and 1300 °C for five hours. Two different bulk compositions with constant Al2O3 contents (60 and 70 mol%, respectively) and varying SiO2 plus B2O3 contents were investigated. X-ray powder diffraction analyses yielded a linear decrease of the lattice parameters with increasing bulk B2O3 content, which was interpreted as to be due to boron incorporation. Related to the increasing boron content, corresponding infrared spectra revealed a slight and continuous shift for most of the absorption bands. These data show that mullite is able to incorporate large amounts of boron into its structure (up to about 20 mol% B2O3 depending on the bulk composition of the starting materials). Infrared analyses suggest that boron is incorporated into the mullite structure in form of planar three-fold coordinated BO3 groups.

  6. Making Mullite Fibers By Airgap Wet Spinning

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S.; Sparks, J. Scott

    1991-01-01

    Proposed process makes continuous mullite fibers retaining structural integrity at temperatures up to and somewhat beyond 1,300 degrees C. Process makes highly pure mullite fibers, without melting and without dangerous solvent.

  7. Chemical vapor deposition of mullite coatings

    DOEpatents

    Sarin, Vinod; Mulpuri, Rao

    1998-01-01

    This invention is directed to the creation of crystalline mullite coatings having uniform microstructure by chemical vapor deposition (CVD). The process comprises the steps of establishing a flow of reactants which will yield mullite in a CVD reactor, and depositing a crystalline coating from the reactant flow. The process will yield crystalline coatings which are dense and of uniform thickness.

  8. Development program to produce mullite fiber insulation

    NASA Technical Reports Server (NTRS)

    Long, W. G.

    1975-01-01

    Processing methods were utilized to form a mullite fiber-Kaowool felt. The formation of a blended felt using the Rotoformer wet-laying method was successful. Felt products were evaluated for tensile strength, thermal stability, thermal conductivity and structural integrity at 1259 C and 1371 C. Textile processing methods failed in an attempt to form a yarn from staple and multifilament mullite fiber due to fiber damage through mechanical handling. The refractoriness of pure Kaowool ceramic fiber is improved with additions of 30% or greater mullite fiber.

  9. Controlled densification of mullite for composite applications.

    SciTech Connect

    Cruse, T. A.

    1999-05-19

    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.

  10. Development of Mullite Substrates and Containers

    NASA Technical Reports Server (NTRS)

    Sibold, J. D.

    1979-01-01

    The mullite-molten silicon interaction was evaluated through fabrication of a series of bodies made with variations in density, alumina-silica ratio, and glass-crystalline ratio. The materials were tested in a sessile drop technique. None of the variations stood up to extended exposure to molten silicon sufficiently to be recommended as a container material. However, directional solidification experiments suggest that, under proper conditions, contamination of the silicon by mullite containers can be minimized. To improve an already good thermal expansion match between mullite and silicon, compositional variations were studied. Altering of the alumina-silica ratio was determined to give a continuously varying thermal expansion. A standard mullite composition was selected and substrates 40 x 4 x .040 inches were fabricated. Slotted substrates of various configurations and various compositions were also fabricated.

  11. Phase transformations in xerogels of mullite composition

    NASA Technical Reports Server (NTRS)

    Hyatt, Mark J.; Bansal, Narottam P.

    1990-01-01

    Monophasic and diphasic xerogels have been prepared as precursors for mullite (3Al203-2Si02). Monophasic xerogel was synthesized from tetraethyl orthosilicate and aluminum nitrate nanohydrate and the diphasic xerogel from colloidal suspension of silica and boehmite. The chemical and structural evolutions, as a function of thermal treatment, in these two types of sol-gel derived mullite precursor powders have been characterized by DTA, TGA, X-ray diffraction, SEM and infrared spectroscopy. Monophasic xerogel transforms to an Al-Si spinel from an amorphous structure at approximately 980 C. The spinel then changes into mullite on further heating. Diphasic xerogel forms mullite at approximately 1360 C. The components of the diphasic powder react independently up to the point of mullite formation. The transformation in the monophasic powder occurs rapidly and yields strongly crystalline mullite with no other phases present. The diphasic powder, however, transforms rather slowly and contains remnants of the starting materials (alpha-Al203, cristobalite) even after heating at high temperatures for long times (1600 C, 6 hr). The diphasic powder could be sintered to high density but not the monophasic powder in spite of its molecular level homogeneity.

  12. Phase transformations in xerogels of mullite composition

    NASA Technical Reports Server (NTRS)

    Hyatt, Mark J.; Bansal, Narottam P.

    1988-01-01

    Monophasic and diphasic xerogels have been prepared as precursors for mullite (3Al2O3-2SiO2). Monophasic xerogel was synthesized from tetraethyl orthosilicate and aluminum nitrate nanohydrate and the diphasic xerogel from colloidal suspension of silica and boehmite. The chemical and structural evolutions, as a function of thermal treatment, in these two types of sol-gel derived mullite precursor powders have been characterized by DTA, TGA, X-ray diffraction, SEM and infrared spectroscopy. Monophasic xerogel transforms to an Al-Si spinel from an amorphous structure at approximately 980 C. The spinel then changes into mullite on further heating. Diphasic xerogel forms mullite at approximately 1360 C. The components of the diphasic powder react independently up to the point of mullite formation. The transformation in the monophasic powder occurs rapidly and yields strongly crystalline mullite with no other phases present. The diphasic powder, however, transforms rather slowly and contains remnants of the starting materials (alpha-Al2O3, cristobalite) even after heating at high temperatures for long times (1600 C, 6 hr). The diphasic powder could be sintered to high density but not the monophasic powder in spite of its molecular level homogeneity.

  13. The modulated average structure of mullite.

    PubMed

    Birkenstock, Johannes; Petříček, Václav; Pedersen, Bjoern; Schneider, Hartmut; Fischer, Reinhard X

    2015-06-01

    Homogeneous and inclusion-free single crystals of 2:1 mullite (Al(4.8)Si(1.2)O(9.6)) grown by the Czochralski technique were examined by X-ray and neutron diffraction methods. The observed diffuse scattering together with the pattern of satellite reflections confirm previously published data and are thus inherent features of the mullite structure. The ideal composition was closely met as confirmed by microprobe analysis (Al(4.82 (3))Si(1.18 (1))O(9.59 (5))) and by average structure refinements. 8 (5) to 20 (13)% of the available Si was found in the T* position of the tetrahedra triclusters. The strong tendencey for disorder in mullite may be understood from considerations of hypothetical superstructures which would have to be n-fivefold with respect to the three-dimensional average unit cell of 2:1 mullite and n-fourfold in case of 3:2 mullite. In any of these the possible arrangements of the vacancies and of the tetrahedral units would inevitably be unfavorable. Three directions of incommensurate modulations were determined: q1 = [0.3137 (2) 0 ½], q2 = [0 0.4021 (5) 0.1834 (2)] and q3 = [0 0.4009 (5) -0.1834 (2)]. The one-dimensional incommensurately modulated crystal structure associated with q1 was refined for the first time using the superspace approach. The modulation is dominated by harmonic occupational modulations of the atoms in the di- and the triclusters of the tetrahedral units in mullite. The modulation amplitudes are small and the harmonic character implies that the modulated structure still represents an average structure in the overall disordered arrangement of the vacancies and of the tetrahedral structural units. In other words, when projecting the local assemblies at the scale of a few tens of average mullite cells into cells determined by either one of the modulation vectors q1, q2 or q3 a weak average modulation results with slightly varying average occupation factors for the tetrahedral units. As a result, the real

  14. Corrosion of Mullite by Molten Salts

    NASA Technical Reports Server (NTRS)

    Jacobson, Nathan S.; Lee, Kang N.; Yoshio, Tetsuo

    1996-01-01

    The interaction of molten salts of different Na2O activities and mullite is examined with furnace and burner tests. The more-acidic molten salts form small amounts of Al2O3; the more-basic molten salts form various Na2O-Al2O3-SiO2 compounds. The results are interpreted using the Na2O-Al203-SiO2 ternary phase diagram, and some possible diffusion paths are discussed. The generally higher melting points of Na2O-Al2O3-SiO2 compounds lead to better behavior of mullite in molten salts, as compared to SiO2-protected ceramics such as SiC. Mullite-coated SiC is discussed, and the corrosion behavior is evaluated.

  15. Functionally graded mullite coatings for gas turbines

    NASA Astrophysics Data System (ADS)

    Kulkarni, Tushar

    The next generation of heat exchangers and gas turbines require high performance materials as they need to operate at higher temperatures for higher efficiency. SiC and Si3N4 are promising candidates as they have excellent high temperature properties. However, when used in complex combustion environments found in gas-turbine applications, these materials have two major concerns; namely hot-corrosion and recession. It is well established that environmental barrier coatings (EBC) can be utilized to overcome these limitations. Although chemical vapor deposited (CVD) mullite (3Al2O 3.2SiO2) coatings developed before this study have shown promise in protecting Si-based substrates, there is concern that the silica content within the mullite coating itself might be susceptible to hot-corrosion and recession during long term exposure to corrosive atmospheres containing Na/V salts and water vapor. There is thus strong motivation to substantially reduce or even virtually eliminate the silica component from the surfaces of mullite coatings that are in direct contact with atmospheres containing corrosive oxides and steam. In this study, CVD has been used to deposit mullite coatings with potential promise to protect Si-based ceramics for high temperature applications. The composition of these functionally graded mullite coatings was varied from silica-rich close to the coating/substrate (SiC) interface for coefficient of thermal expansion match to alumina-rich towards the outer surface of the coating. In the process, the highest alumina-rich mullite ever reported has been deposited. The phase transformation and hot-corrosion behavior of the coatings was also investigated in this work. The coatings show immense potential to protect Si-based ceramics. It is expected that these coatings will have very broad impact by enabling gas turbines to operate at higher temperatures leading to improved fuel efficiency and reduced emissions.

  16. Coating Silicon-Based Ceramics With Durable Mullite

    NASA Technical Reports Server (NTRS)

    Miller, Robert A.; Jacobson, Nathan S.; Lee, Kang N.

    1996-01-01

    Improved plasma-spraying process deposits mullite on silicon carbide substrates. Prevents formation of amorphous mullite by maintaining high temperature of sprayed deposite to allow crystallization to occur. Deposited mullite adheres to substrate and exhibits little or no cracking during thermal cycling. Provides substantially greater resistance to oxidation in dry air and corrosion by molten salt. Process expected useful in depositing mullite on substrates made of other silicon-based ceramics and other ceramic substrates having coefficients of thermal expansion similar to those of mullite.

  17. Microstructure and Mechanical Properties of Porous Mullite

    NASA Astrophysics Data System (ADS)

    Hsiung, Chwan-Hai Harold

    Mullite (3 Al2O3 : 2 SiO2) is a technologically important ceramic due to its thermal stability, corrosion resistance, and mechanical robustness. One variant, porous acicular mullite (ACM), has a unique needle-like microstructure and is the material platform for The Dow Chemical Company's diesel particulate filter AERIFY(TM). The investigation described herein focuses on the microstructure-mechanical property relationships in acicular mullites as well as those with traditional porous microstructures with the goal of illuminating the critical factors in determining their modulus, strength, and toughness. Mullites with traditional pore morphologies were made to serve as references via slipcasting of a kaolinite-alumina-starch slurry. The starch was burned out to leave behind a pore network, and the calcined body was then reaction-sintered at 1600C to form mullite. The samples had porosities of approximately 60%. Pore size and shape were altered by using different starch templates, and pore size was found to influence the stiffness and toughness. The ACM microstructure was varied along three parameters: total porosity, pore size, and needle size. Total porosity was found to dominate the mechanical behavior of ACM, while increases in needle and pore size increased the toughness at lower porosities. ACM was found to have much improved (˜130%) mechanical properties relative to its non-acicular counterpart at the same porosity. A second set of investigations studied the role of the intergranular glassy phase which wets the needle intersections of ACM. Removal of the glassy phase via an HF etch reduced the mechanical properties by ˜30%, highlighting the intergranular phase's importance to the enhanced mechanical properties of ACM. The composition of the glassy phase was altered by doping the ACM precursor with magnesium and neodymium. Magnesium doping resulted in ACM with greatly reduced fracture strength and toughness. Studies showed that the mechanical properties of the

  18. Spectroscopic characteristics of chromium doped mullite glass-ceramics

    SciTech Connect

    Wojtowicz, A.J.; Meng, W.; Lempicki, A.; Beall, G.H.; Hall, D.W.; Chin, T.C.

    1988-06-01

    Characteristics of chromium doped mullite ceramics are discussed with reference to possible laser applications. Dominant features are attributed to large and inherent spectroscopic inhomogeneity of mullite. The spectroscopic data are analyzed using a generalized McCumber theory. The peak stimulated emission cross section is 0.54 x 10/sup -20/ cm/sup 2/. This, together with preliminary single-pass measurements, indicate that gain for mullite is about 2.6 times smaller than gain for alexandrite.

  19. Development of fine diameter mullite fiber

    NASA Technical Reports Server (NTRS)

    Long, W. G.

    1974-01-01

    Results are presented of a program to develop and evaluate mullite fiber with a mean diameter under two microns. The two micron fiber is produced by a blowing process at room temperature from a low viscosity (10-25 poise) solution. The blown fiber was evaluated for dimensional stability in thermal cycling to 1371 C, and was equivalent to the 5 micron spun B and W mullite fiber. An additive study was conducted to evaluate substitutes for the boron. Three levels of chromium, lithium fluoride, and magnesium were added to the standard composition in place of boron and the fiber produced was evaluated for chemical and dimensional stability in thermal cycling to 1371 C. The magnesium was the most chemically stable, but the chrome additive imparted the best dimensional stability.

  20. Stability and phase evolution of mullite in reducing atmosphere

    SciTech Connect

    Naghizadeh, R. Golestani-fard, F.; Rezaie, H.R.

    2011-05-15

    The aim of this study is to investigate the stability of mullite and its phase evolution when heated at 1600-1650 deg. C in reducing atmosphere created by a carbon bed. The stoichiometric mullite (3Al{sub 2}O{sub 3}.2SiO{sub 2}) was synthesized by reacting the proper precursors at 1400 deg. C in air atmosphere. Samples containing the primary mullite and graphite or carbon were prepared by pressing the mix and heated at 1600-1650 deg. C. Products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the stoichiometric mullite could decompose to corundum and alumina-rich mullite. During firing under reducing atmosphere, the stoichiometric mullite became richer in Al{sup 3+} cations. The gaseous SiO compound was found to be released from the sample and reacting with C to form SiC phase. Comparison of general mullite solid solution (Al{sub 4+2x}Si{sub 2-2x}O{sub 10-x}) with alumina-rich mullite obtained from decomposition revealed that x would take different values depending on temperature and atmosphere. The ultimate decomposition product was found to be corundum. - Research Highlights: {yields} This method is a new route for investigation of thermochemical stability of stoichimetric mullite under reducing condition which have done by the authors. {yields} This research has got very good results for stability of mullite at different conditions. {yields} This work has also studied the mechanism of stability of mullite under reducing atmosphere.

  1. Mullite/Mo interfaces formed by Intrusion bonding

    SciTech Connect

    Bartolome, Jose F.; Diaz, Marcos; Moya, Jose S.; Saiz, Eduardo; Tomsia, Antoni P.

    2003-04-30

    The microstructure and strength of Mo/mullite interfaces formed by diffusion bonding at 1650 C has been analyzed. Interfacial metal-ceramic interlocking contributes to flexural strength of approx. 140 MPa as measured by 3 point bending. Saturation of mullite with MoO2 does not affect the interfacial strength.

  2. Development of CVD mullite coatings for Si-based ceramics

    NASA Astrophysics Data System (ADS)

    Auger, Michael Lawrence

    1999-09-01

    To raise fuel efficiencies, the next generation of engines and fuel systems must be lighter and operate at higher temperatures. Ceramic-based materials, which are considerably lighter than metals and can withstand working temperatures of up to 1400sp°C, have been targeted to replace traditional metal-based components. The materials used in combustion environments must also be capable of withstanding erosion and corrosion caused by combustion gases, particulates, and deposit-forming corrodants. With these demanding criteria, silicon-based ceramics are the leading candidate materials for high temperature engine and heat exchanger structural components. However, these materials are limited in gaseous environments and in the presence of molten salts since they form liquid silicates on exposed surfaces at temperatures as low as 800sp°C. Protective coatings that can withstand higher operating temperatures and corrosive atmospheres must be developed for silicon-based ceramics. Mullite (3Alsb2Osb3{*}2SiOsb2) was targeted as a potential coating material due to its unique ability to resist corrosion, retain its strength, resist creep, and avoid thermal shock failure at elevated temperatures. Several attempts to deposit mullite coatings by various processing methods have met with limited success and usually resulted in coatings that have had pores, cracks, poor adherence, and required thermal post-treatments. To overcome these deficiencies, the direct formation of chemically vapor deposited (CVD) mullite coatings has been developed. CVD is a high temperature atomistic deposition technique that results in dense, adherent crystalline coatings. The object of this dissertation was to further the understanding of the CVD mullite deposition process and resultant coating. The kinetics of CVD mullite deposition were investigated as a function of the following process parameters: temperature, pressure, and the deposition reactor system. An empirical kinetic model was developed

  3. Hot Hydrogen Exposure Degradation of the Strength of Mullite

    NASA Technical Reports Server (NTRS)

    Herbell, Thomas P.; Hull, David R.; Garg, Anita

    1996-01-01

    This study deals with the corrosion of near stoichiometric mullite (3Al2O3-2SiO2) by pure dry hydrogen gas. Exposure of the mullite samples was at temperatures of 1050 and 1250 C for times up to 500 hours. Preferential attack of the alumino-silicate glass present in the grain boundaries of the mullite occurred after 125 hours at 1250 C. Hydrogen scrubbing of the SiO2 from the glassy grain boundaries and the mullite grains yielded a porous alumina-rich surface. The room temperature strength increased after short exposure times at 1250 C (up to 125 hours), then decreased by 53 percent after exposure for 500 hours. At 1050 C, all exposure times (25 to 500 hours) decreased the strength. After 500 hours in hydrogen at 1050 C, the room temperature strength of mullite decreased 22 percent. We also observed a rapid 25 percent strength loss after short exposure times at 1050 C. This is attributed to the calcium/hydrogen assisted crystallization of the glassy, grain-boundary phase.

  4. Synthesis of mullite coatings by chemical vapor deposition

    SciTech Connect

    Mulpuri, R.P.; Auger, M.; Sarin, V.K.

    1996-08-01

    Formation of mullite on ceramic substrates via chemical vapor deposition was investigated. Mullite is a solid solution of Al{sub 2}O{sub 3} and SiO{sub 2} with a composition of 3Al{sub 2}O{sub 3}{circ}2SiO{sub 2}. Thermodynamic calculations performed on the AlCl{sub 3}-SiCl{sub 4}-CO{sub 2}-H{sub 2} system were used to construct equilibrium CVD phase diagrams. With the aid of these diagrams and consideration of kinetic rate limiting factors, initial process parameters were determined. Through process optimization, crystalline CVD mullite coatings have been successfully grown on SiC and Si{sub 3}N{sub 4} substrates. Results from the thermodynamic analysis, process optimization, and effect of various process parameters on deposition rate and coating morphology are discussed.

  5. Spectroscopic characteristics of chromium-doped mullite glass-ceramics

    SciTech Connect

    Wojtowicz, A.J.; Meng, W.; Lempicki, A.; Beall, G.H.; Hall, D.W.

    1988-06-01

    The chromium (3+) ion has been widely used as an optical activator in solid-state, tunable laser materials. High octahedral field-stabilization energy and resistance against both oxidation and reduction minimize the dependence of chromium (3+) on the solid-state host matrix. However, the high sensitivity of electronic structure on crystal field strength makes the appropriate choice of host the condition for success. Characteristics of chromium-doped mullite ceramics are discussed with reference to possible laser applications. Dominant features are attributed to large and inherent spectroscopic inhomogeneity of mullite. The spectroscopic data are analyzed using a generalized McCumber theory. The peak-stimulated emission cross section is 0.54 x 10 to the -20 sq cm. This together with preliminary single-pass measurements, indicate that gain for mullite is about 2.6 times smaller than gain for alexandrite.

  6. Mullite coatings for corrosion protection of silicon carbide

    SciTech Connect

    Mulpuri, R.; Sarin, V.K.

    1995-08-01

    SiC based ceramics have been identified as the leading candidate materials for elevated temperature applications in harsh oxidation/corrosion environments. It has been established that a protective coating can be effectively used to avoid problems with excessive oxidation and hot corrosion. However, to date, no coating configuration has been developed that can satisfy the stringent requirements imposed by such applications. Chemical Vapor Deposited (CVD) mullite coatings due to their desirable properties of toughness, corrosion resistance, and a good coefficient of thermal expansion match with SiC are being investigated as a potential candidate. Since mullite has never been successfully grown via CVD, the thermodynamics and kinetics of its formation were initially established and used as a guideline in determining the initial process conditions. Process optimization was carried out using an iterative process of theoretical analysis and experimental work coupled with characterization and testing. The results of theoretical analysis and the CVD formation characteristics of mullite are presented.

  7. Development of CVD Mullite Coatings for SiC Fibers

    SciTech Connect

    Sarin, V.K.; Varadarajan, S.

    2000-03-15

    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.

  8. An exploratory study of the microstructure of mullite fibers

    NASA Technical Reports Server (NTRS)

    Santoro, G. J.; Probst, H. B.; Buzek, B. C.

    1973-01-01

    Mullite fibers of three compositions, ranging from SiO2-rich to Al2O3-rich, were investigated by a number of transmission electron microscopy (TEM) techniques. The fibers were examined in the as-received condition and after subjecting them to thermal exposures as high as 142 C. The investigative techniques used included direct TEM of microtomed sections of mounted fibers and TEM of replicas of polished, chemically etched, and cathodically etched fibers. In addition, X-ray diffraction line broadening analyses was used for determining average crystallite size. A preliminary description of the microstructure of mullite fibers is given.

  9. 29Si and 27Al MAS NMR spectra of mullites from different kaolinites.

    PubMed

    He, Hongping; Guo, Jiugao; Zhu, Jianxi; Yuan, Peng; Hu, Cheng

    2004-04-01

    Mullites synthesized from four kaolinites with different random defect densities have been studied by 27Al and 29Si magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR) and X-ray diffraction (XRD). All these mullites show the same XRD pattern. However, 29Si and 27Al MAS NMR spectra reveal that the mullites derived from kaolinites with high defect densities, have a sillimanite-type Al/Si ordering scheme and are low in silica, whereas those mullites derived from kaolinites with low defect densities, consist of both sillimanite- and mullite-type Al/Si ordering schemes and are rich in silica. PMID:15084323

  10. Method for thermally spraying crack-free mullite coatings on ceramic-based substrates

    NASA Technical Reports Server (NTRS)

    Spitsberg, Irene T. (Inventor); Wang, Hongyu (Inventor); Heidorn, Raymond W. (Inventor)

    2001-01-01

    A process for depositing a mullite coating on a silicon-based material, such as those used to form articles exposed to high temperatures and including the hostile thermal environment of a gas turbine engine. The process is generally to thermally spray a mullite powder to form a mullite layer on a substrate, in which the thermal spraying process is performed so that the mullite powder absorbs a sufficient low level of energy from the thermal source to prevent evaporation of silica from the mullite powder. Processing includes deposition parameter adjustments or annealing to maintain or reestablish phase equilibrium in the mullite layer, so that through-thickness cracks in the mullite layer are avoided.

  11. Method for thermally spraying crack-free mullite coatings on ceramic-based substrates

    NASA Technical Reports Server (NTRS)

    Spitsberg, Irene T. (Inventor); Wang, Hongyu (Inventor); Heidorn, Raymond W. (Inventor)

    2000-01-01

    A process for depositing a mullite coating on a silicon-based material, such as those used to form articles exposed to high temperatures and including the hostile thermal environment of a gas turbine engine. The process is generally to thermally spray a mullite powder to form a mullite layer on a substrate, in which the thermal spraying process is performed so that the mullite powder absorbs a sufficient low level of energy from the thermal source to prevent evaporation of silica from the mullite powder. Processing includes deposition parameter adjustments or annealing to maintain or reestablish phase equilibrium in the mullite layer, so that through-thickness cracks in the mullite layer are avoided.

  12. Thermal cycling characteristics of plasma synthesized mullite films

    SciTech Connect

    Monteiro, O.R.; Hou, P.Y.; Brown, I.G.

    1997-12-01

    The authors have developed a plasma-based technique for the synthesis of mullite and mullite-like films on silicon carbide substrate material. The method, which they refer to as MePIIID (for Metal Plasma Immersion Ion Implantation and Deposition), uses two vacuum arc plasma sources and simultaneous pulse biasing of the substrate in a low pressure oxygen atmosphere. The Al:Si ratio can be controlled via the separate plasma guns, and the film adhesion, structure and morphology can be controlled via the ion energy which in turn is controlled by the pulse bias voltage. The films are amorphous as-deposited, and crystalline mullite is formed by subsequent annealing at 1000 C for 2 hours in air. Adhesion between the aluminum-silicon oxide film and the substrate increases after this first annealing. They have tested the behavior of films when subjected to repetitive thermal cycling between room temperature and 1100 C, and found that the films retain their adhesion and quality. Here they review the plasma synthesis technique and the characteristics of the mullite films prepared in this way, and summarize the status of the thermal cycling experiments.

  13. Mullite-corundum articles based on a phosphate binder

    SciTech Connect

    Zamyatin, S.R.; Tetyaeva, L.P.; Vashtan'yan, G.A.; Belogrudov, A.G.; Domrachev, N.A.

    1987-01-01

    The authors discuss the composition, crystallization, firing, production, and temperature-susceptible properties of a mullite-corundum refractory which incorporates a phosphate binder and is intended for use as a furnace liner. They use a combination of thermal analysis and mechanical testing to optimize the composition as well as its mechanical and heat-resistant properties and present results on its service life and its contribution to the increased thermal efficiency of furnaces in which it is being used.

  14. New generation of plasma-sprayed mullite coatings on silicon carbide

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Miller, Robert A.; Jacobson, Nathan S.

    1995-01-01

    Mullite is promising as a protective coating for silicon-based ceramics in aggressive high-temperature environments. Conventionally plasma-sprayed mullite on SiC tends to crack and debond on thermal cycling. It is shown that this behavior is due to the presence of amorphous mullite in the conventionally sprayed mullite. Heating the SiC substrate during the plasma spraying eliminated the amorphous phase and produced coatings with dramatically improved properties. The new coating exhibits excellent adherence and crack resistance under thermal cycling between room temperature and 1000 to 1400 C. Preliminary tests showed good resistance to Na2CO3-induced hot corrosion.

  15. Copper ions removal from water using functionalized carbon nanotubes–mullite composite as adsorbent

    SciTech Connect

    Tofighy, Maryam Ahmadzadeh; Mohammadi, Toraj

    2015-08-15

    Highlights: • CNTs–mullite composite was prepared via chemical vapor deposition (CVD) method. • The prepared composite was modified with concentrated nitric acid and chitosan. • The modified CNTs–mullite composites were used as novel adsorbents. • Copper ion removal from water by the prepared adsorbents was performed. • Langmuir and Freundlich isotherms and two kinetic models were applied to fit the experimental data. - Abstract: Carbon nanotubes–mullite composite was synthesized by direct growth of carbon nanotubes on mullite particles via chemical vapor deposition method using cyclohexanol and ferrocene as carbon precursor and catalyst, respectively. The carbon nanotubes–mullite composite was oxidized with concentrated nitric acid and functionalized with chitosan and then used as a novel adsorbent for copper ions removal from water. The results demonstrated that modification with concentrated nitric acid and chitosan improves copper ions adsorption capacity of the prepared composite, significantly. Langmuir and Freundlich isotherms and two kinetic models were applied to fit the experimental data. The carbon nanotubes growth on mullite particles to form the carbon nanotubes–mullite composite with further modification is an inherently safe approach for many promising environmental applications to avoid some concerns regarding environment, health and safety. It was found that the modified carbon nanotubes–mullite composite can be considered as an excellent adsorbent for copper ions removal from water.

  16. Effect of high temperature hydrogen exposure on the strength and microstructure of mullite

    NASA Technical Reports Server (NTRS)

    Herbell, Thomas P.; Hull, David; Hallum, Garry M.

    1990-01-01

    The corrosion of near stoichiometric mullite (3Al2O3-2SiO2) by pure dry hydrogen gas was studied at 1050 and 1250 C for times up to 500 hr. The hydrogen preferentially attacked the grain boundaries of the mullite where an aluminosilicate glass was present. Corrosion of the mullite grains was observed after 125 hr at 1250 C. The hydrogen reaction removed SiO2 from the glassy grain boundaries and the mullite grains resulting in a porous alumina rich surface. At 1250 C the strength increased after short exposure times (at least up to 125 hr) and decreased by 53 percent after 500 hr. At 1050 C, all exposure times (25 to 500 hr) decreased the strength. At 500 hr room temperature strength of mullite exposed to 1050 C was reduced by 22 percent. The strength reduction after short exposure times at 1050 C is attributed to crystallization of the grain boundary glass phase.

  17. Preparation and mechanism of nano mullite powders from kaolin via open hydrothermal process.

    PubMed

    Li, Jinhong; Tong, Lingxin; Wang, Xiang

    2014-05-01

    Nano mullite powders have been synthesized from calcined kaolin via open hydrothermal process. The powder product was characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM) with selected area electron diffraction (SAED) analysis. The results indicated that single phase puncheon-shaped nano mullite with about 140-360 nm in length and 50-80 nm in diameter is produced when synthesized in 4 mol/L NaOH solution at 100 degrees C for 4 h. The grain size of mullite decrease slightly with increasing reaction time from 0 h to 4 h. In addition, nuclear magnetic resonance (NMR) analysis confirms presence of Al3+ during the whole reaction process, which indicates that there is an absence of growth units of mullite in the open hydrothermal system and the mullite precursor mainly underwent a solution process during open hydrothermal treatment. PMID:24734655

  18. Development of fibrous monoliths from mullite, alumina, and zirconia powders

    SciTech Connect

    Polzin, B. J.; Cruse, T. A.; Singh, D.; Picciolo, J. J.; Tsaliagos, R. N.; Phelan, P. J.; Goretta, K. C.

    2000-06-29

    Fibrous monoliths (FMs) based on mullite combined with Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3}-stabilized ZrO{sub 2} have been produced. These FMs incorporate duplex cells in which compressive residual stresses were engineered into the surfaces of the cells. The residual stresses should increase average cell strength, which may allow them to achieve mechanical properties comparable to those of Si{sub 3}N{sub 4}/BN FMs. The expected residual stresses have been calculated, and data on sintering and thermal expansion have been gathered. Prototype FMs were produced and their microstructure examined.

  19. Development of low-thermal expansion mullite bodies

    NASA Technical Reports Server (NTRS)

    Leipold, M. H.; Sibold, J. D.

    1982-01-01

    A series of ceramic compositions based on variations in the crystal-glass ratio of a mullite body were developed. The thermal expansion of these compositions varies from 3.7 to 5.0 x 10 to the -6th/deg C to 800 C. The materials are particularly useful for applications involving silicon, in that an identical thermal expansion is available. The high-temperature creep data for the lower-expansion compositions are inferior as a result of their higher glass contents. Raw material sources and fabrication procedures for specific compositions are given.

  20. Silicon carbide whisker-zirconia reinforced mullite and alumina ceramics

    DOEpatents

    Becher, Paul F.; Tiegs, Terry N.

    1987-01-01

    The flexural strength and/or fracture toughness of SiC whisker-reinforced composites utilizing mullite or alumina as the matrix material for the composite are increased by the addition of zirconia in a monoclinic or tetragonal phase to the matrix. The zirconia addition also provides for a lower hot-pressing temperature and increases the flexural strength and/or fracture toughness of the SiC whisker-reinforced composites over SiC whisker-reinforced composites of the similar matrix materials reinforced with similar concentrations of SiC whiskers.

  1. Superstructure of Mullite-type KAl9O14

    PubMed Central

    2013-01-01

    Large whiskers of a new KAl9O14 polymorph with mullite-type structure were synthesized. The chemical composition of the crystals was confirmed by energy-dispersive X-ray spectroscopy, and the structure was determined using single-crystal X-ray diffraction. Nanosized twin domains and one-dimensional diffuse scattering were observed utilizing transmission electron microscopy. The compound crystallizes in space group P21/n (a = 8.1880(8), b = 7.6760(7), c = 8.7944(9) Å, β = 110.570(8)°, V = 517.50(9) Å3, Z = 2). Crystals of KAl9O14 exhibit a mullite-type structure with linear edge-sharing AlO6 octahedral chains connected with groups of two AlO4 tetrahedra and one AlO5 trigonal bipyramid. Additionally, disproportionation of KAl9O14 into K β-alumina and corundum was observed using in situ high-temperature optical microscopy and Raman spectroscopy. PMID:23503683

  2. Mullite+CAS Bond Coat for Environmental Barrier Coatings for Si-Based Ceramics

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Opila, Elizabeth J.; Gray, Hugh R. (Technical Monitor)

    2002-01-01

    Current environmental barrier coatings (EBCs) for silicon-based ceramics consist of a bond coat and a top coat. Mullite bond coat modified by adding low CTE glass ceramics, such as BSAS (xBaO.1xSrO.Al2O3.2SiO2) or CAS (CaO.Al2O3.2SiO2), was developed in the NASA Enabling Propulsion Materials (EPM) Program. EBCs based on mullite+CAS bond coat were characterized using high steam thermal cycling test and high steam isothermal thermogravemitry (TGA) at 1225 C - 13,000 C. The Mullite+CAS bond coat showed far superior durability compared to mullite bond coat, due to enhanced crack resistance. A BSAS top coat provided further improved durability compared to EBCs with a yttria-stabilized zirconia (YSZ) top coat. Still further improvement in the durability was achieved by adding a silicon bond coat between the mullite and the substrate. However, the silicon/mullite+CAS/BSAS EBC showed inferior long-term durability compared to the current state-of-the art EBC (silicon/mullite+BSAS/BSAS EBC), presumably due to the higher CAS-silica chemical reactivity.

  3. Production of continuous mullite fiber via sol-gel processing

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S.; Sparks, J. Scott; Esker, David C.

    1990-01-01

    The development of a continuous ceramic fiber which could be used in rocket engine and rocket boosters applications was investigated at the Marshall Space Flight Center. Methods of ceramic fiber production such as melt spinning, chemical vapor deposition, and precursor polymeric fiber decomposition are discussed and compared with sol-gel processing. The production of ceramics via the sol-gel method consists of two steps, hydrolysis and polycondensation, to form the preceramic, followed by consolidation into the glass or ceramic structure. The advantages of the sol-gel method include better homogeneity and purity, lower preparation temperature, and the ability to form unique compositions. The disadvantages are the high cost of raw materials, large shrinkage during drying and firing which can lead to cracks, and long processing times. Preparation procedures for aluminosilicate sol-gel and for continuous mullite fibers are described.

  4. Compressive Creep and Thermophysical Performance of Mullite Refractories

    SciTech Connect

    Hemrick, JG

    2002-04-01

    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.

  5. Vitre-graf Coating on Mullite. Low Cost Silicon Array Project: Large Area Sillicon Sheet Task

    NASA Technical Reports Server (NTRS)

    Rossi, R. C.

    1979-01-01

    The processing parameters of the Vitre-Graf coating for optimal performance and economy when applied to mullite and graphite as substrates were presented. A minor effort was also performed on slip-cast fused silica substractes.

  6. The ceramic brittleness of the pressed and sintered yttria zirconia-mullite-magnesia system

    NASA Astrophysics Data System (ADS)

    Hakim, Budi L.; Soepriyanto, Syoni; Korda, Akhmad A.; Sunendar, Bambang

    2015-09-01

    The brittleness behaviour of the pressed and sintered Yttria Zirconia-Mullite-Magnesia system has been studied. Specifically, the brittleness index represents a correlation of material properties for predicting mechanical properties such as for the characterization of machinability, wear or erosion resistance. The brittleness index as well as fracture toughness were obtained from indentation testing of the Vickers hardness. In this study, the fracture toughness considered the crack extension mechanism to accommodate Palmqvist crack criteria for the measured data. The additional of Mullite at amount of 15% into 3Y-TZP system significantly reduces the brittleness index while compared to pure Mullite system up to 69%. In the other hand, the additional Mullite 15% by weight into 3Y-TZP system proved an increase of fracture toughness value up to 138% than pure 3Y-TZP system

  7. Corrosion protection of SiC-based ceramics with CVD mullite coatings

    SciTech Connect

    Auger, M.L.; Sarin, V.K.

    1997-12-01

    For the first time, crystalline mullite coatings have been chemically vapor deposited on SiC substrates to enhance its corrosion and 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.

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

    SciTech Connect

    Auger, M.; Hou, P.; Sengupta, A.; Basu, S.; Sarin, V.

    1998-05-01

    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.

  9. Porous acicular mullite obtained by controlled oxidation of waste molybdenum disilicide

    SciTech Connect

    Bučevac, Dušan; Dapčević, Aleksandra; Maksimović, Vesna

    2014-02-01

    Highlights: • Waste MoSi{sub 2} heating elements were used as starting material for fabrication of porous acicular mullite. • Calcined MoSi{sub 2} powder was source of SiO{sub 2} and pore former at the same time. • Porous acicular mullite is promising material for filtration of diesel engine exhaust. • Samples with decent mechanical integrity and porosity of more than 60% were fabricated. - Abstract: Porous acicular mullite was fabricated by using waste MoSi{sub 2} heating element and Al{sub 2}O{sub 3}. Careful calcination of the pulverized heating element led to the formation of a mixture of MoO{sub 3} and amorphous SiO{sub 2}. This mixture was employed as both SiO{sub 2} precursor and pore former. The oxidation of MoSi{sub 2} and mullite formation were studied. The effect of fabrication temperature on phase composition, porosity, grain morphology, and compressive strength of sintered mullite was examined. Pure mullite with porosity of more than 60% and compressive strength of ∼20 MPa was obtained at temperature as low as 1300 °C. The microstructure consisted of elongated, rectangular, prism-like grains which are known to be effective in filtration of diesel engine exhaust. The increase in sintering temperature caused the change of grain morphology and reduction in compressive strength.

  10. Deposition of mullite and mullite-like coatings on silicon carbide by dual-source metal plasma immersion. Topical report, October 1995--September 1996

    SciTech Connect

    Brown, I.G.; Monteiro, O.R.

    1997-04-01

    Mullite and mullite-like coatings on silicon carbide have been produced by a Metal Plasma Immersion Ion Implantation and Deposition (Mepiiid) technique based on two cathodic vacuum arc sources and concurrent pulse biasing of the substrate in an oxygen atmosphere. The deposition was carried out at oxygen partial pressures of between 0.66 and 3.33 Pa. The Al:Si ratio in the films varied from 1:1 to 8:1 and was controlled by varying the pulse duration of the separate plasma guns. High bias voltage was used early in the deposition process in order to produce atomic mixing at the film-substrate interface, while lower bias voltage was used later in the deposition; low ion energy allows control of the physical properties of the film as well as faster deposition rates. The as-deposited films were amorphous, and crystalline mullite was formed by subsequent annealing at 1,100 C for 2 hours in air. Strong adhesion between the mullite and the SiC was achieved, in some cases exceeding the 70 MPa instrumental limit of the pull-tester.

  11. Recycling of fly ash for preparing porous mullite membrane supports with titania addition.

    PubMed

    Dong, Yingchao; Hampshire, Stuart; Zhou, Jian-er; Lin, Bin; Ji, Zhanlin; Zhang, Xiaozhen; Meng, Guangyao

    2010-08-15

    In order to effectively utilize industrial waste fly ash, porous mullite ceramic membrane supports were prepared from fly ash and calcined bauxite with chemically pure titania as sintering additive. The effects of TiO(2) on the sintering behaviors and main properties of porous mullite were studied in detail. Due to the addition of titania, the sintering of the flyash-based mullite was inhibited at low temperatures, but effectively improved at high temperatures, the latter is suitable for preparing porous mullite membrane supports by incomplete sintering. Titania entered into liquid glassy phase with low high-temperature viscosity during sintering, resulting in the improvement of sintering activity, as well as the lowering of secondary mullitization temperature (where 2.0% titania). Between 1300 and 1500 degrees C, with increasing titania content, the samples exhibit increased trends in both linear shrinkage percent and bulk density, but a slightly decreased trend in open porosity, at all sintering temperatures. At 1300-1500 degrees C, the samples sintered at 1450 degrees C for 2h exhibit the lowest shrinkage and bulk density, as well as the highest open porosities in the investigated titania content range of 0-6.0 wt.%. Also, with increasing titania content, the pore size decreases slightly but the three-point flexural strength increases gradually at 1450 degrees C. PMID:20452727

  12. FUNCTIONALLY GRADED ALUMINA/MULLITE COATINGS FOR PROTECTION OF SILICON CARBIDE CERAMIC COMPONENTS FROM CORROSION

    SciTech Connect

    Prof. Stratis V. Sotirchos

    2001-02-01

    The main objective of this research project was 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. Since alumina has excellent resistance to corrosion but coefficient than silicon carbide, the key idea of this project has been to develop graded coatings with composition varying smoothly along their thickness between an inner (base) layer of mullite in contact with the silicon carbide component and an outer layer of pure alumina, which would function as the actual protective coating of the component. (Mullite presents very good adhesion towards silicon carbide and has thermal expansion coefficient very close to that of the latter.)

  13. Environment-oriented low-cost porous mullite ceramic membrane supports fabricated from coal gangue and bauxite.

    PubMed

    Lü, Qikai; Dong, Xinfa; Zhu, Zhiwen; Dong, Yingchao

    2014-05-30

    Porous mullite ceramic supports for filtration membrane were successfully fabricated via recycling of coal gangue and bauxite at sintering temperatures from 1100 to 1500°C with corn starch as pore-forming agent. The dynamic sintering behaviors, phase evolution, shrinkage, porosity and pore size, gas permeation flux, microstructure and mechanical property were systematically studied. A unique volume-expansion stage was observed at increased temperatures from 1276 to 1481°C caused by a mullitization-crystal-growth process. During this stage, open porosity increases and pore size distributions broaden, which result in a maximum of nitrogen gas flux at 1400°C. The X-ray diffraction results reveal that secondary mullitization took place from 1100°C and the major phase is mullite with a content of ∼84.7wt.% at 1400°C. SEM images show that the as-fabricated mullite supports have a porous microstructure composed of sintered glassy particles embedded with inter-locked mullite crystals, which grew gradually with increasing temperature from rod-like into blocky-like morphologies. To obtain mullite membrane supports with sufficient porosity and acceptable mechanical strength, the relationship between porosity and mechanical strength was investigated, which was fitted using a parabolic equation. PMID:24727016

  14. Synthesis and characterization of transition metal-mullite catalysts for nitric oxide (NO) oxidation

    NASA Astrophysics Data System (ADS)

    Thampy, Sampreetha

    AMn2O5 (A = Pr, Sm, Gd, Y, Bi), and (Y, Bi)FeMnO5 mullite prepared by coprecipitation-calcination method are investigated as catalysts for NO oxidation. The effect of precursor stoichiometry, calcination temperature, and coprecipitation pH on phase, specific surface area (SSA) and NO chemisorption are studied. The precursor stoichiometry controlled the oxide phase (mullite vs. perovskite) obtained. In comparison, when the calcination temperature is increased from 750 ºC to 1000 ºC, a tradeoff is observed, where purity of mullite phase increased from 73 % to 100 % but SSA decreased from 30 m2/g to 5 m2/g. Formation of crystalline SmMn2O5 is found to be weakly dependent on pH whereas SSA monotonically increased from 13 m2/g at pH 8.1 to 27 m2/g at pH 13. A strong correlation between NO uptake volume and SSA is found. The highest SSA value (27 m2/g) being associated to a sample showing the highest NO uptake (104 micromol/g). These results suggest that the SSA is the key contributor to higher catalytic performance of TM-mullites.

  15. Neutron-diffraction study up to 1600 °C of 3:2 mullite

    NASA Astrophysics Data System (ADS)

    Brunauer, G.; Frey, F.; Boysen, H.; Schneider, H.; Fischer, P.; Hansen, Th.; Többens, D.; Ehrenberg, H.

    Neutron-diffraction studies were carried out on pure and Cr-doped 3:2 (`sinter') mullite. To learn about structure-property relationships of this refractory material, thermal expansion coefficients and structural parameters were determined by in situ high-temperature investigations. Neutron experiments were performed at the powder diffractometers D2B/ILL, E9/HMI, and HRPT/PSI. All data gave a rather uniform picture of the thermal expansion coefficients: a linear behaviour below 1000 °C and significantly increased (mean) expansion between 1000 and 1600 °C. There is a marked anisotropy of the highest values along the b-axis of the orthorhombic mullite structure. Concerning the structural parameters and the derived bond lengths, there is an expansion of the Al1O6 octahedra, whereas the cross-linking Al2SiO4 tetrahedra stay more or less rigid, but may slightly rotate. Thus a major expansion along the b direction may be qualitatively understood. A structural discussion, however, is affected by the presence of disorder in mullite, in particular in Cr-doped mullite, as it is also reflected by the presence of a modulated diffuse background in the powder patterns.

  16. Possibility of decreasing the activation energy of resistivity of mullite by doping with nickel ion

    NASA Astrophysics Data System (ADS)

    Roy, D.; Das, S.; Nandy, P.

    2012-12-01

    Monophasic mullite samples doped with 0.002 M, 0.02 M, 0.1 M, 0.15 M and 0.2 M of NiCl2 were prepared via sol-gel technique. The prepared gels were dried, grinded, pressed into pellets and sintered at 400 °C, 800 °C, 1000 °C and 1300 °C. The electrical resistivity and activation energy of the composites have been measured and the variation of resistivity with concentration of the nickel ion doping has been investigated. The resistivity decreases with the concentration of nickel ions. X-ray analysis confirms the presence of Ni2+ ions in mullite. The Ni2+ ion, which substitutes Al3+ ion in the octahedral site of mullite structure, can be considered as an efficient factor in reducing the resistivity. The mullite unit cell parameters suggest predominant incorporation of NiCl2 in a glassy phase. The lowest activation energy of resistivity ( E act ) that was achieved is 1.22 eV at 0.02 M.

  17. CVD mullite coatings in high-temperature, high-pressure air-H{sub 2}O[Chemical Vapor Deposition

    SciTech Connect

    Haynes, J.A.; Lance, M.J.; Cooley, K.M.; Ferber, M.K.; Lowden, R.A.; Stinton, D.P.

    2000-03-01

    Crystalline mullite was deposited by chemical vapor deposition (CVD) onto SiC/SiC composites overlaid with CVD SiC. Specimens were exposed to isothermal oxidation tests in high-pressure air +H{sub 2}O at 1,200 C. Unprotected CVD SiC formed silica scales with a dense amorphous inner layer and a thick, porous, outer layer of cristobalite. Thin coatings ({approximately}2{mu}m) of dense CVD mullite effectively suppressed the rapid oxidation of CVD SiC. No microstructural evidence of mullite volatility was observed under these temperature, pressure, and low-flow-rate conditions. Results of this preliminary study indicate that dense, crystalline, high-purity CVD mullite is stable and protective in low-velocity, high-pressure, moisture-containing environments.

  18. In situ formation of sintered cordierite–mullite nano–micro composites by utilizing of waste silica fume

    SciTech Connect

    Khattab, R.M.; EL-Rafei, A.M.; Zawrah, M.F.

    2012-09-15

    Highlights: ► We succeeded to obtain in situ formed sintered cordierite–mullite nano–macro composites from waste and pure materials at 1400 °C. ► Their sinterability was greatly dependent on both firing temperature and composition. ► XRD patterns showed that the optimum temperature required for formation of sintered cordierite–mullite nano–macro composites was achieved at 1400 °C. ► The batch containing 70 wt.% cordierite and 30 wt.% mullite exhibited the best properties. ► Microstructures of the densified composites were composed of nano–macro cordierite–mullite structures. -- Abstract: This study aims at in situ formation of sintered cordierite–mullite nano–macro composites having high technological properties using waste silica fume, calcined ball clay, calcined alumina, and magnesia as starting materials. The starting materials were mixed in different ratios to obtain different cordierite–mullite composite batches in which the cordierite contents ranged from 50 to 100 wt.%. The batches were uni-axially pressed at 100 MPa and sintered at 1350, 1400 and 1450 °C to select the optimum temperature required for cordierite–mullite nano–macro composites formation. The formed phases were identified by X-ray diffraction (XRD) pattern. The sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined. The microstructure of composites has been investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered batches was evaluated. The result revealed that the cordierite–mullite nano–macro composites were in-situ formed at 1400 °C. The batch containing 70 wt.% cordierite showed good physical and mechanical properties.

  19. Powder Injection Molding of Ceria-Stabilized, Zirconia-Toughened Mullite Parts for UAV Engine Components

    NASA Astrophysics Data System (ADS)

    Martin, Renee; Vick, Michael; Enneti, Ravi K.; Atre, Sundar V.

    2013-11-01

    Powder injection molding (PIM) of ceria-stabilized, zirconia-toughened mullite composites were investigated in the present article with the goal of obtaining performance enhancement in complex geometries for energy and transportation applications. A powder-polymer mixture (feedstock) was developed and characterized to determine its suitability for fabricating complex components using the PIM process. Test specimens were injection molded and subsequently debound and sintered. The sintered properties indicated suitable properties for engine component applications used in unmanned aerial vehicles (UAVs). The measured feedstock properties were used in computer simulations to assess the mold-filling behavior for a miniature turbine stator. The results from the measurements of rheological and thermal properties of the feedstock combined with the sintered properties of the ceria-stabilized, zirconia-toughened mullite strongly indicate the potential for enhancing the performance of complex geometries used in demanding operating conditions in UAV engines.

  20. FUNCTIONALLY GRADED ALUMINA/MULLITE COATINGS FOR PROTECTION OF SILICON CARBIDE CERAMIC COMPONENTS FROM CORROSION

    SciTech Connect

    1997-10-01

    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 CO{sub 2} and H{sub 2} 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, we continued the work on the development and construction of the thermogravimetric chemical vapor deposition system that we intend to employ for studying the deposition of alumina, silica, and aluminosilicates (such as mullite) from mixtures of metal chlorides in H{sub 2} and CO{sub 2}. Specifically, we worked on the development of the tubular flow reactor that will be used for producing aluminum chloride for delivery to the chemical vapor deposition system and of the vapor and gas supply system. Various problems arising from condensation of aluminum chlorides in some sections of the supply line were resolved, and we expect to perform experiments using mixtures containing AlCl{sub 3} in the next reporting period. Preliminary experiments on the

  1. An historical mullite fiber-reinforced ceramic composite: Characterization of the wootz' crucible refractory

    SciTech Connect

    Lowe, T.L. ); Merk, N.; Thomas, G. )

    1990-10-01

    Since at least the sixteenth century, the wootz'' ultra-high carbon white cast-iron ingot was produced in India by melting or carburising iron in a crucible. This ingot was forced into sword blades of so-called Damascus steel. The charged crucible was fired in a long (24-hour) single cycle at high temperature (1150-1250{degree}C) in a strongly reducing atmosphere. Raw materials for the refractory vessel are clay and coked'' rice husks. At high temperatures, two phases reinforce the glassy matrix: cristobalite relics of rice husks and a network of mullite crystals. This paper characterizes the microstructure and chemistry of the mullite network in the glassy matrix by means of a combination of techniques: optical microscopy, XRD, SEM, TEM and EDS, and HREM. 13 refs., 11 figs.

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

    SciTech Connect

    Sotirchos, S.V.

    1997-04-01

    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.

  3. Corrosion protection of SiC-based ceramics with CVD mullite coatings

    SciTech Connect

    Sarin, V.; Mulpuri, R.; Auger, M.

    1996-04-20

    SiC based ceramics have been identified as the leading candidate materials for elevated temperature applications in harsh oxidation/corrosion environments. It has been established that a protective coating can be effectively used to avoid problems with excessive oxidation and hot corrosion. However, to date, no coating configuration has been developed that can withstand the rigorous requirements imposed by such applications. Chemical vapor deposited (CVD) mullite coatings due to their desirable properties of toughness, corrosion resistance, and good coefficient of thermal expansion match with SiC are being developed as a potential solution. Formation of mullite on ceramic substrates via chemical vapor deposition was investigated. Thermodynamic calculations performed on the AlCl{sub 3}- SiCl{sub 4}-CO{sub 2}-H{sub 2} system were used to construct equilibrium CVD phase diagrams. Through process optimization, crystalline CVD mullite coatings have been successfully grown on SiC and Si{sub 3}N{sub 4} substrates. Results from the thermodynamic analysis, process optimization, and effect of various process parameters on deposition rate and coating morphology are discussed.

  4. Key Durability Issues with Mullite-Based Environmental Barrier Coatings for Si-Based Ceramics

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.

    1999-01-01

    Plasma-sprayed mullite (3Al2O3 central dot 2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon-based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface, Thus modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

  5. Key Durability Issues with Mullite-Based Environmental Barrier Coatings for Si-Based Ceramics

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.

    2000-01-01

    Plasma-sprayed mullite (3Al2O3.2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon -based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface. Thus the modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while a weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause a premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

  6. Performance of a mullite reusable surface insulation system in a hypersonic stream

    NASA Technical Reports Server (NTRS)

    Hunt, L. R.

    1976-01-01

    The thermal and structural performance of a large panel of mullite reusable surface insulation (RSI) tiles was determined by a series of aerothermal tests in the Langley 8-foot high-temperature structures tunnel. The test panel was designed to represent a portion of the surface structure on a space shuttle orbiter fuselage along a 1,150 K isotherm with the mullite tile system bonded directly to the primary structure. Aerothermal tests were conducted at a free-stream Mach number of 6.7, a total temperature of 1,880 K, a unit Reynolds number of 4.6 million per meter, and dynamic pressure of 62 kPa. The thermal response of the mullite tile was as predicted, and the bond-line temperature did not exceed the design level of 570 K during a typical entry-heat cycle. Geometric irregularities of the tile gaps affected the tile edge temperatures when exposed to hypersonic flow. The tile coating demonstrated good toughness to particle impacts, but the coating cracked and flaked with thermal cycles. The gap filler of woven silica fibers appeared to hinder flow penetration into the gaps and withstood the flow shear of the present tests.

  7. Characterisation of mullite - ZrO2 ceramics prepared by various methods

    NASA Astrophysics Data System (ADS)

    Sedmale, G.; Sperberga, I.; Hmelov, A.; Steins, I.

    2011-10-01

    Mullite - ZrO2 ceramics was sintered from variously prepared powder mixtures -different time milled and hydrothermal synthesized. As sintering aid 8 wt. % illite clay for one part of starting mixtures was added. Two sintering routes was applied for consolidation of powder - spark plasma sintering (SPS) technique and conventional sintering reactions in air. It is shown that the structure of sintered samples for SPS was completed at 1250°C and by conventional - at 1300°C. The developed microstructure both conventional and SPS can be characterized by mullite matrix with evenly distributed ZrO2 grains. For conventionally prepared and sintered samples corundum and ZrO2 tetragonal grains are observed, but for SPS dominates ZrO2 cubic. The microstructure of ceramic samples from hydrothermal synthesized powders and consolidated by SPS is amorphous like, with xenomorfic crystals of mullite and inclusions of ZrO2 cubic grains. It is stated that additive of illite clay promotes the densification. At conventional sintering clay prevents the transformation of ZrO2 tetragonal to ZrO2 monoclinic by cooling of samples, but for SPS promotes formation of ZrO2 cubic. SPS sintered samples processed from conventionally milled powder mixture are characterized by pressure strength.

  8. Mullite Plasma Spraying for In Situ Repair of Cracks in Mullite Refractories: Simultaneous Optimization of Porosity and Thickness by Statistical Design of Experiments

    NASA Astrophysics Data System (ADS)

    Schrijnemakers, A.; Francq, B. G.; Cloots, R.; Vertruyen, B.; Boschini, F.

    2013-10-01

    We report a laboratory-scale study about the suitability of the plasma spraying process for "in situ" repair of cracks in mullite refractories of industrial furnaces. The "design of experiments" approach is used to investigate how the coating porosity and thickness are influenced by six experimental parameters. Arc current, secondary gas (H2) flow rate, and stand-off distance are the most significant parameters for both responses. Several interaction terms also affect significantly the thickness response. The validity of the model equations is discussed both from a statistical point of view and regarding the physical credibility of the main model terms. Additional experiments confirm that the measured properties lie into the prediction intervals provided by the model. Using a set of parameters optimized for minimal porosity and high thickness (relevant for the crack repair application), coatings with 6% porosity and 1070 μm thickness can be prepared reproducibly.

  9. Crystallisation in apatite-mullite glass-ceramics as a function of fluorine content

    NASA Astrophysics Data System (ADS)

    Stanton, Kenneth T.; Hill, Robert G.

    2005-02-01

    Apatite-mullite glass-ceramics are materials prepared by the controlled heat-induced devitrification of glasses of suitable composition and are under investigation for applications in dentistry and orthopaedics. The glasses used here are based on a system with the composition 1.5(5- x)SiO 2·(5- x)Al 2O 3·1.5P 2O 5·(5- x)CaO· xCaF 2. The amount of fluorine in the glasses was varied to investigate the crystallisation behaviour as a function of both fluorine content and temperature. The resultant crystalline phases are fluorapatite [Ca 10(PO 4) 6F 2], mullite [Al 6Si 2O 13] and in some cases, anorthite [CaAl 2Si 2O 8]. Crystal phases were identified using X-ray diffraction (XRD) from both the surface and the bulk of heat-treated monolithic samples and scanning electron microscopy (SEM) was used to image the crystal phase morphologies. Crystallisation characteristics varied widely in terms of apparent nucleation mechanism, crystal phases formed and microstructure. In general, glasses with higher fluorine content devitrified more readily to fluorapatite (FAp) with a higher nucleation density and for glasses with an intermediate to low fluorine content there tended to be an interdependence between FAp and mullite crystallisation. A greater tendency towards anorthite formation, especially at surfaces, was observed for glasses with lower fluorine contents. Furthermore, on decreasing the fluorine content, glasses tended to crystallise by formation of FAp spherulites with increasing diameter and with greater crystal aspect ratio.

  10. Upper Temperature Limit of Environmental Barrier Coatings Based on Mullite and BSAS

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Fox, Dennis S.; Eldridge, Jeffrey I.; Zhu, Dongming; Bansal, Narottam P.; Miller, Robert A.; Robinson, Raymond C.

    2002-01-01

    Current state-of-the-art environmental barrier coatings (EBCs) for Si-based ceramics consist of three layers: a silicon bond coat, an intermediate mullite (3Al2O3-2SiO2) or mullite + BSAS (1-xBaO-xSrO-Al2O3-2SiO2) layer, and a BSAS top coat. Areas of concern for long-term durability are environmental durability, chemical compatibility, silica volatility, phase stability, and thermal conductivity. Variants of this family of EBCs were applied to monolithic SiC and melt infiltrated SiC/SiC composites. Reaction between BSAS and silica results in low melting (approx. 1300 C) glasses at T > 1400 C, which can cause the spallation of the EBC. At temperatures greater than 1400 C, the BSAS top coat also degrades by formation of a porous structure, and it suffers significant recession via silica volatilization in water vapor-containing atmospheres. All of these degradation mechanisms can be EBC life-limiting factors. BSAS undergoes a very sluggish phase transformation (hexagonal celsian to monoclinic celsian), the implications of which are not fully understood at this point. There was evidence of rapid sintering at temperatures as low as 1300 C, as inferred from the sharp increase in thermal conductivity.

  11. Monolithic diphasic gels of mullite by sol-gel process under ultrasound stimulation.

    PubMed

    Vollet, D R; Donatti, D A; Domingos, R N; de Oliveira, I

    1998-06-01

    Diphasic gel in the mullite composition was prepared from a colloidal sol of boehmite mixed with a hydrolyzed tetraethoxisilane (TEOS) solution. The boehmite sol was obtained by peptization of a poorly crystallized or very small mean crystallite size (approximately 34 A) precipitate, resulting from the reaction between solutions of aluminum sulfate and sodium hydroxide. Ultrasound was utilized in the processes of the TEOS hydrolysis and the boehmite peptization, and also for complete homogenization of the mixture to gel. The wet gel is almost clear and monolithic. The gel transparency is lost on drying, when syneresis has ended, so that the interlinked pore structure starts to empty and is recovered upon water re-absorption. Cracking closely accompanies this critical drying process. Differential thermal analysis (DTA) and X-ray diffraction (XRD) show that the solid structure of the gel is composed of an amorphous silica phase, as a matrix, and a colloidal sized crystalline phase of boehmite. Upon heat treatment, the boehmite phase within the gel closely follows the same transition sequence as in pure alumina shifted towards higher temperatures. Orthorhombic mullite formation was detected at 1300 degrees C. PMID:11270341

  12. FUNCTIONALLY GRADED ALUMINA/MULLITE COATINGS FOR PROTECTION OF SILICON CARBIDE CERAMIC COMPONENTS FROM CORROSION

    SciTech Connect

    1998-03-01

    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 CO{sub 2} and H{sub 2} 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 reporting period, the construction and development of the chemical vapor deposition system was completed, and experiments were conducted on the deposition of alumina, silica, and aluminosilicates (such as mullite) from mixtures of AlCl{sub 3} and CH{sub 3}SiCl{sub 3} in CO{sub 2} and H{sub 2}. Work was mainly done on the investigation of the effects of the reaction temperature on the deposition kinetics. It was found that the temperature had a positive effect on the single oxides deposition rates and the codeposition rate. The apparent activation energy values extracted from the deposition rate vs. temperature curves in the high temperature region were similar for the three deposition processes, having a value around 20 kcal/mol. The codeposition rates were higher, by a

  13. Fluorapatite-mullite glass sputter coated Ti6Al4V for biomedical applications.

    PubMed

    Bibby, J K; Bubb, N L; Wood, D J; Mummery, P M

    2005-05-01

    A number of bioactive ceramics have been researched since the development of Bioglass in the 1970's. Fluorapatite mullite has been developed from the dental glass-ceramics used for more general hard tissue replacement. Being brittle in nature, glass-ceramics are currently used mainly as coatings. This paper shows that fluorapatite glass LG112 can be used as a sputtered glass coating on roughened surfaces of Ti6Al4V for possible future use for medical implants. An AFM was used to measure the roughness of the surface before and after coating to determine the change in the topography due to the coating process as this greatly affects cell attachment. The sputter coating partially filled in the artificially roughened surface, changing the prepared topography. Osteoblasts have been successfully grown on the surface of these coatings, showing biocompatibility with bone tissue and therefore potential use in hard tissue repair. PMID:15875245

  14. Changes on electrical and structural properties of polyaniline and polypyrrol by mullite doping

    NASA Astrophysics Data System (ADS)

    González, C. P.; Montaño, A. M.; Estrada, S. E.; Ortiz, C. A.

    2016-02-01

    In this work, the effect of mullite dopant (mull) on the structural and electrical properties of two conductive polymers: polyaniline (PAni) and polypyrrole (PPy), which have great interest in science and materials engineering, has been evaluated. Doped polymers were synthesized with different contents of mineral and at two polymerization times (tP) by an in situ chemical synthesis in acidic aqueous solution and using Ammonium Persulfate (APS) as the reaction initiator. Structural characterization was performed by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The conductivity values (σac) were estimated from Electrochemical Impedance Spectroscopy (EIS). It was found that, at concentrations of work, were obtained higher values σac of conductivity at the highest concentration of the mineral, however, in some compounds the conductivity decreased. The variations in conductivity were attributed to PC-dopant interactions.

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

    SciTech Connect

    PROF. STRATIS V. SOTIRCHOS

    1998-10-01

    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

  16. Prediction of Service Life of Cordierite-Mullite Refractory Materials by Non-Destructive Methods

    NASA Astrophysics Data System (ADS)

    Boccaccini, D. N.; Kamseu, Elie; Volkov-Husoviæ, T. D.; Cannio, M.; Romagnoli, M.; Veronesi, P.; Dlouhy, I.; Boccaccini, A. R.; Leonelli, C.

    2008-02-01

    Ultrasonic pulse velocity testing was used to perform non-destructive quality control of refractory plates used as substrates in fast firing of porcelain whitewares. The measurement of the ultrasonic velocity was used to asses the presence of internal voids or cracks originated from the manufacturing procedure. Image analysis was used to predict thermal stability of the refractory materials. Two cordierite-mullite compositions were investigated that are characterized by different microstructure morphologies and crack propagation behaviour. A brief discussion about the correlation between microstructure, crack propagation behaviour and thermal shock resistance is presented. Moreover, empirical models were developed to predict the service life of refractory plates from measured values of ultrasonic velocities in plates in the as-received state.

  17. Prediction of Service Life of Cordierite-Mullite Refractory Materials by Non-Destructive Methods

    SciTech Connect

    Boccaccini, D. N.; Kamseu, Elie; Cannio, M.; Romagnoli, M.; Veronesi, P.; Leonelli, C.; Volkov-Husoviae, T. D.; Dlouhy, I.; Boccaccini, A. R.

    2008-02-15

    Ultrasonic pulse velocity testing was used to perform non-destructive quality control of refractory plates used as substrates in fast firing of porcelain whitewares. The measurement of the ultrasonic velocity was used to asses the presence of internal voids or cracks originated from the manufacturing procedure. Image analysis was used to predict thermal stability of the refractory materials. Two cordierite-mullite compositions were investigated that are characterized by different microstructure morphologies and crack propagation behaviour. A brief discussion about the correlation between microstructure, crack propagation behaviour and thermal shock resistance is presented. Moreover, empirical models were developed to predict the service life of refractory plates from measured values of ultrasonic velocities in plates in the as-received state.

  18. Parametric Appraisal of Slurry-Sprayed Mullite Coatings for Coating Thickness

    NASA Astrophysics Data System (ADS)

    Verma, R.; Suri, N. M.; Kant, S.

    2016-07-01

    The slurry spray technique (SST) has been employed to deposit mullite-based coatings on ASTM 1018 low-carbon steel substrate for environmental barrier coating applications. A Taguchi L18 orthogonal array is adopted for optimization of the identified process variables and material parameters, namely stamping pressure, fly-ash content, and sintering additive, time, and temperature. The measured thickness of the produced coatings was chosen as the response characteristic for the present study. The optimum values of the process variables were predicted by employing analysis of variance based on raw data and the signal-to-noise (S/N) ratio. Based on analysis of the experimental results, the effect of each parameter level on the coating thickness is discussed. It is observed that the sintering temperature had a strong influence on the maximum coating thickness of the slurry-sprayed coating. The as-sprayed coatings fabricated using SST demonstrated splat morphology with continuous interface, suggesting good adherence to the substrate.

  19. Constraining 17O and 27Al NMR spectra of high-pressure crystals and glasses: New data for jadeite, pyrope, grossular, and mullite

    USGS Publications Warehouse

    Kelsey, K.E.; Stebbins, J.F.; Du, L.-S.; Hankins, B.

    2007-01-01

    The 17O NMR spectra of glasses quenched from melts at high pressure are often difficult to interpret due to overlapping peaks and lack of crystalline model compounds. High-pressure aluminosilicate glasses often contain significant amounts of [5]Al and [6]Al, thus these high-pressure glasses must contain oxygen bonded to high-coordinated aluminum. The 17O NMR parameters for the minerals jadeite, pyrope, grossular, and mullite are presented to assist interpretation of glass spectra and to help test quantum chemical calculations. The 17O NMR parameters for jadeite and grossular support previous peak assignments of oxygen bonded to Si and high-coordinated Al in high-pressure glasses as well as quantum chemical calculations. The oxygen tricluster in mullite is very similar to the previously observed tricluster in grossite (CaAl4 O7) and suspected triclusters in glasses. We also present 27Al NMR spectra for pyrope, grossular, and mullite.

  20. Development of a zirconia-mullite based ceramic for recuperator applications

    SciTech Connect

    Gonzalez, J.M. )

    1992-12-01

    GTE Products Corporation developed a compact ceramic high temperature recuperator for recovering heat from relatively clean exhaust gases at temperatures up to 2500F. The DOE program allowed GTE to improve the technical and economic characteristics of the recuperator and stimulate industrial acceptance of the recuperator as an energy-saving technology. From January 1981 to December 1984, 561 recuperators were installed by GTE on new or retrofitted furnaces. With over 1200 units sold commercially between 1981 and 1990, GTE has documented the effect (long and short term) of corrosive attack from alkalies and lead. One objective of this contract was to develop Z-1000 a zirconia-mullite mixed oxide ceramic for use in ceramic recuperator applications susceptible to corrosion. To first and second pass of the ceramic recuperator would utilize the current cordierite-mixed-oxide ceramic. A Z-1000 matrix element would be used in the preheated air side's third pass (exhaust inlet). Thermal stresses on Z-1000 cross flow module could be minimized by selecting appropriate heat transfer surface areas for each pass. A large surface area for first and second pass (cordierite section) could provide for sufficient heat transfer for 50% effectiveness. A surface area that generates minimal heat transfer in the third pass (Z-1000) section is envisioned. Heat transferred in this section reduces the differential temperature across the matrix and the thermal stresses. Hence, thermal shock resistance of the material in the third pass becomes less critical; however, its corrosion resistance must be sufficient to withstand corrosive attack. This modular design could utilize a field repairable, disposable matrix. This report is concerned with process technology development for fabricating such a matrix, and a series of corrosion tests that established the potential corrosion resistance of the Z-1000 ceramic.

  1. Indirect selective laser sintering of an apatite-mullite glass-ceramic for potential use in bone replacement applications.

    PubMed

    Goodridge, R D; Dalgarno, K W; Wood, D J

    2006-01-01

    The feasibility of using indirect selective laser sintering (SLS) to produce parts from glass-ceramic materials for bone replacement applications has been investigated. A castable glass based on the system SiO2 x Al2O3 x P2O5 x CaO x CaF2 that crystallizes to a glass-ceramic with apatite and mullite phases was produced, blended with an acrylic binder, and processed by SLS. Green parts with good structural integrity were produced using a wide range of processing conditions, allowing both monolayer and multilayer components to be constructed. Following SLS the parts were post-processed to remove the binder and to crystallize fully the material, evolving the apatite and mullite phases. The parts were heated to 1200 degrees C using a number of different time-temperature profiles, following which the processed material was analysed by differential thermal analysis, X-ray diffraction, and scanning electron microscopy, and tested for flexural strength. An increase in strength was achieved by infiltrating the brown parts with a resorbable phosphate glass, although this altered the crystal phases present in the material. PMID:16459446

  2. Effects of soda-lime-silica waste glass on mullite formation kinetics and micro-structures development in vitreous ceramics.

    PubMed

    Marinoni, Nicoletta; D'Alessio, Daniela; Diella, Valeria; Pavese, Alessandro; Francescon, Ferdinando

    2013-07-30

    The effects of soda-lime waste glass, from the recovery of bottle glass cullet, in partial replacement of Na-feldspar for sanitary-ware ceramic production are discussed. Attention is paid to the mullite growth kinetics and to the macroscopic properties of the final output, the latter ones depending on the developed micro-structures and vitrification grade. Measurements have been performed by in situ high temperature X-ray powder diffraction, scanning electron microscopy, thermal dilatometry, water absorption and mechanical testing. Glass substituting feldspar from 30 to 50 wt% allows one (i) to accelerate the mullite growth reaction kinetics, and (ii) to achieve macroscopic features of the ceramic output that comply with the latest technical requirements. The introduction of waste glass leads to (i) a general saving of fuel and reduction of the CO2-emissions during the firing stage, (ii) a preservation of mineral resources in terms of feldspars, and (iii) an efficient management of the bottle glass refuse by readdressing a part of it in the sanitary-ware manufacturing. PMID:23624427

  3. Site-Resolved Spectroscopy of CHROMIUM(3): Mullite Class-Ceramics

    NASA Astrophysics Data System (ADS)

    Knutson, Robert Andrew

    A variety of techniques were employed to study the site distribution of Cr^{3+} doped mullite glass-ceramic and to identify individual spectroscopic features with the site species from which they originate. The influence of various site parameters such as ligand field strength, symmetry, and ^4 T_2-^2E energy gap on the emission was analyzed. Line-narrowed R-line fluorescence spectra were taken. From these spectra the homogeneous linewidth of the R-line emission was determined. The laser-resonant emission was accompanied by a vibronic sideband and an R_1 emission satellite which originates from ions that have their R_2 transition in resonance with the laser. From these spectra the mean phonon energy and average E-2A splitting were determined. Comparison of adsorption, luminescence, and excitation spectra revealed a broad distribution of Cr^ {3+} environments and demonstrated partial site selectivity of the inhomogeneous ^4T_2 adsorption peak, with lower energy excitation pumping ions at corresponding lower field sites. The ^4T_2 absorption was modeled as a distribution of "Pekarian" functions. This model was then used to fit the luminescence data. Electron paramagnetic resonance spectra revealed features in the glass-ceramic which are typical of glass hosts, suggesting that there are Cr^{3+ } ions in extremely disordered environments in this material. These may represent ions in the glass -crystal interface region. Studies of the decay kinetics revealed that higher excitation energies excite longer-lived fluorescence. This behavior was analyzed in terms of the various radiative and nonradiative relaxation models. The quantum efficiency was measured using a recently developed photocaloric technique. The results reveal that the glass-ceramics are much more efficient than glass hosts. Longer excitation wavelengths were seen to pump less efficient emission, possibly because low efficiency ions at low field sites in disordered environments are preferentially excited at

  4. Synthesis and processing of Al{sub 2}O{sub 3}/Al composites by in situ reaction of aluminum and mullite

    SciTech Connect

    Fahrenholtz, W.G.; Ewsuk, K.G.; Loehman, R.E.; Tomsia, A.P.

    1995-02-01

    Al{sub 2}O{sub 3}/Al composites, were formed by reacting molten aluminum metal with dense mullite ceramic preforms. The composites produced by this reactive metal penetration process (RMP) have a two phase, interpenetrating microstructure in which both the ceramic and the metal are continuous in three dimensions. Scanning electron microscopy (SEM) micrographs of composites produced by RMP show a fine microstructure comprised of interlocked metal and ceramic phases, with a feature size of approximately 2 {mu}m. RMP is a relatively rapid process with metal penetration rates of nearly 5 mm/hour at 1100{degrees}C after a short incubation period. An activation energy of 92 kJ/mole was calculated from reaction rate data. Transmission electron microscopy (TEM) micrographs reveal that aluminum metal penetrates along the mullite grain boundaries before reaction with the mullite grains, indicating that diffusion along grain boundaries may be the rate limiting step for the reaction. Thermodynamic information, results of microstructure analyses, and kinetic data indicate that RMP proceeds in 4 stages: (1) Al melting and the formation of a thermodynamically stable metal/ceramic interface; (2) depletion of oxygen from the grain boundaries intersecting the ceramic/metal interface; (3) Al metal penetration into the ceramic preform along grain boundaries; and (4) Al reaction with and conversion of individual mullite grains.

  5. Ab initio calculations of mechanical, thermodynamic and electronic structure properties of mullite, iota-alumina and boron carbide

    NASA Astrophysics Data System (ADS)

    Aryal, Sita Ram

    The alumino-silicate solid solution series (Al 4+2xSi2-2 xO10-x) is an important class of ceramics. Except for the end member (x=0), Al2 SiO5 the crystal structures of the other phases, called mullite, have partially occupied sites. Stoichiometric supercell models for the four mullite phases 3Al2O 3 · 2SiO2 · 2Al 2O3 · SiO2, 4 Al2O3· SiO 2, 9Al2O3 · SiO2, and iota-Al2 O3 (iota-alumina) are constructed starting from experimentally reported crystal structures. A large number of models were built for each phase and relaxed using the Vienna ab initio simulation package (VASP) program. The model with the lowest total energy for a given x was chosen as the representative structure for that phase. Electronic structure and mechanical properties of mullite phases were studied via first-principles calculations. Of the various phases of transition alumina, iota-Al 2O3 is the least well known. In addition structural details have not, until now, been available. It is the end member of the aluminosilicate solid solution series with x=1. Based on a high alumina content mullite phase, a structural model for iota- Al2O3 is constructed. The simulated x-ray diffraction (XRD) pattern of this model agrees well with a measured XRD pattern. The iota-Al2 O3 is a highly disordered ultra-low-density phase of alumina with a theoretical density of 2854kg/m3. Using this theoretically constructed model, elastic, thermodynamic, electronic, and spectroscopic properties of iota-Al2 O3 have been calculated and compared it with those of alpha- Al2O3 and gamma- Al2O3. Boron carbide (B4C) undergoes an amorphization under high velocity impacts. The mechanism of amorphization is not clear. Ab initio methods are used to carry out large-scale uniaxial compression simulations on two polytypes of stoichiometric boron carbide (B4C), B 11C-CBC, and B12- CCC where B11C or B12 is the 12-atom icosahedron and CBC or CCC is the three-atom chain. The simulations were performed on large supercells of 180 atoms

  6. A low-cost mullite-titania composite ceramic hollow fiber microfiltration membrane for highly efficient separation of oil-in-water emulsion.

    PubMed

    Zhu, Li; Chen, Mingliang; Dong, Yingchao; Tang, Chuyang Y; Huang, Aisheng; Li, Lingling

    2016-03-01

    Oil-in-water (O/W) emulsion is considered to be difficult to treat. In this work, a low-cost multi-layer-structured mullite-titania composite ceramic hollow fiber microfiltration membrane was fabricated and utilized to efficiently remove fine oil droplets from (O/W) emulsion. In order to reduce membrane cost, coal fly ash was effectively recycled for the first time to fabricate mullite hollow fiber with finger-like and sponge-like structures, on which a much more hydrophilic TiO2 layer was further deposited. The morphology, crystalline phase, mechanical and surface properties were characterized in details. The filtration capability of the final composite membrane was assessed by the separation of a 200 mg·L(-1) synthetic (O/W) emulsion. Even with this microfiltration membrane, a TOC removal efficiency of 97% was achieved. Dilute NaOH solution backwashing was used to effectively accomplish membrane regeneration (∼96% flux recovery efficiency). This study is expected to guide an effective way to recycle waste coal fly ash not only to solve its environmental problems but also to produce a high-valued mullite hollow fiber membrane for highly efficient separation application of O/W emulsion with potential simultaneous functions of pure water production and oil resource recovery. PMID:26748205

  7. High Temperature Elastic Properties of Single Crystal Mullite (Approximately 2.5Al2O3.SiO2) by Brillouin Spectroscopy

    NASA Technical Reports Server (NTRS)

    Palko, James W.; Sayir, Ali; Sinogeikin, Stanislav V.; Kriven, Waltraud M.; Bass, Jay D.; Farmer, Serene C. (Technical Monitor)

    2001-01-01

    The complete elastic tensor of mullite has been determined by brillouin spectroscopy at room temperature and elevated temperatures up to 1200C. Equivalent, isotropic moduli (bulk, shear, and Young's) have been calculated. The room temperature values obtained using Voigt-Reuss-Hill averaging are: K(sub VRH) = 173.5 + 6.9 GPa, G(sub VRH) = 88.0 + 3.5 GPa, E(sub VRH) = 225.9 + 9.0 GPa. All moduli show relatively gradual decreases with temperature. The temperature derivatives obtained for the equivalent, isotropic moduli are: dK(sub VRH)/dT = - 17.5 + 2.5 MPa/deg. C, dG(sub VRH)/dT = -8.8 + 1.4 MPa/deg. C, dE(sub VRH)/dT = -22.6 + 2.8 MPa/deg C. Substantial differences between bulk properties calculated from the single crystal measurements in this study and the properties reported in the literature for polycrystalline sintered mullite are identified, indicating the importance of factors such as microstructure, intergranular phases, and composition to the elasticity of mullite ceramics.

  8. Constraining Oxygen-17 NMR Spectra of High Pressure Crystals and Glasses: New Data for Jadeite, Pyrope, Grossular, and Mullite

    NASA Astrophysics Data System (ADS)

    Kelsey, K. E.; Stebbins, J. F.; Du, L.; Hankins, B.

    2005-12-01

    17O NMR is a direct way of analyzing the immediate environment around oxygen atoms and can provide information on cation ordering, mixing, and network connectivity in glasses and disordered crystals. Due to overlapping peaks and lack of data on crystalline model compounds, 17O NMR spectra of high pressure glasses have been difficult to interpret. Additionally, data on crystalline model compounds are needed to test the validity of quantum chemical calculations. In this study, 17O NMR spectra were collected for crystalline jadeite, pyrope, grossular, and mullite in order to determine the parameters for oxygen bonded to [6]Al in a variety of environments. Jadeite contains three oxygen sites: oxygen bonded to [4]Si, Na, and two [6]Al atoms (O1), oxygen bonded to [4]Si, Na, and [6]Al atoms (O2), and oxygen bonded to two [4]Si and two Na atoms (O3). The NMR parameters for O1 are CQ = 3.3 MHz, δ = 64 ppm, and ν = 0.9; for O2 are CQ = 4.1 MHz, δ = 59 ppm, and ν = 0.15; and for O3 are CQ = 5.0 MHz, δ = 60 ppm, and ν = 0.15. The parameters for O2 are similar to interpretations of recent data for this kind of site in high pressure sodium aluminosilicate glasses (δ = 59 ppm) and to quantum chemical calculations (Lee et al., 2004, J. Phys. Chem., 108, 5897). Pyrope and grossular each contain one oxygen site, oxygen bonded to [4]Si, [6]Al, and two M2+ cations. The 17O NMR parameters for pyrope are CQ = 3.4 MHz, δ = 84 ppm, and ν = 0.3 and for grossular are CQ = 4.1 MHz, δ = 102 ppm, and ν = 0.4. In grossular, the NMR peak for oxygens bonded to [4]Si, Ca, and high coordinated Al seems to fall between those for "normal" bridging and non bridging oxygens, as reported for high pressure CAS glasses by Allwardt et al. (2005). These data will also be useful to help understand Ca-Mg ordering in the pyrope-grossular solid solutions. Mullite contains four oxygen environments: oxygen bonded to three tetrahedral Al or Si (Oc*), oxygen bonded to two tetrahedral Al or Si (Oc), and

  9. Processing of an apatite-mullite glass-ceramic and an hydroxyapatite/phosphate glass composite by selective laser sintering.

    PubMed

    Lorrison, J C; Dalgarno, K W; Wood, D J

    2005-08-01

    The work presented details the results of an investigation into the feasibility of using Selective Laser Sintering (SLS) to directly produce customised bioceramic implants. The materials used were bioactive in nature and included a glass-ceramic and a combination of hydroxyapatite and phosphate glass. The glass-ceramic was selected from the range of apatite-mullite materials in the SiO2.Al2O3.CaO.CaF2.P2O5 series, due to their potentially suitable biological and mechanical properties. The hydroxyapatite and phosphate glass combination was chosen to allow an alternative production approach to be investigated. The viability of using both these materials with the SLS process was assessed and the process route and resulting material properties characterised using a variety of techniques including Differential Thermal Analysis (DTA), X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The results obtained indicate that it was possible to produce multiple layer components from both materials using the SLS process. The glass-ceramic materials could only be processed at very low scan speeds and powers, yielding relatively brittle components. It was though possible to produce parts from the hydroxyapatite and phosphate glass combination across a much wider range of parameters, producing parts which had a greater potential for possible implant production. PMID:15965749

  10. Development of a zirconia-mullite based ceramic for recuperator applications. DOE/ORNL Ceramic Technology Project

    SciTech Connect

    Gonzalez, J.M.

    1992-12-01

    GTE Products Corporation developed a compact ceramic high temperature recuperator for recovering heat from relatively clean exhaust gases at temperatures up to 2500F. The DOE program allowed GTE to improve the technical and economic characteristics of the recuperator and stimulate industrial acceptance of the recuperator as an energy-saving technology. From January 1981 to December 1984, 561 recuperators were installed by GTE on new or retrofitted furnaces. With over 1200 units sold commercially between 1981 and 1990, GTE has documented the effect (long and short term) of corrosive attack from alkalies and lead. One objective of this contract was to develop Z-1000 a zirconia-mullite mixed oxide ceramic for use in ceramic recuperator applications susceptible to corrosion. To first and second pass of the ceramic recuperator would utilize the current cordierite-mixed-oxide ceramic. A Z-1000 matrix element would be used in the preheated air side`s third pass (exhaust inlet). Thermal stresses on Z-1000 cross flow module could be minimized by selecting appropriate heat transfer surface areas for each pass. A large surface area for first and second pass (cordierite section) could provide for sufficient heat transfer for 50% effectiveness. A surface area that generates minimal heat transfer in the third pass (Z-1000) section is envisioned. Heat transferred in this section reduces the differential temperature across the matrix and the thermal stresses. Hence, thermal shock resistance of the material in the third pass becomes less critical; however, its corrosion resistance must be sufficient to withstand corrosive attack. This modular design could utilize a field repairable, disposable matrix. This report is concerned with process technology development for fabricating such a matrix, and a series of corrosion tests that established the potential corrosion resistance of the Z-1000 ceramic.

  11. Mullitization in Al{sub 2}O{sub 3}-SiC nanocomposite: A case study of high temperature oxidation

    SciTech Connect

    Wang, J.; Ponton, C.B.; Marquis, P.M.

    1996-03-15

    Alumina-SiC nanocomposites, which offer a better mechanical performance than conventional ceramic materials, are a class of potentially important structural materials. Unfortunately, alumina-SiC nanocomposite is a thermodynamically metastable system at elevated temperatures. The SiC particles, especially those near the sample surface, are susceptible to oxidation at temperatures above 1,000 C, forming silica which may subsequently react with the alumina matrix. The objective of the present work is to investigate the mullitization reaction between the oxidation-led nano-silica particles and alumina matrix in an alumina-5 vol% SiC nanocomposite

  12. Sintering behavior of mullite with addition of SiO2-MgO-Y2O3-SrCO3

    NASA Astrophysics Data System (ADS)

    Lim, Chang-Bin; Yeo, Dong-Hun; Shin, Hyo-Soon

    2013-12-01

    As the size of semiconducting silicon (Si) wafers increases, that of the ceramic substrate, which is main part of a semiconductor probing system, has also increased. The increased number of layers due to high integrity of Si wafers and the narrow pattern linewidths for impedance matching require the use of Cu-Mo conducting paste, rather than conventional Mo paste, for low electrical resistivity. For co-firing of a Cu-Mo electrode with a ceramic substrate, a green ceramic substrate with a printed pattern must be sintered at a temperature below 1400 °C. To obtain a mullite composition that can be co-fired with a Cu-Mo electrode at a temperature below 1400 °C, we added 1.0 wt% of SiO2, 1.0 wt% of MgO, 1.5 wt% of Y2O3, and 7.0 wt% of SrCO3 to a commercial mullite composition, and we sintered the specimen with that composition at 1350 °C in a reducing atmosphere to obtain a density of 3.20 g/cm3. The sintered specimen's coefficient of thermal expansion at temperatures from room temperature to 200 °C was 4.53 ppm/°C, which is acceptable for a semiconductor probing system.

  13. Fabrication of mullite-bonded porous SiC ceramics from multilayer-coated SiC particles through sol-gel and in-situ polymerization techniques

    NASA Astrophysics Data System (ADS)

    Ebrahimpour, Omid

    In this work, mullite-bonded porous silicon carbide (SiC) ceramics were prepared via a reaction bonding technique with the assistance of a sol-gel technique or in-situ polymerization as well as a combination of these techniques. In a typical procedure, SiC particles were first coated by alumina using calcined powder and alumina sol via a sol-gel technique followed by drying and passing through a screen. Subsequently, they were coated with the desired amount of polyethylene via an in-situ polymerization technique in a slurry phase reactor using a Ziegler-Natta catalyst. Afterward, the coated powders were dried again and passed through a screen before being pressed into a rectangular mold to make a green body. During the heating process, the polyethylene was burnt out to form pores at a temperature of about 500°C. Increasing the temperature above 800°C led to the partial oxidation of SiC particles to silica. At higher temperatures (above 1400°C) derived silica reacted with alumina to form mullite, which bonds SiC particles together. The porous SiC specimens were characterized with various techniques. The first part of the project was devoted to investigating the oxidation of SiC particles using a Thermogravimetric analysis (TGA) apparatus. The effects of particle size (micro and nano) and oxidation temperature (910°C--1010°C) as well as the initial mass of SiC particles in TGA on the oxidation behaviour of SiC powders were evaluated. To illustrate the oxidation rate of SiC in the packed bed state, a new kinetic model, which takes into account all of the diffusion steps (bulk, inter and intra particle diffusion) and surface oxidation rate, was proposed. Furthermore, the oxidation of SiC particles was analyzed by the X-ray Diffraction (XRD) technique. The effect of different alumina sources (calcined Al2O 3, alumina sol or a combination of the two) on the mechanical, physical, and crystalline structure of mullite-bonded porous SiC ceramics was studied in the

  14. Coatings for mullite insulation

    NASA Technical Reports Server (NTRS)

    Bolinger, P. N.; Rauch, H. W., Sr.

    1976-01-01

    Series of coatings provides hard, impermeable, waterproof layer. Inclusion of color oxides imparts high emittance to surface. Refractory fillers investigated include TiO2, BaO.ZrO2, SrO.TiO2 ziron, spodumene, petalite, and kryptonite. Colorants include Cr2O3, NiO, and CoO.

  15. Characterization of the Microstructure of an AlN-Mullite-Al2O3 Ceramic Layer on WCu Composite Alloy for Microelectronic Application

    NASA Astrophysics Data System (ADS)

    Zhu, Jiandong; An, Rong; Wang, Chunqing; Zhang, Wei; Wen, Guangwu

    2015-11-01

    An AlN composite ceramic layer was designed and fabricated on WCu substrates by hydrolysis-assisted solidification and firing. First, the surface of WCu substrates were pre-coated with polycarbosilane/AlN ceramic layers by spinning; the layers were then fabricated by firing. The phase composition, microstructure, and element distribution of the ceramic layer and interfacial reaction layer were investigated by use of scanning electron microscopy, energy-dispersive spectroscopy and x-ray diffraction. The results showed that the ceramic layers were composed of AlN, mullite, and Al2O3. There were many nanocrystalline rods on the surface of the ceramic layers. The Cr layer prevented the WCu substrate from reacting with water vapor during firing, and the Ni layer prevented diffusion of tungsten into the Cr layer. Study of the cross section of the ceramic layer fired on the Cr/Ni/WCu substrate revealed a perfect interfacial reaction layer.

  16. Role of Y{sub 2}O{sub 3}, CaO, MgO additives on structural and microstructural behavior of zirconia/mullite aggregates

    SciTech Connect

    Mishra, D. K.; Prusty, Sasmita; Mohapatra, B. K.; Singh, S. K.; Behera, S. N.

    2012-07-23

    Zirconia mullite (MUZ), Y{sub 2}O{sub 3}-MUZ, CaO-MUZ and MgO-MUZ composites, synthesized through plasma fusion technique, are becoming important due to their commercial scale of production within five minutes of plasma treatment from sillimanite, zircon and alumina mixture. The X-ray diffraction studies reveal the monoclinic zirconia phase in MUZ composite whereas mixed monoclinic, tetragonal and cubic phases of zirconia have been observed in Y{sub 2}O{sub 3}, CaO, MgO added MUZ composites. The Y{sub 2}O{sub 3}, CaO and MgO additives act as sintering aids to favour the transformation and stabilisation of tetragonal and cubic zirconia phases at room temperature. These additives also play a key role in the development of various forms of microstructure to achieve dense MUZ composites.

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

    SciTech Connect

    SUGAMA, T.; BROTHERS, L.E.; VAN DE PUTTE, T.R.

    2006-06-01

    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.

  18. The effect of ZrO2 and TiO 2 on solubility and strength of apatite-mullite glass-ceramics for dental applications.

    PubMed

    Fathi, Hawa M; Miller, Cheryl; Stokes, Christopher; Johnson, Anthony

    2014-03-01

    The effect of ZrO2 and TiO2 on the chemical and mechanical properties of apatite-mullite glass-ceramics was investigated after sample preparation according to the ISO (2768:2008) recommendations for dental ceramics. All materials were characterized using differential thermal analysis, X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. X-ray fluorescence spectroscopy was used to determine the concentrations of elements present in all materials produced. The chemical solubility test and the biaxial flexural strength (BFS) test were then carried out on all the samples. The best solubility value of 242 ± 61 μg/cm(2) was obtained when HG1T was heat-treated for 1 h at the glass transition temperature plus 20 °C (Tg + 20 °C) followed by 5 h at 1200 °C. The highest BFS value of 174 ± 38 MPa was achieved when HG1Z and HG1Z+T were heat-treated for 1 h at the Tg + 20 °C followed by 7 h at 1200 °C. The present study has demonstrated that the addition of TiO2 to the reference composition showed promise in both the glass and heat-treated samples. However, ZrO2 is an effective agent for developing the solubility or the mechanical properties of an apatite-mullite glass-ceramic separately but does not improve the solubility and the BFS simultaneously. PMID:24249630

  19. Fabrication of mullite-bonded porous SiC ceramics from multilayer-coated SiC particles through sol-gel and in-situ polymerization techniques

    NASA Astrophysics Data System (ADS)

    Ebrahimpour, Omid

    In this work, mullite-bonded porous silicon carbide (SiC) ceramics were prepared via a reaction bonding technique with the assistance of a sol-gel technique or in-situ polymerization as well as a combination of these techniques. In a typical procedure, SiC particles were first coated by alumina using calcined powder and alumina sol via a sol-gel technique followed by drying and passing through a screen. Subsequently, they were coated with the desired amount of polyethylene via an in-situ polymerization technique in a slurry phase reactor using a Ziegler-Natta catalyst. Afterward, the coated powders were dried again and passed through a screen before being pressed into a rectangular mold to make a green body. During the heating process, the polyethylene was burnt out to form pores at a temperature of about 500°C. Increasing the temperature above 800°C led to the partial oxidation of SiC particles to silica. At higher temperatures (above 1400°C) derived silica reacted with alumina to form mullite, which bonds SiC particles together. The porous SiC specimens were characterized with various techniques. The first part of the project was devoted to investigating the oxidation of SiC particles using a Thermogravimetric analysis (TGA) apparatus. The effects of particle size (micro and nano) and oxidation temperature (910°C--1010°C) as well as the initial mass of SiC particles in TGA on the oxidation behaviour of SiC powders were evaluated. To illustrate the oxidation rate of SiC in the packed bed state, a new kinetic model, which takes into account all of the diffusion steps (bulk, inter and intra particle diffusion) and surface oxidation rate, was proposed. Furthermore, the oxidation of SiC particles was analyzed by the X-ray Diffraction (XRD) technique. The effect of different alumina sources (calcined Al2O 3, alumina sol or a combination of the two) on the mechanical, physical, and crystalline structure of mullite-bonded porous SiC ceramics was studied in the

  20. Thermal stability of mullite RMn₂O₅ (R  =  Bi, Y, Pr, Sm or Gd): combined density functional theory and experimental study.

    PubMed

    Li, Chenzhe; Thampy, Sampreetha; Zheng, Yongping; Kweun, Joshua M; Ren, Yixin; Chan, Julia Y; Kim, Hanchul; Cho, Maenghyo; Kim, Yoon Young; Hsu, Julia W P; Cho, Kyeongjae

    2016-03-31

    Understanding and effectively predicting the thermal stability of ternary transition metal oxides with heavy elements using first principle simulations are vital for understanding performance of advanced materials. In this work, we have investigated the thermal stability of mullite RMn2O5 (R  =  Bi, Pr, Sm, or Gd) structures by constructing temperature phase diagrams using an efficient mixed generalized gradient approximation (GGA) and the GGA  +  U method. Simulation predicted stability regions without corrections on heavy elements show a 4-200 K underestimation compared to our experimental results. We have found the number of d/f electrons in the heavy elements shows a linear relationship with the prediction deviation. Further correction on the strongly correlated electrons in heavy elements could significantly reduce the prediction deviations. Our corrected simulation results demonstrate that further correction of R-site elements in RMn2O5 could effectively reduce the underestimation of the density functional theory-predicted decomposition temperature to within 30 K. Therefore, it could produce an accurate thermal stability prediction for complex ternary transition metal oxide compounds with heavy elements. PMID:26932942

  1. Thermal stability of mullite RMn2O5 (R  =  Bi, Y, Pr, Sm or Gd): combined density functional theory and experimental study

    NASA Astrophysics Data System (ADS)

    Li, Chenzhe; Thampy, Sampreetha; Zheng, Yongping; Kweun, Joshua M.; Ren, Yixin; Chan, Julia Y.; Kim, Hanchul; Cho, Maenghyo; Kim, Yoon Young; Hsu, Julia W. P.; Cho, Kyeongjae

    2016-03-01

    Understanding and effectively predicting the thermal stability of ternary transition metal oxides with heavy elements using first principle simulations are vital for understanding performance of advanced materials. In this work, we have investigated the thermal stability of mullite RMn2O5 (R  =  Bi, Pr, Sm, or Gd) structures by constructing temperature phase diagrams using an efficient mixed generalized gradient approximation (GGA) and the GGA  +  U method. Simulation predicted stability regions without corrections on heavy elements show a 4-200 K underestimation compared to our experimental results. We have found the number of d/f electrons in the heavy elements shows a linear relationship with the prediction deviation. Further correction on the strongly correlated electrons in heavy elements could significantly reduce the prediction deviations. Our corrected simulation results demonstrate that further correction of R-site elements in RMn2O5 could effectively reduce the underestimation of the density functional theory-predicted decomposition temperature to within 30 K. Therefore, it could produce an accurate thermal stability prediction for complex ternary transition metal oxide compounds with heavy elements.

  2. Anisotropic thermal expansion and anharmonic phonon behavior of mullite-type Bi{sub 2}Ga{sub 4}O{sub 9}

    SciTech Connect

    Murshed, M. Mangir Gesing, Thorsten M.

    2013-09-01

    Graphical abstract: - Highlights: • Anisotropic lattice thermal expansion of Bi{sub 2}Ga{sub 4}O{sub 9} was modeled using extended Grüneisen first-order approximation. • The model includes harmonic, quasi-harmonic and intrinsic anharmonic contributions to the internal energy. • Temperature dependent Raman frequency shift and line-width was analyzed using symmetric phonon decay channel. - Abstract: We report the lattice thermal expansion and the temperature-dependent phonon behavior of the mullite-type Bi{sub 2}Ga{sub 4}O{sub 9} complex oxide. The thermal expansion was studied using composite data collected from powder and single crystal X-ray diffraction between 100 K and 1273 K. The lattice expansion occurred in the order of a < c < b. The anisotropic expansion behavior was monitored with respect to thermal expansion coefficients and the anisotropy factor. The volume thermal expansion was expressed using an extended Grüneisen first-order approximation to the zero-pressure equation of state; the model includes harmonic, quasi-harmonic and intrinsic anharmonic contributions to the internal energy as a function of temperature. The temperature dependent Raman spectra were collected from a single crystal between 78 K and 1273 K. The shift of the frequencies and the broadening of the line-widths with increasing temperature helped to analyze the anharmonicity and the thermal behavior of some phonons.

  3. Chromium substitution in mullite type bismuth aluminate: Bi2CrxAl4-xO9 with 0≤x≤2.0

    NASA Astrophysics Data System (ADS)

    Debnath, Tapas; Ullah, Ahamed; Rüscher, Claus H.; Hussain, Altaf

    2014-12-01

    Nominal compositions Bi2CrxAl4-xO9 with 0.0≤x≤2.0 (Δx=0.2) were prepared using appropriate amounts of nitrates dissolved in glycerine and heated at 800 °C for 24 h as we previously used for the preparation of solid solution series Bi2Mx/M‧4-xO9 (M/M‧=Fe/Al, Ga/Al and Fe/Ga). The samples were characterized using XRD, FTIR and optical microscopic techniques. Analyses of XRD data show mullite type single phase can be prepared up to x=1.2. The lattice parameters (a, b and c) increases with increasing Cr content. Further increase in x (i.e., x≥1.4) show the presence of some additional phases indicating a limiting value for Cr doping is in the range of 1.2≤x<1.4. The effect of Cr incorporation could also be observed in the infrared absorption spectra via systematic hard mode shifts of certain lattice modes, e.g. the Bi-O related vibration changes from 96 cm-1 to 93 cm-1 with increasing x up to 1.2 and certain intensity changes together with shift in peak positions. Interestingly, the absence of any splitting and shift of the high energy IR absorption peak at 821 cm-1 as assigned to the characteristic tetrahedral type dimer, Al2O7, indicate that the Cr thus partially substitutes only the octahedrally coordinated Al. This is confirmed by Rietveld structure refinements, too.

  4. First-Principles Investigations of the Structure, Electronic, and Optical Properties of Mullite-Type Orthorhombic Bi2M4O9 (M = Al(3+), Ga(3+)).

    PubMed

    Zahedi, Ehsan; Xiao, Bing; Shayestefar, Mohadese

    2016-05-16

    The structure, electronic band structure, density of state, projected wave function, and optical properties of mullite-type orthorhombic Bi2M4O9 (M = Al(3+), Ga(3+)) crystals have been studied by applying density functional theory based on the Vanderbilt ultrasoft pseudopotential in the frame of the generalized gradient approximation as an exchange-correlation function. Satisfactory agreement between experimental and theoretical results indicates that the used method and conditions are suitable. M-O bonds in tetrahedral MO4 environments are stronger and more covalent with respect to octahedral MO6; also Bi-O bonds in both studied structures are almost ionic in nature. The photocatalytic activity of Bi2Al4O9 and Bi2Ga4O9 is enhanced due to unequal values of Mulliken charges on the O atoms in MO4, MO6, and BiO6E groups. Bi2Al4O9 and Bi2Ga4O9 are direct and indirect band gap semiconductors with band gaps of 2.71 and 2.86 eV, respectively. Higher photocatalytic activity of Bi2Al4O9 is inferable from the lower effective masses of photogenerated carriers around the conduction band minimum and valence band maximum, in comparison with Bi2Ga4O9. The presence of M and O orbitals in the valence and conduction bands reveals that symmetry breaking in the MO4 and MO6 units has an important role in separating charges and increasing photocatalytic activity. Photocatalytic activities of Bi2Al4O9 and Bi2Ga4O9 for decomposition of organic pollutants and generation of hydrogen from water splitting are confirmed from band edge potentials. PMID:27139249

  5. Structural, electrical and multiferroic properties of La-doped mullite Bi{sub 2}Fe{sub 4}O{sub 9} thin films

    SciTech Connect

    Raghavan, C.M.; Kim, J.W.; Kim, J.-W.; Kim, S.S.

    2015-10-15

    Highlights: • Chemical solution deposited La-doped Bi{sub 2}Fe{sub 4}O{sub 9} thin film. • Structural, electrical and multiferroic properties were investigated. • La-doped Bi{sub 2}Fe{sub 4}O{sub 9} exhibited enhanced electrical and multiferroic properties. - Abstract: Thin films of (Bi{sub 2−x}La{sub x})Fe{sub 4}O{sub 9} (x = 0 and x = 0.05) were prepared on Pt(1 1 1)/Ti/SiO{sub 2}/Si(1 0 0) substrates by using a chemical solution deposition method to investigate structural, microstructural, electrical and multiferroic properties. Both the thin films were crystallized in mullite type phases with orthorhombic structures containing no secondary and impurity phases, which was confirmed by X-ray diffraction and Raman spectroscopy studies. The (Bi{sub 1.95}La{sub 0.05})Fe{sub 4}O{sub 9} thin film exhibited improved electrical and multiferroic properties at room-temperature. The leakage current density of the (Bi{sub 1.95}La{sub 0.05})Fe{sub 4}O{sub 9} thin film was one order of magnitude lower than that of the Bi{sub 2}Fe{sub 4}O{sub 9} thin film. Furthermore, in the thin film form, (Bi{sub 2−x}La{sub x})Fe{sub 4}O{sub 9} exhibited better stability against electrical breakdowns and enhanced multiferroic properties.

  6. Near-infrared luminescence and color tunable chromophores based on Cr(3+)-doped mullite-type Bi2(Ga,Al)4O9 solid solutions.

    PubMed

    Liu, Chengyin; Xia, Zhiguo; Chen, Mingyue; Molokeev, Maxim S; Liu, Quanlin

    2015-02-16

    Cr(3+)-activated mullite-type Bi2Ga(4-x)Al(x)O9 (x = 0, 1, 2, 3, and 4) solid solutions were prepared by the solid state reaction, and their spectroscopic properties were investigated in conjunction with the structural evolution. Under excitation at 610 nm, Bi2[Ga(4-y)Al(y)]3.97O9:0.03Cr(3+) (y = 0, 1, 2, 3, and 4) phosphors exhibited broad-band near-infrared (NIR) emission peaking at ∼710 nm in the range 650-850 nm, and the optimum Cr(3+) concentrations and concentration quenching mechanism were determined. Except for the interesting NIR emission, the body color changed from white (at x = 0) to green (at x = 0.08) for Bi2Ga(4-x)O9:xCr(3+), and from light yellow (at x = 0) to deep brown (at x = 0.08) for Bi2Al(4-x)O9:xCr(3+), respectively. Moreover, as a result of variable Al/Ga ratio, the observed body color for Bi2[Ga(4-y)Al(y)]3.97O9:0.03Cr(3+) (y = 0, 1, 2, 3, and 4) varied from deep brown to green. The relationship between the observed colors and their diffuse reflectance spectra were also studied for the understanding of the different absorption bands. The results indicated that Cr(3+)-doped Bi2Ga(4-x)Al(x)O9 solid solutions appeared as the bifunctional materials with NIR phosphors and color-tunable pigments. PMID:25622046

  7. Synthesis, structure and magnetic ordering of the mullite-type Bi2Fe(4-x)CrxO9 solid solutions with a frustrated pentagonal Cairo lattice.

    PubMed

    Rozova, M G; Grigoriev, V V; Bobrikov, I A; Filimonov, D S; Zakharov, K V; Volkova, O S; Vasiliev, A N; Antipov, E V; Tsirlin, A A; Abakumov, A M

    2016-01-21

    Highly homogeneous mullite-type solid solutions Bi2Fe(4-x)CrxO9 (x = 0.5, 1, 1.2) were synthesized using a soft chemistry technique followed by a solid-state reaction in Ar. The crystal structure of Bi2Fe3CrO9 was investigated using X-ray and neutron powder diffraction, transmission electron microscopy and (57)Fe Mössbauer spectroscopy (S.G. Pbam, a = 7.95579(9) Å, b = 8.39145(9) Å, c = 5.98242(7) Å, RF(X-ray) = 0.022, RF(neutron) = 0.057). The ab planes in the structure are tessellated with distorted pentagonal loops built up by three tetrahedrally coordinated Fe sites and two octahedrally coordinated Fe/Cr sites, linked together in the ab plane by corner-sharing forming a pentagonal Cairo lattice. Magnetic susceptibility measurements and powder neutron diffraction show that the compounds order antiferromagnetically (AFM) with the Néel temperatures decreasing upon increasing the Cr content from TN ∼ 250 K for x = 0 to TN ∼ 155 K for x = 1.2. The magnetic structure of Bi2Fe3CrO9 at T = 30 K is characterized by a propagation vector k = (1/2,1/2,1/2). The tetrahedrally coordinated Fe cations form singlet pairs within dimers of corner-sharing tetrahedra, but spins on the neighboring dimers are nearly orthogonal. The octahedrally coordinated (Fe,Cr) cations form antiferromagnetic up-up-down-down chains along c, while the spin arrangement in the ab plane is nearly orthogonal between nearest neighbors and collinear between second neighbors. The resulting magnetic structure is remarkably different from the one in pure Bi2Fe4O9 and features several types of spin correlations even on crystallographically equivalent exchange that may be caused by the simultaneous presence of Fe and Cr on the octahedral site. PMID:26661379

  8. Thermal expansion of mullite-type Bi{sub 2}Al{sub 4}O{sub 9}: A study by X-ray diffraction, vibrational spectroscopy and density functional theory

    SciTech Connect

    Mangir Murshed, M.; Mendive, Cecilia B.; Curti, Mariano; Šehović, Malik; Friedrich, Alexandra; Fischer, Michael; Gesing, Thorsten M.

    2015-09-15

    Polycrystalline Bi{sub 2}Al{sub 4}O{sub 9} powder samples were synthesized using the glycerine method. Single crystals were produced from the powder product in a Bi{sub 2}O{sub 3} melt. The lattice thermal expansion of the mullite-type compound was studied using X-ray diffraction, Raman spectroscopy and density functional theory (DFT). The metric parameters were modeled using Grüneisen approximation for the zero pressure equation of state, where the temperature-dependent vibrational internal energy was calculated from the Debye characteristic frequency. Both the first-order and second-order Grüneisen approximations were applied for modeling the volumetric expansion, and the second-order approach provided physically meaningful axial parameters. The phonon density of states as well as phonon dispersion guided to set the characteristic frequency for simulation. The experimental infrared and Raman phonon bands were compared with those calculate from the DFT calculations. Selective Raman modes were analyzed for the thermal anharmonic behaviors using simplified Klemens model. The respective mode Grüneisen parameters were calculated from the pressure-dependent Raman spectra. - Graphical abstract: Crystal structure of mullite-type Bi{sub 2}Al{sub 4}O{sub 9} showing the edge-sharing AlO{sub 6} octahedra running parallel to the c-axis. - Highlights: • Thermal expansion of Bi{sub 2}Al{sub 4}O{sub 9} was studied using XRD, FTIR, Raman and DFT. • Metric parameters were modeled using Grüneisen approximation. • Phonon DOS and phonon dispersion helped to set the Debye frequency. • Mode Grüneisen parameters were calculated from the pressure-dependent Raman spectra. • Anharmonicity was analyzed for some selective Raman modes.

  9. Chromium substitution in mullite type bismuth aluminate: Bi{sub 2}Cr{sub x}Al{sub 4−x}O{sub 9} with 0≤x≤2.0

    SciTech Connect

    Debnath, Tapas; Ullah, Ahamed; Rüscher, Claus H.; Hussain, Altaf

    2014-12-15

    Nominal compositions Bi{sub 2}Cr{sub x}Al{sub 4−x}O{sub 9} with 0.0≤x≤2.0 (Δx=0.2) were prepared using appropriate amounts of nitrates dissolved in glycerine and heated at 800 °C for 24 h as we previously used for the preparation of solid solution series Bi{sub 2}M{sub x}/M′{sub 4−x}O{sub 9} (M/M′=Fe/Al, Ga/Al and Fe/Ga). The samples were characterized using XRD, FTIR and optical microscopic techniques. Analyses of XRD data show mullite type single phase can be prepared up to x=1.2. The lattice parameters (a, b and c) increases with increasing Cr content. Further increase in x (i.e., x≥1.4) show the presence of some additional phases indicating a limiting value for Cr doping is in the range of 1.2≤x<1.4. The effect of Cr incorporation could also be observed in the infrared absorption spectra via systematic hard mode shifts of certain lattice modes, e.g. the Bi–O related vibration changes from 96 cm{sup −1} to 93 cm{sup −1} with increasing x up to 1.2 and certain intensity changes together with shift in peak positions. Interestingly, the absence of any splitting and shift of the high energy IR absorption peak at 821 cm{sup −1} as assigned to the characteristic tetrahedral type dimer, Al{sub 2}O{sub 7}, indicate that the Cr thus partially substitutes only the octahedrally coordinated Al. This is confirmed by Rietveld structure refinements, too. - Graphical abstract: Structural model of Cr doped bismuth aluminate, Bi{sub 2}Cr{sub x}Al{sub 4−x}O{sub 9}. - Highlights: • Chromium doped bismuth aluminate, Bi{sub 2}Cr{sub x}Al{sub 4−x}O{sub 9} with mullite type structure are synthesized. • The samples are characterized by XRD and FTIR techniques. • Cr can replace only certain amount of octahedrally coordinated Al in Bi{sub 2}Al{sub 4}O{sub 9} under present experimental conditions.

  10. Mechanochemical-thermal preparation and structural studies of mullite-type Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} solid solutions

    SciTech Connect

    Da Silva, K.L.; Sepelak, V.; Duevel, A.; Paesano, A.; Hahn, H.; Litterst, F.J.; Heitjans, P.; Becker, K.D.

    2011-05-15

    A series of Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} solid solutions (0{<=}x{<=}1), prepared by mechanochemical processing of Bi{sub 2}O{sub 3}/Ga{sub 2}O{sub 3}/Al{sub 2}O{sub 3} mixtures and subsequent annealing, was investigated by XRD, EDX, and {sup 27}Al MAS NMR. The structure of the Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} solid solutions is found to be orthorhombic, space group Pbam (No. 55). The lattice parameters of the Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} series increase linearly with increasing gallium content. Rietveld refinement of the XRD data as well as the analysis of the {sup 27}Al MAS NMR spectra show a preference of gallium cations for the tetrahedral sites in Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9}. As a consequence, this leads to a far from random distribution of Al and Ga cations across the whole series of solid solutions. -- Graphical Abstract: Mullite-type Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} mixed crystals (0{<=}x{<=}1) prepared by a combined mechanochemical-thermal route possess a non-random distribution of Ga{sup 3+} and Al{sup 3+} cations over the sites of tetrahedral (T) and octahedral [O] coordination, characterized by the preference of Ga{sup 3+} (Al{sup 3+}) for tetrahedral (octahedral) sites. Display Omitted Highlights: {yields} Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} (0{<=}x{<=}1) were synthesized via mechanochemical-thermal route. {yields} The lattice parameters of Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} increase linearly with gallium content. {yields} Quantitative information on the cation distribution in Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} is derived. {yields} Ga{sup 3+} and Al{sup 3+} show the preference for tetrahedral and octahedral sites, respectively.

  11. 3-D woven, mullite matrix, composite filter

    SciTech Connect

    Lane, J.E.; Painter, C.J.; Radford, K.C. LeCostaouec, J.F.

    1995-12-01

    Westinghouse, with Techniweave as a major subcontractor, is conducting a three-phase program aimed at providing advanced candle filters for a 1996 pilot scale demonstration in one of the two hot gas filter systems at Southern Company Service`s Wilsonville PSD Facility. The Base Program (Phases I and II) objective is to develop and demonstrate the suitability of the Westinghouse/Techniweave next generation composite candle filter for use in Pressurized Fluidized Bed Combustion (PFBC) and/or Integrated Gasification Combined Cycle (IGCC) power generation systems. The Optional Task (Phase M, Task 5) objective is to fabricate, inspect and ship to Wilsonville Hot gas particulate filters are key components for the successful commercializaion of advanced coal-based power-generation systems such as Pressurized Fluidized-bed Combustion (PFBC), including second-generation PFBC, and Integrated Gasification Combined Cycles (IGCC). Current generation monolithic ceramic filters are subject to catastrophic failure because they have very low resistance to crack propagation. To overcome this problem, a damage-tolerant ceramic filter element is needed.

  12. Crystal-chemistry of mullite-type aluminoborates Al{sub 18}B{sub 4}O{sub 33} and Al{sub 5}BO{sub 9}: A stoichiometry puzzle

    SciTech Connect

    Fisch, Martin; Armbruster, Thomas; Rentsch, Daniel; Libowitzky, Eugen; Pettke, Thomas

    2011-01-15

    Orthorhombic Al{sub 2}O{sub 3}-rich aluminoborate is an important ceramic material for which two slightly different compositions have been assumed: Al{sub 5}BO{sub 9} (5Al{sub 2}O{sub 3}:B{sub 2}O{sub 3}) and Al{sub 18}B{sub 4}O{sub 33} (9Al{sub 2}O{sub 3}:2B{sub 2}O{sub 3}). The formula Al{sub 18}B{sub 4}O{sub 33} (=Al{sub 4.91}B{sub 1.09}O{sub 9}) was derived from results of chemical analyses when crystal structure data were not yet available. Subsequent structural investigations indicated Al{sub 5}BO{sub 9} composition. Nevertheless, Al{sub 18}B{sub 4}O{sub 33} was still accepted as the correct stoichiometry assuming that additional B replaces 9% Al. Powder samples of both compositions and ones with excess boron were prepared by solid state reactions between {alpha}-Al{sub 2}O{sub 3} and B{sub 2}O{sub 3}/H{sub 3}BO{sub 3} at temperatures above 1100 {sup o}C and single-crystals were grown from flux at 1100 and 1550 {sup o}C. Products were investigated by single-crystal and powder XRD, {sup 11}B and {sup 27}Al solid-state MAS-NMR, Raman and FTIR spectroscopy as well as Laser-ablation ICP-MS. No indication of the predicted 9% B{yields}Al substitution was found. LA ICP-MS indicated 12.36(27) wt% B{sub 2}O{sub 3} corresponding to Al{sub 4.97}B{sub 1.03}O{sub 9}. Hence, the suggested Al{sub 18}B{sub 4}O{sub 33} stoichiometry can be excluded for all synthesized samples. A very low amount of Al vacancies at a five-fold coordinated site are likely, charge balanced by an additional nearby three-fold coordinated B site. All evidences indicate that the title compound should be reported as Al{sub 5-x}B{sub 1+x}O{sub 9} with x<0.038(6), which is close to Al{sub 5}BO{sub 9}. -- Graphical abstract: A chemical composition of Al{sub 18}B{sub 4}O{sub 33}=Al{sub 4.91}B{sub 1.09}O{sub 9}=9Al{sub 2}O{sub 3}:2B{sub 2}O{sub 3} has been assumed for mullite-type aluminoborate with Al{sub 5}BO{sub 9} structure. However, samples prepared by different routes showed compositions close to 5Al

  13. Mullite fiber reinforced reaction bonded Si3N4 composites

    NASA Technical Reports Server (NTRS)

    Saleh, T.; Sayir, A.; Lightfoot, A.; Haggerty, J.

    1996-01-01

    Fracture toughnesses of brittle ceramic materials have been improved by introducing reinforcements and carefully tailored interface layers. Silicon carbide and Si3N4 have been emphasized as matrices of structural composites intended for high temperature service because they combine excellent mechanical, chemical, thermal and physical properties. Both matrices have been successfully toughened with SiC fibers, whiskers and particles for ceramic matrix composite (CMC) parts made by sintering, hot pressing or reaction forming processes. These SiC reinforced CMCs have exhibited significantly improved toughnesses at low and intermediate temperature levels, as well as retention of properties at high temperatures for selected exposures; however, they are vulnerable to attack from elevated temperature dry and wet oxidizing atmospheres after the matrix has cracked. Property degradation results from oxidation of interface layers and/or reinforcements. The problem is particularly acute for small diameter (-20 tim) polymer derived SiC fibers used for weavable toes. This research explored opportunities for reinforcing Si3N4 matrices with fibers having improved environmental stability; the findings should also be applicable to SiC matrix CMCs.

  14. Series of compositions Bi{sub 2}(M'{sub x}M{sub 1-x}){sub 4}O{sub 9} (M', M=Al, Ga, Fe; 0{<=}x{<=}1) with mullite-type crystal structure: Synthesis, characterization and {sup 18}O/{sup 16}O exchange experiment

    SciTech Connect

    Debnath, T.; Ruescher, C.H.; Fielitz, P.; Ohmann, S.; Borchardt, G.

    2010-11-15

    Series of compositions Bi{sub 2}(M'{sub x}M{sub 1-x}){sub 4}O{sub 9} with x=0.0, 0.1,..., 1.0 and M'/M=Ga/Al, Fe/Al and Fe/Ga were synthesized by dissolving appropriate amounts of corresponding metal nitrate hydrates in glycerine, followed by gelation, calcination and final heating at 800 {sup o}C for 24 h. The new compositions with M'/M=Ga/Al form solid-solution series, which are isotypes to the two other series M'/M=Fe/Al and Fe/Ga. The XRD data analysis yielded in all cases a linear dependence of the lattice parameters related on x. Rietveld structure refinements of the XRD patterns of the new compounds, Bi{sub 2}(Ga{sub x}Al{sub 1-x}){sub 4}O{sub 9} reveal a preferential occupation of Ga in tetrahedral site (4 h). The IR absorption spectra measured between 50 and 4000 cm{sup -1} of all systems show systematic shifts in peak positions related to the degree of substitution. Samples treated in {sup 18}O{sub 2} atmosphere (16 h at 800 {sup o}C, 200 mbar, 95% {sup 18}O{sub 2}) for {sup 18}O/{sup 16}O isotope exchange experiments show a well-separated IR absorption peak related to the M-{sup 18}O{sub c}-M vibration, where O{sub c} denotes the common oxygen of two tetrahedral type MO{sub 4} units. The intensity ratio of M-{sup 18}O{sub c}/M-{sup 16}O{sub c} IR absorption peaks and the average crystal sizes were used to estimate the tracer diffusion coefficients of polycrystalline Bi{sub 2}Al{sub 4}O{sub 9} (D=2x10{sup -22} m{sup 2}s{sup -1}), Bi{sub 2}Fe{sub 4}O{sub 9} (D=5x10{sup -21} m{sup 2}s{sup -1}), Bi{sub 2}(Ga/Al){sub 4}O{sub 9} (D=2x10{sup -21} m{sup 2}s{sup -1}) and Bi{sub 2}Ga{sub 4}O{sub 9} (D=2x10{sup -20} m{sup 2}s{sup -1}). - Graphical abstract: Fig. Perspective view of the mullite-type Bi{sub 2}(M'{sub x}M{sub 1-x}){sub 4}O{sub 9} unit cell (M', M=Al, Ga, Fe). Display Omitted

  15. Coated article and method of making

    NASA Technical Reports Server (NTRS)

    Wang, Hongyu (Inventor); Lee, Kang Neung (Inventor)

    2002-01-01

    An article includes a silicon-containing substrate and a modified mullite coating. The modified mullite coating comprises mullite and a modifier component that reduces cracks in the modified mullite coating. The article can further comprise a thermal barrier coating applied to the modified mullite coating. The modified mullite coating functions as a bond coating between the external environmental/thermal barrier coating and the silicon-containing substrate. In a method of forming an article, a silicon-containing substrate is formed and a modified mullite coating is applied. The modified mullite coating comprises mullite and a modifier component that reduces cracks in the modified mullite coating.

  16. Coated article and method of making

    NASA Technical Reports Server (NTRS)

    Wang, Hongyu (Inventor); Lee, Kang Neung (Inventor)

    2003-01-01

    An article includes a silicon-containing substrate and a modified mullite coating. The modified mullite coating comprises mullite and a modifier component that reduces cracks in the modified mullite coating. The article can further comprise a thermal barrier coating applied to the modified mullite coating. The modified mullite coating functions as a bond coating between the external environmental/thermal barrier coating and the silicon-containing substrate. In a method of forming an article, a silicon-containing substrate is formed and a modified mullite coating is applied. The modified mullite coating comprises mullite and a modifier component that reduces cracks in the modified mullite coating.

  17. Crystal-chemistry of mullite-type aluminoborates Al 18B 4O 33 and Al 5BO 9: A stoichiometry puzzle

    NASA Astrophysics Data System (ADS)

    Fisch, Martin; Armbruster, Thomas; Rentsch, Daniel; Libowitzky, Eugen; Pettke, Thomas

    2011-01-01

    Orthorhombic Al 2O 3-rich aluminoborate is an important ceramic material for which two slightly different compositions have been assumed: Al 5BO 9 (5Al 2O 3:B 2O 3) and Al 18B 4O 33 (9Al 2O 3:2B 2O 3). The formula Al 18B 4O 33 (=Al 4.91B 1.09O 9) was derived from results of chemical analyses when crystal structure data were not yet available. Subsequent structural investigations indicated Al 5BO 9 composition. Nevertheless, Al 18B 4O 33 was still accepted as the correct stoichiometry assuming that additional B replaces 9% Al. Powder samples of both compositions and ones with excess boron were prepared by solid state reactions between α-Al 2O 3 and B 2O 3/H 3BO 3 at temperatures above 1100 °C and single-crystals were grown from flux at 1100 and 1550 °C. Products were investigated by single-crystal and powder XRD, 11B and 27Al solid-state MAS-NMR, Raman and FTIR spectroscopy as well as Laser-ablation ICP-MS. No indication of the predicted 9% B→Al substitution was found. LA ICP-MS indicated 12.36(27) wt% B 2O 3 corresponding to Al 4.97B 1.03O 9. Hence, the suggested Al 18B 4O 33 stoichiometry can be excluded for all synthesized samples. A very low amount of Al vacancies at a five-fold coordinated site are likely, charge balanced by an additional nearby three-fold coordinated B site. All evidences indicate that the title compound should be reported as Al 5- xB 1+ xO 9 with x<0.038(6), which is close to Al 5BO 9.

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

    SciTech Connect

    Shanmugham, S.; Liaw, P.K.; Stinton, D.P.; Besmann, T.M.; More, K.L.; Bleier, A.; Porter, W.D.; Misture, S.T.

    1996-05-01

    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.

  19. Environmental Barrier Coatings Having a YSZ Top Coat

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Gray, Hugh (Technical Monitor)

    2002-01-01

    Environmental barrier coatings (EBCs) with a Si bond coat, a yttria-stabilized zirconia (YSZ) top coat, and various intermediate coats were investigated. EBCs were processed by atmospheric pressure plasma spraying. The EBC durability was determined by thermal cycling tests in water vapor at 1300 C and 1400 C, and in air at 1400 C and 1500 C. EBCs with a mullite (3Al2O3 (dot) 2SiO2) + BSAS (1 - xBaO (dot) xSrO (dot) Al2O3 (dot) 2SiO2) intermediate coat were more durable than EBCs with a mullite intermediate coat, while EBCs with a mullite/BSAS duplex intermediate coat resulted in inferior durability. The improvement with a mullite + BSAS intermediate coat was attributed to enhanced compliance of the intermediate coat due to the addition of a low modulus BSAS second phase. Mullite + BSAS/YSZ and BSAS/YSZ interfaces produced a low melting (less than 1400 C) reaction product, which is expected to degrade the EBC performance by increasing the thermal conductivity. EBCs with a mullite + BSAS / graded mullite + YSZ intermediate coat showed the best durability among the EBCs investigated in this study. This improvement was attributed to diffused CTE (Coefficient of Thermal Expansion) mismatch stress and improved chemical stability due to the compositionally graded mullite+YSZ layer.

  20. Thin-wall hollow ceramic spheres from slurries. Quarterly project status report, 1 January--31 March 1991

    SciTech Connect

    Chapman, A.T.; Cochran, J.K.

    1991-12-31

    The hollow sphere materials were alumina, mullite, and mullite- ZrO{sub 2} (the Zr reduced the high-temperature thermal conductivity). During this phase, three major tasks were emphasized: Use of opacifiers (Zr oxide) to reduce the high-temperature thermal conductivity of the sphere, convert the slurries from organic-based to aqueous-based, and technology transfer to industry.

  1. Chemical and morphological changes of reusable surface insulation coatings as a function of convectively heated cyclic testing

    NASA Technical Reports Server (NTRS)

    Leiser, D. B.; Stewart, D. A.; Goldstein, H. E.

    1973-01-01

    The effects of convective heating upon reusable surface insulation coatings were studied utilizing scanning electron microscopy, X-ray fluorescence, and X-ray diffraction. Samples of coated silica, mullite, and ceramic mullite fiber were cycled in an arc plasma stream up to 15 times for 15 minutes per cycle at surface temperatures simulating those on the space shuttle vehicle. The surfaces of ceramic mullite fiber and mullite coatings were roughened substantially by the convectively heated environment while the silica was significantly smoothed after testing. Scanning electron microscopy also showed surface cracking of varying degrees in all of the coatings. The surface chemistry of the coatings as examined by X-ray fluorescence revealed that significant changes in composition were occurring during cycling, particularly within the mullite coating.

  2. Degradation Of Environmental Barrier Coatings (EBC) Due To Chemical and Thermal Expansion Incompatibility

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; King, Deboran (Technical Monitor)

    2001-01-01

    Current environmental barrier coatings (EBCs) consist of multiple layers, with each layer having unique properties to meet the various requirements for successful EBCs. As a result, chemical and thermal expansion compatibility between layers becomes an important issue to maintaining durability. Key constituents in current EBCs are mullite (3Al2O3-2SiO2), BSAS (BaO(1-x)-SrO(x)-Al2O3-2SiO2), and YSZ (ZrO2-8 wt.% Y2O3). The mullite-BSAS combination appears benign although significant diffusion occurs. Mullite-YSZ and BSAS-YSZ combinations do not react up to 1500 C. Thermally grown SiO2- BSAS and mullite-BSAS-YSZ combinations are most detrimental, forming low melting glasses. Thermal expansion mismatch between YSZ and mullite or BSAS causes severe cracking and delamination.

  3. Multilayer article having stabilized zirconia outer layer and chemical barrier layer

    NASA Technical Reports Server (NTRS)

    Lee, Kang N. (Inventor); Bansal, Narottam P. (Inventor)

    2004-01-01

    A multilayer article includes a substrate that includes at least one of a ceramic compound and a Si-containing metal alloy. An outer layer includes stabilized zirconia. Intermediate layers are located between the outer layer and the substrate and include a mullite-containing layer and a chemical barrier layer. The mullite-containing layer includes 1) mullite or 2) mullite and an alkaline earth metal aluminosilicate. The chemical barrier layer is located between the mullite-containing layer and the outer layer. The chemical barrier layer includes at least one of mullite, hafnia, hafnium silicate and rare earth silicate (e.g., at least one of RE.sub.2 SiO.sub.5 and RE.sub.2 Si.sub.2 O.sub.7 where RE is Sc or Yb). The multilayer article is characterized by the combination of the chemical barrier layer and by its lack of a layer consisting essentially of barium strontium aluminosilicate between the mullite-containing layer and the chemical barrier layer. Such a barium strontium aluminosilicate layer may undesirably lead to the formation of a low melting glass or unnecessarily increase the layer thickness with concomitant reduced durability of the multilayer article. In particular, the chemical barrier layer may include at least one of hafnia, hafnium silicate and rare earth silicate.

  4. Transformation toughened ceramics for the heavy duty diesel engine technology program, phase 2

    NASA Technical Reports Server (NTRS)

    Musikant, S.; Samanta, S. C.; Architetto, P.; Feingold, E.

    1985-01-01

    The objective of this program is to develop an insulating structural ceramic for application in a heavy duty adiabatic diesel engine. The approach is to employ transformation toughening (TT) by additions of zirconia-hafnia solid solution (ZHSS). The feasibility of using ZHSS as a toughening agent in mullite and alumina has been demonstrated in Phase 1 of this work. Based on Phase 1 results, a decision was made to concentrate the Phase 2 effort on process optimization of the TT mullite. A strong factor in that decision was the low thermal conductivity and high thermal shock resistance of the mullite. Results of the Phase 2 effort indicate that optimum toughening of mullite by additions of ZHSS is difficult to achieve due to apparent sensitivity to morphology. The 48 ksi room temperature modulus-of-rupture (MOR) achieved in selected specimens is approximately 50% of the original strength target. The MOR deteriorated to 34 ksi at 800 C.

  5. Crystallization of a barium-aluminosilicate glass

    NASA Technical Reports Server (NTRS)

    Drummond, C. H., III; Lee, W. E.; Bansal, N. P.; Hyatt, M. J.

    1989-01-01

    The crystallization of a celsian glass composition was investigated as a possible high-temperature ceramic matrix material. Heat treatments invariably resulted in crystallization of the hexaclesian phase unless a flux, such as lithia, was added or a nucleating agent used (e.g., celsian seeds). TEM analysis revealed complex microstructures. Glasses with Mo additions contained hexacelsian, mullite, and an Mo-rich glass. Li2O additions stabilized celsian but mullite and Mo-rich glass were still present.

  6. New environmental barrier coating system on carbon-fiber reinforced silicon carbide composites

    NASA Astrophysics Data System (ADS)

    Latzel, S.; Vaßen, R.; Stöver, D.

    2005-06-01

    Carbon-fiber-reinforced silicon carbide composites (C/SiC) are promising materials for high-temperature, light weight structural components. However, a protective coating and environmental barrier coating (EBC) are necessary to prevent the oxidation of the carbon and the reaction of the formed silica scale with water vapor. Current EBC systems use multiple layers, each serving unique requirements. However, any mismatch in the coefficients of thermal expansion (CTE) creates internal stresses and might lead to crack formation. In this case, oxygen and water vapor penetrate through the EBC, reducing the lifetime of the component. Mullite (Al6Si2O13) is used in many known EBC systems on silicon-based ceramics either as an EBC itself or as a bondcoat. Due to its low CTE and its sufficient thermal cycling behavior, mullite was chosen in this investigation as a first layer. As mullite suffers loss of SiO2 when exposed to water vapor at high temperatures, an additional protective top coat is needed to complete the EBC system. Different oxides were evaluated to serve as top coat, especially high-temperature oxides with low coefficients of thermal expansion (LCTE). An EBC containing mullite as bondcoat and the LCTE oxide La2Hf2O7 as a top coat is proposed. Both layers were applied via atmospheric plasma spraying. In this paper, results of the influence of processing conditions on the microstructure of single mullite and LCTE oxide layers as well as mullite/LCTE oxide systems are presented. Special emphasis was directed toward the crystallinity of the mullite layer and, in the top layer, toward low porosity and reduced crack density.

  7. Ceramic-metal composite formation by reactive metal penetration

    SciTech Connect

    Loehman, R.E.; Ewsuk, K.G.; Fahrenholtz, W.G.; Lakshman, B.B.

    1996-11-01

    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.

  8. Development of iron oxide and titania treated fly ash based ceramic and its bioactivity.

    PubMed

    Sultana, Parveen; Das, Sukhen; Bhattacharya, Alakananda; Basu, Ruma; Nandy, Papiya

    2012-08-01

    The increasing accumulation of fly ash from thermal power plants poses a major problem to the environment. The present work reflects the novel utilization of this profusely available industrial waste in the form of an antibacterial hard ceramic material by treating fly ash with ferric oxide (Fe2O3) and titania (TiO2) during sintering process at 1600 °C. The developed material shows more than 90% bacterial reduction against both Gram-positive and Gram-negative bacteria. The mechanism of their antibacterial action was studied by transmission electron microscopy (TEM) image analysis of the bacterial cross-section. The developed ceramic material acquires hardness due to the enhancement of the natural mullite content in the matrix. The mullite content and the crystallinity of mullite have shown their increasing trend with increasing concentration of the metal oxide during sintering process. A maximum of ~37% increase in mullite was obtained for 7% w/w Fe2O3 and TiO2. Metal oxide lowered the activation energy of the reaction and enhanced the reaction rate of alumina (Al2O3)-silica (SiO2) to form mullite which increases the hardness. The study highlights novel utilization of fly ash as a hard ceramic antibacterial product (bioceramics) for both structural and hygiene applications in an eco-friendly way. PMID:24364932

  9. Evaluation of reusable surface insulation for space shuttle over a range of heat-transfer rate and surface temperature

    NASA Technical Reports Server (NTRS)

    Chapman, A. J.

    1973-01-01

    Reusable surface insulation materials, which were developed as heat shields for the space shuttle, were tested over a range of conditions including heat-transfer rates between 160 and 620 kW/sq m. The lowest of these heating rates was in a range predicted for the space shuttle during reentry, and the highest was more than twice the predicted entry heating on shuttle areas where reusable surface insulation would be used. Individual specimens were tested repeatedly at increasingly severe conditions to determine the maximum heating rate and temperature capability. A silica-base material experienced only minimal degradation during repeated tests which included conditions twice as severe as predicted shuttle entry and withstood cumulative exposures three times longer than the best mullite material. Mullite-base materials cracked and experienced incipient melting at conditions within the range predicted for shuttle entry. Neither silica nor mullite materials consistently survived the test series with unbroken waterproof surfaces. Surface temperatures for a silica and a mullite material followed a trend expected for noncatalytic surfaces, whereas surface temperatures for a second mullite material appeared to follow a trend expected for a catalytic surface.

  10. Kinetics of evaporation and gel formation in thin films of ceramic precursors.

    PubMed

    Gu, Yu; Chen, Zhaoxi; Borodinov, Nikolay; Luzinov, Igor; Peng, Fei; Kornev, Konstantin G

    2014-12-01

    Precursors derived from the hydrolysis of organic or inorganic salts have been widely used to produce ceramic coatings for a broad variety of applications. When applying the liquid precursors to the substrates, it is extremely challenging to control the film uniformity and homogeneity. The rate of solvent evaporation at different locations is different, causing the viscosity variation and flows in the film. There is very limited knowledge about the viscosity change in evaporating ceramic precursors. Therefore, it is crucial to understand the effect of evaporation on viscosity variation in thin films and droplets. We use magnetic rotational spectroscopy to study the time dependence of viscosity in mullite precursors. A correlation between the viscosity change and evaporation kinetics is revealed. This correlation was used to relate the change of viscosity to the concentration of mullite. A master curve relating viscosity to the mullite concentration was constructed and used to propose a possible scenario of the viscosity increase during solvent evaporation. PMID:25397585

  11. The geochemistry and bioreactivity of fly-ash from coal-burning power stations.

    PubMed

    Jones, Timothy; Wlodarczyk, Anna; Koshy, Lata; Brown, Patrick; Shao, Longyi; BéruBé, Kelly

    2009-07-01

    Fly-ash is a byproduct of the combustion of coal in power stations for the generation of electricity. The fly-ash forms from the melting of incombustible minerals found naturally in the coal. The very high coal combustion temperatures result in the formation of microscopic glass particles from which minerals such as quartz, haematite and mullite can later recrystallize. In addition to these minerals, the glassy fly-ash contains a number of leachable metals. Mullite is a well-known material in the ceramics industry and a known respiratory hazard. Macroscopically mullite can be found in a large range of morphologies; however microscopic crystals appear to favour a fibrous habit. Fly-ash is a recognized bioreactive material in rat lung, generating hydroxyl radicals, releasing iron, and causing DNA damage. However, the mechanisms of the bioreactivity are still unclear and the relative contributions of the minerals and leachable metals to that toxicity are not well known. PMID:19604058

  12. Refractory Oxide Coatings on Sic Ceramics

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Jacobson, Nathan S.; Miller, Robert A.

    1994-01-01

    Silicon carbide with a refractory oxide coating is potentially a very attractive ceramic system. It offers the desirable mechanical and physical properties of SiC and the environmental durability of a refractory oxide. The development of a thermal shock resistant plasma-sprayed mullite coating on SiC is discussed. The durability of the mullite/SiC in oxidizing, reducing, and molten salt environments is discussed. In general, this system exhibits better behavior than uncoated SiC. Areas for further developments are discussed.

  13. Pillared smectite clay coatings for ceramic-matrix composites

    SciTech Connect

    Jagota, S.; Harmer, M.A.; Lemon, M.F.; Jagota, A.; McCarron, E.M. III.

    1995-08-01

    This paper describes a novel route for the low-temperature formation of mullite, from pillared smectite clay precursors, for use as fiber coatings in ceramic-matrix composites. In particular, alumina-pillared bentonite converts in part to mullite at the unusually low temperature of about 800 C. The clay precursors display excellent film-forming capability and have been coated onto silicon carbide fibers. Mechanical tests on composites of the coated fibers and a borosilicate glass demonstrate their success as debond coatings, suggesting that this approach is a viable and simple route to oxide coatings for fibers.

  14. Thin film cadmium telluride solar cells

    SciTech Connect

    Chu, T.L.; Chu, S.S.; Xi, X.J.; Yang, Y.T.

    1983-05-01

    Cadmium telluride films have been deposited on coated graphite and mullite substrates by the direct combination of the vapors of the elements in a hydrogen atmosphere. The properties of nearly stoichiometric films on mullite substrates were measured by the van der Pauw technique in the temperature range of 25/sup 0/ - 150/sup 0/C. The deposition of n-type cadmium telluride by using hydrogen iodide as a dopant and the deposition of p-type cadmium telluride films by using arsine or phosphine as a dopant were studied. Schottky barrier solar cells were prepared from n-type cadmium telluride films and heterojunction cells from p-type cadmium telluride films.

  15. Oxidation-resistant interfacial coatings for continuous fiber ceramic composites

    SciTech Connect

    Stinton, D.P.; Besmann, T.M.; Bleier, A.; Shanmugham, S.; Liaw, P.K.

    1995-08-01

    Continuous fiber ceramic composites mechanical behavior are influenced by the bonding characteristics between the fiber and the matrix. Finite modeling studies suggest that a low-modulus interfacial coating material will be effective in reducing the residual thermal stresses that are generated upon cooling from processing temperatures. Nicalon{trademark}/SiC composites with carbon, alumina and mullite interfacial coatings were fabricated with the SiC matrix deposited using a forced-flow, thermal gradient chemical vapor infiltration process. Composites with mullite interfacial coatings exhibited considerable fiber pull-out even after oxidation and have potential as a composite system.

  16. Ceramic-bonded abrasive grinding tools

    DOEpatents

    Holcombe, Jr., Cressie E.; Gorin, Andrew H.; Seals, Roland D.

    1994-01-01

    Abrasive grains such as boron carbide, silicon carbide, alumina, diamond, cubic boron nitride, and mullite are combined with a cement primarily comprised of zinc oxide and a reactive liquid setting agent and solidified into abrasive grinding tools. Such grinding tools are particularly suitable for grinding and polishing stone, such as marble and granite.

  17. Ceramic-bonded abrasive grinding tools

    DOEpatents

    Holcombe, C.E. Jr.; Gorin, A.H.; Seals, R.D.

    1994-11-22

    Abrasive grains such as boron carbide, silicon carbide, alumina, diamond, cubic boron nitride, and mullite are combined with a cement primarily comprised of zinc oxide and a reactive liquid setting agent and solidified into abrasive grinding tools. Such grinding tools are particularly suitable for grinding and polishing stone, such as marble and granite.

  18. Article Including Environmental Barrier Coating System

    NASA Technical Reports Server (NTRS)

    Lee, Kang N. (Inventor)

    2015-01-01

    An enhanced environmental barrier coating for a silicon containing substrate. The enhanced barrier coating may include a bond coat doped with at least one of an alkali metal oxide and an alkali earth metal oxide. The enhanced barrier coating may include a composite mullite bond coat including BSAS and another distinct second phase oxide applied over said surface.

  19. Preparation and gas separation properties of zeolite T membrane.

    PubMed

    Cui, Ying; Kita, Hidetoshi; Okamoto, Ken-ichi

    2003-09-01

    Zeolite T membranes were synthesized on tubular porous mullite tubes by hydrothermal synthesis. The membranes selectively permeated carbon dioxide from CO2/CH4 and CO2/N2 mixtures with high separation performances, which were due to combined effects of molecular sieving and competitive adsorption. PMID:13678177

  20. Abundances and distribution of minerals and elements in high-alumina coal fly ash from the Jungar Power Plant, Inner Mongolia, China

    USGS Publications Warehouse

    Dai, S.; Zhao, L.; Peng, S.; Chou, C.-L.; Wang, X.; Zhang, Y.; Li, D.; Sun, Y.

    2010-01-01

    The fly ash from the Jungar Power Plant, Inner Mongolia, China, is unique because it is highly enriched in alumina (Al2O3>50%). The fly ash mainly consists of amorphous glass and mullite and trace amounts of corundum, quartz, char, calcite, K-feldspar, clay minerals, and Fe-bearing minerals. The mullite content in fly ash is as high as 37.4% because of high boehmite and kaolinite contents in feed coal. Corundum is a characteristic mineral formed during the combustion of boehmite-rich coal.Samples from the economizer were sieved into six size fractions (<120, 120-160, 160-300, 300-360, 360-500, and >500 mesh) and separated into magnetic, mullite+corundum+quartz (MCQ) and glass phases for mineralogical and chemical analysis. The corundum content increases but amorphous glass decreases with decreasing particle size. Fractions of small particle sizes are relatively high in mullite, probably because mullite was formed from fine clay mineral particles under high-temperature combustion condition. Similarly, fine corundum crystals formed in the boiler from boehmite in feed coal. The magnetic phase consists of hematite, magnetite, magnesioferrite, and MgFeAlO4 crystals. The MCQ phase is composed of 89% mullite, 6.1% corundum, 4.5% quartz, and 0.5% K-feldspar.Overall, the fly ash from the power plant is significantly enriched in Al2O3 with an average of 51.9%, but poor in SiO2, Fe2O3, CaO, MgO, Na2O, P2O5, and As. Arsenic, TiO2, Th, Al2O3, Bi, La, Ga, Ni, and V are high in mullite, and the magnetic matter is enriched in Fe2O3, CaO, MnO, TiO2, Cs, Co, As, Cd, Ba, Ni, Sb, MgO, Zn, and V. The remaining elements are high in the glass fraction. The concentration of K2O, Na2O, P2O5, Nb, Cr, Ta, U, W, Rb, and Ni do not clearly vary with particle size, while SiO2 and Hg decrease and the remaining elements clearly increase with decreasing particle size. ?? 2009 Elsevier B.V.

  1. Thermal/chemical stability of ceramic cross flow filter materials

    SciTech Connect

    Alvin, M.A.; Bahovchin, D.M.; Lippert, T.E.; Tressler, R.E.; McNerney, K.B.

    1992-01-01

    Westinghouse has undertaken a two phase program to determine possible long-term, high temperature influence that advanced coal-based power system environments may have on the stability of the ceramic cross flow filter elements. During the past year, we have principally focused our efforts on developing an understanding of the stability of the alumina/mullite filter material at high temperature (i.e., 870, 980, and 1100[degrees]C) under oxidizing conditions which contain gas phase alkali species. The alumina/mullite cross flow liter material that has consistently been used throughout the flow-through gas phase alkali testing segment of this program, consists of mullite rods or needles that are embedded within an amorphous phase which contains corundum (Al[sub 2]O[sub 3]) and anorthite (CaAl[sub 2]Si[sub 2]O[sub 8]). Due to the rapid cooling rate that was used to produce the alumina/mullite filter disc material from high fire, the matrix consists of 59.6 wt% mullite, 30.5 wt% amorphous, 5.1 wt% anorthite, and 4.8 wt% alumina. The relatively low, as-fabricated, hot strength of this material (841[plus minus]259 psi at 870[degrees]C) is a direct result of the high amorphous content which softens at temperatures of 870[degrees]C. Load versus deflection curves as a function of temperature indicate that this material is relatively brittle up to temperatures of 600[degrees]C. Both a loss of strength, as well as plastic deformation of the matrix occurs at [approximately]700[degrees]C. If cross flow filters are manufactured from an alumina/mullite matrix that contains an [approximately]30.5 wt% amorphous content, we suspect that the plastic nature of the glass phase could potentially serve as a substrate for fines collection during initial filter operation at 700[degrees]C. Similarly the plastic nature could potentially cause deformation of the liter under load.

  2. Thermal/chemical stability of ceramic cross flow filter materials

    SciTech Connect

    Alvin, M.A.; Bahovchin, D.M.; Lippert, T.E.; Tressler, R.E.; McNerney, K.B.

    1992-11-01

    Westinghouse has undertaken a two phase program to determine possible long-term, high temperature influence that advanced coal-based power system environments may have on the stability of the ceramic cross flow filter elements. During the past year, we have principally focused our efforts on developing an understanding of the stability of the alumina/mullite filter material at high temperature (i.e., 870, 980, and 1100{degrees}C) under oxidizing conditions which contain gas phase alkali species. The alumina/mullite cross flow liter material that has consistently been used throughout the flow-through gas phase alkali testing segment of this program, consists of mullite rods or needles that are embedded within an amorphous phase which contains corundum (Al{sub 2}O{sub 3}) and anorthite (CaAl{sub 2}Si{sub 2}O{sub 8}). Due to the rapid cooling rate that was used to produce the alumina/mullite filter disc material from high fire, the matrix consists of 59.6 wt% mullite, 30.5 wt% amorphous, 5.1 wt% anorthite, and 4.8 wt% alumina. The relatively low, as-fabricated, hot strength of this material (841{plus_minus}259 psi at 870{degrees}C) is a direct result of the high amorphous content which softens at temperatures of 870{degrees}C. Load versus deflection curves as a function of temperature indicate that this material is relatively brittle up to temperatures of 600{degrees}C. Both a loss of strength, as well as plastic deformation of the matrix occurs at {approximately}700{degrees}C. If cross flow filters are manufactured from an alumina/mullite matrix that contains an {approximately}30.5 wt% amorphous content, we suspect that the plastic nature of the glass phase could potentially serve as a substrate for fines collection during initial filter operation at 700{degrees}C. Similarly the plastic nature could potentially cause deformation of the liter under load.

  3. Protective coating for alumina-silicon carbide whisker composites

    DOEpatents

    Tiegs, Terry N.

    1989-01-01

    Ceramic composites formed of an alumina matrix reinforced with silicon carbide whiskers homogenously dispersed therein are provided with a protective coating for preventing fracture strength degradation of the composite by oxidation during exposure to high temperatures in oxygen-containing atmospheres. The coating prevents oxidation of the silicon carbide whiskers within the matrix by sealing off the exterior of the matrix so as to prevent oxygen transport into the interior of the matrix. The coating is formed of mullite or mullite plus silicon oxide and alumina and is formed in place by heating the composite in air to a temperature greater than 1200.degree. C. This coating is less than about 100 microns thick and adequately protects the underlying composite from fracture strength degradation due to oxidation.

  4. Growth and feeding response of Pseudoplusia includens (Lepidoptera:Noctuidae) to host plants grown in controlled carbon dioxide atmospheres

    SciTech Connect

    Lincoln, D.E.; Sionit, N.; Strain, B.R.

    1984-12-01

    Rising atmospheric carbon dioxide may alter plant/herbivore interactions. The projected rise in atmospheric carbon dioxide is expected to increase plant productivity, but little evidence is available regarding effects on insect feeding or growth. Leaves of soybean plants grown under three carbon dioxide regimes (350, 500, and 650 ..mu..l/liter) were fed to soybean looper larvae. Larvae fed at increasingly higher rates on plants from elevated carbon dioxide atmospheres: 80% greater rates on leaves from the 650 ..mu..l/liter treatment than on leaves from the 350 ..mu..l/litter treatment. Variation in larval feeding was related to the leaf content of nitrogen and water and to the leaf-specific weight, each of which was altered by the carbon dioxide growth regime of the soybean plants. This study suggests that the impact of herbivores may increase as the level of atmospheric carbon dioxide rises.

  5. Theoretical study of production of unique glasses in space. [kinetic relationships describing nucleation and crystallization phenomena

    NASA Technical Reports Server (NTRS)

    Larsen, D. C.; Sievert, J. L.

    1975-01-01

    The potential of producing the glassy form of selected materials in the weightless, containerless nature of space processing is examined through the development of kinetic relationships describing nucleation and crystallization phenomena. Transformation kinetics are applied to a well-characterized system (SiO2), an excellent glass former (B2O3), and a poor glass former (Al2O3) by conventional earth processing methods. Viscosity and entropy of fusion are shown to be the primary materials parameters controlling the glass forming tendency. For multicomponent systems diffusion-controlled kinetics and heterogeneous nucleation effects are considered. An analytical empirical approach is used to analyze the mullite system. Results are consistent with experimentally observed data and indicate the promise of mullite as a future space processing candidate.

  6. Interfacial and colloidal aspects of aqueous suspensions containing oxidic powders. Final report

    SciTech Connect

    Bleier, Alan

    1984-01-01

    This program addressed ceramics and colloid science research needs that underscore the physicochemical principles which govern the processing of oxide ceramic powders. Materials systems emphasized silica, alumina, zirconia, and mullite. The surface charge characteristics of the cited solids were determined using potentiometric techniques. Interfacial chemical reactions were thermodynamically evaluated. Zeta potential trends and values for silica and alumina systems were predicted reasonably well. Some surface behavior of mullite could be predicted from those of the constituent, silicon and aluminum oxides. Guidelines were generated for these problems and for a more complete description of the electrical double layers surrounding oxide ceramic powders in aqueous media. These efforts ultimately indicated that charge regulation is important to the processing of ceramics. A charge regulation model suggests that the electrostatic stabilizing effect of surface charge may critically depend on the volume concentration of powder.

  7. Dip coating process: Silicon sheet growth development for the large-area silicon sheet task of the low-cost silicon solar array project

    NASA Technical Reports Server (NTRS)

    Heaps, J. D.; Maciolek, R. B.; Harrison, W. B.; Wolner, H. A.; Hendrickson, G.; Nelson, L. D.

    1976-01-01

    To date, an experimental dip-coating facility was constructed. Using this facility, relatively thin (1 mm) mullite and alumina substrates were successfully dip-coated with 2.5 - 3.0 ohm-cm, p-type silicon with areas of approximately 20 sq cm. The thickness and grain size of these coatings are influenced by the temperature of the melt and the rate at which the substrate is pulled from the melt. One mullite substrate had dendrite-like crystallites of the order of 1 mm wide and 1 to 2 cm long. Their axes were aligned along the direction of pulling. A large variety of substrate materials were purchased or developed enabling the program to commence a substrate definition evaluation. Due to the insulating nature of the substrate, the bottom layer of the p-n junction may have to be made via the top surface. The feasibility of accomplishing this was demonstrated using single crystal wafers.

  8. Results of scientific achievements for production

    SciTech Connect

    Primachenko, V.V.

    1988-07-01

    During recent years the Aluminosilicate Refractory Laboratory of the Ukrainian Scientific-Research Institute for Refractories together with refractory, metallurgical, and other plants has solved a number of problems on the technology and service of refractories. This paper reviews those achievements. A method for producing refractories, vibrocasting, was developed and was found to increase labor productivity by two or three times. The properties of vibrocast refractory parts and materials are discussed and compared to those of pressed and pneumatically rammed refractories. A number of new high-quality forms of refractory production were introduced for fused mullite and heat-resistant mullite-corundum refractories. Increasing the service life of coke oven doors by using an unreinforced block liner and mechanizing their installation and removal was also discussed. The economic savings obtained via these and other developments are cited.

  9. Cadmium telluride films on foreign substrates

    SciTech Connect

    Chu, T.L.; Chu, S.S.; Pauleau, Y.; Murthy, K.; Stokes, E.D.; Russell, P.E.

    1983-01-01

    Thin films of cadmium telluride have been deposited on mullite and tungsten-coated graphite substrates at 500--700 /sup 0/C by the direct combination of cadmium and tellurium in a hydrogen atmosphere. Their microstructure and crystallographic properties were studied. The importance of controlling the Cd/Te molar ratio in the reaction mixture to obtain nearly stoichiometric films was demonstrated. The electrical properties of nonstoichiometric and nearly stoichiometric films on mullite substrates were measured by the van der Pauw technique. Schottky barriers were used to measure the electrical properties of cadmium telluride films on W/graphite substrates. The effective intragrain minority carrier diffusion length in n-type films was measured by the scanned electron beam method using a Schottky barrier structure.

  10. Chemical-vapor-infiltrated silicon nitride, boron nitride, and silicon carbide matrix composites

    SciTech Connect

    Ventri, R.D.; Galasso, F.S. )

    1990-07-01

    This paper reports composites of carbon/chemical-vapor-deposited (CVD) Si{sub 3}N{sub 4}, carbon/CVD BN, mullite/CVD SiC, and SiC yarn/CVD SiC prepared to determine if there were inherent toughness in these systems. The matrices were deposited at high enough temperatures to ensure that they were crystalline, which should make them more stable at high temperatures. The fiber-matrix bonding in the C/Si{sub 3}N{sub 4} composite appeared to be too strong; the layers of BN in the matrix of the C/BN were too weakly bonded; and the mullite/SiC composite was not as tough as the SiC/SiC composites. Only the SiC yarn/CVD SiC composite exhibited both strength and toughness.

  11. Internally Cooled Monolithic Silicon Nitride Aerospace Components

    NASA Technical Reports Server (NTRS)

    Best, Jonathan E.; Cawley, James D.; Bhatt, Ramakrishna T.; Fox, Dennis S.; Lang, Jerry (Technical Monitor)

    2000-01-01

    A set of rapid prototyping (RP) processes have been combined with gelcasting to make ceramic aerospace components that contain internal cooling geometry. A mold and core combination is made using a MM6Pro (Sanders Prototyping, Inc.) and SLA-250/40 (3Dsystems, Inc.). The MM6Pro produces cores from ProtoBuild (trademarked) wax that are dissolved in room temperature ethanol following gelcasting. The SLA-250/40 yields epoxy/acrylate reusable molds. Parts produced by this method include two types of specimens containing a high density of thin long cooling channels, thin-walled cylinders and plates, as well as a model hollow airfoil shape that can be used for burner rig evaluation of coatings. Both uncoated and mullite-coated hollow airfoils has been tested in a Mach 0.3 burner rig with cooling air demonstrating internal cooling and confirming the effectiveness of mullite coatings.

  12. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2001-01-01

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composition comprises a plurality of hollow oxide-based spheres of various dimensions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substrates are also provided.

  13. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2004-01-13

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composition comprises a plurality of hollow oxide-based spheres of various dimensions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substrates are also provided.

  14. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2000-01-01

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composite comprises a plurality of hollow oxide-based spheres of varios dimentions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substates are also provided.

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

    SciTech Connect

    1997-01-09

    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.

  16. Near-net-shape processing of metal-ceramic composites by reactive metal penetration

    SciTech Connect

    Fahrenholtz, W.G.; Ewsuk, K.G.; Ellerby, D.T.; Loehman, R.E.

    1996-09-01

    Metal-ceramic composites were made to near-net shape by reacting phase-pure mullite and mullite-glass preforms with molten Al using a reactive metal penetration process. Conversion of the two ceramic preforms to Al{sub 2}O{sub 3}/Al composites was accompanied by a 0.32% volume expansion and a 1.42% volume shrinkage, respectively. Molar volume and density calculations made assuming a net-shape reaction estimate {approximately}17 and {approximately}27 vol% Al to be present in the two composites after reaction. Results from quantitative stereology measurements used to quantify the concentration of metal in the reactively formed composites validate the calculations.

  17. Hydridosiloxanes as precursors to ceramic products

    DOEpatents

    Blum, Yigal D.; Johnson, Sylvia M.; Gusman, Michael I.

    1997-01-01

    A method is provided for preparing ceramic precursors from hydridosiloxane starting materials and then pyrolyzing these precursors to give rise to silicious ceramic materials. Si--H bonds present in the hydridosiloxane starting materials are catalytically activated, and the activated hydrogen atoms may then be replaced with nonhydrogen substituents. These preceramic materials are pyrolyzed in a selected atmosphere to give the desired ceramic product. Ceramic products which may be prepared by this technique include silica, silicon oxynitride, silicon carbide, metal silicates, and mullite.

  18. Development and assessment of two-phase porous matrices for use in all-oxide ceramic composites

    NASA Astrophysics Data System (ADS)

    Fujita, Hiroki

    The study focuses on a class of all-oxide continuous-fiber ceramic composite (CFCC) in which damage tolerance is derived from a highly-porous matrix, without an interphase at the fiber-matrix boundary. It includes experiments and analyses on both a representative oxide CFCC (developed earlier at UCSB) and a series of alumina-mullite matrices. The first part of the thesis addresses the stability of the porosity against densification and the associated implications for long-term durability at elevated temperatures. For this purpose, changes in the mechanical properties of the CFCC following 1000 hour exposure at 1000--1200°C were examined. Despite evidence of some strengthening of the matrix, the tensile properties in the 0°/90° orientation, including strength and failure strain, are unchanged. This strengthening is manifested to a more significant extent in the composite properties in the +/-45° orientation. The remainder of the thesis focuses on the assessment of weakly bonded mixtures of mullite and alumina as candidate matrices. Stability against densification is accomplished by using mullite particles as the major phase. This stability arises from the sluggish sintering kinetics of mullite. The matrix is strengthened by adding alumina, either as small particulates in the starting slurry or by subsequent impregnation and pyrolysis of a precursor solution. The modulus and the toughness of both types of mixtures as well as the changes in these properties following aging at 1200°C are examined. Models based on bonded particle aggregates are presented, assessed and calibrated. When coupled with a crack deflection parameter, the models are useful in determining the conditions under which damage tolerance is lost, because of excessive strengthening of the matrix. The implications of these results in matrix design are discussed.

  19. Material for a luminescent solar concentrator

    DOEpatents

    Andrews, L.J.

    1984-01-01

    A material for use in a luminescent solar concentrator, formed by ceramitizing the luminescent ion Cr/sup 3 +/ with a transparent ceramic glass containing mullite. The resultant material has tiny Cr/sup 3 +/-bearing crystallites dispersed uniformly through an amorphous glass. The invention combines the high luminescent efficiency of Cr/sup 3 +/ in the crystalline phase with the practical and economical advantages of glass technology.

  20. Aluminosilicates with varying alumina-silica ratios: synthesis via a hybrid sol-gel route and structural characterisation.

    PubMed

    Nampi, Padmaja Parameswaran; Moothetty, Padmanabhan; Berry, Frank John; Mortimer, Michael; Warrier, Krishna Gopakumar

    2010-06-01

    Aluminosilicates with varying Al2O3:SiO2 molar ratios (3:1, 3:2, 3:3 and 3:4) have been synthesized using a hybrid sol-gel route using boehmite sol as the precursor for alumina and tetraethyl orthosilicate (TEOS) as the precursor for silica. The synthesis of boehmite sol from aluminium nitrate, and its use as the alumina precursor, is cost effective compared to alkoxide precursors. Structural aspects, including bonding and coordination, are studied in detail for samples calcined in the temperature range 400-1400 °C using both NMR and FTIR spectroscopy: the results are correlated with phase formation data (spinel and high temperature phases) obtained from XRD and thermal analysis. FTIR results show a broadening of peaks at 800 °C indicating a disordered distribution of octahedral sites caused by crosslinking between AlO6 octahedral and SiO4 tetrahedral units prior to the formation of mullite. (27)Al MAS NMR spectra are consistent with a progressive decrease in the number of AlO6 polyhedra with increasing temperature corresponding to Al in these units being forced to adopt a tetrahedral coordination due to the increasing presence of similarly coordinated Si species. XRD results confirm the formation of pure mullite at 1250 °C for a 3Al2O3:2SiO2 system. At 1400 °C, phase pure mullite is observed for all compositions except 3Al2O3:SiO2 where α-Al2O3 is the major phase with traces of mullite. The synthesis of aluminosilicates through a hybrid sol-gel route and the detailed insight into structural features gained from spectroscopic and diffraction techniques contributes further to the development of these materials in applications ranging from nanocatalysts to high-temperature ceramics. PMID:20411190

  1. Hydridosiloxanes as precursors to ceramic products

    DOEpatents

    Blum, Y.D.; Johnson, S.M.; Gusman, M.I.

    1997-06-03

    A method is provided for preparing ceramic precursors from hydridosiloxane starting materials and then pyrolyzing these precursors to give rise to silicious ceramic materials. Si-H bonds present in the hydridosiloxane starting materials are catalytically activated, and the activated hydrogen atoms may then be replaced with nonhydrogen substituents. These preceramic materials are pyrolyzed in a selected atmosphere to give the desired ceramic product. Ceramic products which may be prepared by this technique include silica, silicon oxynitride, silicon carbide, metal silicates, and mullite.

  2. Ceramic joining

    SciTech Connect

    Loehman, R.E.

    1996-04-01

    This paper describes the relation between reactions at ceramic-metal interfaces and the development of strong interfacial bonds in ceramic joining. Studies on a number of systems are described, including silicon nitrides, aluminium nitrides, mullite, and aluminium oxides. Joints can be weakened by stresses such as thermal expansion mismatch. Ceramic joining is used in a variety of applications such as solid oxide fuel cells.

  3. Low cost silicon-on-ceramic photovoltaic solar cells

    NASA Technical Reports Server (NTRS)

    Koepke, B. G.; Heaps, J. D.; Grung, B. L.; Zook, J. D.; Sibold, J. D.; Leipold, M. H.

    1980-01-01

    A technique has been developed for coating low-cost mullite-based refractory substrates with thin layers of solar cell quality silicon. The technique involves first carbonizing one surface of the ceramic and then contacting it with molten silicon. The silicon wets the carbonized surface and, under the proper thermal conditions, solidifies as a large-grained sheet. Solar cells produced from this composite silicon-on-ceramic material have exhibited total area conversion efficiencies of ten percent.

  4. Microstructure Study For Optimization Of Dielectric Property Of Electrical Porcelain

    SciTech Connect

    Tak, S. K.; Shekhawat, M. S.; Mangal, R.

    2010-06-29

    Five sample mixtures of kaolin, ball clay, feldspar and Quartz were formulated and porcelain samples fabricated. Crystalline phases and mullite morphology were studied using XRD and SEM respectively. A composition of 30% kaolin, 15% ball clay, 30% feldspar and 25% quartz yielded a body with high dielectric strength of 19 kV/mm compare to an ISO graded product having dielectric strength 14.6 KV/mm after firing at 1225 deg. C.

  5. Microstructure Study For Optimization Of Dielectric Property Of Electrical Porcelain

    NASA Astrophysics Data System (ADS)

    Tak, S. K.; Shekhawat, M. S.; Mangal, R.

    2010-06-01

    Five sample mixtures of kaolin, ball clay, feldspar and Quartz were formulated and porcelain samples fabricated. Crystalline phases and mullite morphology were studied using XRD and SEM respectively. A composition of 30% kaolin, 15% ball clay, 30% feldspar and 25% quartz yielded a body with high dielectric strength of 19kV/mm compare to an ISO graded product having dielectric strength 14.6 KV/mm after firing at 1225°C.

  6. Extruded ceramic honeycomb and method

    DOEpatents

    Day, J. Paul

    1995-04-04

    Extruded low-expansion ceramic honeycombs comprising beta-spodumene solid solution as the principal crystal phase and with less than 7 weight percent of included mullite are produced by compounding an extrusion batch comprising a lithium aluminosilicate glass powder and a clay additive, extruding a green honeycomb body from the batch, and drying and firing the green extruded cellular honeycomb to crystallize the glass and clay into a low-expansion spodumene ceramic honeycomb body.

  7. Investigation of interlayer materials for the microwave joining of SiC

    SciTech Connect

    Silberglitt, R.; Palaith, D. ); Black, W.M.; Sa'adaldin, H.S. ); Katz, J.D.; Blake, R.D. )

    1991-01-01

    Microwave joining of ceramics has the potential for increased speed and convenience. Joints have been made in alumina, mullite and silicon nitride with flexure strength approaching, and in some cases exceeding, that of the as received material in a fraction of the time that is customarily required with conventional techniques. This paper describes the initial results of investigations aimed at applying microwave joining to SiC and other carbide ceramics. 8 refs., 5 figs.

  8. Solid-phase extraction of plant thionins employing aluminum silicate based extraction columns.

    PubMed

    Hussain, Shah; Güzel, Yüksel; Pezzei, Cornelia; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

    2014-08-01

    Thionins belong to a family of cysteine-rich, low-molecular-weight (∼5 KDa) biologically active proteins in the plant kingdom. They display a broad cellular toxicity against a wide range of organisms and eukaryotic cell lines. Thionins protect plants against different pathogens, including bacteria and fungi. A highly selective solid-phase extraction method for plant thionins is reported deploying aluminum silicate (3:2 mullite) powder as a sorbent in extraction columns. Mullite was shown to considerably improve selectivity compared to a previously described zirconium silicate embedded poly(styrene-co-divinylbenzene) monolithic polymer. Due to the presence of aluminum(III), mullite offers electrostatic interactions for the selective isolation of cysteine-rich proteins. In comparison to zirconium(IV) silicate, aluminum(III) silicate showed reduced interactions towards proteins which resulted into superior washings of unspecific compounds while still retaining cysteine-rich thionins. In the presented study, European mistletoe, wheat and barley samples were subjected to solid-phase extraction analysis for isolation of viscotoxins, purothionins and hordothionins, respectively. Matrix-assisted laser desorption/ionization time of flight mass spectroscopy was used for determining the selectivity of the sorbent toward thionins. The selectively retained thionins were quantified by colorimetric detection using the bicinchoninic acid assay. For peptide mass-fingerprint analysis tryptic digests of eluates were examined. PMID:24913248

  9. The study of aluminum loss and consequent phase transformation in heat-treated acid-leached kaolin

    SciTech Connect

    Foo, Choo Thye; Mahmood, Che Seman; Mohd Salleh, Mohamad Amran

    2011-04-15

    This study investigates the effect of Al leaching during Fe removal from kaolin to mullite. Heat-treated kaolin was obtained by heating natural kaolin at 400, 500, 600, 700, 800 and 900 deg. C. The heat-treated kaolin was then leached at 100 deg. C with 4 M, 3 M, 2 M, 1 M, 0.2 M solution of H{sub 2}SO{sub 4} and 0.2 M solution of oxalic acid. The dried samples were sintered to 1300 deg. C for 4 h at a heating rate of 10 deg. C min{sup -1}. X-ray diffractometry and differential thermal analysis were used to study the phase transformation of kaolin to mullite. It was found that 700 deg. C is the optimum preheat-treatment temperature to leach out Fe and also Al for both types of the acids used. The majority of the 4 M sulfuric acid-treated kaolins formed the cristobalite phase when sintered. On the other hand, 1 M, 0.2 M sulfuric acid and 0.2 M oxalic acid leached heat-treated kaolin formed mullite and quartz phase after sintering. - Research Highlights: {yields} Preheat-treatment of kaolin improves the leachability of unwanted iron. {yields} The optimum preheat-treatment temperature is 700 deg. C. {yields} Sintered 4 M sulfuric acid-treated kaolin majorly formed the cristobalite phase. {yields} Sintered 0.2 M oxalic acid-treated kaolin formed lesser amorphous silicate phase.

  10. Comprehensive Study on Ceramic Membranes for Low-Cost Microbial Fuel Cells.

    PubMed

    Pasternak, Grzegorz; Greenman, John; Ieropoulos, Ioannis

    2016-01-01

    Microbial fuel cells (MFCs) made with different types of ceramic membranes were investigated to find a low-cost alternative to commercially available proton exchange membranes. The MFCs operated with fresh human urine as the fuel. Pyrophyllite and earthenware produced the best performance to reach power densities of 6.93 and 6.85 W m(-3), respectively, whereas mullite and alumina achieved power densities of 4.98 and 2.60 W m(-3), respectively. The results indicate the dependence of bio-film growth and activity on the type of ceramic membrane applied. The most favourable conditions were created in earthenware MFCs. The performance of the ceramic membranes was related to their physical and chemical properties determined by environmental scanning electron microscopy and energy dispersive X-ray spectroscopy. The cost of mullite, earthenware, pyrophyllite and alumina was estimated to be 13.61, 4.14, 387.96 and 177.03 GBP m(-2), respectively. The results indicate that earthenware and mullite are good substitutes for commercially available proton exchange membranes, which makes the MFC technology accessible in developing countries. PMID:26692569

  11. Sintering and Interface Strain Tolerance of Plasma-Sprayed Thermal and Environmental Barrier Coatings

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Leissler, George W.; Miller, Robert A.

    2003-01-01

    Ceramic thermal and environmental barrier coatings will be more aggressively designed to protect gas turbine engine hot section SiC/SiC Ceramic Matrix Composite (CMC) components in order to meet future engine higher fuel efficiency and lower emission goals. A coating system consisting of a zirconia-based oxide topcoat (thermal barrier) and a mullite/BSAS silicate inner coat (environmental barrier) is often considered a model system for the CMC applications. However, the coating sintering, and thermal expansion mismatch between the zirconia oxide layer and the silicate environmental barrier/CMC substrate will be of major concern at high temperature and under thermal cycling conditions. In this study, the sintering behavior of plasma-sprayed freestanding zirconia-yttria-based thermal barrier coatings and mullite (and/or barium-strontium-aluminosilicate, i.e., BSAS) environmental barrier coatings was determined using a dilatometer in the temperature range of 1200-1500 C. The effects of test temperature on the coating sintering kinetics were systematically investigated. The plasma-sprayed zirconia-8wt.%yttria and mullite (BSAS) two-layer composite coating systems were also prepared to quantitatively evaluate the interface strain tolerance of the coating system under thermal cycling conditions based on the dilatomentry. The cyclic response of the coating strain tolerance behavior and interface degradation as a function of cycle number will also be discussed.

  12. Comprehensive Study on Ceramic Membranes for Low‐Cost Microbial Fuel Cells

    PubMed Central

    Pasternak, Grzegorz; Greenman, John

    2016-01-01

    Abstract Microbial fuel cells (MFCs) made with different types of ceramic membranes were investigated to find a low‐cost alternative to commercially available proton exchange membranes. The MFCs operated with fresh human urine as the fuel. Pyrophyllite and earthenware produced the best performance to reach power densities of 6.93 and 6.85 W m−3, respectively, whereas mullite and alumina achieved power densities of 4.98 and 2.60 W m−3, respectively. The results indicate the dependence of bio‐film growth and activity on the type of ceramic membrane applied. The most favourable conditions were created in earthenware MFCs. The performance of the ceramic membranes was related to their physical and chemical properties determined by environmental scanning electron microscopy and energy dispersive X‐ray spectroscopy. The cost of mullite, earthenware, pyrophyllite and alumina was estimated to be 13.61, 4.14, 387.96 and 177.03 GBP m−2, respectively. The results indicate that earthenware and mullite are good substitutes for commercially available proton exchange membranes, which makes the MFC technology accessible in developing countries. PMID:26692569

  13. Evaluation of Interfacial Interactions Between Ti-6Al-4V and Mold Use Ti-Added Backup Coat in Investment Casting

    NASA Astrophysics Data System (ADS)

    Cheng, Xu; Chai, Lianjing; Wu, Guoqing; Wang, Hong; Nan, Hai

    2016-05-01

    In this article, the chemical inertness of shell using Ti-added mullite backup coat against molten Ti-6Al-4V (Ti64) alloy was investigated. The metal/shell interfacial microstructures and compositions were characterized using an optical microscope, scanning electron microscope, roughness tester, and X-ray diffractometer; the hardened layer thickness was evaluated using a microhardness tester. By adding titanium powder into the mullite backup coat, the alpha case and hardened layer thickness of the Ti64 castings were largely reduced with good surface finishing. Silicon ions, from the backup coat, penetrated into the alloy and coarsened the β lath at the metal/shell interfacial area. The Ti powder in the mullite backup coat oxidized and interacted with silica during mold firing and casting, which reduced the silicon and oxygen concentrations at the metal/shell interfacial area. The oxygen penetration depth is thicker than the alpha case layer thickness, and around 0.26 wt pct, oxygen can obviously coarsen the alpha lath at the metal/shell interfacial area during investment casting.

  14. Processing and properties of prismatic composites that exhibit a threshold strength

    NASA Astrophysics Data System (ADS)

    Snyder, Mark Richard

    Incorporating thin compressive layers into ceramic composites allows for the arrest of cracks and produces a stress below which failure cannot occur, or threshold strength. This concept has been proven in laminar structures for cracks propagating in one direction. Here, a method for producing a threshold strength in multiple directions is addressed. This was accomplished by using composites consisting of alumina prismatic rods separated by a matrix of thin mullite/alumina layers that develop residual compressive stresses upon cooling from the sintering temperature. A colloidal processing method of producing these architectures was developed. This method consisted of making alumina fibers by extruding a plastically deformable consolidated, alumina body, coating the fibers with a mixture of mullite and alumina and consolidating the coated fibers into void free composites. This method was characterized to isolate the conditions necessary for producing composites. Consolidation of the fibers was accomplished by lowering the flow stress of the fibers and by eliminating the trapped pockets of air between them. Composites with varying residual stresses were produced by varying the thickness and mullite content of the compressive layers. Assessment of the residual stress state was performed by piezospectroscopy and indentation studies. The residual stress measurements were found to coincide with the behavior predicted by theoretical modeling and finite element analysis. Prismatic composites were shown to exhibit both crack arrest and flaw insensitive mechanical behavior. An equation for the propagation of a crack through a semi-circular compressive layer was developed. This model accurately described the average strength when the crack was observed to propagate straight through the compressive layers. In cases where the crack deflected or bifurcated, the model underestimated the average measured strengths. It was shown that increasing the volume fraction of mullite in the

  15. Selection of fluxing agent for coal ash and investigation of fusion mechanism: a first-principles study

    SciTech Connect

    Jie Li; Mei-Fang Du; Zhong-Xiao Zhang; Rong-Qing Guan; Yu-Shuang Chen; Ting-Yu Liu

    2009-01-15

    An approach based on the ab initio quantum chemical modeling (CASTEP, generalized gradient approximation (GGA), and density functional theory (DFT)) was first employed to guide the selection of the appropriate fluxing agent to reduce the coal ash melting temperature. Two kinds of typical Chinese coal ash A and B with a high-melting temperature were chosen as the investigated subjects. Result of the calculation shows that mullite mineral, which is the main component of coal ash, is easier to combine with an electron acceptor than with an electron donor. Because the cations of borax (Na{sub 2}B{sub 4}O{sub 7}10H{sub 2}O) and limestone can act as electron acceptors, borax and limestone were selected as the fluxing agents in our experiment. Results of the experiment show that the melting temperatures of coal ash A and B are both decreased by borax and limestone, respectively. Moreover, borax has a better fluxing effect than limestone under the same conditions. The further numerical study on the coal ash fusing mechanism indicates that the Na{sup +} and Ca{sup 2+} cations, as acceptors, can enter into the crystal lattice of mullite mainly through O(7) and O(8) and then cause the Al(6)-O(8) and Al(5)-O(7) bonds to rupture in the (AlO{sub 6})-octahedron. From this, mullite is forced to transform to feldspar and corundum minerals that have a low binding energy. Because of the phase change of minerals in the coal ash, the coal ash melting temperature is decreased by adding borax and limestone. 27 refs., 8 figs., 3 tabs.

  16. Copper sludge from printed circuit board production/recycling for ceramic materials: a quantitative analysis of copper transformation and immobilization.

    PubMed

    Tang, Yuanyuan; Lee, Po-Heng; Shih, Kaimin

    2013-08-01

    The fast development of electronic industries and stringent requirement of recycling waste electronics have produced a large amount of metal-containing waste sludge. This study developed a waste-to-resource strategy to beneficially use such metal-containing sludge from the production and recycling processes of printed circuit board (PCBs). To observe the metal incorporation mechanisms and phase transformation processes, mixtures of copper industrial waste sludge and kaolinite-based materials (kaolinite and mullite) were fired between 650 and 1250 °C for 3 h. The different copper-hosting phases were identified by powder X-ray diffraction (XRD) in the sintered products, and CuAl2O4 was found to be the predominant hosting phase throughout the reactions, regardless of the strong reduction potential of copper expected at high temperatures. The experimental results indicated that CuAl2O4 was generated more easily and in larger quantities at low-temperature processing when using the kaolinite precursor. Maximum copper transformations reached 86% and 97% for kaolinite and mullite systems, respectively, when sintering at 1000 °C. To monitor the stabilization effect after thermal process, prolonged leaching tests were carried out using acetic acid with an initial pH value of 2.9 to leach the sintered products for 20 days. The results demonstrated the decrease of copper leachability with the formation of CuAl2O4, despite different sintering behavior in kaolinite and mullite systems. This study clearly indicates spinel formation as the most crucial metal stabilization mechanism when sintering copper sludge with aluminosilicate materials, and suggests a promising and reliable technique for reusing metal-containing sludge as ceramic materials. PMID:23796110

  17. Development of low dielectric constant alumina-based ceramics for microelectronic substrates

    SciTech Connect

    Wu, S. J.

    1993-05-01

    The performance of high speed computers depends not only on IC chips, but also on the signal propagation speed between these chips. The signal propagation delay in a computer is determined by the dielectric constant of the substrate material to which the IC chips are attached. In this study, a ceramic substrate with a low dielectric constant (k {approx} 5.0) has been developed. When compared with the traditional alumina substrate (k {approx} 10.0), the new material corresponds to a 37% decrease in the signal propagation delay. Glass hollow spheres are used to introduce porosity (k = 1.0) to the alumina matrix in a controlled manner. A surface coating technique via heterogeneous nucleation in aqueous solution has been used to improve the high temperature stability of these spheres. After sintering at 1,400 C, isolated spherical pores are uniformly distributed in the almost fully dense alumina matrix; negligible amounts of matrix defects can be seen. All pores are isolated from each other. Detailed analyses of the chemical composition find that the sintered sample consists of {alpha}-alumina, mullite and residual glass. Mullite is the chemical reaction product of alumina and the glass spheres. Residual glass exists because current firing conditions do not complete the mullitization reaction. The dielectric constant of the sintered sample is measured and then compared with the predicted value using Maxwell`s model. Mechanical strength is evaluated by a four-point bending test. Although the flexural strength decreases exponentially with porosity, samples with 34% porosity (k {approx} 5.0) still maintain adequate mechanical strength for the proper operation of a microelectronic substrate.

  18. The physicochemistry and toxicology of CFA particles.

    PubMed

    Jones, Tim; Brown, Patrick; BéruBé, Kelly; Wlodarczyk, Anna; Longyi, Shao

    2010-01-01

    The term "technogenic particles" is used to describe airborne particulate matter (PM) produced during industrial processes. The most common of these is "fly ash" produced during combustion of solid and liquid fossil fuels. Coal fly ash is derived from the mineral and metal contaminants within coal in which particles (1) are distinctly spherical in shape, (2) are composed of 60-90% glass, and (3) often contain a range of contaminant metals. In addition, particles may contain recrystallized minerals, mainly quartz, mullite, and hematite; both quartz and mullite are recognized respiratory hazards. Fly ash particles from both UK and Chinese coal-burning power stations were characterized by field emission-scanning electron microscopy (morphology and size), x-ray diffraction (crystallinity and minerals), and inductively coupled plasma-mass spectroscopy (elemental composition). PM(10) samples were separated from bulk fly ash by a dry dust separator system. The plasmid scission assay (PSA) was used to measure damage produced by fly ash to plasmid bacteriophage PhiX174 RF DNA. The supercoiled DNA was either damaged or severely damaged by reactive oxygen species (ROS) generated by the fly ash at different concentrations. Geochemical analyses confirmed that the fly ash particles are predominantly glass, with a minor component of the minerals quartz, hematite, and mullite. Fly ash particles also contained a range of metals contaminants; however, these were mostly bound into the glass with only a small proportion potentially bioaccessible. PSA data showed that fly ash exhibited significant oxidative capacity when compared to negative control (MB H(2)O), indicating that ROS are likely to be the driving force underlying fly ash bioreactivity. PMID:20155577

  19. Contribution of aluminas and aluminosilicates to the formation of PCDD/Fs on fly ashes.

    PubMed

    Potter, Phillip M; Dellinger, Barry; Lomnicki, Slawomir M

    2016-02-01

    Chlorinated aromatics undergo surface-mediated reactions with metal oxides to form Environmentally Persistent Free Radicals (EPFRs) which can further react to produce polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs). Previous work using laboratory-made fly ash surrogates composed of transition metal oxides deposited on silica powder has confirmed their ability to mimic fly ash in the production of PCDD/Fs. However, little is known about the propensity of aluminas and aluminosilicates, other components of fly ash, to form PCDD/Fs. A fly ash sample containing both alumina and mullite, an aluminosilicate, was tested for PCDD/F formation ability and compared to PCDD/F yields from the thermal degradation of 2-monochlorophenol (2-MCP) precursor over γ-alumina, α-alumina, and mullite. A packed-bed flow reactor was used to investigate the thermal degradation of 2-MCP over the various catalysts at 200-600 °C. Fly ash gave similar PCDD/F yields to surrogates made with similar transition metal content. γ-alumina, which is thermodynamically unfavorable, was very catalytically active and gave low PCDD/F yields despite a high destruction of 2-MCP. Mullite and α-alumina, the thermodynamically favorable form of alumina, yielded higher concentrations of dioxins and products with a higher degree of chlorine substitution than γ-alumina. The data suggest that certain aluminas and aluminosilicates, commonly found in fly ash, are active catalytic surfaces in the formation of PCDD/Fs in the post-flame cool zones of combustion systems and should be considered as additional catalytic surfaces active in the process. PMID:26615490

  20. Novel, inorganic composites using porous, alkali-activated, aluminosilicate binders

    NASA Astrophysics Data System (ADS)

    Musil, Sean

    Geopolymers are an inorganic polymeric material composed of alumina, silica, and alkali metal oxides. Geopolymers are chemical and fire resistant, can be used as refractory adhesives, and are processed at or near ambient temperature. These properties make geopolymer an attractive choice as a matrix material for elevated temperature composites. This body of research investigated numerous different reinforcement possibilities and variants of geopolymer matrix material and characterized their mechanical performance in tension, flexure and flexural creep. Reinforcements can then be chosen based on the resulting properties to tailor the geopolymer matrix composites to a specific application condition. Geopolymer matrix composites combine the ease of processing of polymer matrix composites with the high temperature capability of ceramic matrix composites. This study incorporated particulate, unidirectional fiber and woven fiber reinforcements. Sodium, potassium, and cesium based geopolymer matrices were evaluated with cesium based geopolymer showing great promise as a high temperature matrix material. It showed the best strength retention at elevated temperature, as well as a very low coefficient of thermal expansion when crystallized into pollucite. These qualities made cesium geopolymer the best choice for creep resistant applications. Cesium geopolymer binders were combined with unidirectional continuous polycrystalline mullite fibers (Nextel(TM) 720) and single crystal mullite fibers, then the matrix was crystallized to form cubic pollucite. Single crystal mullite fibers were obtained by the internal crystallization method and show excellent creep resistance up to 1400°C. High temperature flexural strength and flexural creep resistance of pollucite and polycrystalline/single-crystal fibers was evaluated at 1000-1400°C.

  1. Phase transformations in 40-60-GPa shocked gneisses from the Haughton Crater (Canada): An Analytical Transmission Electron Microscopy (ATEM) study

    NASA Technical Reports Server (NTRS)

    Martinez, I.; Guyot, F.; Schaerer, U.

    1992-01-01

    In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.

  2. Dip-coated sheet silicon solar cells

    NASA Technical Reports Server (NTRS)

    Heaps, J. D.; Maciolek, R. B.; Zook, J. D.; Scott, M. W.

    1976-01-01

    A cost-effective method is being developed for producing solar cell quality sheet silicon by dip coating inexpensive ceramic substrates with a thin layer of large grain silicon. Mullite (Aluminum Silicate) ceramic substrates coated with a thin layer of graphite have been dipped into molten silicon to produce 20-150 micron thick layers having grain sizes as large as .4 cm x 4 cm. With these silicon layers photovoltaic diodes have been fabricated with measured and inherent conversion efficiencies of 4% and 7%, respectively.

  3. Micromechanical stresses in SiC-reinforced Al2O3 composites

    NASA Technical Reports Server (NTRS)

    Li, Zhuang; Bradt, Richard C.

    1989-01-01

    Applying an Eshelby (1957) approach, the internal micromechanical stresses within an SiC-inclusion-reinforced (platelet to whisker geometries) polycrystalline alumina matrix composite were calculated. The results are compared to the experimental residual stress measurements of a SiC-whisker-reinforced Al2O3 by Predecki, et al. (in press) and found to be in excellent agreement. The calculations are then extended to SiC-reinforced composites with polycrystalline mullite, silicon nitride, and cordierite matrices. It is concluded that the internal stresses are significantly influenced by the inclusion geometry as well as the thermoelastic differences between the inclusion and the matrix and also the volume fraction.

  4. Crystallization paths in SiO2-Al2O3-CaO system as a genotype of silicate materials

    NASA Astrophysics Data System (ADS)

    Lutsyk, V. I.; Zelenaya, A. E.

    2013-12-01

    The phases trajectories in the fields of primary crystallization of cristobalite (SiO2cr), tridymite (SiO2tr), mullite (3Al2O3-2SiO2) and in a field of liquid immiscibility are analyzed on a basis of computer model for T-x-y diagram of SiO2-Al2O3-CaO system. The concentration fields with unique set of microconstituents and the fields without individual crystallization schemes and microconstituents are revealed.

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

    SciTech Connect

    Fahrenholtz, W.F.; Ewsuk, K.G.; Loehman, R.E.

    1996-12-31

    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 from {approximately}90 to {approximately}200 kJ/mole.

  6. Performance and stability of advanced monolithic and fiber reinforced composite candle filters during PCFBC operation

    SciTech Connect

    Alvin, M.A.

    1996-12-31

    Advanced clay bonded silicon carbide, alumina/mullite and CVI-SiC fiber reinforced composite porous ceramic candle filters have been identified for use in pressurized circulating fluidized-bed combustion (PCFBC) systems where operating temperatures approach 870--900 C. In this paper the author will discuss the performance of these filter elements, and explore the response and stability of the advanced filter materials after 540 hours of operation in Foster Wheeler`s PCFBC system in Karhula, Finland. The potential use of the advanced filter materials for extended operating life in high temperature, pressurized, coal-fired process applications will also be addressed.

  7. Rigid separator lead acid batteries

    SciTech Connect

    Cannone, A.G.; Salkind, A.J.; Stempin, J.L.; Wexell, D.R.

    1996-11-01

    Lead acid cells assembled with extruded separators displayed relatively uniform capacity and voltage parameters through 100{sup +} cycles of charge/discharge. This contrasts to failure of control cells with glass mat separators after 60 cycles. The mullite/alumina separators with 50, 60, and 70% porosity separators appear suitable for both flooded and sealed lead acid cell applications. The advantages of the rigid ceramic separators over fiber mat materials are in the uniformity of capacity and voltage, the ease of cell assembly, and the probability that firm stacking pressure on the active material will yield greater cycle life, especially at elevated temperatures.

  8. Interface engineering for the passivation of c-Si with O3-based atomic layer deposited AlOx for solar cell application

    NASA Astrophysics Data System (ADS)

    Lee, Hyunju; Tachibana, Tomihisa; Ikeno, Norihiro; Hashiguchi, Hiroki; Arafune, Koji; Yoshida, Haruhiko; Satoh, Shin-ichi; Chikyow, Toyohiro; Ogura, Atsushi

    2012-04-01

    We have investigated the effects of deposition temperature and post-annealing on the passivation performance of AlOx films deposited by O3-based atomic layer deposition for crystalline Si. We found that the dramatic enhancement in the passivation performance of room-temperature deposited AlOx films by post-annealing is due to the phase transformation of aluminum silicate to mullite in an AlOx interlayer and the resulting self-aligned AlOx/SiOx interface. This result is interesting for the fabrication of high-performance silicon solar cells with AlOx passivation layers.

  9. Oxidation-resistant interface coatings for Nicalon/SiC composites

    SciTech Connect

    Stinton, D.P.; Besmann, T.M.; Lowden, R.A.; Liaw, P.K.; Shanmugham, S.

    1997-12-01

    Nicalon/SiC composites with thin C and C/oxide/C interfaces were fabricated. The oxide layers, mullite and Al{sub 2}O{sub 3}-TiO{sub 2}, were deposited by a sol-gel process, while the C layer was deposited by a chemical vapor infiltration method. The fabricated composites were flexure tested in both as-processed and oxidized conditions. Composites with C and C/oxide/C interfaces retained graceful failure even after 500 h oxidation at 1000 C, but with reduced flexural strengths.

  10. Method of depositing a coating on Si-based ceramic composites

    NASA Technical Reports Server (NTRS)

    Wang, Hongyu (Inventor); Lau, Yuk-Chiu (Inventor); Spitsberg, Irene (Inventor); Henry, Arnold T. (Inventor)

    2004-01-01

    A process of depositing a coating system suitable for use as an environmental barrier coating on various substrate materials, particularly those containing silicon and intended for high temperature applications such as the hostile thermal environment of a gas turbine engine. The process comprises depositing a first coating layer containing mullite, and preferably a second coating layer of an alkaline earth aluminosilicate, such as barium-strontium-aluminosilicate (BSAS), by thermal spraying while maintaining the substrate at a temperature of 800.degree. C. or less, preferably 500.degree. C. or less, by which a substantially crack-free coating system is produced with desirable mechanical integrity.

  11. Determination of anisotropy and multimorphology in fly ash based geopolymers

    NASA Astrophysics Data System (ADS)

    Khan, M. Irfan; Azizli, Khairun; Sufian, Suriati; Man, Zakaria; Siyal, Ahmer Ali; Ullah, Hafeez

    2015-07-01

    In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

  12. Oxidation behavior in reaction-bonded aluminum-silicon alloy/alumina powder compacts

    SciTech Connect

    Yokota, S.H.

    1992-12-01

    Goal of this research is to determine the feasibility of producing low-shrinkage mullite/alumina composites by applying the reaction-bonded alumina (RBAO) process to an aluminum-silicon alloy/alumina system. Mirostructural and compositional changes during heat treatment were studied by removing samples from the furnace at different steps in the heating schedule and then using optical and scanning electron microscopy, EDS and XRD to characterize the powder compacts. Results suggest that the oxidation behavior of the alloy compact is different from the model proposed for the pure Al/alumina system.

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

    SciTech Connect

    Nowok, J.W.; Hurley, J.P.

    1995-03-01

    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.

  14. Enhancement of oxidation resistance of silicon carbide by high-dose and multi-energy aluminum implantation

    SciTech Connect

    Yang, Z.; Du, H.; Libera, M.; Withrow, S.P.; Casas, L.M.; Lareau, R.T.

    1993-12-31

    High-dose and multi-energy aluminum implantation of {alpha}-SiC (0001) was carried out to achieve a broad aluminum distribution extending from the sample surface to a depth of approximately 350 nm. Oxidation resistance of the implanted crystals was studied in 1 atm flowing oxygen at 1300C. Aluminum implantation resulted in a 45% improvement in the oxidation resistance of {alpha}-SiC as compared with unimplanted crystals due to the formation of structurally dense mullite (3Al{sub 2}O{sub 3}.2SiO{sub 2}) in the oxidation scale.

  15. Synthesis of hydroxy sodalite from coal fly ash using waste industrial brine solution.

    PubMed

    Musyoka, Nicholas M; Petrik, Leslie F; Balfour, Gillian; Gitari, Wilson M; Hums, Eric

    2011-01-01

    The effect of using industrial waste brine solution instead of ultra pure water was investigated during the synthesis of zeolites using three South African coal fly ashes as Si feedstock. The high halide brine was obtained from the retentate effluent of a reverse osmosis mine water treatment plant. Synthesis conditions applied were; ageing of fly ash was at 47 ° C for 48 hours, and while the hydrothermal treatment temperature was set at 140 ° C for 48 hours. The use of brine as a solvent resulted in the formation of hydroxy sodalite zeolite although unconverted mullite and hematite from the fly ash feedstock was also found in the synthesis product. PMID:22175873

  16. Determination of anisotropy and multimorphology in fly ash based geopolymers

    SciTech Connect

    Khan, M. Irfan Azizli, Khairun Sufian, Suriati Man, Zakaria Siyal, Ahmer Ali Ullah, Hafeez

    2015-07-22

    In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

  17. High Temperature Aerogels in the Al2O3-SiO2 System

    NASA Technical Reports Server (NTRS)

    Hurwitz, Frances I.; Aranda, Denisse V.; Gallagher, Meghan E.

    2008-01-01

    Al2O3-SiO2 aerogels are of interest as constituents of thermal insulation systems for use at high temperatures. Al2O3 and mullite aerogels are expected to crystallize at higher temperatures than their SiO2 counterparts, hence avoiding the shrinkages that accompany the formation of lower temperature SiO2 phases and preserving pore structures into higher temperature regimes. The objective of this work is to determine the influence of processing parameters on shrinkage, gel structure (including surface area, pore size and distribution) and pyrolysis behavior.

  18. Effect of mineralizers on the sintering of porcelain bodies (a review)

    SciTech Connect

    Maslennikova, G.N.; Koneshova, T.I.

    1987-11-01

    The authors assess the effects of a wide range of mineralizing agents on the structure formation of porcelain in order to arrive at optimal crystallization and structure parameters for the resulting porcelain crystals and to determine those agents which best contribute to the energy efficiency of the sintering process. The assessment is carried out specifically for the kinetics of mullite formation. Reagents tested include salts of sodium, potassium, lithium, calcium, magnesium, zinc, and aluminum, and the oxides of chromium, titanium, iron, zirconium, molybdenum, boron, and tin.

  19. Thermal Conductivity and Thermal Gradient Cyclic Behavior of Refractory Silicate Coatings on SiC/SiC Ceramic Matrix Composites

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

    2001-01-01

    Plasma-sprayed mullite and BSAS coatings have been developed to protect SiC/SiC ceramic matrix composites from high temperature environmental attack. In this study, thermal conductivity and thermal barrier functions of these coating systems are evaluated using a laser high-heat-flux test rig. The effects of water vapor on coating thermal conductivity and durability are studied by using alternating furnace and laser thermal gradient cyclic tests. The influence of laser high thermal-gradient cycling on coating failure modes is also investigated.

  20. Reactions and microstructure at ceramic/metal interfaces

    SciTech Connect

    Tomsia, A.P.; Loehman, R.E.

    1993-12-31

    Reactions of Ti and Zr with AlN, Al{sub 2}O{sub 3} and mullite were studied. The substrates were selected to represent a simple nitride (AlN), a simple oxide (Al{sub 2}O{sub 3}), and a complex oxide (mullite). The activities of the Ti and Zr were varied by dissolving them at 1 and 5 wt.% in the 72Ag-28Cu eutectic composition, which is otherwise unreactive with the ceramics. Reactions were studied by measuring the variation of the alloy contact angle on the ceramic with time at temperature and by determining the compositions of interfacial reaction products. The reaction products were determined by SEM-EDS, EPMA and XRD hose analysis. Contact angles were lower for Ti alloys than for those containing Zr. Reaction products were primarily the nitrides of Zr and Ti for reaction with AlN and the respective oxides for reaction with Al{sub 2}O{sub 3}.Complex alloy phases were found in the metal away from the ceramic-metal reaction zone.

  1. Microstructural characterization and influence of manufacturing parameters on technological properties of vitreous ceramic materials

    SciTech Connect

    Njoya, D.; Hajjaji, M.; Bacaoui, A.; Njopwouo, D.

    2010-03-15

    Microstructure of vitreous ceramic samples manufactured from kaolinitic-clay and feldspars raw materials from Cameroon was investigated in the range 1150-1250 deg. C by X-ray diffraction and scanning electron microscopy and by measuring some technological properties. Moreover, the simultaneous influence of feldspars content, heating temperature and soaking time on water absorption and firing shrinkage was evaluated by adopting the response surface methodology (Doehlert matrix), using the New Efficient Methodology for Research using Optimal Design (NEMROD) software. The results show that a spinel phase, mullite, glassy phase and some amount of hematite were formed. However, the spinel phase and potassic feldspar, as compared to the sodic one, disappeared at moderate firing temperature and soaking time. Apparently, mullite developed from spinel phase, which is formed from the demixion of metakaolin. On the other hand, it is found that the effects of fluxing content and firing temperature on the measured properties were almost similar and more influent than soaking time. Antagonistic and synergetic interactions existed between the considered parameters, and their importance differed for the considered properties. By using this mathematical tool, suitable operating conditions for manufacturing vitreous bodies were determined.

  2. Evaluation of ceramic filter material, selection for application

    SciTech Connect

    Alvin, M.A.; Tressler, R.E.; Lippert, T.E.; Diaz, E.S.

    1993-09-01

    Field testing in several of the Westinghouse Advanced Particulate Filtration (APF) systems has indicated that the oxide-based materials are more susceptible to thermal shock which results from system transients (i.e., combustion of char or reducing gases; system startup/turbine transients). The current clay bonded silicon carbide filter materials have a higher thermal shock resistance, but appear to be more susceptible to high temperature creep, as well as to changes that occur within the binder phase(s). Strength has frequently been used to assess what effects advanced coal fired process systems have on the stability and projected life of the various porous ceramic filter materials (Tables 1 and 2). Based on the numerous phase changes that occur, and the influence of pulse cleaning on the thermal fatigue characteristics of both the alumina/mullite and clay bonded silicon carbide filter materials, alternate material properties as thermal conductivity, thermal coefficient of expansion, elastic modulus, fracture toughness, and emissivity as a function of thermal/chemical aging are now being considered as critical factors for projecting filter durability and operating life. Table 3 provides a summary of the as-manufactured material properties for the alumina/mullite and clay bonded silicon carbide filter materials which have been used in the Westinghouse`s APF systems. Effort is currently being directed to determine how these properties change during thermal aging of the filters in various subpilot and pilot plant systems.

  3. High temperature alkali corrosion of ceramics in coal gas: Final report

    SciTech Connect

    Pickrell, G.R.; Sun, T.; Brown, J.J. Jr.

    1994-12-31

    There are several ceramic materials which are currently being considered for use as structural elements in coal combustion and coal conversion systems because of their thermal and mechanical properties. These include alumina (refractories, membranes, heat engines); silicon carbide and silicon nitride (turbine engines, internal combustion engines, heat exchangers, particulate filters); zirconia (internal combustion engines, turbine engines, refractories); and mullite and cordierite (particulate filters, refractories, heat exchangers). High temperature alkali corrosion has been known to cause premature failure of ceramic components used in advanced high temperature coal combustion systems such as coal gasification and clean-up, coal fired gas turbines, and high efficiency heat engines. The objective of this research is to systematically evaluate the alkali corrosion resistance of the most commonly used structural ceramics including silicon carbide, silicon nitride, cordierite, mullite, alumina, aluminum titanate, and zirconia. The study consists of identification of the alkali reaction products and determination of the kinetics of the alkali reactions as a function of temperature and time. 145 refs., 29 figs., 12 tabs.

  4. Testing of the Westinghouse hot gas filter at Ahlstrom Pyropower Corporation

    SciTech Connect

    Lippert, T.; Alvin, M.A.; Bruck, G.J.; Isaksson, J.; Dennis, R.A.; Brown, R.A.

    1995-12-31

    A single cluster Westinghouse hot gas filter has been tested for over 2050 hours on Ahlstrom Pyropower Corporation`s Pressurized Circulating Fluidized Bed (PCFB) 10 MW test facility at Karhula, Finland. This filter system, which houses 128 ceramic candles in three plenums, takes the full flow from the PCFB. Two candle types, an alumina/mullite candle manufactured by Coors Ceramics and a clay bonded SiC candle manufactured by Refractron Corporation were evaluated over a range of filtration face velocities, dust loadings, coal types and temperatures. Both candle systems allowed less than 3 ppmw to exit the candles with inlet dust loadings as high as 18,000 ppm. Stable pressure drop across the filter in the steady state was achieved with less than 60 in wg (150 mbar) for either candle system. Pulse cleaning air pressure was less than 435 psi (30 bar) when the plant was operated at 145 to 175 psi (10 to 12 bar). Improvements to the flow distribution in the filter housing and fine tuning of the pulsing system were incorporated. The alumina/mullite candles accumulated around 750 hours at operating temperatures to 1,650 F (900 C). The SiC accumulated about 1,300 hours at temperatures to 1,560 F (850 C). Strength measurements and SEM examination of the candle material have been conducted to help evaluate long-term ceramic candle filter material stability. All metal structures within the filter assembly performed as designed.

  5. New Measurements of Activation Volume in Olvine Under Anhydrous Conditions

    SciTech Connect

    Durham, W.; Mei, S; Kohlstedt, D; Wang, L; Dixon, N

    2009-01-01

    A new cell assembly for the deformation-DIA (D-DIA) shows promise for limiting the water content of samples and providing a more mechanically stable environment for deformation. The 6-mm cubic cell consists of a 6-mm diameter mullite sphere cradled in a web of unfired pyrophyllite. The pyrophyllite flows during initial compression of the D-DIA to form gaskets between the six anvils while the mullite flows to become a nearly cubic-shaped pressure medium. Measurements on olivine indicate more than one order of magnitude drop in water content to <40 ppm H/Si compared with the boron-epoxy medium. Improved mechanical stability is achieved by elimination of the thermocouple from the assembly and determination of temperature from calibration curves of furnace power vs. temperature. Three samples of polycrystalline orthopyroxene-buffer San Carlos olivine have been deformed in high-temperature creep in the new cell, at pressures of 2.7-4.9 GPa and temperatures near 1473 K. Strength is consistent with that measured in the gas-apparatus at lower pressures. Over the pressure range investigated we resolve an activation volume for creep of dry olivine of V* = 9.5 {+-} 7 x 10-6 m3/mol.

  6. Dip coating process: Silicon sheet growth development for the large-area silicon sheet task of the low-cost silicon solar array project

    NASA Technical Reports Server (NTRS)

    Heaps, J. D.; Maciolek, R. B.; Zook, J. D.; Harrison, W. B.; Scott, M. W.; Hendrickson, G.; Wolner, H. A.; Nelson, L. D.; Schuller, T. L.; Peterson, A. A.

    1976-01-01

    The technical and economic feasibility of producing solar cell quality sheet silicon by dip-coating one surface of carbonized ceramic substrates with a thin layer of large grain polycrystalline silicon was investigated. The dip-coating methods studied were directed toward a minimum cost process with the ultimate objective of producing solar cells with a conversion efficiency of 10% or greater. The technique shows excellent promise for low cost, labor-saving, scale-up potentialities and would provide an end product of sheet silicon with a rigid and strong supportive backing. An experimental dip-coating facility was designed and constructed, several substrates were successfully dip-coated with areas as large as 25 sq cm and thicknesses of 12 micron to 250 micron. There appears to be no serious limitation on the area of a substrate that could be coated. Of the various substrate materials dip-coated, mullite appears to best satisfy the requirement of the program. An inexpensive process was developed for producing mullite in the desired geometry.

  7. Friction and wear of oxide-ceramic sliding against IN-718 nickel base alloy at 25 to 800 C in atmospheric air

    NASA Technical Reports Server (NTRS)

    Sliney, Harold E.; Deadmore, Daniel L.

    1989-01-01

    The friction and wear of oxide-ceramics sliding against the nickel base alloy IN-718 at 25 to 800 C were measured. The oxide materials tested were mullite (3Al2O3.2SiO2); lithium aluminum silicate (LiAlSi(x)O(y)); polycrystalline monolithic alpha alumina (alpha-Al2O3); single crystal alpha-Al2O3 (sapphire); zirconia (ZrO2); and silicon carbide (SiC) whisker-reinforced Al2O3 composites. At 25 C the mullite and zirconia had the lowest friction and the polycrystalline monolithic alumina had the lowest wear. At 800 C the Al2O3-8 vol/percent SiC whisker composite had the lowest friction and the Al2O3-25 vol/percent SiC composite had the lowest wear. The friction of the Al2O3-SiC whisker composites increased with increased whisker content while the wear decreased. In general, the wear-resistance of the ceramics improve with their hardness.

  8. Evaluation of the interfacial mechanical properties in fiber-reinforced ceramic composites

    SciTech Connect

    Ferber, M.K.; Wereszczak, A.A.; Riester, L.; Lowden, R.A.; Chawla, K.K.

    1993-06-01

    The present study examined the application of a micro-indentation technique to the measurement of interfacial properties in fiber reinforced ceramic composites. Specific fiber/matrix systems included SiC/glass, SiC/macro-defect-free (MDF) cement, SiC/SiC, and mullite/glass. The effect of fiber coatings upon the interfacial properties was also investigated. These properties, which included the debond strength, interfacial shear stress, and residual axial fiber stress, were evaluated by measuring the force-displacement curves generated during load-unload cycles. Estimates of these three stress values were obtained by matching the experimental force-displacement curves with data predicted from an existing model. In general the SiC/glass composites exhibited the lowest values of the interfacial shear and debond stresses. The sliding characteristics of the SiC/MDF cement and SiC/SiC composites were strongly influenced by the residual axial stress and the nature of the fiber coating. In the case of the mullite/glass composite, the high values of the interfacial shear and debond stresses reduced the measurement sensitivity, thereby increasing the uncertainty in the estimates of the interfacial properties. 17 refs, 6 figs, 1 tab.

  9. Coating system to permit direct brazing of ceramics

    DOEpatents

    Cadden, Charles H.; Hosking, F. Michael

    2003-01-01

    This invention relates to a method for preparing the surface of a ceramic component that enables direct brazing using a non-active braze alloy. The present invention also relates to a method for directly brazing a ceramic component to a ceramic or metal member using this method of surface preparation, and to articles produced by using this brazing method. The ceramic can be high purity alumina. The method comprises applying a first coating of a silicon-bearing oxide material (e.g. silicon dioxide or mullite (3Al.sub.2 O.sub.3.2SiO.sub.2) to the ceramic. Next, a thin coating of active metal (e.g. Ti or V) is applied. Finally, a thicker coating of a non-active metal (e.g. Au or Cu) is applied. The coatings can be applied by physical vapor deposition (PVD). Alternatively, the active and non-active metals can be co-deposited (e.g. by sputtering a target made of mullite). After all of the coatings have been applied, the ceramic can be fired at a high temperature in a non-oxidizing environment to promote diffusion, and to enhance bonding of the coatings to the substrate. After firing, the metallized ceramic component can be brazed to other components using a conventional non-active braze alloy. Alternatively, the firing and brazing steps can be combined into a single step. This process can replace the need to perform a "moly-manganese" metallization step.

  10. Effect of thermal treatment on the nano-structure and phase transformation of metakaolin-based geopolymers.

    PubMed

    Kim, Yongsung; Kang, Seunggu

    2014-11-01

    Enhancement of the mechanical strength of metakaolin-based geopolymers activated with NaOH was attempted by calcining metakaolin at a higher temperature than that commonly reported. Increasing the calcination temperature from 750 degrees C to 1150 degrees C promoted the recrystallization of mullite. Two type of zeolite of sodium aluminum silicate hydrates were found in the geopolymers made of metakaolin calcined at 750 degrees C-1050 degrees C. The h-zeolite [Na6(AlSiO4)6 x H2O] was not found in the geopolymer made of metakaolin calcined above 900 degrees C, while Z-zeolite [Na2O x Al2O3 x SiO2 x H2O] remained in specimens calcined at up to 1050 degrees C, All zeolite disappeared above 1150 degrees C. The pozzolanic reaction generates very small particles of 10-30 nm on the surface of metakaolin grains of 0.2-0.6 μm, rendering the matrix denser by binding the grains. The maximum compressive strength was revealed with the geopolymer made of metakaolin calcined at 1050 degrees C. The reason for the increased strength of the geopolymer obtained using higher calcination temperature is thought to be the combined effects of matrix hardening by geopolymeric reaction and reinforcement by mullite crystal phases. PMID:25958625

  11. On the Enclathration of NaB(OH)4 in the β-Cages of Sodalite: Crystallization Kinetics and Crystal Structure

    NASA Astrophysics Data System (ADS)

    Buhl, J.-Ch.; Mundus, C.; Löns, J.; Hoffmann, W.

    1994-12-01

    The hydrothermal formation of sodium hydroxyborate enclathrated sodalite synthesized from an initial ternary mixture of mullite, cristobalite and corundum has been investigated. Depending on temperature and pressure the compound Na7.5[AlSiO4]6[B(OH)4]1.5 · 2H2O could be synthesized in form of polycrystalline powder as well as in form of single crystals. The kinetics of the sodalite growth could be determined at 423 K and 473 K. 29Si-and 27Al MAS NMR was shown to be the preferred method to describe the conversion into sodalite quantitatively. Evidence for the first formation of polycrystalline sodalite has been found after the total dissolution of mullite and cristobalite. Single crystal X-ray diffraction data were used for the structure determination and refinement. The position and orientation of the hydroxyborate anions within the sodalite's /β-cages could only be found in the course of a "rigid body" refinement with constraints for the B(OH)4 tetrahedron. The boron atoms are located in an off-centre position within the sodalite cages. One out of the four oxygen atoms of the hydroxyborate group is positioned near the centre of a face of the sodium tetrahedron, whereas the three remaining oxygen atoms are near to the middle of its edges.

  12. Processing and characterization of multi-cellular monolithic bioceramics for bone regenerative scaffolds

    NASA Astrophysics Data System (ADS)

    Ari-Wahjoedi, Bambang; Ginta, Turnad Lenggo; Parman, Setyamartana; Abustaman, Mohd Zikri Ahmad

    2014-10-01

    Multicellular monolithic ceramic body is a ceramic material which has many gas or liquid passages partitioned by thin walls throughout the bulk material. There are many currently known advanced industrial applications of multicellular ceramics structures i.e. as supports for various catalysts, electrode support structure for solid oxide fuel cells, refractories, electric/electronic materials, aerospace vehicle re-entry heat shields and biomaterials for dental as well as orthopaedic implants by naming only a few. Multicellular ceramic bodies are usually made of ceramic phases such as mullite, cordierite, aluminum titanate or pure oxides such as silica, zirconia and alumina. What make alumina ceramics is excellent for the above functions are the intrinsic properties of alumina which are hard, wear resistant, excellent dielectric properties, resists strong acid and alkali attacks at elevated temperatures, good thermal conductivities, high strength and stiffness as well as biocompatible. In this work the processing technology leading to truly multicellular monolithic alumina ceramic bodies and their characterization are reported. Ceramic slip with 66 wt.% solid loading was found to be optimum as impregnant to the polyurethane foam template. Mullitic ceramic composite of alumina-sodium alumino disilicate-Leucite-like phases with bulk and true densities of 0.852 and 1.241 g cm-3 respectively, pore linear density of ±35 cm-1, linear and bulk volume shrinkages of 7-16% and 32 vol.% were obtained. The compressive strength and elastic modulus of the bioceramics are ≈0.5-1.0 and ≈20 MPa respectively.

  13. Corrosion protection of SiC-based ceramics with CVDMullite coatings

    SciTech Connect

    Sarin, V.; Auger, M.

    1997-05-01

    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.

  14. Improvement of Reusable Surface Insulation (RSI) materials

    NASA Technical Reports Server (NTRS)

    Blome, J. C.

    1972-01-01

    The mullite fiber based hardened compacted fibers (HCF) type of reusable surface insulation was further developed for use in the Space Shuttle Program. Two hundred fifty formulations of fiber mixtures, fillers, binders, and organic processing aids were made using mullite fibers as the basic ingredient. Most of the work was accomplished on 15-lb/cu ft material. It was established that higher density materials are stronger with strength values as high as 250 lb/sq in. in tension. New measurement techniques and equipment were developed for accurate determination of strength and strain to failure. Room temperature to 2300 F stress-strain relationships were made. The room temperature tensile modulus of elasticity is 61,700 lb/sq in. and the strain at failure is 0.165 percent, typically, when measured longitudinally parallel to the long axes of the fibers. Thermal insulating effectiveness was increased 20 percent by reducing the diameter of some of the fibers in the material. Improvements were made in density uniformity and strength uniformity in a block of HCF by mixing improvements and by the use of organic additives. Specifications were established on the materials and processes used in making the insulation.

  15. Lightweight proppants for deep-gas-well stimulation. Third annual report, July 1, 1981-June 30, 1982

    SciTech Connect

    Cutler, R.A.; Enniss, D.O.; Swartz, G.C.; Jones, A.H.

    1983-04-01

    The need exists for lower-density, less-expensive proppants for use in hydraulic-fracturing treatments. Ceramics, fabricated as fully sintered or hollow spheres, are the best materials for obtaining economical proppants with adequate strength. Fabrication techniques are described for fabricating solid-porcelain proppants and hollow-ceramic proppants. Porcelain proppants made by mix-pelletization techniques have good characteristics for propping wells with closure stresses to 96.5 MPa (14,000 psi). The properties of porcelain proppants are compared with twelve commercially available or experimental proppants. Several of the proppants evaluated had adequate conductivity for most hydraulic-fracturing jobs and are less expensive than bauxite. A single-fluid nozzle, counter-current spray-drying technique was used to make hollow, spherical proppants. Alumina was used as the ceramic raw material for these spray-drying experiments, but the same technique can be used with other ceramic materials. Hollow proppants with strengths comparable to sand have been spray dried but further optimization of spray drying parameters is needed to achieve proppants with concentric voids and improved strength. Bauxite, mullite, alumina and mullite rods were fast fired in a plasma in order to see if it is feasible to sinter these materials rapidly. Fast firing appears to be an alternative method of sintering proppants and may reduce costs, thereby making proppants more cost competitive with sand. 42 figures, 20 tables.

  16. Illinois basin coal fly ashes. 2. Equilibria relationships and qualitative modeling of ash-water reactions

    USGS Publications Warehouse

    Roy, W.R.; Griffin, R.A.

    1984-01-01

    Alkaline and acidic Illinois Basin coal fly ash samples were each mixed with deionized water and equilibrated for about 140 days to simulate ash ponding environments. Common to both equilibrated solutions, anhydrite solubility dominated Ca2+ activities, and Al3+ activities were in equilibrium with both matrix mullite and insoluble aluminum hydroxide phases. Aqueous silica activities were controlled by both mullite and matrix silicates. The pH of the extract of the acidic fly ash was 4.1 after 24 h but increased to a pH value of 6.4 as the H2SO4, assumed to be adsorbed to the particle surfaces, was exhausted by the dissolution of matrix iron oxides and aluminosilicates. The activities of aqueous Al3+ and iron, initially at high levels during the early stages of equilibration, decreased to below analytical detection limits as the result of the formation of insoluble Fe and Al hydroxide phases. The pH of the extract of the alkaline fly ash remained above a pH value of 10 during the entire equilibration interval as a result of the hydrolysis of matrix oxides. As with the acidic system, Al3+ activities were controlled by amorphous aluminum hydroxide phases that began to form after about 7 days of equilibration. The proposed mechanisms and their interrelations are discussed in addition to the solubility diagrams used to deduce these relationships. ?? 1984 American Chemical Society.

  17. Thermal Conductivity of Ceramic Thermal Barrier and Environmental Barrier Coating Materials

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Bansal, Narottam P.; Lee, Kang N.; Miller, Robert A.

    2001-01-01

    Thermal barrier and environmental barrier coatings (TBC's and EBC's) have been developed to protect metallic and Si-based ceramic components in gas turbine engines from high temperature attack. Zirconia-yttria based oxides and (Ba,Sr)Al2Si2O8(BSAS)/mullite based silicates have been used as the coating materials. In this study, thermal conductivity values of zirconia-yttria- and BSAS/mullite-based coating materials were determined at high temperatures using a steady-state laser heat flux technique. During the laser conductivity test, the specimen surface was heated by delivering uniformly distributed heat flux from a high power laser. One-dimensional steady-state heating was achieved by using thin disk specimen configuration (25.4 mm diam and 2 to 4 mm thickness) and the appropriate backside air-cooling. The temperature gradient across the specimen thickness was carefully measured by two surface and backside pyrometers. The thermal conductivity values were thus determined as a function of temperature based on the 1-D heat transfer equation. The radiation heat loss and laser absorption corrections of the materials were considered in the conductivity measurements. The effects of specimen porosity and sintering on measured conductivity values were also evaluated.

  18. Mineralogy and thermal properties of kaolin from the San José (Oruro, Bolivia)

    NASA Astrophysics Data System (ADS)

    Alfonso, Pura; Garcia-Valles, Maite; Martínez, Salvador; Amando Penedo, Lucio; Elvys Trujillo, Juan

    2016-04-01

    The San José mine, Oruro, Bolivia is known for provided a broad diversity of minerals. The San José Sn deposit is a Sn-Ag deposit composed of veins hosted in a complex of Miocene domes from monzonitic to dioritic composition within rhyolitic volcanic rocks hosted in Tertiary sedimentary rocks. Advanced argillitic alteration. is widespread in the surroundings of the deposit. Kaolinitization reach industrial importance and the kaolinitized rock is exploited, however it was not already been characterised. In this study we present a preliminary mineralogical and thermal characterization to determine the industrial applications of these kaolinitic materials. A sampling of the kaolinitized rocks in outcrops from the mining area was undertaken. The chemical composition of major and trace elements was determined by X-ray fluorescence (XRF). Mineralogy was obtained by powder diffraction X-ray (XRD) and infrared spectroscopy (FTIR). Quantitative determination of phases was obtained by the Rietveld refinement method using the Fullprof software. Thermal properties were determined by differential thermal analysis-thermo gravimetry (DTA -TG) and dilatometry. Mineral phases determined are mainly quartz (54-55 wt. %), kaolinite (7-8 wt. %), K-feldspar (8-19 wt. %), muscovite (16-17 wt. %), plagioclase up to 3 wt. %, alunite up to 8 wt% and gypsum up to 4 wt%. DTA -TG show a first endothermic event related to the dehydration of gypsum, with a loss weight of 0.4 wt%. An endothermic peak corresponding to the loss of the OH- groups of kaolinite occurs about 520 °C and an exothermic, at 980 °C, due to the crystallization of the mullite phase. The endothermic peak is attributed to the transformation of kaolinite in metakaolinite: Al2Si2O5 (OH)4  Al2Si2O7 + 2H2O and the dehydroxilation of alunite; the loss weight associated with this event is 2.9-3.2 wt%. The exothermic peak is caused by the formation of mullite: 3Al2Si2O7  Al6Si2O13 + 4SiO2. Another loss weight, of 3wt%, is

  19. Synthesis of low-temperature, fast, single-firing body for porcelain stoneware tiles with coal gangue.

    PubMed

    Qiangwei Wei; Wenyuan Gao; Xinguo Sui

    2010-10-01

    Coal gangue is a major industrial solid waste in China, causing great environment pollution. According to phase diagram theory, a low-temperature, fast, single-firing body mix for porcelain stoneware tiles was designed in the quaternary system CaO--MgO--Al₂O₃--SiO₂, using coal gangue as the main raw material. The coal gangue was from Baishan city, Jilin province and mainly composed of kaolinite and quartz. Mineralogical compositions and microstructures of some selected samples sintered at different temperatures were identified with X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results indicated that the optimal body mix was the one containing 34 wt% coal gangue sintered at 1170°C for about 1 h, with rupture strength of 43 MPa and water absorption of 0.22%. The main crystalline phases of the sintered body were quartz, anorthite and mullite. PMID:19942651

  20. Thermodynamic analysis of chemical stability of ceramic materials in hydrogen-containing atmospheres at high temperatures

    NASA Technical Reports Server (NTRS)

    Misra, Ajay K.

    1990-01-01

    The chemical stability of several ceramic materials in hydrogen-containing environments was analyzed with thermodynamic considerations in mind. Equilibrium calculations were made as a function of temperature, moisture content, and total system pressure. The following ceramic materials were considered in this study: SiC, Si3N4, SiO2, Al2O3, mullite, ZrO2, Y2O3, CaO, MgO, BeO, TiB2, TiC, HfC, and ZrC. On the basis of purely thermodynamic arguments, upper temperature limits are suggested for each material for long-term use in H2-containing atmospheres.

  1. Structure-activity relationships of mineral dusts as heterogeneous nuclei for ammonium sulfate crystallization from supersaturated aqueous solutions.

    PubMed

    Martin, S T; Schlenker, J; Chelf, J H; Duckworth, O W

    2001-04-15

    Mineral inclusions, present in aqueous atmospheric salt droplets, regulate crystallization when relative humidity decreases by providing a surface for heterogeneous nucleation and thus reducing the critical supersaturation. Although laboratory studies have quantified these processes to some extent, the diverse atmospheric mineralogy presents more chemical systems than practically feasible for direct study. Structure--activity relationships are necessary. To that end, in the present work the interactions of ammonium sulfate with corundum, hematite, mullite, rutile, anatase, and baddeleyite were studied by diffuse reflectance fourier transform infrared spectroscopy (DRIFTS) and by epitaxial modeling. The spectroscopic results show that shifts in sulfate peak positions due to chemisorption are not a correlative indicator of the efficacy of heterogeneous nucleation. In contrast, epitaxial modeling results of unreconstructed surfaces explain the sequence of critical supersaturations for constant particle size. If validated by further work, this computer modeling method would provide an important structure--activity tool for the estimation of heterogeneous nucleation properties of the atmospheric mineralogy. PMID:11329712

  2. Silicon carbide whisker reinforced ceramic composites and method for making same

    DOEpatents

    Wei, George C. [Oak Ridge, TN

    1989-01-24

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties especially increased fracture toughness. In the formation of these ceramic composites, the single crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al.sub.2 O.sub.3, mullite, or B.sub.4 C. The mixtures which contain a homogeneous disperson of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1600.degree. to 1950.degree. C. with pressing times varying from about 0.75 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness of up to about 9 MP.am.sup.1/2 which represents as much as a two-fold increase over that of the matrix material.

  3. Silicon carbide whisker reinforced ceramic composites and method for making same

    DOEpatents

    Wei, George C.

    1993-01-01

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties especially increased fracture toughness. In the formation of these ceramic composites, the single crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al.sub.2 O.sub.3, mullite, or B.sub.4 C. The mixtures which contain a homogeneous disperson of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1600.degree. to 1950.degree. C. with pressing times varying from about 0.075 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness of up to about 9 MPa.m.sup.1/2 which represents as much as a two-fold increase over that of the matrix material.

  4. Silicon carbide whisker reinforced ceramic composites and method for making same

    DOEpatents

    Wei, George C.

    1985-01-01

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties especially increased fracture toughness. In the formation of these ceramic composites, the single crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al.sub.2 O.sub.3, mullite, or B.sub.4 C. The mixtures which contain a homogeneous dispersion of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1600.degree. to 1950.degree. C. with pressing times varying from about 0.75 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness of up to about 9 MPa.m.sup.1/2 which represents as much as a two-fold increase over that of the matrix material.

  5. Status of reusable surface insulation thermal protection system technology programs

    NASA Technical Reports Server (NTRS)

    Greenshields, D. H.; Meyer, A. J.; Tillian, D. J.

    1972-01-01

    The development of three low-density rigidized insulation materials for the shuttle TPS application is reported. These materials consist of one high purity silica system and two systems based on mullite, an aluminum silicate. Both systems consist of fibers joined together with appropriate binders to obtain a rigidized insulation composite. Both material systems require the application of a glassy coating to provide a wear resistant, high emittance surface and to prevent the absorption of water by the fiber matrix. The technology program has addressed the development of water impervious coatings, methods of assembling the materials in design concepts while minimizing the thermal stress in the insulation, achieving compatibility between the RSI material and the structural system, and test evaluations to demonstrate the feasibility of the surface insulation concept.

  6. Ceramic technology for solar thermal receivers

    NASA Technical Reports Server (NTRS)

    Kudirka, A. A.; Smoak, R. H.

    1981-01-01

    The high-temperature capability, resistance to corrosive environments and non-strategic nature of ceramics have prompted applications in the solar thermal field whose advantages over metallic devices of comparable performance may begin to be assessed. It is shown by a survey of point-focusing receiver designs employing a variety of ceramic compositions and fabrication methods that the state-of-the-art in structural ceramics is not sufficiently advanced to fully realize the promised benefits of higher temperature capabilities at lower cost than metallic alternatives. The ceramics considered include alumina, berylia, magnesia, stabilized zirconia, fused silica, silicon nitride, silicon carbide, mullite and cordierite, processed by such methods as isostatic pressing, dry pressing, slip casting, extrusion, calendaring and injection molding.

  7. Development of Refractory Silicate-YSZ Dual Layer TBCs

    NASA Technical Reports Server (NTRS)

    He, Yirong; Lee, N.; Tewari, Surendra; Miller, Robert A.

    1999-01-01

    Development of advanced thermal barrier coatings (TBCs) is the most promising approach for increasing the efficiency and performance of gas turbine engines by enhancing the temperature capability of hot section metallic components. Spallation of the yttria-stabilized zirconia (YSZ) top coat, induced by the oxidation of the bond coat coupled with the thermal expansion mismatch strain, is considered to be the ultimate failure mode for current state-of-the-art TBCS. Enhanced oxidation resistance of TBCs can be achieved by reducing the oxygen conductance of TBCs below that of thermally grown oxide (TGO) alumina scale. One approach is incorporating an oxygen barrier having an oxygen conductance lower than that of alumina scale. Mullite, rare earth silicates and glass ceramics have been selected as potential candidates for the oxygen barrier. This paper presents the results of cyclic oxidation studies of oxygen barrier/YSZ dual layer TBCs.

  8. Oxidation-resistant interface coatings for SiC/SiC composites

    SciTech Connect

    Stinton, D.P.; Kupp, E.R.; Hurley, J.W.; Lowden, R.A.

    1996-08-01

    The characteristics of the fiber-matrix interfaces in ceramic matrix composites control the mechanical behavior of these composites. Finite element modeling (FEM) was performed to examine the effect of interface coating modulus and coefficient of thermal expansion on composite behavior. Oxide interface coatings (mullite and alumina-titania) produced by a sol-gel method were chosen for study as a result of the FEM results. Amorphous silicon carbide deposited by chemical vapor deposition (CVD) is also being investigated for interface coatings in SiC-matrix composites. Processing routes for depositing coatings of these materials were developed. Composites with these interfaces were produced and tested in flexure both as-processed and after oxidation to examine the suitability of these materials as interface coatings for SiC/SiC composites in fossil energy applications.

  9. Silicon carbide whisker reinforced ceramic composites and method for making same

    DOEpatents

    Wei, G.C.

    1989-01-24

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties especially increased fracture toughness. In the formation of these ceramic composites, the single crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al{sub 2}O{sub 3}, mullite, or B{sub 4}C. The mixtures which contain a homogeneous dispersion of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1,600 to 1,950 C with pressing times varying from about 0.75 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness which represents as much as a two-fold increase over that of the matrix material.

  10. Development of low-expansion ceramics with strength retention to elevated temperatures. Final report

    SciTech Connect

    Hirschfeld, D.A.; Brown, J.J. Jr.

    1994-09-01

    The development of advanced engines has resulted in the need for new ceramic compositions which exhibit thermo-mechanical properties suitable for the engine environment, e.g., low thermal expansion, stability to 1,200 C, and thermal shock resistance. To meet these goals, a two phase research program was instituted. In the first phase, new oxide ceramics were identified in the AlPO{sub 4}-{beta}-eucryptite, {beta}-cristobalite, mullite and zircon systems. This research focused on screening and property characterization of ceramics in the four systems. The most promising compositions in the AlPO{sub 4}-{beta}-eucryptite and zircon systems were then further evaluated and developed in the second phase with the goal of being ready for prototype testing in actual engines. Of the compositions, calcium magnesium zirconium phosphate (zircon system) exhibits the most desirable properties and is presently being developed for commercialization.

  11. PEO of pre-anodized Al-Si alloys: Corrosion properties and influence of sealings

    NASA Astrophysics Data System (ADS)

    Mohedano, M.; Matykina, E.; Arrabal, R.; Mingo, B.; Pardo, A.

    2015-08-01

    Voltage-controlled PEO coatings were developed on A356 aluminum alloys (gravity-cast and rheocast) with a pre-anodized layer. The influence of the alloy manufacturing process and the effect of Si-rich phase on the structure and composition of the oxide layers were evaluated using SEM, EDS and XRD. The pre-anodized oxide layer preserves the microstructure of the substrate due to the presence of secondary phases that have a different behavior relative to the matrix during anodizing. PEO coatings consisted of a mixture of α-Al2O3, γ-Al2O3 and mullite. The corrosion behavior and the effectiveness of different sealing techniques based on salts of nickel, cobalt, cerium and phosphonic acid were also studied. Post-treatments improved the hydrophobic properties of the coatings and showed a beneficial effect, significantly increasing the coating impedance and thereby reducing the susceptibility to corrosion.

  12. Design and Development of a Ceramic Hot-Gas Filter for Fossil Energy

    SciTech Connect

    Vaubert, V.

    2001-02-14

    Advanced coal-fueled, power generation systems utilizing pressurized fluidized bed combustion (PFBC) and integrated gasification combined cycle (IGCC) technologies are currently being developed for high-efficiency, low emissions, and low-cost power generation. In spite of the advantages of these promising technologies, the severe operating environment often leads to material degradation and loss of performance in the barrier filters used for particle entrapment. To address this problem a monolithic cross-flow ceramic hot-gas filter is being designed and developed. Because of testing necessities, a hot-gas candle-filter which integrates the requirements of the cross-flow filter will be fabricated first. As a result, a high-purity, stoichiometric mullite, nine inch long, closed-end, candle-filter prototype was fabricated at Oak Ridge National Laboratory (ORNL) using gelcasting technology.

  13. Dilithium dialuminium trisilicate Crystalline Phase Prepared from Coal Fly Ash

    NASA Astrophysics Data System (ADS)

    Yao, Zhitong; Xia, Meisheng; Ye, Ying

    2012-06-01

    The dilithium dialuminium trisilicate phase Li2Al2Si3O10 was prepared using coal fly ash and lithium hydroxide monohydrate LiOH·H2O as precursors. The influences of various preparation conditions on Li2Al2Si3O10 forming were investigated. The results showed that the optimum additive amount of LiOH·H2O was about 20%. The onset of calcining temperature and time was identified as 980 °C and 1 h, respectively. XRD analysis indicated that the content of Li2Al2Si3O10 phase increased at the expense of quartz and mullite, with calcining temperatures increasing and time extending. SEM observation revealed that the calcined samples were drastically interlocked together with the prolonging of time. The obtained Li2Al2Si3O10 phase was well crystallized and with small grain size.

  14. Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier Coatings

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Choi, Sung R.; Eldridge, Jeffrey I.; Lee, Kang N.; Miller, Robert A.

    2003-01-01

    In this paper, surface cracking and interface reactions of a BSAS coating and a multi-layer ZrO2-8wt%Y2O3 and mullite/BSAS/Si thermal and environmental barrier coating system on SiC/SiC ceramic matrix composites were characterized after long-term combined laser thermal gradient and furnace cyclic tests in a water vapor containing environment. The surface cracking was analyzed based on the coating thermal gradient sintering behavior and thermal expansion mismatch stress characteristics under the thermal cyclic conditions. The interface reactions, which were largely enhanced by the coating surface cracking in the water vapor environment, were investigated in detail, and the reaction phases were identified for the coating system after the long-term exposure. The accelerated coating delamination failure was attributed to the increased delamination driving force under the thermal gradient cyclic loading and the reduced interface adhesion due to the detrimental interface reactions.

  15. Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier Coatings

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Choi, Sung R.; Eldridge, Jeffrey I.; Lee, Kang N.; Miller, Robert A.

    2003-01-01

    In this paper, surface cracking and interface reactions of a BSAS coating and a multi-layer ZTO2-8wt%Y2O3 and mullite/BSAS/Si thermal and environmental barrier coating system on SiC/SiC ceramic matrix composites were characterized after long-term combined laser thermal gradient and furnace cyclic tests in a water vapor containing environment. The surface cracking was analyzed based on the coating thermal gradient sintering behavior and thermal expansion mismatch stress characteristics under the thermal cyclic conditions. The interface reactions, which were largely enhanced by the coating surface cracking in the water vapor environment, were investigated in detail, and the reaction phases were identified for the coating system after the long- term exposure. The accelerated coating delamination failure was attributed to the increased delamination driving force under the thermal gradient cyclic loading and the reduced interface adhesion due to the detrimental interface reactions.

  16. Effect of hydrogen on the strength and microstructure of selected ceramics

    NASA Technical Reports Server (NTRS)

    Herbell, Thomas P.; Eckel, Andrew J.; Hull, David R.; Misra, Ajay K.

    1990-01-01

    Ceramics in monolithic form and as composite constituents in the form of fibers, matrices, and coatings are currently being considered for a variety of high-temperature applications in aeronautics and space. Many of these applications involve exposure to a hydrogen-containing environment. The compatibility of selected ceramics in gaseous high-temperature hydrogen is assessed. Environmental stability regimes for the long term use of ceramic materials are defined by the parameters of temperature, pressure, and moisture content. Thermodynamically predicted reactions between hydrogen and several monolithic ceramics are compared with actual performance in a controlled environment. Morphology of hydrogen attack and the corresponding strength degradation is reported for silicon carbide, silicon nitride, alumina, magnesia, and mullite.

  17. A facile approach to pure-phase Bi2Fe4O9 nanoparticles sensitive to visible light

    NASA Astrophysics Data System (ADS)

    Wang, X.; Zhang, M.; Tian, P.; Chin, W. S.; Zhang, C. M.

    2014-12-01

    Pure-phase Bi2Fe4O9 nanoparticles with mullite-type structure were successfully fabricated through a facile and environmentally benign sol-gel process. According to the UV-Vis diffuse reflection spectrum, the multiband structure and the band edge position of the nanoparticles were confirmed, indicating the prominent absorption in the expanded visible-light region. As compared to the bulk, the visible-light-driven photocatalytic activity of the obtained nanoparticles was improved by 30-fold. The much improved photocatalytic efficiency of the sample mainly owed to the small crystal size and the multiband characteristic as well as the adding of H2O2 as electron scavenger and a source of hydroxide free radicals instead of Fenton-like reaction, leading to a low recombination of the photogenerated e-/h+ pairs.

  18. Comparison of Refractory Performance in Black Liquor Gasifiers and a Smelt Test System

    SciTech Connect

    Peascoe, RA

    2001-09-25

    Prior laboratory corrosion studies along with experience at the black liquor gasifier in New Bern, North Carolina, clearly demonstrate that serious material problems exist with the gasifier's refractory lining. Mullite-based and alumina-based refractories used at the New Bern facility suffered significant degradation even though they reportedly performed adequately in smaller scale systems. Oak Ridge National Laboratory's involvement in the failure analysis, and the initial exploration of suitable replacement materials, led to the realization that a simple and reliable, complementary method for refractory screening was needed. The development of a laboratory test system and its suitability for simulating the environment of black liquor gasifiers was undertaken. Identification and characterization of corrosion products were used to evaluate the test system as a rapid screening tool for refractory performance and as a predictor of refractory lifetime. Results from the test systems and pl ants were qualitatively similar.

  19. Microstructures and Abrasive Properties of the Oxide Coatings on Al6061 Alloys Prepared by Plasma Electrolytic Oxidation in Different Electrolytes

    NASA Astrophysics Data System (ADS)

    Wang, Kai; Byun, Sangsik; Lee, Chan Gyu; Koo, Bon Heun; Wang, Yi Qi; Song, Jung Il

    Al2O3 coatings were prepared on T6-tempered Al6061 alloys substrate under a hybrid voltage (AC 200 V-60 Hz and DC 260 V value) by plasma electrolytic oxidation (PEO) in 30 min. The effects of different electrolytes on the abrasive behaviors of the coatings were studied by conducting dry ball-on-disk wear tests. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to investigate the coating microstructure. XRD analysis results show that the coatings mainly consist of α- and γ-Al2O3, and some mullite and AlPO4 phase in Na2SiO3 and Na3PO4 containing electrolytes, respectively. The wear test results show that the coatings which were PEO-treated in Na3PO4 containing electrolyte presented the most excellent abrasive resistance property.

  20. Multilayer Article Characterized by Low Coefficient of Thermal Expansion Outer Layer

    NASA Technical Reports Server (NTRS)

    Lee, Kang N. (Inventor)

    2004-01-01

    A multilayer article comprises a substrate comprising a ceramic or a silicon-containing metal alloy. The ceramic is a Si-containing ceramic or an oxide ceramic with or without silicon. An outer layer overlies the substrate and at least one intermediate layer is located between the outer layer and thc substrate. An optional bond layer is disposed between thc 1 least one intermediate layer and thc substrate. The at least one intermediate layer may comprise an optional chemical barrier layer adjacent the outer layer, a mullite-containing layer and an optional chemical barrier layer adjacent to the bond layer or substrate. The outer layer comprises a compound having a low coefficient of thermal expansion selected from one of the following systems: rare earth (RE) silicates; at least one of hafnia and hafnia-containing composite oxides; zirconia-containing composite oxides and combinations thereof.

  1. Environmental Barrier Coatings for Silicon-Based Ceramics

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Fox, Dennis S.; Robinson, Raymond C.; Bansal, Narottam P.

    2001-01-01

    Silicon-based ceramics, such as SiC fiber-reinforced SiC (SiC/SiC ceramic matrix composites (CMC) and monolithic silicon nitride (Si3N4), are prime candidates for hot section structural components of next generation gas turbine engines. Silicon-based ceramics, however, suffer from rapid surface recession in combustion environments due to volatilization of the silica scale via reaction with water vapor, a major product of combustion. Therefore, application of silicon-based ceramic components in the hot section of advanced gas turbine engines requires development of a reliable method to protect the ceramic from environmental attack. An external environmental barrier coating (EBC) is considered a logical approach to achieve protection and CP long-term stability. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 Wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program (5). They consist of three layers, a silicon first bond coat, a mullite or a mullite + BSAS (BaO(1-x)-SrO(x)-Al2O3-2SiO2) second bond coat, and a BSAS top coat. The EPM EBCs were applied on SiC/SiC CMC combustor liners in three Solar Turbines (San Diego, CA) Centaur 50s gas turbine engines. The combined operation of the three engines has accumulated over 24,000 hours without failure (approximately 1,250 C maximum combustor liner temperature), with the engine in Texaco, Bakersfield, CA, accumulating about 14,000 hours. As the

  2. Silicon carbide whisker reinforced composites and method for making same

    DOEpatents

    Wei, G.C.

    1984-02-09

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties, especially increased fracture toughness. In the formation of these ceramic composites, the single-crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al/sub 2/O/sub 3/, mullite, or B/sub 4/C. The mixtures which contain a homogeneous dispersion of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1600 to 1950/sup 0/C with pressing times varying from about 0.75 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness of up to about 9 MPa.m/sup 1/2/ which represents as much as a two-fold increase over that of the matrix material.

  3. Silicon carbide whisker reinforced ceramic composites and method for making same

    DOEpatents

    Wei, George C.

    1993-11-16

    The present invention is directed to the fabrication of ceramic composites which possess improved mechanical properties especially increased fracture toughness. In the formation of these ceramic composites, the single crystal SiC whiskers are mixed with fine ceramic powders of a ceramic material such as Al.sub.2 O.sub.3, mullite, or B.sub.4 C. The mixtures which contain a homogeneous disperson of the SiC whiskers are hot pressed at pressures in a range of about 28 to 70 MPa and temperatures in the range of about 1600.degree. to 1950.degree. C. with pressing times varying from about 0.075 to 2.5 hours. The resulting ceramic composites show an increase in fracture toughness of up to about 9 MPa.m.sup.1/2 which represents as much as a two-fold increase over that of the matrix material.

  4. Oxidation-resistant interface coatings for SiC/SiC composites

    SciTech Connect

    Stinton, D.P.; Kupp, E.R.; Hurley, J.W.

    1996-06-01

    The characteristics of the fiber-matrix interfaces in ceramic matrix composites control the mechanical behavior of these composites. Finite element modeling (FEM) was performed to examine the effect of interface coating modulus and coefficient of thermal expansion on composite behavior. Oxide interface coatings (mullite and alumina-titania) produced by a sol-gel method were chosen for study as a result of the FEM results. Amorphous silicon carbide deposited by chemical vapor deposition (CVD) is also being investigated for interface coatings in SiC-matrix composites. Processing routes for depositing coatings of these materials were developed. Composites with these interfaces were produced and tested in flexure both as-processed and after oxidation to examine the suitability of these materials as interface coatings for SiC/SiC composites in fossil energy applications.

  5. Amorphous and nanostructured silica and aluminosilicate spray-dried microspheres

    NASA Astrophysics Data System (ADS)

    Todea, M.; Turcu, R. V. F.; Frentiu, B.; Tamasan, M.; Mocuta, H.; Ponta, O.; Simon, S.

    2011-08-01

    Amorphous silica and aluminosilicate microspheres with diameters in the 0.1-20 μm range were produced by spray drying method. SEM, TEM and AFM images showed the spherical shape of the obtained particles. Based on thermal analysis data, several heat treatments have been applied on the as-prepared samples in order to check the amorphous state stability of the microspheres and to develop nanosized crystalline phases. As-prepared microspheres remain amorphous up to 1400 °C. By calcination at 1400 °C, cristobalite type nanocrystals are developed on silica sample, while in aluminosilicate sample first are developed mullite type nanocrystals and only after prolonged treatment are developed also cristobalite type nanocrystals. 29Si and 27Al MAS NMR results show that the local order around aluminum and silicon atoms strongly depend on the thermal history of the microspheres.

  6. Dip-coating process: Silicon sheet growth development for the large-area silicon sheet task of the low-cost silicon solar array project

    NASA Technical Reports Server (NTRS)

    Zook, J. D.; Heaps, J. D.; Maciolek, R. B.; Koepke, B. G.; Gutter, C. D.; Schuldt, S. B.

    1977-01-01

    The objective of this research program is to investigate the technical and economic feasibility of producing solar-cell-quality sheet silicon by coating one surface of carbonized ceramic substrates with a thin layer of large-grain polycrystalline silicon from the melt. The past quarter demonstrated significant progress in several areas. Seeded growth of silicon-on-ceramic (SOC) with an EFG ribbon seed was demonstrated. Different types of mullite were successfully coated with silicon. A new method of deriving minority carrier diffusion length, L sub n from spectral response measurements was evaluated. ECOMOD cost projections were found to be in good agreement with the interim SAMIS method proposed by JPL. On the less positive side, there was a decrease in cell performance which we believe to be due to an unidentified source of impurities.

  7. Tailoring of Boehmite-Derived Aluminosilicate Aerogel Structure and Properties: Influence of Ti Addition

    NASA Technical Reports Server (NTRS)

    Hurwitz, Frances I.; Guo, Haiquan; Sheets, Erik J.; Miller, Derek R.; Newlin, Katy N.

    2010-01-01

    Aluminosilicate aerogels offer potential for extremely low thermal conductivities at temperatures greater than 900 C, beyond where silica aerogels reach their upper temperature limits. Aerogels have been synthesized at various Al:Si ratios, including mullite compositions, using Boehmite (AlOOH) as the Al source, and tetraethoxy orthosilicate as the Si precursor. The Boehmite-derived aerogels are found to form by a self-assembly process of AlOOH crystallites, with Si-O groups on the surface of an alumina skeleton. Morphology, surface area and pore size varies with the crystallite size of the starting Boehmite powder, as well as with synthesis parameters. Ternary systems, including Al-Si-Ti aerogels incorporating a soluble Ti precursor, are possible with careful control of pH. The addition of Ti influences sol viscosity, gelation time pore structure and pore size distribution, as well as phase formation on heat treatment.

  8. Silver-hafnium braze alloy

    DOEpatents

    Stephens, Jr., John J.; Hosking, F. Michael; Yost, Frederick G.

    2003-12-16

    A binary allow braze composition has been prepared and used in a bonded article of ceramic-ceramic and ceramic-metal materials. The braze composition comprises greater than approximately 95 wt % silver, greater than approximately 2 wt % hafnium and less than approximately 4.1 wt % hafnium, and less than approximately 0.2 wt % trace elements. The binary braze alloy is used to join a ceramic material to another ceramic material or a ceramic material, such as alumina, quartz, aluminum nitride, silicon nitride, silicon carbide, and mullite, to a metal material, such as iron-based metals, cobalt-based metals, nickel-based metals, molybdenum-based metals, tungsten-based metals, niobium-based metals, and tantalum-based metals. A hermetic bonded article is obtained with a strength greater than 10,000 psi.

  9. Prevention of trace and major element leaching from coal combustion products by hydrothermally-treated coal ash

    SciTech Connect

    Adnadjevic, B.; Popovic, A.; Mikasinovic, B.

    2009-07-01

    The most important structural components of coal ash obtained by coal combustion in 'Nikola Tesla A' power plant located near Belgrade (Serbia) are amorphous alumosilicate, alpha-quartz, and mullite. The phase composition of coal ash can be altered to obtain zeolite type NaA that crystallizes in a narrow crystallization field (SiO{sub 2}/Al{sub 2}O{sub 3}; Na{sub 2}O/SiO{sub 2}; H{sub 2}O/Na{sub 2}O ratios). Basic properties (crystallization degree, chemical composition, the energy of activation) of obtained zeolites were established. Coal ash extracts treated with obtained ion-exchange material showed that zeolites obtained from coal ash were able to reduce the amounts of iron, chromium, nickel, zinc, copper, lead, and manganese in ash extracts, thus proving its potential in preventing pollution from dump effluent waters.

  10. Reliability Analysis of Brittle, Thin Walled Structures

    SciTech Connect

    Jonathan A Salem and Lynn Powers

    2007-02-09

    One emerging application for ceramics is diesel particulate filters being used order to meet EPA regulations going into effect in 2008. Diesel particulates are known to be carcinogenic and thus need to be minimized. Current systems use filters made from ceramics such as mullite and corderite. The filters are brittle and must operate at very high temperatures during a burn out cycle used to remove the soot buildup. Thus the filters are subjected to thermal shock stresses and life time reliability analysis is required. NASA GRC has developed reliability based design methods and test methods for such applications, such as CARES/Life and American Society for Testing and Materials (ASTM) C1499 “Standard Test Method for Equibiaxial Strength of Ceramics.”

  11. Preparation and Oxidation of ZrB2/SiC/Zr2Al4C5 Multi-phase Ceramics with Spark Plasma Sintering

    NASA Astrophysics Data System (ADS)

    Guo, Qilong; Li, Junguo; Ma, Zhiyu; Nie, Ye; Shen, Qiang; Zhang, Lianmeng

    2013-03-01

    The ZrB2/SiC/Zr2Al4C5 multi-phase ceramics were fabricated by spark plasma sintering (SPS) at 1800 °C for 3 min under 20 MPa in an vacuum. Oxidation behavior of multi-phase ceramics were investigated using thermo gravimetric analysis (TGA) from 20 °C to 1500 °C and muffle furnace in stagnant air at 1200 °C. Samples were analyzed after oxidation by X-ray diffraction (XRD), scanning electron microscopy (SEM) along with energy dispersive spectroscopy (EDS) to determine the reaction products and to observe the microstructure. The results showed that the aluminium borate and mullite crystallize on the surface in the samples oxidized. The effect of Zr2Al4C5 content on the oxidation resistance of the ZrB2 ceramics were discussed respectively, and oxidation mechanism was also analysised.

  12. Fundamental alloy design of oxide ceramics and their composites. [Annual] report, May 1, 1990--August 31, 1992

    SciTech Connect

    Chen, I.W.

    1992-12-31

    The main research was on microstructural development of oxide ceramics. Projects were completed and the publications given. Abstracts are given on: Reactive CeO{sub 2}powders by homogeneous precipitation, SiC whisker-reinforced lithium aluminosilicate composite, solute drag on grain boundary in ionic solids (space charge effect), in-situ alumina/aluminate platelet composites, exaggerated texture and grain growth of superplastic silicon nitride (SiAlON), hot extrusion of ceramics, control of grain boundary pinning in Al{sub 2}O{sub 3}/ZrO{sub 2} composites with Ce{sup 3+}/Ce{sup 4+} doping, superplastic forming of ceramic composites, computer simulation of final stage sintering (model, kinetics, microstructure, effect of initial pore size), development of superplastic structural ceramics, and superplastic flow of two-phase ceramics containing rigid inclusions (zirconia/mullite composites). A proposed research program is outlined: materials, solute drag, densification and coarsening, and grain boundary electrical behavior.

  13. Fundamental alloy design of oxide ceramics and their composites

    SciTech Connect

    Chen, I.W.

    1992-01-01

    The main research was on microstructural development of oxide ceramics. Projects were completed and the publications given. Abstracts are given on: Reactive CeO[sub 2]powders by homogeneous precipitation, SiC whisker-reinforced lithium aluminosilicate composite, solute drag on grain boundary in ionic solids (space charge effect), in-situ alumina/aluminate platelet composites, exaggerated texture and grain growth of superplastic silicon nitride (SiAlON), hot extrusion of ceramics, control of grain boundary pinning in Al[sub 2]O[sub 3]/ZrO[sub 2] composites with Ce[sup 3+]/Ce[sup 4+] doping, superplastic forming of ceramic composites, computer simulation of final stage sintering (model, kinetics, microstructure, effect of initial pore size), development of superplastic structural ceramics, and superplastic flow of two-phase ceramics containing rigid inclusions (zirconia/mullite composites). A proposed research program is outlined: materials, solute drag, densification and coarsening, and grain boundary electrical behavior.

  14. Fundamental studies on the nature and properties of ceramic fiber insulation

    NASA Technical Reports Server (NTRS)

    Mueller, J. I.; Whittemore, O. J., Jr.; Scott, W. D.; Miller, A. D.; Smiser, L. W.; Leiser, D. B.

    1975-01-01

    Silica and mullite fibers used to fabricate reusable surface insulation (RSI) for the space shuttle orbiter may devitrify/recrystallize within the temperature range anticipated upon reentry. This is shown to be dependent upon impurity level, temperature, and time at temperature. It is determined that the effects of the material improvement and optimization program are positive. The degree of crystallinity is shown to have a predominant effect upon the strength of fabricated RSI tile, and limits are determined. Models are developed to predict tensile strengths and shrinkage rates of silica tile based upon readily measurable parameters. Thermal cycling which simulates reentry results in an increase in the crystallinity and in the porosity of tile coatings.

  15. Spatio-temporal behaviour of atomic-scale tribo-ceramic films in adaptive surface engineered nano-materials.

    PubMed

    Fox-Rabinovich, G; Kovalev, A; Veldhuis, S; Yamamoto, K; Endrino, J L; Gershman, I S; Rashkovskiy, A; Aguirre, M H; Wainstein, D L

    2015-01-01

    Atomic-scale, tribo-ceramic films associated with dissipative structures formation are discovered under extreme frictional conditions which trigger self-organization. For the first time, we present an actual image of meta-stable protective tribo-ceramics within thicknesses of a few atomic layers. A mullite and sapphire structure predominates in these phases. They act as thermal barriers with an amazing energy soaking/dissipating capacity. Less protective tribo-films cannot sustain in these severe conditions and rapidly wear out. Therefore, a functional hierarchy is established. The created tribo-films act in synergy, striving to better adapt themselves to external stimuli. Under a highly complex structure and non-equilibrium state, the upcoming generation of adaptive surface engineered nano-multilayer materials behaves like intelligent systems - capable of generating, with unprecedented efficiency, the necessary tribo-films to endure an increasingly severe environment. PMID:25740153

  16. Low temperature environmental degradation of zirconia ceramics

    NASA Astrophysics Data System (ADS)

    Zhao, Zhenbo

    2005-11-01

    The low temperature environmental degradation (LTED) of yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) has been prevented, or at least retarded, by using both bulk doping and surface doping methods with either cation, or anion, stabilizers. The introduction of both mullite and alumina into 3Y-TZP by a bulk-doping method was found to be effective in suppressing the tetragonal-->monoclinic transformation induced by water during hydrothermal treatment thus giving rise to better mechanical properties. The beneficial effects of alumina on the phase stability of the 3Y-TZP ceramic are considered to be due to the increase in the elastic modulus of the constraining matrix, as well as to the segregation of A12O3 at grain boundaries. The LTED transformation kinetics as determined by x-ray diffraction (XRD) and White Light Interferometer (WLI) analysis showed that the isothermal tetragonal-to-monoclinic transformation starts from the surface and has an incubation-nucleation-growth mechanism which can be described by the Johnson-Mehl-Avrami equation. The degradation of Y-TZP ceramic after hydrothermal treatment can be effectively overcome by surface doping by a solid diffusion method with tetravalent dopants: CeO2 and GeO2; with trivalent dopants: La2O 3 and Fe2O3; and with divalent dopants: CuO and MgO. For surface CeO2-, GeO2- and Fe2O 3-doping, this degradation inhibition behaviour is attributed to a localized increase in cation stabilizer content which satisfies the requirements for stabilization of the tetragonal phase. However, in each case, the stability mechanisms are different. For surface La2O3doping, surface doping overcomes the formation of La2O3 and La 2Zr2O7 since the extra La2O3 can further diffuse to the center of the 3Y-TZP ceramic. For CuO-doping, small amounts of CuO form a liquid that can act as a conduit for the re-distribution of yttria. In the case of surface MgO modification, the stabilization results from the isolated nature of the

  17. Processing and mechanical behavior of Nicalon{reg_sign}/SiC composites with sol-gel derived oxide interfacial coatings

    SciTech Connect

    Shanmugham, S.; Liaw, P.K.

    1996-10-01

    Recent analytical and finite element modeling studies have indicated that low modulus interface materials are desirable for obtaining Nicalon/SiC composites with good toughness. Two oxides, Al titanate and mullite, were chosen on this basis as interface materials. The oxide and C coatings were deposited by sol-gel and CVD, respectively. Nicalon/SiC composites with oxide/C and C/oxide/C interfaces were fabricated and evaluated for flexure strength in the as-processed and oxidized conditions. Composites with C/oxide/C interfaces retained considerable strength and damage-tolerant behavior even after 500 h oxidation at 1000 C in air. The C/oxide/C interface shows promise as a viable oxidation-resistant interface alternative to C or BN interfaces.

  18. Ocular surface foreign bodies: novel findings mimicking ocular malignant melanoma

    PubMed Central

    Maudgil, A; Wagner, B E; Rundle, P; Rennie, I G; Mudhar, H S

    2014-01-01

    Purpose Malignant melanoma of the eye is an uncommon condition that is important to recognise. We describe three cases in which ocular foreign bodies have masqueraded as ocular malignant melanoma. Methods Interventional case reports. Results Case 1 describes diathermy-induced carbon particle implantation, during plaque therapy for the treatment of uveal melanoma, mimicking recurrence with extra-scleral invasion. Case 2 shows a foreign body called ‘mullite' mimicking conjunctival melanoma. Case 3 demonstrates a conjunctival foreign body called ‘illite' that mimicked a limbal melanocytic lesion, clinically thought to be either melanocytoma or melanoma. Conclusion This report highlights the importance of careful history taking, examination, and appropriate biopsy in cases of suspected malignant melanoma, to prevent unnecessary and potentially radical treatment. PMID:25104745

  19. Sensors for ceramic components in advanced propulsion systems

    NASA Technical Reports Server (NTRS)

    Koller, A. C.; Bennethum, W. H.; Burkholder, S. D.; Brackett, R. R.; Harris, J. P.

    1995-01-01

    This report includes: (1) a survey of the current methods for the measurement of surface temperature of ceramic materials suitable for use as hot section flowpath components in aircraft gas turbine engines; (2) analysis and selection of three sensing techniques with potential to extend surface temperature measurement capability beyond current limits; and (3) design, manufacture, and evaluation of the three selected techniques which include the following: platinum rhodium thin film thermocouple on alumina and mullite substrates; doped silicon carbide thin film thermocouple on silicon carbide, silicon nitride, and aluminum nitride substrates; and long and short wavelength radiation pyrometry on the substrates listed above plus yttria stabilized zirconia. Measurement of surface emittance of these materials at elevated temperature was included as part of this effort.

  20. Development of a monolithic ceramic cross flow filter

    SciTech Connect

    Larsen, D.A.

    1995-12-01

    High-temperature, high-pressure particulate control is required to protect turbine equipment and to meet environmental stack emissions standards in coal-fueled power systems. Ceramic cross flow filters have high surface area per unit volume for removing particulates from these hot gas streams. A one-piece monolithic ceramic cross flow filter is needed. Mullite bonded, porous, permeable alumina ceramics were made on a lab scale with the Blasch injection forming process. Permeability and other initial targeted property requirements were achieved: >200 cd (<1 iwg/fpm), room temperature modulus of rupture >1000 psi, particle size 100/200 mesh, pore size 20 microns. It is concluded that it is feasible to use the proprietary Blasch process to form cross flow filters.

  1. Advanced Environmental Barrier Coatings Development for Si-Based Ceramics

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Choi, R. Sung; Robinson, Raymond C.; Lee, Kang N.; Bhatt, Ramakrishna T.; Miller, Robert A.

    2005-01-01

    Advanced environmental barrier coating concepts based on multi-component HfO2 (ZrO2) and modified mullite systems are developed for monolithic Si3N4 and SiC/SiC ceramic matrix composite (CMC) applications. Comprehensive testing approaches were established using the water vapor cyclic furnace, high pressure burner rig and laser heat flux steam rig to evaluate the coating water vapor stability, cyclic durability, radiation and erosion resistance under simulated engine environments. Test results demonstrated the feasibility and durability of the environmental barrier coating systems for 2700 to 3000 F monolithic Si3N4 and SiC/SiC CMC component applications. The high-temperature-capable environmental barrier coating systems are being further developed and optimized in collaboration with engine companies for advanced turbine engine applications.

  2. Investigation of the mineral components of porcelain raw material and their phase evolution during a firing process by using a Rietveld quantitative analysis

    NASA Astrophysics Data System (ADS)

    Kim, Jaegyeom; Heo, Eunae; Kim, Seung-Joo; Kim, Jong-Young

    2016-01-01

    A ceramic raw material for white porcelain and its phase evolution during a firing process were investigated by using Rietveld method based on powder X-ray diffraction data. The raw material was mainly composed of five mineral phases: quartz (SiO2), microcline (KAlSi3O8), albite (NaAlSi3O8), muscovite (KAl2(AlSi3O10)(OH)2), and kaolinite (Al2Si2O5(OH)4). The amount of each mineral phase could be determined by using Rietveld quantitative phase analyses. During the firing process, the microcline, albite, muscovite and kaolinite phases started to react with each other to produce the mullite phase embedded in an amorphous matrix. The amount of quartz remained nearly unchanged until a temperature above 1200 °C; then, it converted to an amorphous phase at higher temperatures.

  3. Thermal expansion of laminated, woven, continuous ceramic fiber/chemical-vapor-infiltrated silicon carbide matrix composites

    NASA Technical Reports Server (NTRS)

    Eckel, Andrew J.; Bradt, Richard C.

    1990-01-01

    Thermal expansions of three two-dimensional laminate, continuous fiber/chemical-vapor-infiltrated silicon carbide matrix composites reinforced with either FP-Alumina (alumina), Nextel (mullite), or Nicalon (Si-C-O-N) fibers are reported. Experimental thermal expansion coefficients parallel to a primary fiber orientation were comparable to values calculated by the conventional rule-of-mixtures formula, except for the alumina fiber composite. Hysteresis effects were also observed during repeated thermal cycling of that composite. Those features were attributed to reoccurring fiber/matrix separation related to the micromechanical stresses generated during temperature changes and caused by the large thermal expansion mismatch between the alumina fibers and the silicon carbide matrix.

  4. Ceramic thermal barrier coating for rapid thermal cycling applications

    DOEpatents

    Scharman, Alan J.; Yonushonis, Thomas M.

    1994-01-01

    A thermal barrier coating for metal articles subjected to rapid thermal cycling includes a metallic bond coat deposited on the metal article, at least one MCrAlY/ceramic layer deposited on the bond coat, and a ceramic top layer deposited on the MCrAlY/ceramic layer. The M in the MCrAlY material is Fe, Ni, Co, or a mixture of Ni and Co. The ceramic in the MCrAlY/ceramic layer is mullite or Al.sub.2 O.sub.3. The ceramic top layer includes a ceramic with a coefficient of thermal expansion less than about 5.4.times.10.sup.-6 .degree.C.sup.-1 and a thermal conductivity between about 1 J sec.sup.-1 m.sup.-1 .degree.C.sup.-1 and about 1.7 J sec.sup.-1 m.sup.-1 .degree.C.sup.-1.

  5. Corrosion resistance of ceramic materials in pyrochemical reprocessing condition by using molten salt for spent nuclear oxide fuel

    NASA Astrophysics Data System (ADS)

    Takeuchi, M.; Kato, T.; Hanada, K.; Koizumi, T.; Aose, S.

    2005-02-01

    The corrosion resistance of ceramic materials in pyrochemical reprocessing using molten salts was discussed through the thermodynamic calculation and corrosion test. The corrosion test was basically carried out in alkali molten salt under chlorine gas. In addition, the effects of oxygen, carbon and main fission product's chlorides on ceramics corrosion were evaluated in that condition. Most of ceramic oxides showed good chemical stability on chlorine, oxygen and uranyl chloride from thermodynamic calculation results. On the other hand, from corrosion test result, silicon nitride, mullite (Al6Si2O13) and cordierite (Mg2Al3(AlSi5O18)) have a good corrosion resistance which is corresponding to 0.1 mm/y or less. No cracks on the materials were observed and flexural strength did not drop remarkably after 480 h corrosion testing in molten salt under Cl2 O2 atmosphere.

  6. Spatio-temporal behaviour of atomic-scale tribo-ceramic films in adaptive surface engineered nano-materials

    NASA Astrophysics Data System (ADS)

    Fox-Rabinovich, G.; Kovalev, A.; Veldhuis, S.; Yamamoto, K.; Endrino, J. L.; Gershman, I. S.; Rashkovskiy, A.; Aguirre, M. H.; Wainstein, D. L.

    2015-03-01

    Atomic-scale, tribo-ceramic films associated with dissipative structures formation are discovered under extreme frictional conditions which trigger self-organization. For the first time, we present an actual image of meta-stable protective tribo-ceramics within thicknesses of a few atomic layers. A mullite and sapphire structure predominates in these phases. They act as thermal barriers with an amazing energy soaking/dissipating capacity. Less protective tribo-films cannot sustain in these severe conditions and rapidly wear out. Therefore, a functional hierarchy is established. The created tribo-films act in synergy, striving to better adapt themselves to external stimuli. Under a highly complex structure and non-equilibrium state, the upcoming generation of adaptive surface engineered nano-multilayer materials behaves like intelligent systems - capable of generating, with unprecedented efficiency, the necessary tribo-films to endure an increasingly severe environment.

  7. Strong, damage tolerant oxide-fiber/oxide matrix composites

    NASA Astrophysics Data System (ADS)

    Bao, Yahua

    cationic polyelectrolytes to have a positive surface charge and then dipped into diluted, negatively-charged AlPO4 colloidal suspension (0.05M) at pH 7.5. Amorphous AlPO4 (crystallizes to tridymite- and cristobalite-forms at 1080°C) nano particles were coated on fibers layer-by-layer using an electrostatic attraction protocol. A uniform and smooth coating was formed which allowed fiber pullout from the matrix of a Nextel 720/alumina mini-composite hot-pressed at 1250°C/20MPa. Reaction-bonded mullite (RBM), with low formation temperature and sintering shrinkage was synthesized by incorporation of mixed-rare-earth-oxide (MREO) and mullite seeds. Pure mullite formed with 7.5wt% MREO at 1300°C. Introduction of 5wt% mullite seeds gave RBM with less than 3% shrinkage and 20% porosity. AlPO4-coated Nextel 720/RBM composites were successful fabricated by EPID and pressureless sintering at 1300°C. Significant fiber pullout occurred and the 4-point bend strength was around 170MPa (with 25-30vol% fibers) at room temperature and 1100°C and a Work-of-Fracture 7KJ/m2. At 1200°C, the composite failed in shear due to the MREO-based glassy phase in the matrix. AlPO4-coated Nextel 720 fiber/aluminosilicate (no MREO) showed damage tolerance at 1200°C with a bend strength 170MPa.

  8. A new method for measurement of the vitrification rate of earthenware texture by scanning electron microscope.

    PubMed

    Moon, Eun Jung; Kim, Su Kyeong; Han, Min Su; Lee, Eun Woo; Heo, Jun Su; Lee, Han Hyoung

    2013-08-01

    A new method for determining the vitrification rate of pottery depending on the firing temperature was devised using secondary electron images (SEI) of scanning electron microscope (SEM). Several tests were performed to establish the appropriate operating conditions of SEM and reproducibility as well as to examine the applicability of the method. The grayscale values converted from each pixel of SEI were used to determine the vitrification rate of pottery, which in our study were artificially fired specimens composed of three types of clay. A comparison between the vitrification rate value and appearance temperature of minerals shows that mullite formation starts at 1,100°C, during which the vitrification rate rapidly increases by over 10%. In consequence, the result presented here demonstrates that the new method can be applied to estimate the firing temperature of pottery. PMID:23920198

  9. Alumina composites for oxide/oxide fibrous monoliths

    SciTech Connect

    Cruse, T. A.; Polzin, B. J.; Picciolo, J. J.; Singh, D.; Tsaliagos, R. N.; Goretta, K. C.

    2000-03-01

    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.

  10. Valorization of sugarcane bagasse ash: producing glass-ceramic materials.

    PubMed

    Teixeira, S R; Magalhães, R S; Arenales, A; Souza, A E; Romero, M; Rincón, J M

    2014-02-15

    Some aluminosilicates, for example mullite and wollastonite, are very important in the ceramic and construction industries. The most significant glass-ceramic for building applications has wollastonite as the main crystal phase. In this work we report on the use of sugarcane bagasse ash (SCBA) to produce glass-ceramics with silicates as the major crystalline phases. The glasses (frits) were prepared by mixing ash, limestone (calcium and magnesium carbonates) and potassium carbonate as the fluxing agent. X-ray fluorescence was used to determine the chemical composition of the glasses and their crystallization was assessed by using thermal analysis (DTA/DSC/TGA) and X-ray diffraction. The results showed that glass-ceramic material can be produced with wollastonite as the major phase, at a temperature lower than 900 °C. PMID:24463731

  11. [Fly ash and its biological effects. 3. Exposure to dust of workers in the energy-generating industry (power plants and thermoelectric power stations)].

    PubMed

    Wojtczak, J; Bielichowska, G; Stroszejn-Mrowca, G; Tenerowicz, B

    1989-01-01

    An evaluation of exposure to dust of workers employed at typical work-stands in power industry plants was made. Mean concentrations of respirable dust determined at 14 different work-posts range from 0.45 to 8.95 mg/m3, and of total dust from 1.55 to 85.0 mg/m3. Mean content of free crystalline silica in dust samples is less than 10%. At the work-stands where ash dust was encountered, the presence of respirable fibres at concentration below 0.2 fibre/cm3 was observed. In all ash samples alpha-quartz and mullite were found: in some of them also kaolinite and orthoclase were traced. Only at five out of all 14 work-stands examined mean concentration of respirable dust was lower than the hygienic standard value. PMID:2560803

  12. Creep of Refractory Fibers and Modeling of Metal and Ceramic Matrix Composite Creep Behavior

    NASA Technical Reports Server (NTRS)

    Tewari, S.N.

    1995-01-01

    Our concentration during this research was on the following subprograms. (1) Ultra high vacuum creep tests on 218, ST300 and WHfC tungsten and MoHfC molybdenum alloy wires, temperature range from 1100 K to 1500 K, creep time of 1 to 500 hours. (2) High temperature vacuum tensile tests on 218, ST300 and WHfC tungsten and MoHfC molybdenum alloy wires. (3) Air and vacuum tensile creep tests on polycrystalline and single crystal alumina fibers, such as alumina-mullite Nextel fiber, yttrium aluminum ganet (YAG) and Saphikon, temperature range from 1150 K to 1470 K, creep time of 2 to 200 hours. (4) Microstructural evaluation of crept fibers, TEM study on the crept metal wires, SEM study on the fracture surface of ceramic fibers. (5) Metal Matrix Composite creep models, based on the fiber creep properties and fiber-matrix interface zone formation.

  13. Plasma electrolytic oxidation coating of synthetic Al-Mg binary alloys

    SciTech Connect

    Tarakci, Mehmet

    2011-12-15

    The binary Al-Mg synthetic alloys were prepared in a vacuum/atmosphere controlled furnace with the addition of 0.5, 1, 2, 4, 7, and 15 wt.% pure Mg into pure aluminum as substrate material. The surfaces of the Al-Mg alloys and pure aluminum were coated for 120 min by plasma electrolytic oxidation in the same electrolyte of 12 g/L sodium silicate and 2 g/L KOH in distilled water. The coating was characterized by X-ray diffraction, scanning electron microscopy, profilometry and Vickers microhardness measurements. There regions of loose outer layer, dense inner layer with precipitate like particles of {alpha}-Al{sub 2}O{sub 3} and a thin transition layer were identified for the coated samples. The coating thickness increases from 85 to 150 {mu}m with Mg contents in the alloys. The surface morphology becomes more porous and consequently surface roughness tends to increase with plasma electrolytic oxidation treatment and further with Mg content. The increase in magnesium content reduces the formation of {alpha}-Al{sub 2}O{sub 3} and crystalline mullite phases in the coating and decreases microhardness of coating. The Mg concentration is constant throughout the other loose and dense regions of coating though it gradually decreases in the thin inner region. - Research Highlights: Black-Right-Pointing-Pointer The average thickness of PEO coating of Al-Mg alloys increases with Mg content. Black-Right-Pointing-Pointer The addition of Mg reduces and prevents the formation of {alpha}-Al{sub 2}O{sub 3} and mullite. Black-Right-Pointing-Pointer The surface roughness increases with Mg content in the Al-Mg alloys. Black-Right-Pointing-Pointer The hardness values of the coating decreases with the Mg amount in the substrate. Black-Right-Pointing-Pointer The Mg concentration is constant throughout the main regions of coating.

  14. The high temperature creep behavior of oxides and oxide fibers

    NASA Technical Reports Server (NTRS)

    Jones, Linda E.; Tressler, Richard E.

    1991-01-01

    A thorough review of the literature was conducted on the high-temperature creep behavior of single and polycrystalline oxides which potentially could serve as fiber reinforcements in ceramics or metal matrix applications. Sapphire when oriented with the basal plane perpendicular to the fiber axis (c-axis oriented) is highly creep resistant at temperatures in excess of 1600 C and applied loads of 100 MPa and higher. Pyramidal slip is preferentially activated in sapphire under these conditions and steady-state creep rates in the range of 10(exp -7) to 10 (exp -8)/s were reported. Data on the creep resistance of polycrystalline beryllia suggest that C-axiz oriented single crystal beryllia may be a viable candidate as a fiber reinforcement material; however, the issure of fabricability and moisture sensitivity must be addressed for this material. Yttrium aluminum garnet (YAG) also appears to be a fiber candidate material having a high resistance to creep which is due to it's complex crystal structure and high Peierl resistance. The high creep resistance of garnet suggests that there may be other complex ternary oxides such as single crystal mullite which may also be candidate materials for fiber reinforcements. Finally, CVD and single crystal SiC, although not oxides, do possess a high resistance to creep in the temperature range between 1550 and 1850 C and under stresses of 110 to 220 MPa. From a review of the literature, it appears that for high creep resistant applications sapphire, silicon carbide, yttrium aluminum garnet, mullite, and beryllia are desirable candidate materials which require further investigation.

  15. Processing and Characterizing Alumina/Aluminum Composites with Tailored Microstructures Formed by Reactive Metal Penetration

    SciTech Connect

    Corral, E.; Ellerby, D.; Ewsuk, K.; Fahrenholtz, B.; Loehman, R.

    1999-01-28

    In industry, the need to maximize energy efficiency depends on the availability of suitable advanced materials. Ceramic composites are exemplary materials for many advanced engineering applications because they exhibit good thermal stability, oxidation resistance and enhanced toughness. Presently, ceramic composite fabrication processes are costly, often requiring high temperatures and pressures to achieve reasonable densities. Our research is focused on developing a processing technique, that will allow production of alumina/aluminum composites using relatively low temperatures and without the application of an external force, thus reducing the processing costs. Our composites were formed using Reactive Metal Penetration (RMP), which is a process involving the reaction of molten Al with a dense ceramic preform. The result is a near net shape ceramic/metal composite with interpenetrating phases. The volume fraction of metal in the composites was varied by doping an aluminosilicate ceramic preform with silica. For this study we fabricated composites using pure mullite and mullite doped with 23 and 42 weight percent silica, yielding 18, 25, and 30 volume percent metal in the composites, respectively. Optical and Scanning Electron Microscopy were used to characterize the homogeneity and scale of the microstructure. The scale of the microstructure varied with preform composition, the reaction temperature and with secondary heat treatments. Four-point bend testing was used to evaluate the influence of microstructure on strength and reliability. During these studies a gradient in the microstructure was observed, which we further characterized using microhardness testing. Alumina/aluminum composites formed by RMP show higher toughness then monolithic alumina and have the potential for improved reliability when compared to monolithic ceramics.

  16. Residual stress analysis of multilayer environmental barrier coatings.

    SciTech Connect

    Harder, B.; Almer, J.; Weyant, C.; Lee, K.; Faber, K.; Northwestern Univ.; Rolls-Royce Corp.

    2009-02-01

    Silicon-based ceramics (SiC, Si{sub 3}N{sub 4}) are promising materials systems for high-temperature structural applications in gas turbine engines. However, the silica layer that forms on these materials is susceptible to attack from water vapor present in combustion environments. To protect against this degradation, environmental barrier coatings (EBCs) have been developed to shield the underlying substrate and prevent degradation. Here we report on elastic and thermal properties, as well as internal stresses of candidate multilayer coatings, as measured in situ using microfocused high-energy X-rays in a transmission diffraction geometry. Doped aluminosilicate coatings were investigated for their stability on a SiC/SiC melt-infiltrated substrate. The coatings consisted of a Ba{sub 1-x}Sr{sub x}Al{sub 2}Si{sub 2}O{sub 8} topcoat with a mullite or mullite+SrAl{sub 2}Si{sub 2}O{sub 8} interlayer, and a silicon bond coat. A numerical model was used to compare the stress results with an ideal coating system. Experiments were carried out on as-sprayed and heat-treated samples in order to analyze the strain and phase evolution as a function of multilayer depth and temperature. The phase transformation of the topcoat promoted healing of cracks in the EBC and reduced stresses in the underlying layers and the addition of SAS to the interlayer reduced stresses in thermally cycled coatings, but did not stop cracks from forming.

  17. Sodium sulfate corrosion of silicon carbide fiber-reinforced lithium aluminosilicate glass-ceramic matrix composites. Master's thesis

    SciTech Connect

    Maldia, L.C.

    1993-12-01

    Sodium sulfate hot corrosion of a SiC fiber-reinforced lithium aluminosilicate (LAS) glass-ceramic matrix composite was studied using Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD). Changes in the microstructural chemical composition of the specimens were investigated. The samples provided by Naval Air Warfare Center (NAWC), Warminster, PA were grouped as follows: (1) as-received, (2) Na2SO4 salt-coated and heat-treated in oxygen, (3) noncoated and heat-treated in oxygen, (4) Na2SO4. Salt-coated and heat-treated in argon, and (5) noncoated and heat-treated in argon. Heat treatment was performed by NAWC for 100 hours at 900 deg C. Experimental data obtained indicated that the presence of Na2SO4 in an oxidative environment resulted in rapid corrosion of the matrix and SiC fibers and in the latter rings of SiO2 replaced what had previously been SiC. There was very limited degradation of the fibers and matrix exposed at the surface in the noncoated sample heat-treated in oxygen and in the salt-coated sample heat-treated in argon. A significant reduction in the amount of mullite in the matrices of all heat-treated samples was observed. Mullite dissolved into either the glassy phase or into the Beta-spodumene matrix. Lastly, the presence of distinct magnesium silicate crystalline phases in the salt-coated and heat-treated in oxygen sample implies that the MgO at the surface reacted with the SiO2 in the matrix.

  18. Zr doped anatase supported reticulated ceramic foams for photocatalytic water purification

    SciTech Connect

    Plesch, G.; Vargová, M.; Vogt, U.F.; Gorbár, M.; Jesenák, K.

    2012-07-15

    Highlights: ► Thick photocatalytic anatase films on macroporous reticulated ceramic foams. ► Alumina and alumina–mullite macroporous reticulated foams as photocatalyst support. ► Zr doping significantly improves the TiO{sub 2} film activity in phenol photomineralization. ► Comparison of photocatalytic activity of thick films and powder suspensions. -- Abstract: Titanium dioxide films were deposited on macroporous reticulated Al{sub 2}O{sub 3} and alumina–mullite foams with pore sizes of 15 ppi (pores per inch). Coatings were prepared from suspensions of precursor powders of Aeroxide{sup ®} P25 nanopowder and precipitated TiO{sub 2} by using a dip coating process. The TiO{sub 2} forms films with a thickness of ∼2–20 μm. The photocatalytic activity was characterized as the mineralization rate of an aqueous phenol solution under UVA irradiation by the TOC technique. Precipitated TiO{sub 2} films have nearly the same photocatalytic activity as a titania suspension, in which powder aggregates have a size comparable with the thickness of the films. Samples made of Aeroxide{sup ®} P25 nanopowder, in which the size of aggregates is ∼0.1 μm show higher efficiency of photodecomposition in suspensions with films. The doping of precipitated anatase with Zr(IV) in the atomic ratio Zr/Ti = 0.008 significantly improves the photocatalytic activity of the foam supported titania. Zr doped anatase films show better performance as the films prepared only from Aeroxide{sup ®} P25 nanopowder.

  19. Interfacial coatings for ceramic-matrix composites -- Volume 2. Final report

    SciTech Connect

    Sambasivan, S.

    1998-06-09

    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). Other interesting concepts with intensive material development efforts are also being pursued and a brief discussion of these are given in the main text. While demonstration of new interface concepts seems to be the primary objective in most studies, difficulties in processing of interface coatings and designing reliable test methods for determining interface properties have actually retarded the progress. Some of the concepts appear to be simple in nature but require sophisticated processing schemes to develop the coatings. Multilayered coatings with each layer serving specific function are also being proposed. Recent studies also show that significant degradation in fiber strength (30--50%) can result from merely applying the interface coating. These factors have compounds the complexity of interface tailoring in CMCs leading to a need for specific solution for a specific CMC system.

  20. Quantitative, chemical, and mineralogical characterization of flue gas desulfurization by-products.

    PubMed

    Laperche, Valérie; Bigham, Jerry M

    2002-01-01

    The objective of this study was to demonstrate that simple fractionation and selective dissolution techniques can be used to provide detailed chemical and mineralogical analyses of flue gas desulfurization by-products. The material studied was a mine grout prepared as a 1:1 mixture (wt./wt.) of fly ash (FA) and filter cake (FC) with hydrated lime (50 g kg(-1)) added to improve handling. The hydrated lime was composed mostly of calcite (CaCO3), portlandite [Ca(OH)2], lime (CaO), and brucite [Mg(OH)2] (515, 321, 55, and 35 g kg(-1), respectively) and had low (<6 g kg(-1)) concentrations of most trace elements. The FC contained hannebachite (CaSO3 x 0.5H2O) (786 g kg(-1)) with smaller quantities (<10 g kg(-1)) of calcite, quartz (SiO2), brucite, and gypsum (CaSO4 x 2H2O). Except for B and Cu, trace element concentrations were comparable to those in the hydrated lime. The FA contained both magnetic (222 g kg(-1)) and nonmagnetic (778 g kg(-1)) fractions. The former was composed mostly of hematite (Fe2O3), magnetite (Fe3O4), and glass (272, 293, and 287 g kg(-1), respectively), whereas the latter was enriched in glass, quartz, and mullite (Al6Si2O13) (515, 243, and 140 g kg(-1), respectively). Etching with 1% HF showed that 60 to 100% of trace elements were concentrated in the glass, although some metals (Co, Cr, and Mn) were clearly enriched in the magnetic phase. The aged grout contained 147 g kg(-1) ettringite [Ca6Al2(SO4)3(OH)12 x 26H2O] in addition to 314 g kg(-1) hannebachite and 537 g kg(-1) insoluble phases (mullite, quartz, hematite, magnetite, and glass). PMID:12026103

  1. Processing and characterization of multi-cellular monolithic bioceramics for bone regenerative scaffolds

    SciTech Connect

    Ari-Wahjoedi, Bambang; Ginta, Turnad Lenggo; Parman, Setyamartana; Abustaman, Mohd Zikri Ahmad

    2014-10-24

    Multicellular monolithic ceramic body is a ceramic material which has many gas or liquid passages partitioned by thin walls throughout the bulk material. There are many currently known advanced industrial applications of multicellular ceramics structures i.e. as supports for various catalysts, electrode support structure for solid oxide fuel cells, refractories, electric/electronic materials, aerospace vehicle re-entry heat shields and biomaterials for dental as well as orthopaedic implants by naming only a few. Multicellular ceramic bodies are usually made of ceramic phases such as mullite, cordierite, aluminum titanate or pure oxides such as silica, zirconia and alumina. What make alumina ceramics is excellent for the above functions are the intrinsic properties of alumina which are hard, wear resistant, excellent dielectric properties, resists strong acid and alkali attacks at elevated temperatures, good thermal conductivities, high strength and stiffness as well as biocompatible. In this work the processing technology leading to truly multicellular monolithic alumina ceramic bodies and their characterization are reported. Ceramic slip with 66 wt.% solid loading was found to be optimum as impregnant to the polyurethane foam template. Mullitic ceramic composite of alumina-sodium alumino disilicate-Leucite-like phases with bulk and true densities of 0.852 and 1.241 g cm{sup −3} respectively, pore linear density of ±35 cm{sup −1}, linear and bulk volume shrinkages of 7-16% and 32 vol.% were obtained. The compressive strength and elastic modulus of the bioceramics are ≈0.5-1.0 and ≈20 MPa respectively.

  2. Isotope study on diffusion in CaSO{sub 4} formed during sorbent-flue-gas reaction

    SciTech Connect

    Hsia, C.; St. Pierre, G.R.; Fan, L.S.

    1995-10-01

    In sorbent-flue-gas reactions, porous CaO sorbent particles are used to capture SO{sub 2} by formation of CaSO{sub 4}. Because of the large molar volume of CaSO{sub 4}, the internal surface area which is originally available for reaction diminishes as CaSO{sub 4} forms. Once the CaSO{sub 4} layer forms, further sorbent sulfation is believed to be controlled by the product layer diffusion process. It has been suggested that the product layer diffusion occurs by gaseous diffusion (Simons and Garman, 1976) and by ionic diffusion (Bhatia and Perlmutter, 1981). In this work, a two-stage sulfation experiment using {sup 32}SO{sub 2} and {sup 34}SO{sub 2} was performed. For the first stage of sulfation, at 1,300 C, 5,000 ppm {sup 32}SO{sub 2}/air mixture was passed into the mullite tube and circulated out through the bubbler continuously. This stage lasted for 14 days. When the first stage was terminated, the tablets were removed from the furnace and examined. At the beginning of the second stage sulfation, 5,000 ppm {sup 32}SO{sub 2}/air mixture was first used during the heating period. As soon as the tube temperature reached 1,300 C, the mechanical pump was turned on and the pressure in the tube was reduced immediately. Upon the completion of the evacuation, isotope gas 75%{sup 34}SO{sub 2}-25%{sup 32}SO{sub 2} was introduced into the mullite tube. Appropriate amount of air was also introduced into the tube such that the total SO{sub 2} concentration was roughly 5,000 ppm. The second stage sulfation lasted for three days. The SIMS analysis was performed by Microelectronics Center in North Carolina.

  3. Design of sintered, tough, oxide laminate and fibrous monolithic composites

    NASA Astrophysics Data System (ADS)

    Kim, Dong-Kyu

    Tough, oxide, laminated and fibrous monolithic composites were fabricated by using tape casting and co-extrusion technique, respectively. Mullite (3Al 2O3·2SiO2), alumina (Al2O 3), 50 vol% alumina · 50 vol% YAG (yttrium aluminum garnet, Y 3Al5O12) in situ composite, 50 vol% alumina · 50 vol% mullite in situ composite, zirconia (ZrO 2), and nickel aluminate (NiAl2O4) were used as matrix materials. Aluminum phosphate (AlPO4), alumina platelets, and 50 vol% alumina · 50 vol% leucite (KAlSi2O6) were chosen as high temperature applicable interphase materials. ICP (Inductively coupled plasma) data indicated no extensive decomposition of AlPO4 heat treated at 1600 and 1800°C. The AlPO4 worked as a stable, porous, weak, crack deflecting interphase material with three point bending strength of 1.5 MPa and 61% of theoretical density after heat treatment at 1600°C for 10h. The 50 vol% alumina · 50 vol% YAG in situ composite had a bending strength of 361 MPa after sintering at the condition of 1700°C/5h. A : B (C) : D (E) bimodal designs were proposed to increase the toughness of the laminated composites. 1 : 5 (6) : 12 (1) bimodal laminated composite had a bending strength and a work of fracture of 142 MPa and 0.51 KJ/m2, respectively. Fibrous monolithic composites with different interphase thickness and interphase composition were fabricated. 2-, 3- and mixed-layer fibrous monolithic composites were made.

  4. Stabilization of nickel by aluminum- and iron-rich ceramic materials: Reaction pathways and product leaching behavior

    NASA Astrophysics Data System (ADS)

    Shih, Kaimin

    The feasibility of stabilizing nickel-laden sludge with commonly available ceramic precursors was investigated. Nickel aluminate spinel (NiAl2O 4) was the immobilization phase produced when NiO was sintered with aluminum-rich precursors, including gamma-Al2O3, corundum, kaolinite and mullite. Analogously, nickel ferrite spinel (NiFe2O 4) was the stable phase produced by firing NiO with hematite, as an iron-rich precursor. By using gamma-Al2O3 as the precursor, the NiAl2O4 formation mechanism was a reaction between NiO and gamma-Al2O3 at lower temperatures (990°C), while the reaction was between NiO and corundum at higher temperatures. When sintering NiO with kaolinite, nickel can be efficiently incorporated in NiAl2O4 by two mechanisms: (i) a low temperature reaction with a defect spinel, and (ii) a high temperature reaction with mullite. Nickel-incorporation efficiency was quantitatively estimated by powder X-ray Diffraction (XRD) analysis. With 3-hours sintering, NiFe2O 4 (trevorite) formation took place above 600°C with more than 95% nickel incorporation efficiency achieved above 1000°C; while NiAl 2O4 crystallized above 1000°C with an efficiency >90% above 1250°C. In using kaolinite and mullite as precursors, nickel is not incorporated in any silicon-containing phase. The kinetic factors responsible for nickel incorporation efficiency from different precursors were revealed through investigation of product microstructures. Moreover, four raw material mixing procedures were compared, with the ball-milled slurries demonstrating the highest nickel incorporation efficiency. Prolonged leach tests of NiO, NiAl2O4, NiFe 2O4 and sintered kaolinite + NiO samples were carried out using the TCLP extraction fluids #1 and #2 to evaluate the durability of sintered products. Over longer leaching periods, spinel proved superior to NiO for immobilization of nickel, although NiFe2O4 appears slightly more leachable than NiAl2O4. With TCLP extraction fluid #1 (pH 4.9), the

  5. Properties and utilization aspects of fly ash from a anthracite coal-fired power plant in northwestern Henan Province, P. R. China

    SciTech Connect

    Sun Junmin; Li Yuqiong

    1998-12-31

    Jiaozuo power plant, located in northwestern Henan province, is one of the largest plants in the power network of central China. It is equipped with 6{times}200MW generating sets fed by the anthracite coal from Shanxi province. Up to 0.8 million tons of fly ash, bottom ash, and boiler slag are produced annually and less than 20% of them was used beneficially. Fly ash is separated into floating spheres, magnetic spheres, settling spheres and unburnt carbon; the contents of the fractions are 0.7%, 0.62%, 91.68% and 7%, respectively. Bottom ash and separated fly ash were analyzed with SEM, XRD and wet chemical method. Morphologically, floating spheres are large cenospheres. Settling spheres are spheroids with smooth surfaces, most of them are less than 10 {micro}m in diameter. Magnetic spheres present rough surfaces with intergrowth of hematite and magnetite crystals. Unburnt carbon is predominantly infusible char, reflecting the high coalification degree of the feed coal. Mineralogically, the content and crystal size of mullite in bottom ash are greater than in floating and settling spheres. Chemically, floating spheres contain more Al{sub 2}O{sub 3} and SiO{sub 2} and less Fe{sub 2}O{sub 3}, CaO, MgO, K{sub 2}O in comparison with bottom ash and settling spheres, which indicates that floating spheres are originated from the minerals with high melting point and viscosity. To date, fly ash from this power plant has been used in sticky soil amendment, brick production by mixing with coal waste; highway pavement; railway tunnel construction and thermal insulation material production using floating spheres. Other applications must be developed to recycle the high fly ash output. Small settling spheres, especially those less than 10{micro}m in diameter, have great potential in concrete and functional filling, so the separation and utilization of very small settling spheres should be emphasized. Additionally, bottom ash may be used for synthesis of mullite.

  6. Paragenesis of unusual Fe-cordierite (sekaninaite)-bearing paralava and clinker from the Kuznetsk coal basin, Siberia, Russia

    NASA Astrophysics Data System (ADS)

    Grapes, Rodney; Korzhova, Sophia; Sokol, Ella; Seryotkin, Yurii

    2011-08-01

    Sekaninaite (XFe > 0.5)-bearing paralava and clinker are the products of ancient combustion metamorphism in the western part of the Kuznetsk coal basin, Siberia. The combustion metamorphic rocks typically occur as clinker beds and breccias consisting of vitrified sandstone-siltstone clinker fragments cemented by paralava, resulting from hanging-wall collapse above burning coal seams and quenching. Sekaninaite-Fe-cordierite (XFe = 95-45) is associated with tridymite, fayalite, magnetite, ± clinoferrosilite and ±mullite in paralava and with tridymite and mullite in clinker. Unmelted grains of detrital quartz occur in both rocks (<3 vol% in paralavas and up to 30 vol% in some clinkers). Compositionally variable siliceous, K-rich peraluminous glass is <30% in paralavas and up to 85% in clinkers. The paralavas resulted from extensive fusion of sandstone-siltstone (clinker), and sideritic/Fe-hydroxide material contained within them, with the proportion of clastic sediments ≫ ferruginous component. Calculated dry liquidus temperatures of the paralavas are 1,120-1,050°C and 920-1,050°C for clinkers, with calculated viscosities at liquidus temperatures of 101.6-7.0 and 107.0-9.8 Pa s, respectively. Dry liquidus temperatures of glass compositions range between 920 and 1,120°C (paralava) and 920-960°C (clinker), and viscosities at these temperatures are 109.7-5.5 and 108.8-9.7 Pa s, respectively. Compared with worldwide occurrences of cordierite-sekaninaite in pyrometamorphic rocks, sekaninaite occurs in rocks with XFe (mol% FeO/(FeO + MgO)) > 0.8; sekaninaite and Fe-cordierite occur in rocks with XFe 0.6-0.8, and cordierite (XFe < 0.5) is restricted to rocks with XFe < 0.6. The crystal-chemical formula of an anhydrous sekaninaite based on the refined structure is | {{{K}}_{0.02} } |({{Fe}}_{1.54}^{2 + } {{Mg}}_{0.40} {{Mn}}_{0.06} )_{Upsigma 2.00}M [({{Al}}_{1.98} {{Fe}}_{0.02}^{2 + } {{Si}}_{1.00} )_{Upsigma 3.00}^{T1} ({{Si}}_{3.94} {{Al}}_{2.04} {{Fe}}_{0

  7. Phase transformations and residual stresses in environmental barrier coatings

    NASA Astrophysics Data System (ADS)

    Harder, Bryan J.

    Silicon-based ceramics (SiC, Si3N4) are promising materials for high-temperature structural applications in turbine engines. However, the silica layer that forms on these materials is susceptible to attack from water vapor present in combustion environments. To protect against this degradation, environmental barrier coatings (EBCs) were developed to protect the underlying substrate. In the case of silicon carbide (SiC), multilayer coating systems consist of a Ba1-xSrxAl2Si 2O8 (BSAS) topcoat, a mullite or mullite + SrAl2Si 2O8 (SAS) interlayer, and a silicon bond coat. In this work, biaxial strains were measured on as-sprayed and heat-treated samples to analyze the stress and phase evolution in the coating system as a function of depth and temperature. Models were used to compare the results with an ideal coating system. In the assprayed state, tensile stresses as high as 175 MPa were measured, and cracking was observed. After thermally cycling the samples, stresses were significantly reduced and cracks in the topcoat had closed. The addition of SAS to the interlayer increased the compressive stress in the BSAS topcoat in thermally-cycled samples, which was desirable for EBC applications. The BSAS topcoat transformed from the as-deposited hexacelsian state to the stable celsian above 1200°C. This phase transformation is accompanied by a CTE reduction. The kinetics of the hexacelsian-to-celsian transformation were quantified for freestanding plasma-sprayed BSAS. Activation energies for bulk bars and crushed powder were determined to be ˜340 kJ/mol and ˜500 kJ/mol, respectively. X-ray diffraction and electron backscatter diffraction were used to establish how microstructural constraints reduce the transformation energy. Barrier coating lifetime and stability are also influenced by exposure to reactive, low-melting point calcium-magnesium-aluminosilicate (CMAS) deposits formed from dust and sand. Multilayer doped aluminosilicate coatings and bulk BSAS material were

  8. Feasible voltage-tap based quench detection in a Ag/Bi-2212 coil enabled by fast 3D normal zone propagation

    DOE PAGESBeta

    Shen, Tengming; Ye, Liyang; Li, Pei

    2016-07-01

    For this study, small insert solenoids have been built using a commercial Ag/Bi-2212 multifilamentary round wire, insulated with a new thin TiO2– polymer coating insulation (thickness in ~20 μm versus ~100 μm for a commonly used mullite braided sleeve insulation), and characterized in background magnetic field up to 14 T at 4.2 K to explore the high-field performance and quench detection of Bi-2212 magnets. The coil has no visible leakage and no electrical shorts after reaction, and it carries 280 A/mm-2 in a background field 14 T and generates an additional 1.7 T. A notable result is that, despite normalmore » zones propagate slowly along the conductor, the hot spot temperature upon detection increases only from 40 K to 60 K when the resistive quench detection voltage threshold increases from 0.1 V to 1 V for all operating current density investigated, showing that quench detection using voltage taps is feasible for this coil. This is in a strong contrast to a coil we previously built to the same specifications but from wires insulated with the mullite braided sleeve insulation, for which the hot spot temperature upon detection increases from ~80 K to ~140 K while increasing from the detection voltage threshold from 0.1 V to 1 V, and thus for which quench detection using voltage taps presents significant risks, consistent with the common belief that the effectiveness of quench detection using voltage taps for superconducting magnets built using high temperature superconductors is seriously compromised by their slow normal zone propagation. This striking difference is ascribed to the fast transverse quench propagation enabled by thin insulation and improved thermal coupling between conductor turns. Finally, this work demonstrates that quench detection for high-temperature superconducting magnets highly depends on the design and construction of the coils such as insulation materials used and this dependence should be factored into the overall magnet design.« less

  9. Feasible voltage-tap based quench detection in a Ag/Bi-2212 coil enabled by fast 3D normal zone propagation

    NASA Astrophysics Data System (ADS)

    Shen, Tengming; Ye, Liyang; Li, Pei

    2016-08-01

    Small insert solenoids have been built using a commercial Ag/Bi-2212 multifilamentary round wire, insulated with a new thin TiO2–polymer coating insulation (thickness of ∼20 μm versus ∼100 μm for a commonly used mullite braided sleeve insulation), and characterized in a background magnetic field up to 14 T at 4.2 K to explore the high-field performance and quench detection of Bi-2212 magnets. The coil has no visible leakage and no electrical shorts after reaction, and it carries 280 A mm‑2 in a background field of 14 T and generates an additional 1.7 T. A notable result is that, despite normal zones propagating slowly along the conductor, the hot spot temperature upon detection increases only from 40 K to 60 K when the resistive quench detection voltage threshold increases from 0.1 V to 1 V for all operating current density investigated, showing that quench detection using voltage taps is feasible for this coil. This is in strong contrast to a coil we have previously built to the same specifications but from wires insulated with mullite braided sleeve insulation, for which the hot spot temperature upon detection increases from ∼80 K to ∼140 K while increasing the detection voltage threshold from 0.1 V to 1 V, and thus for which quench detection using voltage taps presents significant risks, consistent with the common belief that the effectiveness of quench detection using voltage taps for superconducting magnets built using high-temperature superconductors is seriously compromised by their slow normal zone propagation. This striking difference is ascribed to the fast transverse quench propagation enabled by thin insulation and the improved thermal coupling between conductor turns. This work demonstrates that quench detection for high-temperature superconducting magnets highly depends on the design and construction of the coils such as the insulation materials used and this dependence should be factored into the overall magnet design.

  10. Measurement and Analysis of Narrow-Band Surface Acoustic Waves in Ceramic Environmental Barrier Coatings

    NASA Astrophysics Data System (ADS)

    Steen, T. L.; Basu, S. N.; Sarin, V. K.; Murray, T. W.

    2008-02-01

    A laser-based ultrasonic system is used to measure the mechanical properties and thickness of mullite environmental barrier coatings deposited on SiC substrates. Narrow-band surface acoustic waves (SAWs) are generated with an amplitude modulated laser source, and a photorefractive crystal based interferometer coupled to a lock-in amplifier is used to detect the resulting surface displacement. The complex displacement field is mapped over a source-to-receiver distance of approximately 500 μm in order to extract the wavelength of the SAW at a given excitation frequency, from which the phase velocity is determined. Dispersion curves measured over a frequency range of 100-180 MHz are used to extract mean values for the elastic modulus and thickness of the coating over the measurement region. These values are compared to the mean elastic modulus and thickness of the coating measured using nanoindentation and optical microscopy, respectively. It is shown that porosity in the substrate can have a significant impact on the experimental results, particularly over short measurement distances. Experiments on SiC with 1-4% porosity show a linear increase of the mean SAW velocity with decreasing porosity. Additionally, measurements made on a sample with a given bulk porosity indicate that the SAW velocity varies locally, leading to additional error in the measurement of coating properties. This error can be reduced through spatially averaging the velocity measurements.

  11. A study of surface tension driven segregation in monotectic alloy systems

    NASA Technical Reports Server (NTRS)

    Andrews, J. Barry; Andrews, Rosalia N.; Gowens, Terrell F.

    1988-01-01

    The compatibilities of various monotectic alloy systems with several different crucible materials were evaluated. The study was carried out using small candidate alloy samples of compositions that produced fifty volume percent of each liquid phase at the monotectic temperature. Compatibility was based on the evaluation of the wetting tendency of the two immiscible phases with the crucible material in a one-g solidified sample. Three types of wetting phenomena were observed during the evaluation. Type 1 indicates an alloy-crucible combination where the L2 phase preferentially wets the crucible material. Since L2 is usually the minority phase in desirable alloys, this material combination would be difficult to process and is therefore considered incompatible. Type 2 behavior indicates an alloy-crucible combination where the L1 phase preferentially wets the crucible material. This type of combination is considered compatible since surface tension effects should aid in processing the alloy to a useful form. Type 3 indicates any combination that leads to major reactions between the alloy and crucible material, gas entrapment, or separation of the metal from the crucible wall. Additional compatibility evaluations would have to be carried out on combinations of this category. The five alloy systems studied included aluminum-bismuth, copper-lead, aluminum-indium, aluminum-lead and cadmium-gallium. The systems were combined with crucibles of alumina, boron nitride, mullite, quartz, silicon carbide and zirconia.

  12. Crack-resistant Al2O3-SiO2 glasses.

    PubMed

    Rosales-Sosa, Gustavo A; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

    2016-01-01

    Obtaining "hard" and "crack-resistant" glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3-(100-x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3-SiO2 glasses. In particular, the composition of 60Al2O3 • 40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses. PMID:27053006

  13. Effect of size of man-made and natural mineral fibers on chemiluminescent response in human monocyte-derived macrophages.

    PubMed Central

    Ohyama, M; Otake, T; Morinaga, K

    2001-01-01

    Fiber size is an important factor in the tumorigenicity of various mineral fibers and asbestos fibers in animal experiments. We examined the time course of the ability to induce lucigenin-dependent chemiluminescence (CL) from human monocyte-derived macrophages exposed to Japan Fibrous Material standard reference samples (glass wool, rock wool, micro glass fiber, two types of refractory ceramic fiber, refractory mullite fiber, potassium titanium whisker, silicon carbide whisker, titanium oxide whisker, and wollastonite). We determined how fiber length or width might modify the response of cells. We found that the patterns of time-dependent increase of CL (sigmoid type) were similar for each sample except wollastonite. We observed a strong correlation between geometric-mean length and ability to induce CL in seven samples > 6 microm in length over the time course (largest r(2) = 0.9760). Although we also observed a close positive correlation between geometric-mean width and the ability to induce CL in eight samples < 1.8 microm in width at 15 min (r(2) = 0.8760), a sample of 2.4 microm in width had a low ability to induce CL. Moreover, the relationship between width and the rate of increase in ability to induce CL had a negative correlation at 30-60 min (largest r(2) = 0.7473). Our findings suggest that the release of superoxide from macrophages occurs nonspecifically for various types of mineral fibers depending on fiber length. PMID:11675268

  14. Strength testing of hot gas filters: Volume 6. Final report

    SciTech Connect

    Faber, K.T.

    1998-06-09

    The strength of various ceramic hot gas filter materials has been evaluated by four laboratories: Argonne National Laboratory, DuPont Lanxide, Southern Research Institute and Babcock and Wilcox. The filter materials under study include (a) a Nextel{trademark}/SiC composite filter (from 3M), (b) PRD-66, an all oxide layered microstructure of alumina, mullite, cordierite and some amorphous material by DuPont Lanxide, (c) a Babcock and Wilcox material consisting of an oxide composite of chopped fibers (Saffil) and continuous Nextel fibers, (d-f) monolithic and recrystallized SiC materials and an alumino/aluminosilicate material by IFPM, and (g) a monolithic SiC by the Pall Corporation. Not all four organizations tested each of the materials. PRD-66 was tested by three of the four. Four tests were used to evaluate properties of the candle filter materials. They included (a) the C-ring test, (b) the O-ring test, (c) the burst test and (d) the axial compression test. Each organization identified above did not perform all four tests. The objective of the study described here was to (a) provide an evaluation of the test methods used for hot gas filters to determine which is best for hot gas filter evaluation and (b) evaluate the discrepancies in results from tests run at different laboratories. No material ranking was made here, nor requested.

  15. Stability of polycrystalline Nextel 720 fiber

    SciTech Connect

    Das, G.

    1996-12-31

    The microstructure and tensile properties of polycrystalline Nextel 720 fiber (85 wt.% Al{sub 2}O{sub 3} - 15 wt-% SiO{sub 2}), both crystallized and precrystallized, were evaluated following prolonged thermal exposure at 982{degrees}C in air. The room temperature tensile strengths of Nextel 720 fibers did not appear to suffer degradation for exposures up to 3000 h and the microstructure remained unaffected by thermal exposures. The tensile strength of precrystallized Nextel 720 fiber was also determined at room temperature following heat treatments at 1093-1427{degrees}C in air. The precrystallized Nextel 720 fiber started to show a slight loss of strength after heat treatment at 1093{degrees}C/4 h and the strength deterioration was exacerbated for heat treatments at 1204{degrees}C/4 h and above. Microstructural characterization by x-ray and transmission electron microscopy (TEM) revealed the formation of mullite in heat treated precrystallized Nextel 720 fiber at 1204{degrees}C and a coarsening of microstructure above 1204{degrees}C. The degradation of strength in precrystallized Nextel 720 fiber heat treated at 1204{degrees}C/4 h and above may be attributed to phase instability and grain coarsening. Fractographs showed that fracture originated predominantly at the fiber surface.

  16. Hollow proppants and a process for their manufacture

    DOEpatents

    Jones, A.H.; Cutler, R.A.

    1985-10-15

    Hollow, fine-grained ceramic proppants are less expensive and improve fracture control when compared to conventional proppants (dense alumina, mullite, bauxite, zirconia, etc.). Hollow proppants of the present invention have been fabricated by spray drying, followed by sintering in order to obtain a dense case and a hollow core. These proppants generally have high sphericity and roundness (Krumbein sphericity and roundness greater than 0.8), have diameters on average between 2,250 and 125 [mu]m, depending on proppant size required, and have strength equal to or greater than that of sand. The hollow core, the size of which can be controlled, permits better fracture control in hydraulic fracturing treatments since the proppant can be transported in lower viscosity fluids. Hollow proppants produced at the same cost/weight as conventional proppants also provide for lower costs, since less weight is required to fill the same volume. The fine-grained (preferably less than 5 [mu]m in diameter) ceramic case provides the strength necessary to withstand closure stresses and prevent crushing. 6 figs.

  17. ADVANCED HOT GAS FILTER DEVELOPMENT

    SciTech Connect

    E.S. Connolly; G.D. Forsythe

    1998-12-22

    Advanced, coal-based power plants will require durable and reliable hot gas filtration systems to remove particulate contaminants from the gas streams to protect downstream components such as turbine blades from erosion damage. It is expected that the filter elements in these systems will have to be made of ceramic materials to withstand goal service temperatures of 1600 F or higher. Recent demonstration projects and pilot plant tests have indicated that the current generation of ceramic hot gas filters (cross-flow and candle configurations) are failing prematurely. Two of the most promising materials that have been extensively evaluated are clay-bonded silicon carbide and alumina-mullite porous monoliths. These candidates, however, have been found to suffer progressive thermal shock fatigue damage, as a result of rapid cooling/heating cycles. Such temperature changes occur when the hot filters are back-pulsed with cooler gas to clean them, or in process upset conditions, where even larger gas temperature changes may occur quickly and unpredictably. In addition, the clay-bonded silicon carbide materials are susceptible to chemical attack of the glassy binder phase that holds the SiC particles together, resulting in softening, strength loss, creep, and eventual failure.

  18. Use of a variable frequency source with a single-mode cavity to process ceramic filaments

    SciTech Connect

    Vogt, G.J.; Regan, A.H.; Rohlev, A.S.; Curtin, M.T.

    1995-09-01

    Rapid feedback control is needed for practical microwave processing of continuous ceramic oxide filaments to regulate the process temperature where the -dielectric properties of the filaments change rapidly with temperature. These dielectric changes can produce large rapid changes in the resonant frequency, the reflectivity, and the power density of the cavity. A broadband traveling wave tube (TWT) amplifier provides a highly versatile process control platform for filament processing. By comparing a RF signal from the cavity to a reference signal from the TWT, phase information can be used in a negative feedback loop to allow the oscillator to track the cavity frequency as it shifts due to the changing dielectric constant in the filaments being heated. By sampling the electric field level in the cavity with a detector, amplitude control can be done to maintain a constant absorbed power in a fiber tow, which is important for controlling the tow heating and temperature. This paper describes the design and testing of feedback controller with mullite rods in a single-mode TE{sub 10n} resonator driven by a commercial TWT.

  19. Tension-Compression Fatigue of a Nextel™720/alumina Composite at 1200 °C in Air and in Steam

    NASA Astrophysics Data System (ADS)

    Lanser, R. L.; Ruggles-Wrenn, M. B.

    2016-02-01

    Tension-compression fatigue behavior of an oxide-oxide ceramic-matrix composite was investigated at 1200 °C in air and in steam. The composite is comprised of an alumina matrix reinforced with Nextel™720 alumina-mullite fibers woven in an eight harness satin weave (8HSW). The composite has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. Tension-compression fatigue behavior was studied for cyclical stresses ranging from 60 to 120 MPa at a frequency of 1.0 Hz. The R ratio (minimum stress to maximum stress) was -1.0. Fatigue run-out was defined as 105 cycles and was achieved at 80 MPa in air and at 70 MPa in steam. Steam reduced cyclic lives by an order of magnitude. Specimens that achieved fatigue run-out were subjected to tensile tests to failure to characterize the retained tensile properties. Specimens subjected to prior cyclic loading in air retained 100 % of their tensile strength. The steam environment severely degraded tensile properties. Tension-compression cyclic loading was considerably more damaging than tension-tension cyclic loading. Composite microstructure, as well as damage and failure mechanisms were investigated.

  20. High temperature filter materials

    SciTech Connect

    Alvin, M.A.; Lippert, T.E.; Bachovchin, D.M.; Tressler, R.E.

    1992-12-01

    Objectives of this program are to identify the potential long-term thermal/chemical effects that advanced coal-based power generating system environments have on the stability of porous ceramic filter materials, as well as to assess the influence of these effects on filter operating performance and life. We have principally focused our efforts on developing an understanding of the stability of the alumina/mullite filter material at high temperature (i.e., 870, 980, and 1100{degrees}C) under oxidizing conditions which contain gas phase alkali species. Testing has typically been performed in two continuous flow-through, high temperature test facilities at the Westinghouse Science and Technology Center, using 7 cm diameter {times} 6.4 mm thick discs. (Alvin, 1992) Each disc of ceramic filter material is exposed for periods of 100 to 3,000 hours in duration. Additional efforts have been performed at Westinghouse to broaden our understanding of the stability of cordierite, cordierite-silicon nitride, reaction and sintered silicon nitride, and clay bonded silicon carbide under similar simulated advanced coal fired process conditions. The results of these efforts are presented in this paper.

  1. Filter component assessment

    SciTech Connect

    Alvin, M.A.; Lippert, T.E.; Diaz, E.S.; Smeltzer, E.W.

    1995-11-01

    The objectives of this program are to provide a more ruggedized filter system that utilizes porous ceramic filters which have improved resistance to damage resulting from crack propagation, thermal fatigue and/or thermal excursions during plant or process transient conditions, and/or mechanical ash bridging events within the candle filter array. As part of the current Phase 1, Task 1, effort of this program, Westinghouse is evaluating the filtration characteristics, mechanical integrity, and corrosion resistance of the following advanced or second generation candle filters for use in advanced coal-fired process applications: 3M CVI-SiC composite--chemical vapor infiltration of silicon carbide into an aluminosilicate Nextel{trademark} 312 fiber preform; DuPont PRD-66--filament wound candle filter structure containing corundum, cordierite, cristobalite, and mullite; DuPont SiC-SiC--chemical infiltration of silicon carbide into a silicon carbide Nicalon{trademark} fiber mat or felt preform; and IF and P Fibrosic{trademark}--vacuum infiltrated oxide-based chopped fibrous matrix. Results to date are presented.

  2. High temperature filter materials

    SciTech Connect

    Alvin, M.A.; Lippert, T.E.; Bachovchin, D.M. . Science and Technology Center); Tressler, R.E. )

    1992-01-01

    Objectives of this program are to identify the potential long-term thermal/chemical effects that advanced coal-based power generating system environments have on the stability of porous ceramic filter materials, as well as to assess the influence of these effects on filter operating performance and life. We have principally focused our efforts on developing an understanding of the stability of the alumina/mullite filter material at high temperature (i.e., 870, 980, and 1100[degrees]C) under oxidizing conditions which contain gas phase alkali species. Testing has typically been performed in two continuous flow-through, high temperature test facilities at the Westinghouse Science and Technology Center, using 7 cm diameter [times] 6.4 mm thick discs. (Alvin, 1992) Each disc of ceramic filter material is exposed for periods of 100 to 3,000 hours in duration. Additional efforts have been performed at Westinghouse to broaden our understanding of the stability of cordierite, cordierite-silicon nitride, reaction and sintered silicon nitride, and clay bonded silicon carbide under similar simulated advanced coal fired process conditions. The results of these efforts are presented in this paper.

  3. Crack-resistant Al2O3–SiO2 glasses

    PubMed Central

    Rosales-Sosa, Gustavo A.; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

    2016-01-01

    Obtaining “hard” and “crack-resistant” glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3–(100–x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3–SiO2 glasses. In particular, the composition of 60Al2O3•40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses. PMID:27053006

  4. Preparation of Functionally Graded Materials (FGMs) Using Coal Fly Ash and NiCr-Based Alloy Powder by Spark Plasma Sintering (SPS)

    SciTech Connect

    Kaneko, Gen-yo; Kitagawa, Hiroyuki; Hasezaki, Kazuhiro; Ito, Yuji; Kakuda, Hideaki

    2008-02-15

    Functionally Graded Materials (FGMs) were prepared by spark plasma sintering (SPS) using coal fly ash and NiCr alloy powder. The coal fly ash was produced by the Misumi Coal Thermal Power Station (Chugoku Electric Power Co., Inc.), with 80 wt% nickel and 20 wt% chromium (Fukuda Metal Foil and Powder Co., Ltd.) used as source materials. The sintering temperature in the graphite die was 1000 deg. C. X-ray diffraction patterns of the sintered coal fly ash materials indicated that mullite (3Al{sub 2}O{sub 3}{center_dot}2SiO{sub 2}) and silica (SiO{sub 2}) phases were predominant. Direct joining of coal fly ash and NiCr causes fracture at the interface. This is due to the mismatch in the thermal expansion coefficients (CTE). A crack in the FGM was observed between the two layers with a CTE difference of over 4.86x10{sup -6} K{sup -1}, while a crack in the FGM was difficult to detect when the CTE difference was less than 2.77x10{sup -6} K{sup -1}.

  5. Performance evaluation of porous radiant gas burners

    SciTech Connect

    Speyer, R.F.; Lin, Wen-Yi; Agarwal, G.

    1995-12-31

    A porous radiant burner testing facility was built, consisting of temperature and gas composition measurements as a function of position, as well as spectral and total radiosity measurements. Uncombusted hydrocarbons were detected within the flame support layer for only low flow rates (e.g 7.1 1/min for a reticulated ceramic flame support layer); only combustion products mixed with the atmosphere were detected at higher rates. Radiosity increased with increasing flow rate via increasing surface temperatures, while burner efficiencies decreased because of less effectual heat transfer of combustion product gases to solid surfaces. Stainless steel screen-based flame support layers demonstrated optimum performance as compared to ceramic and metal tube-based, and reticulated ceramic-based flame support layers. Increased turbulent flow and surface area for convective heat transfer between the base surface and the end of the flame support layer were factors attributed to improved burner radiosity and efficiency. The greybody temperatures and emittances of burners were determined using a simplex algorithm fit of spectral radiosity data to Planck`s equation. The significantly higher and more grey emittance (hence radiosity) of CoAl$-(2)$O$-(4)$-coated mullite flame support tubes, as compared to alumina tubes of identical geometry, was demonstrated using this method.

  6. Characterization of ceramics materials mixed with Co3O4

    NASA Astrophysics Data System (ADS)

    Guzmán, A. F.; Landínez Téllez, D. A.; Roa-Rojas, J.; Fajardo, F.

    2014-04-01

    We have performed the preparation, structural, electrical and mechanical characterizations of ceramic materials composed of kaolinite Al2(Si2O5)(OH)4 and alumina (Al2O3) mixed with different concentrations of cobalt oxide (Co3O4). Ceramic samples were prepared from a base concentration of alumina 30% and kaolinite 70%, mixed with various concentrations of cobalt oxide in steps of 4% up to a value of 20%. The samples were sintered by the standard solid-state reaction method at a temperature of 1350 °C. In all samples with cobalt was found the presence of mullite. It was determined that alumina and cristobalite decreased when the cobalt concentration was increased due to the formation of the cobalt spinel. In order to determine the crystal structure of the samples, crystallographic analysis from X-ray diffraction experiments and also the semi-quantitative phase analysis were performed. Results were compared with theoretical parameters through the PowderCell 2.4 software. By increasing the concentration of cobalt oxide was found a significant increase in the resistance of materials to friction wear and a small decrease on the mean value of the dielectric constant. Through flexion measurements is observed the increases of the elasticity modulus by about 45% for the sample with 4% of cobalt oxide when compared with the samples without cobalt.

  7. Ceramic Coating Inspection Using Laser-Based Ultrasonics and Nanoindentation

    SciTech Connect

    Steen, T. L.; Murray, T. W.; Basu, S. N.; Sarin, V. K.

    2007-03-21

    A combination of laser-based ultrasonic (LBU) inspection and nanoindentation testing is used to evaluate the thickness uniformity and through-thickness mechanical property distributions in 5-20 {mu}m thick CVD environmental barrier coatings. Mullite (3Al2O3{center_dot}2SiO2) coatings grown on silicon carbide substrates are studied in order to provide feedback on the growth process under a range of operating conditions. Nanoindentation tests are performed on polished coating cross sections, and the depth dependence of the elastic modulus of each coating is found. In the LBU experiments, a modulated continuous wave (CW) source is used for surface wave generation. The source is held at a fixed temporal frequency as it is scanned over the surface of the coating. At each temporal frequency of interest, the spatial frequencies of the acoustic modes are found, allowing for phase velocities to be determined. The mean values of elastic moduli found using the LBU approach compare well with the nanoindentation results.

  8. Chemical and mechanical consequences of environmental barrier coating exposure to calcium-magnesium-aluminosilicate.

    SciTech Connect

    Harder, B.; Ramirez-Rico, J.; Almer, J. D.; Kang, L.; Faber, K.

    2011-06-01

    The success of Si-based ceramics as high-temperature structural materials for gas turbine applications relies on the use of environmental barrier coatings (EBCs) with low silica activity, such as Ba{sub 1-x}Sr{sub x}Al{sub 2}Si{sub 2}O{sub 8} (BSAS), which protect the underlying components from oxidation and corrosion in combustion environments containing water vapor. One of the current challenges concerning EBC lifetime is the effect of sandy deposits of calcium-magnesium-aluminosilicate (CMAS) glass that melt during engine operation and react with the EBC, changing both its composition and stress state. In this work, we study the effect of CMAS exposure at 1300 C on the residual stress state and composition in BSAS-mullite-Si-SiC multilayers. Residual stresses were measured in BSAS multilayers exposed to CMAS for different times using high-energy X-ray diffraction. Their microstructure was studied using a combination of scanning electron microscopy and transmission electron microscopy techniques. Our results show that CMAS dissolves the BSAS topcoat preferentially through the grain boundaries, dislodging the grains and changing the residual stress state in the topcoat to a nonuniform and increasingly compressive stress state with increasing exposure time. The presence of CMAS accelerates the hexacelsian-to-celsian phase transformation kinetics in BSAS, which reacts with the glass by a solution-reprecipitation mechanism. Precipitates have crystallographic structures consistent with Ca-doped celsian and Ba-doped anorthite.

  9. In-situ stress analysis of multilayer environmental barrier coatings.

    SciTech Connect

    Harder, B. J.; Almer, J.; Lee, K. N.; Faber, K. T.; Northwestern Univ.; Rolls-Royce Corp.

    2009-06-01

    The biaxial stress and thermal expansion of multilayer doped-aluminosilicate environmental barrier coatings were measured in situ during cooling using microfocused high-energy X-rays in transmission. Coating stresses during cooling from 1000 C were measured for as-sprayed and thermally cycled samples. In the as-sprayed state, tensile stresses as high as 75 MPa were measured in the doped-aluminosilicate topcoat at 375 C, after which a drop in the stress occurred accompanied by through-thickness cracking of the two outermost layers. After thermally cycling the samples, the stress in the topcoat was reduced to approximately 50 MPa, and there was no drop in stress upon cooling. This stress reduction was attributed to a crystallographic phase transformation of the topcoat and the accompanying change in thermal expansion coefficient. The addition of a doped aluminosilicate to the mullite layer did not lower the stress in the topcoat, but may offer increased durability due to an increased compressive stress.

  10. Transformation of Ba-Al-Si precursors to celsian by high-temperature oxidation and annealing

    NASA Astrophysics Data System (ADS)

    Schmutzler, Hans J.; Sandhage, Kenneth H.

    1995-02-01

    Celsian (monoclinic BaO · A12O3 · 2SiO2) is being considered as a matrix material for ceramic composites used in high-temperature structural applications. The present article describes the synthesis of celsian by the oxidation and annealing of solid, malleable, metallic Ba-Al-Si precursors. The phase and microstructural evolution after various stages of oxidation at 300 °C to 1260 °C in pure oxygen at 1 atm pressure have been examined by X-ray diffraction (XRD) and electron microprobe analyses (EPMA). Barium peroxide, BaO2, formed rapidly during oxidation at 300 °C, with aluminum and silicon remaining largely as unoxidized particles in a BaO2 matrix. Between 300 °C and 500 °C, barium orthosilicate, Ba2Si04, formed by a solid-state reaction between barium peroxide and unoxidized silicon. Further exposure to temperatures between 500 °C and 1200 °C resulted in the oxidation of aluminum and of residual silicon. The oxidized silicon reacted with the barium orthosilicate matrix to yield higher silica-containing barium silicates that, in turn, reacted with alumina or mullite to form metastable hexacelsian (hexagonal BaO-A12O3 · 2SiO2). Celsian was then obtained by further exposure to peak temperatures ≤1260°C.

  11. Transformation toughened ceramics for the heavy duty diesel engine technology program

    NASA Technical Reports Server (NTRS)

    Musikant, S.; Feingold, E.; Rauch, H.; Samanta, S.

    1984-01-01

    The objective of this program is to develop an advanced high temperature oxide structural ceramic for application to the heavy duty diesel engine. The approach is to employ transformation toughening by additions of ZrO.5HfO.5O2 solid solution to the oxide ceramics, mullite (2Al2O3S2SiO2) and alumina (Al2O3). The study is planned for three phases, each 12 months in duration. This report covers Phase 1. During this period, processing techniques were developed to incorporate the ZrO.5HfO.5O2 solid solution in the matrices while retaining the necessary metastable tetragonal phase. Modulus of rupture and of elasticity, coefficient of thermal expansion, fracture toughness by indent technique and thermal diffusivity of representative specimens were measured. In Phase 2, the process will be improved to provide higher mechanical strength and to define the techniques for scale up to component size. In Phase 3, full scale component prototypes will be fabri-]cated.

  12. Surface modification of oil fly ash and its application in selective capturing of carbon dioxide

    NASA Astrophysics Data System (ADS)

    Yaumi, Ali L.; Hussien, Ibnelwaleed A.; Shawabkeh, Reyad A.

    2013-02-01

    Oil fly ash from power generation plants was activated with 30% NH4OH and used for selective adsorption of carbon dioxide from CO2/N2 mixture. The treated samples were characterized for their surface area, morphology, crystalline phase, chemical composition and surface functional groups. Energy dispersive X-ray analysis showed an increase in the carbon contents from 45 to 73 wt% as a result of leaching out metal oxides. XRD proved that chemical activation of ash resulted in diminishing of major crystalline phases of zeolite, and other alumino-silicates leaving only quartz and mullite. BET analysis showed an increase in surface area from 59 to 318 m2/g after chemical activation and the pore volume increased from 0.0368 to 0.679 cm3/g. This increase in pore volume is supported by the results of SEM, where more micropores were opened with well-defined particle sizes and porous structure. The TGA of the treated fly ash showed stability at higher temperature as the weight loss decreased with increasing temperature. For treated ash, the FTIR displayed new peaks of amine functional group. The treated ash was used for the removal of CO2 from CO2/N2 mixture and the maximum adsorption/capturing capacity was found to be 240 mg/g. This capacity increases with increase in initial gas concentration, inlet flow rate and temperature suggesting the endothermic nature of the interaction between the gas molecules and the surface of the ash.

  13. Feasibility and process scale-up low cost alumina fibers for advanced Re-usable Surface Insulation (RSI)

    NASA Technical Reports Server (NTRS)

    Pearson, A.

    1975-01-01

    The objective of this program was to establish feasibility of a process to produce low cost aluminum oxide fibers having sufficient strength, flexibility, and thermal stability for multiple re-use at temperatures to 1480 C in advanced RSI type heat shields for reentry vehicles. Using bench-scale processing apparatus, the Alcoa 'Saphiber' process was successfully modified to produce nominally 8 microns diameter polycrystalline alpha-alumina fiber. Thermal stability was demonstrated in vacuum reheating tests to 1371 C and in atmospheric reheating to 1483 C. Individual fiber properties of strength, modulus, and flexibility were not determined because of friability and short length of the fiber. Rigidized tile produced from fiber of nominally 8, 20 and 40 micron diameter had thermal conductivities significantly higher than those of RSI SiO2 or mullite at relatively low temperature but became comparable above about 1000 C. Tile densities were high due to short fiber length, especially in the coarser diameter fiber. No significant effect of fiber diameter on thermal properties could be determined form the data. Mechanical properties of tiles deteriorated as fiber diameter increased.

  14. Crystallization kinetics of BaO-Al2O3-SiO2 glasses

    NASA Technical Reports Server (NTRS)

    Bansal, Narottam P.; Hyatt, Mark J.

    1988-01-01

    Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

  15. Environmental Barrier Coatings for Ceramics and Ceramic Composites

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.; Fox, Dennis; Eldridge, Jeffrey; Robinson, R. Craig; Bansal, Narottam

    2004-01-01

    One key factor that limits the performance of current gas turbine engines is the temperature capability of hot section structural components. Silicon-based ceramics, such as SiC/SiC composites and monolithic Si3N4, are leading candidates to replace superalloy hot section components in the next generation gas turbine engines due to their excellent high temperature properties. A major stumbling block to realizing Si-based ceramic hot section components is the recession of Si-based ceramics in combustion environments due to the volatilization of silica scale by water vapor. An external environmental barrier coating (EBC) is the most promising approach to preventing the recession. Current EBCs are based on silicon, mullite (3A12O3-2SiO2) and BSAS (barium strontium aluminum silicate with celsian structure). Volatility of BSAS, BSAS-silica chemical reaction, and low melting point of silicon limit the durability and temperature capability of current EBCs. Research is underway to develop EBCs with longer life and enhanced temperature capability. Understanding key issues affecting the performance of current EBCs is necessary for successful development of advanced EBCs. These issues include stress, chemical compatibility, adherence, and water vapor stability. Factors that affect stress are thermal expansion mismatch, phase stability, chemical stability, elastic modulus, etc. The current understanding on these issues will be discussed.

  16. Durability and Design Issues of Thermal/environmental Barrier Coatings on Sic/sic Ceramic Matrix Composites Under 1650 C Test Conditions

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Choi, Sung R.; Ghosn, Louis J.; Miller, Robert A.

    2004-01-01

    Ceramic thermal/environmental barrier coatings for SiC-based ceramics will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. However, the coating durability remains a major concern with the ever-increasing temperature requirements. Currently, advanced T/EBC systems, which typically include a high temperature capable zirconia- (or hahia-) based oxide top coat (thermal barrier) on a less temperature capable mullite/barium-strontium-aluminosilicate (BSAS)/Si inner coat (environmental barrier), are being developed and tested for higher temperature capability Sic combustor applications. In this paper, durability of several thermal/environmental barrier coating systems on SiC/SiC ceramic matrix composites was investigated under laser simulated engine thermal gradient cyclic, and 1650 C (3000 F) test conditions. The coating cracking and delamination processes were monitored and evaluated. The effects of temperature gradients and coating configurations on the ceramic coating crack initiation and propagation were analyzed using finite element analysis (FEA) models based on the observed failure mechanisms, in conjunction with mechanical testing results. The environmental effects on the coating durability will be discussed. The coating design approach will also be presented.

  17. Current Issues with Environmental Barrier Coatings for Ceramics and Ceramic Composites

    NASA Technical Reports Server (NTRS)

    Lee, Kang N.

    2004-01-01

    The environmental barrier coating (EBC) for SiC/SiC ceramic matrix composites and Si3N4 ceramics is an emerging field as the application of silicon-based ceramics in the gas turbine engine hot section is on the horizon, both for aero and industrial gas turbines. EBC is an enabling technology for silicon-based ceramics because these materials without an EBC cannot be used in combustion environments due to rapid surface recession. Significant progress in EBC development has been made during the last decade through various government-sponsored programs. Current EBCs are based on silicon, mullite (3Al2O3-2SiO2) and BSAS (barium strontium aluminum silicate with celsian structure). Volatility of BSAS, BSAS-silica chemical reaction, and low melting point of silicon limit temperature capability of current EBCs to about 1350 C for long-term applications. There is a need for higher temperature EBCs as the temperature capability of silicon-based ceramics continue to increase. Therefore, research is underway to develop EBCs with improved temperature capability compared to current EBCs. The current status and issues with the advanced EBC development efforts will be discussed.

  18. Delamination Mechanisms of Thermal and Environmental Barrier Coatings on SiC/SiC Ceramic Matrix Composites

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Choi, Sung R.; Lee, Kang N.; Miller, Robert A.

    2003-01-01

    Advanced ceramic thermal harrier coatings will play an increasingly important role In future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. However, the coating durability issue remains a major concern with the ever-increasing temperature requirements. In this paper, thermal cyclic response and delamination failure modes of a ZrO2-8wt%Y2O3 and mullite/BSAS thermaVenvironmenta1 barrier coating system on SiC/SiC ceramic matrix composites were investigated using a laser high-heat-flux technique. The coating degradation and delamination processes were monitored in real time by measuring coating apparent conductivity changes during the cyclic tests under realistic engine temperature and stress gradients, utilizing the fact that delamination cracking causes an apparent decrease in the measured thermal conductivity. The ceramic coating crack initiation and propagation driving forces under the cyclic thermal loads, in conjunction with the mechanical testing results, will be discussed.

  19. Crack Driving Forces in a Multilayered Coating System for Ceramic Matrix Composite Substrates

    NASA Technical Reports Server (NTRS)

    Ghosn, Louis J.; Zhu, Dongming; Miller, Robert A.

    2005-01-01

    The effects of the top coating thickness, modulus and shrinkage strains on the crack driving forces for a baseline multilayer Yttria-Stabilized-Zirconia/Mullite/Si thermal and environment barrier coating (TEBC) system for SiC/SiC ceramic matrix composite substrates are determined for gas turbine applications. The crack driving forces increase with increasing modulus, and a low modulus thermal barrier coating material (below 10 GPa) will have no cracking issues under the thermal gradient condition analyzed. Since top coating sintering increases the crack driving forces with time, highly sintering resistant coatings are desirable to maintain a low tensile modulus and maintain a low crack driving force with time. Finite element results demonstrated that an advanced TEBC system, such as ZrO2/HfO2, which possesses improved sintering resistance and high temperature stability, exhibited excellent durability. A multi-vertical cracked structure with fine columnar spacing is an ideal strain tolerant coating capable of reducing the crack driving forces to an acceptable level even with a high modulus of 50 GPa.

  20. Delamination Mechanisms of Thermal and Environmental Barrier Coatings on SiC/SiC Ceramic Matrix Composites

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Choi, Sung R.; Lee, Kang N.; Miller, Robert A.

    1990-01-01

    Advanced ceramic thermal barrier coatings will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. However, the coating durability issue remains a major concern with the ever-increasing temperature requirements. In this paper, thermal cyclic response and delamination failure modes of a ZrO2-8wt%Y2O3 and mullite/BSAS thermal/environmental barrier coating system on SiC/SiC ceramic matrix composites were investigated using a laser high-heat-flux technique. The coating degradation and delamination processes were monitored in real time by measuring coating apparent conductivity changes during the cyclic tests under realistic engine temperature and stress gradients, utilizing the fact that delamination cracking causes an apparent decrease in the measured thermal conductivity. The ceramic coating crack initiation and propagation driving forces under the cyclic thermal loads, in conjunction with the mechanical testing results, will be discussed.

  1. Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Choi, Sung R.; Eldridge, Jeffrey I.; Lee, Kang N.; Miller, Robert A.

    1990-01-01

    In this paper, surface cracking and interface reactions of a ZrO2-8wt%Y2O3 and mullite/BSAS/Si thermal and environmental barrier coating system on SiC/SiC ceramic matrix composites were characterized after long-term combined laser thermal gradient and furnace cyclic tests in a water vapor containing environment. The surface cracking was analyzed based on the coating thermal gradient sintering behavior and thermal expansion mismatch stress characteristics under the thermal cyclic conditions. The interface reactions that were largely enhanced by the coating surface cracking in the water vapor environment were investigated in detail, and the reaction phases were identified for the coating system after the long-term exposure. The accelerated coating delamination failure was attributed to the increased delamination driving force under the thermal gradient cyclic loading and the reduced interface adhesion due to the detrimental interface reactions. The coating design issues will also be discussed based on the observed failure mechanisms under the high-heat-flux test conditions.

  2. Recycling and utilisation of industrial solid waste: an explorative study on gold deposit tailings of ductile shear zone type in China.

    PubMed

    Liu, Rui; Huang, Fei; Du, Runxiang; Zhao, Chunming; Li, Yongli; Yu, Haoran

    2015-06-01

    Tailings are solid waste arising from mineral processing. This type of waste can cause severe damage to the environment during stockpiling as a result of the leaching of something harmful into the ecosystem. Gold deposit of ductile shear zone type is an important type of gold deposit, and the recycling of its tailings has been challenging researchers for a long time. In this article, the characteristics of this type of tailings were systematically studied by using modern technical means. Considering the characteristics of the tailings, clay was selected to make up for the shortcomings of the tailings and improve their performance. Water and raw materials were mixed to produce green bodies, which are subsequently sintered into ceramic bodies at 980 °C~1020 °C (sintering temperature). The results showed that some new kinds of mineral phases, such as mullite, anorthite and orthoclase, appear in ceramic bodies. Furthermore, the ceramic bodies have a surface hardness of 5 to 6 (Mohs scale), and their water absorption and modulus of rupture can meet some technical requirements of ceramic materials described in ISO 13006-2012 and GB 5001-1985. These gold mine tailings can be made into ceramic tiles, domestic ceramic bodies, and other kinds of ceramic bodies for commercial and industrial purposes after further improvements. PMID:26060235

  3. Sodium sulfate corrosion of silicon carbide fiber-reinforced calcium aluminosilicate glass-ceramic matrix composites. Master's thesis

    SciTech Connect

    Newton, P.J.

    1994-03-01

    Hot corrosion effects of Sodium Sulfate (NaSO4) coated Calcium Aluminosilicate (CAS)/Silicon Carbide (SiC) reinforced glass-ceramic matrix composite were investigated using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDX) and X-ray Diffraction (XRD). The samples provided by the Naval Air Warfare Center (NAWC) were unidirectional SiC/CAS as follows: (1) as received, (2) uncoated in air, (3) Na2SO4, coated in air and (4) Na2SO4 coated in argon. A heat treatment was conducted at 900 deg C for 100 hours. Experimental observations indicated that the Na2S04 coating in an oxidising environment had severely corroded the silicon fiber resulting in a silica rich, Nepheline, Wollastonite, Rankinite, Albite and glassy phases. In the argon atmosphere fiber degradation was present although less severe than in the oxygen environment. Similar phases of silica rich, Nepheline, Albite, Rankinite, Mullite, Pseudo-Wollastonite and a glassy region were present. Minimal fiber and matrix degradation was observed in the uncoated sample beat treated in air. Calcium aluminosilicate, SiC Fiber reinforced composites.

  4. Formation and use of coal combustion residues from three types of power plants burning Illinois coals

    USGS Publications Warehouse

    Demir, I.; Hughes, R.E.; DeMaris, P.J.

    2001-01-01

    Coal, ash, and limestone samples from a fluidized bed combustion (FBC) plant, a pulverized coal combustion (PC) plant, and a cyclone (CYC) plant in Illinois were analyzed to determine the combustion behavior of mineral matter, and to propose beneficial uses for the power plant ashes. Pyrite and marcasite in coal were converted during combustion to glass, hematite and magnetite. Calcite was converted to lime and anhydrite. The clay minerals were altered to mullite and glass. Quartz was partially altered to glass. Trace elements in coal were partially mobilized during combustion and, as a result, emitted into the atmosphere or adsorbed on fly ash or on hardware on the cool side of the power plants. Overall, the mobilities of 15 trace elements investigated were lower at the FBC plant than at the other plants. Only F and Mn at the FBC plant, F, Hg, and Se at the PC plant and Be, F, Hg, and Se at the CYC plant had over 50% of their concentrations mobilized. Se and Ge could be commercially recovered from some of the combustion ashes. The FBC ashes could be used as acid neutralizing agents in agriculture and waste treatment, and to produce sulfate fertilizers, gypsum wall boards, concrete, and cement. The PC and CYC fly ashes can potentially be used in the production of cement, concrete, ceramics, and zeolites. The PC and CYC bottom ashes could be used in stabilized road bases, as frits in roof shingles, and perhaps in manufacturing amber glass. ?? 2001 Elsevier Science Ltd. All rights reserved.

  5. Experimental observations of thermal spikes in microwave processing of ceramic oxide fibers

    SciTech Connect

    Vogt, G.J.; Unruh, W.P.; Thomas, J.R. Jr.

    1994-04-01

    Microwave heating of alumina/silica fiber tows in a single-mode microwave cavity at 2.45 GHz have produced a surprising thermal spike behavior on the fiber bundles. During a thermal spike, a ``hot spot`` on the tow brightens rapidly, persists for a few seconds, and rapidly extinguishs. A hot spot can encompass the entire tow in the cavity or just a localized portion of the tow. Some local hot spots propagate along the fiber. Thermal spikes are triggered by relatively small (<15%) increases in power, thus having obvious implications for the development of practical microwave fiber processing systems. A tow can be heated through several successive thermal spikes, after which the tow is left substantially cooler than it was originally, although the applied microwave electric field is much larger. X-ray diffraction studies show that after each temperature spike there is a partial phase transformation of the tow material into mullite. After several excursions the tow has been largely transformed to the new, less lossy phase and is more difficult to heat. Heating experiments with Nextel 550 tows are examined for a pausible explanation of this microwave heating behavior.

  6. Numerical Modeling of Suspension HVOF Spray

    NASA Astrophysics Data System (ADS)

    Jadidi, M.; Moghtadernejad, S.; Dolatabadi, A.

    2016-02-01

    A three-dimensional two-way coupled Eulerian-Lagrangian scheme is used to simulate suspension high-velocity oxy-fuel spraying process. The mass, momentum, energy, and species equations are solved together with the realizable k-ɛ turbulence model to simulate the gas phase. Suspension is assumed to be a mixture of solid particles [mullite powder (3Al2O3·2SiO2)], ethanol, and ethylene glycol. The process involves premixed combustion of oxygen-propylene, and non-premixed combustion of oxygen-ethanol and oxygen-ethylene glycol. One-step global reaction is used for each mentioned reaction together with eddy dissipation model to compute the reaction rate. To simulate the droplet breakup, Taylor Analogy Breakup model is applied. After the completion of droplet breakup, and solvent evaporation/combustion, the solid suspended particles are tracked through the domain to determine the characteristics of the coating particles. Numerical simulations are validated against the experimental results in the literature for the same operating conditions. Seven or possibly eight shock diamonds are captured outside the nozzle. In addition, a good agreement between the predicted particle temperature, velocity, and diameter, and the experiment is obtained. It is shown that as the standoff distance increases, the particle temperature and velocity reduce. Furthermore, a correlation is proposed to determine the spray cross-sectional diameter and estimate the particle trajectories as a function of standoff distance.

  7. Sintering aids for yttria partially stabilized zirconia

    SciTech Connect

    Montross, C.S.

    1987-01-01

    High-purity yttria partially stabilized zirconia does not sinter readily. Commercial production of the powder and finished parts has allowed contamination by silica and aluminosilicates to enhance the sintering via a liquid-phase mechanism at 1400/sup 0/C. This research analyzed several simple metal oxides as possible nonglassy sintering aids to enhance the sintering of high-purity yttria partially stabilized zirconia, Y-PSZ, without the deleterious effects of the glass contamination. Of the metal oxides analyzed: iron oxide, bismuth oxide, chromia, niobia, tantala, tungsten oxide and mullite, only one metal oxide, iron oxide resulted in enhanced sintering. The iron oxide doped Y-PSZ exhibited better sinterability than high purity Y-PSZ and equivalent/better sinterability than glass doped Y-PSZ. The iron oxide doped Y-PSZ had a higher tetragonal content at lower sintering temperatures and at lower densities than glass doped Y-PSZ. This resulted in higher fracture toughness at lower temperatures than the glass doped Y-PSZ. Additionally, the iron oxide doped Y-PSZ showed a better resistance to low temperature high humidity degradation than glass doped Y-PSZ under identical conditions. Problems of bloating common to high surface area ultra fine powders and exhibited by the glass doped Y-PSZ were not alleviated by the use of the nonglassy metal oxide sintering aids.

  8. Fly ash from a Mexican mineral coal. II. Source of W zeolite and its effectiveness in arsenic (V) adsorption.

    PubMed

    Medina, Adriana; Gamero, Prócoro; Almanza, José Manuel; Vargas, Alfredo; Montoya, Ascención; Vargas, Gregorio; Izquierdo, María

    2010-09-15

    Coal-fired plants in Coahuila (Mexico) produce highly reactive fly ash (MFA), which is used in a one-step process as a raw material in producing zeolite. We explored two routes in the synthesis of zeolite: (a) direct MFA zeolitization, which resulted in the formation of W zeolite with KOH and analcime with NaOH and (b) a MFA fusion route, which resulted in the formation of zeolite W or chabazite with KOH and zeolite X or P with NaOH. No residual crystalline phases were present. When LiOH was employed, ABW zeolite with quartz and mullite were obtained. For both zeolitization routes, the nature of the alkali (KOH, NaOH, LiOH), the alkali/MFA ratio (0.23-1.46), and the crystallization temperature and time (90-175 degrees C; 8-24 h) were evaluated. Additionally, the effect of temperature and time on MFA fusion was studied. W zeolite was obtained by both zeolitization methods. The direct route is preferred because it is a straightforward method using soft reaction conditions that results in a high yield of low cost zeolites with large crystal agglomerates. It was demonstrated that aluminum modified W zeolite has the ability to remove 99% of the arsenic (V) from an aqueous solution of Na(2)HAsO(4).7H(2)O originally containing 740 ppb. PMID:20537461

  9. Fly ash from a Mexican mineral coal I: Mineralogical and chemical characterization.

    PubMed

    Medina, Adriana; Gamero, Prócoro; Querol, Xavier; Moreno, Natalia; De León, Beatriz; Almanza, Manuel; Vargas, Gregorio; Izquierdo, María; Font, Oriol

    2010-09-15

    The properties of coal fly ash are strongly dependent on the geological origin and the combustion process of the coal. It is important to characterize regional fly ash in detail to ascertain its potential uses as raw material in the production of high value products. The physicochemical properties of fly ash coming from the "Jose Lopez Portillo" coal-fired power plant, Coahuila, Mexico (MFA), are presented in this work. A detailed study of trace elements, the chemical composition of the amorphous phase, thermal stability and the leaching of contaminant elements under different conditions are included. MFA is composed of mullite, quartz, calcite, magnetite and an amorphous phase. This material contains mainly silica (59.6%), alumina (22.8%) and magnetite (5.6%). Its amorphous phase (78.3%) has a high silica (49.4%) and alumina (14.4%) content. According to its mineralogical and chemical composition, MFA is potentially useful as a raw material for making cement, silica, and alumina, as well as low silica/alumina ratio zeolites. Deleterious elements could be removed during the zeolitization process or with an additional acid treatment. Because of its morphological properties and structural and thermal stability, MFA can be used in thermal isolation and refractory materials and as a support for heterogeneous catalysts. PMID:20546994

  10. Simultaneous reduction of particulate matter and NO(x) emissions using 4-way catalyzed filtration systems.

    PubMed

    Swanson, Jacob J; Watts, Winthrop F; Newman, Robert A; Ziebarth, Robin R; Kittelson, David B

    2013-05-01

    The next generation of diesel emission control devices includes 4-way catalyzed filtration systems (4WCFS) consisting of both NOx and diesel particulate matter (DPM) control. A methodology was developed to simultaneously evaluate the NOx and DPM control performance of miniature 4WCFS made from acicular mullite, an advanced ceramic material (ACM), that were challenged with diesel exhaust. The impact of catalyst loading and substrate porosity on catalytic performance of the NOx trap was evaluated. Simultaneously with NOx measurements, the real-time solid particle filtration performance of catalyst-coated standard and high porosity filters was determined for steady-state and regenerative conditions. The use of high porosity ACM 4-way catalyzed filtration systems reduced NOx by 99% and solid and total particulate matter by 95% when averaged over 10 regeneration cycles. A "regeneration cycle" refers to an oxidizing ("lean") exhaust condition followed by a reducing ("rich") exhaust condition resulting in NOx storage and NOx reduction (i.e., trap "regeneration"), respectively. Standard porosity ACM 4-way catalyzed filtration systems reduced NOx by 60-75% and exhibited 99.9% filtration efficiency. The rich/lean cycling used to regenerate the filter had almost no impact on solid particle filtration efficiency but impacted NOx control. Cycling resulted in the formation of very low concentrations of semivolatile nucleation mode particles for some 4WCFS formulations. Overall, 4WCFS show promise for significantly reducing diesel emissions into the atmosphere in a single control device. PMID:23550802

  11. Growth of alumina/metal composites into porous ceramics by the oxidation of aluminum

    SciTech Connect

    Watari, Takanori; Mori, Koichiro; Torikai, Toshio; Matsuda, Ohsaku . Dept. of Applied Chemistry)

    1994-10-01

    Ductile metal is incorporated into brittle ceramics to improve their fracture toughness. Of the many methods for fabricating ceramic/metal composites, the oxidation of a molten alloy (DIMOX process) is particularly interesting because it affords (1) ease of composite production, (2) low cost, and (3) near-net-shape capability. Alumina/metal composites were grown into the pores of porous alumina, porous aluminosilicate, and porous silicon carbide substrates through the oxidation of Al-Si (5 wt %) powder compacts coated with magnesia powder (11 mg/cm[sup 2]). The thickness of the resulting composite increased with oxidation time and temperature, and was proportional to (pore size)[sup 0.5] on using porous alumina. The composite thickness was more than 2 times larger in the silicon carbide and about 4 times larger in the aluminosilicate than in the alumina at 1,523 K for 1 h. The products using these three types of substrates consisted of alumina, aluminum, and silicon, except that a silicon carbide phase occurred when using the silicon carbide substrate. Silica and mullite in the aluminosilicate substrate changed to silicon and alumina, and silica in the silicon carbide substrate changed to silicon because of the reduction by aluminum.

  12. Process for preparing ceramic-metal composite bodies

    SciTech Connect

    Breslin, M.C.

    1993-05-25

    A process for forming an aluminum/ceramic composite is described comprising the non-vapor phase oxidation of molten aluminum achieved by contacting the molten aluminum to a sacrificial ceramic body, wherein the molten aluminum is at a temperature at least 300 degrees above the melting point of aluminum but below the softening point of the ceramic body, wherein the sacrificial ceramic body is a material selected from the group consisting of silica, quartz, sand, wollastonite, mullite, silicate glass, fluorosilicate glass, fluoroborosilicate glass, aluminosilicate glass, calcium silicate glass, calcium aluminum silicate glass, calcium aluminum fluorosilicate glass, titanium dioxide, titanium carbide, zirconium dioxide, magnesium oxide, silicon nitride, silicon carbide, zirconium carbide, zirconium nitride, metal sulfides, and mixtures thereof, whereby the sacrificial ceramic body at least partially oxidizes the aluminum to form an aluminum oxide ceramic component, and wherein molten aluminum flows into the aluminum oxide ceramic component, and wherein the sacrificial ceramic body is at least partially reduced, whereby an aluminum/ceramic composite is produced possessing a near net shape relative to the shape of the sacrificial ceramic body.

  13. Anisotropic lattice thermal expansion of PbFeBO4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

    DOE PAGESBeta

    Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

    2014-11-01

    We present the lattice thermal expansion of mullite-type PbFeBO4 in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. Moreover, the unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies ofmore » the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO4, FeO6 and BO3 polyhedra as a function of temperature.« less

  14. Thermodynamic effects of calcium and iron oxides on crystal phase formation in synthetic gasifier slags containing from 0 to 27wt.% V2O3

    DOE PAGESBeta

    Nakano, Jinichiro; Duchesne, Marc; Bennett, James; Kwong, Kyei -Sing; Nakano, Anna; Hughes, Robin

    2014-11-15

    Thermodynamic phase equilibria in synthetic slags (Al2O3–CaO–FeO–SiO2–V2O3) were investigated with 0–27 wt.% vanadium oxide corresponding to industrial coal–petroleum coke (petcoke) feedstock blends in a simulated gasifier environment. Samples encompassing coal–petcoke mixed slag compositions were equilibrated at 1500 °C in a 64 vol.% CO/36 vol.% CO2 atmosphere (Po2 ≈ 10–8 atm at 1500 °C) for 72 h, followed by rapid water quench, then analyzed by inductively coupled plasma optical emission spectrometry, X-ray diffractometry, and scanning electron microscopy with wavelength dispersive spectroscopy. With increasing CaO content, FeO content, or both; the slag homogeneity region expanded and a composition range exhibiting crystals wasmore » reduced. The mullite (Al6Si2O13) crystalline phase was not present in the slags above 9 wt.% FeO while the karelianite (V2O3) crystalline phase was always present in compositions studied if a sufficient amount of vanadium existed in the slag. Furthermore, based on the present experimental equilibrium evaluation, a set of isothermal phase diagrams showing effects of CaO and FeO on thermodynamic phase stabilities in the vanadium-bearing slags is proposed. Some uses of the diagrams for potential industrial practice are discussed.« less

  15. Tension-Compression Fatigue of a Nextel™720/alumina Composite at 1200 °C in Air and in Steam

    NASA Astrophysics Data System (ADS)

    Lanser, R. L.; Ruggles-Wrenn, M. B.

    2016-08-01

    Tension-compression fatigue behavior of an oxide-oxide ceramic-matrix composite was investigated at 1200 °C in air and in steam. The composite is comprised of an alumina matrix reinforced with Nextel™720 alumina-mullite fibers woven in an eight harness satin weave (8HSW). The composite has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. Tension-compression fatigue behavior was studied for cyclical stresses ranging from 60 to 120 MPa at a frequency of 1.0 Hz. The R ratio (minimum stress to maximum stress) was -1.0. Fatigue run-out was defined as 105 cycles and was achieved at 80 MPa in air and at 70 MPa in steam. Steam reduced cyclic lives by an order of magnitude. Specimens that achieved fatigue run-out were subjected to tensile tests to failure to characterize the retained tensile properties. Specimens subjected to prior cyclic loading in air retained 100 % of their tensile strength. The steam environment severely degraded tensile properties. Tension-compression cyclic loading was considerably more damaging than tension-tension cyclic loading. Composite microstructure, as well as damage and failure mechanisms were investigated.

  16. Incorporation of zinc for fabrication of low-cost spinel-based composite ceramic membrane support to achieve its stabilization.

    PubMed

    Li, Lingling; Dong, Xinfa; Dong, Yingchao; Zhu, Li; You, Sheng-Jie; Wang, Ya-Fen

    2015-04-28

    In order to reduce environment risk of zinc, a spinel-based porous membrane support was prepared by the high-temperature reaction of zinc and bauxite mineral. The phase evolution process, shrinkage, porosity, mechanical property, pore size distribution, gas permeation flux and microstructure were systematically studied. The XRD results, based on a Zn/Al stoichiometric composition of 1/2, show a formation of ZnAl2O4 structure starting from 1000°C and then accomplished at 1300°C. For spinel-based composite membrane, shrinkage and porosity are mainly influenced by a combination of an expansion induced by ZnAl2O4 formation and a general densification due to amorphous liquid SiO2. The highest porosity, as high as 44%, is observed in ZnAl4 membrane support among all the investigated compositions. Compared with pure bauxite (Al), ZnAl4 composite membrane support is reinforced by ZnAl2O4 phase and inter-locked mullite crystals, which is proved by the empirical strength-porosity relationships. Also, an increase in average pore diameter and gas flux can be observed in ZnAl4. A prolonged leaching experiment reveals the zinc can be successfully incorporated into ceramic membrane support via formation of ZnAl2O4, which has substantially better resistance toward acidic attack. PMID:25655422

  17. Scaling up the Single Transducer Thickness-Independent Ultrasonic Imaging Method for Accurate Characterization of Microstructural Gradients in Monolithic and Composite Tubular Structures

    NASA Technical Reports Server (NTRS)

    Roth, Don J.; Carney, Dorothy V.; Baaklini, George Y.; Bodis, James R.; Rauser, Richard W.

    1998-01-01

    Ultrasonic velocity/time-of-flight imaging that uses back surface reflections to gauge volumetric material quality is highly suited for quantitative characterization of microstructural gradients including those due to pore fraction, density, fiber fraction, and chemical composition variations. However, a weakness of conventional pulse-echo ultrasonic velocity/time-of-flight imaging is that the image shows the effects of thickness as well as microstructural variations unless the part is uniformly thick. This limits this imaging method's usefulness in practical applications. Prior studies have described a pulse-echo time-of-flight-based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples that eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material microstructure in plate-like samples of silicon nitride, metal matrix composite, and polymer matrix composite. In this study, the method is engineered for inspection of more complex-shaped structures-those having (hollow) tubular/curved geometry. The experimental inspection technique and results are described as applied to (1) monolithic mullite ceramic and polymer matrix composite 'proof-of-concept' tubular structures that contain machined patches of various depths and (2) as-manufactured monolithic silicon nitride ceramic and silicon carbide/silicon carbide composite tubular structures that might be used in 'real world' applications.

  18. Simultaneous leaching and carbon sequestration in constrained aqueous solutions

    SciTech Connect

    Phelps, Tommy Joe; Moon, Ji Won; Roh, Yul; Cho, Kyu Seong

    2011-01-01

    The behavior of metal ions leaching and precipitated mineral phases of metal-rich fly ash (FA) was examined in order to evaluate microbial impacts on carbon sequestration and metal immobilization. The leaching solutions consisted of aerobic deionized water (DW) and artificial eutrophic water (AEW) that was anaerobic, organic- and mineral-rich, and higher salinity as is typical of bottom water in eutrophic algae ponds. The Fe- and Ca-rich FAs were predominantly composed of quartz, mullite, portlandite, calcite, hannebachite, maghemite, and hematite. After 86 days, only Fe and Ca contents exhibited a decrease in leaching solutions while other major and trace elements showed increasing or steady trends in preference to the type of FA and leaching solution. Ca-rich FA showed strong carbon sequestration efficiency ranging up to 32.3 g CO(2)/kg FA after 86 days, corresponding to almost 65% of biotic carbon sequestration potential under some conditions. Variations in the properties of FAs such as chemical compositions, mineral constituents as well as the type of leaching solution impacted CO(2) capture. Even though the relative amount of calcite increased sixfold in the AEW and the relative amount of mineral phase reached 37.3 wt% using Ca-rich FA for 86 days, chemical sequestration did not accomplish simultaneous precipitation and sequestration of several heavy metals.

  19. Heated blends of phosphate waste: Microstructure characterization, effects of processing factors and use as a phosphorus source for alfalfa growth.

    PubMed

    Loutou, M; Hajjaji, M; Mansori, M; Favotto, C; Hakkou, R

    2016-07-15

    Microstructure of expandable lightweight aggregates (LWAs), which was composed of phosphate waste (PW), cement kiln dust (CKD) and raw clay (RC) was investigated, and the effects of processing factors (temperature, waste content, soaking time) on their physical properties were quantified by using response surface methodology (RSM). The potential use of LWAs as a phosphorus source was assessed through the use of seeds of alfalfa. It was found that the main minerals of the waste, namely carbonates and fluorapatite, were involved in the formation of labradorite/anorthite and melt respectively. Stability of mullite- the main constituent of CKD- was sensitive to the melt content. The assemblage of the identified phases was discussed based on the CaO-SiO2-Al2O3 phase diagram. The results of RSM showed that the change of compressive strength, firing shrinkage and water absorption of LWAs versus processing factors was well described with a polynomial model and the weights of the effects of the factors increased in the following order: sintering temperature > waste content (in the case of PW-RC) > soaking time. On the other hand, it was found that due to the release of phosphorus by soil-embedded pellets, the growth of alfalfa plants improved, and the rate enhanced in this order: PW-RC > PW-CKD > PW-CKD-RC. The absorbed quantity of phosphorus (0.12%) was still lower than the common uptake amount. PMID:27100329

  20. Crystallization kinetics of BaO-Al2O3-SiO2 glasses

    NASA Technical Reports Server (NTRS)

    Bansal, Narottam P.; Hyatt, Mark J.

    1989-01-01

    Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

  1. Thermal Gradient Cyclic Behavior of a Thermal/Environmental Barrier Coating System on SiC/SiC Ceramic Matrix Composites

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

    2002-01-01

    Thermal barrier and environmental barrier coatings (TBCs and EBCs) will play a crucial role in future advanced gas turbine engines because of their ability to significantly extend the temperature capability of the ceramic matrix composite (CMC) engine components in harsh combustion environments. In order to develop high performance, robust coating systems for effective thermal and environmental protection of the engine components, appropriate test approaches for evaluating the critical coating properties must be established. In this paper, a laser high-heat-flux, thermal gradient approach for testing the coatings will be described. Thermal cyclic behavior of plasma-sprayed coating systems, consisting of ZrO2-8wt%Y2O3 thermal barrier and NASA Enabling Propulsion Materials (EPM) Program developed mullite+BSAS/Si type environmental barrier coatings on SiC/SiC ceramic matrix composites, was investigated under thermal gradients using the laser heat-flux rig in conjunction with the furnace thermal cyclic tests in water-vapor environments. The coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after the tests. The coating failure mechanisms are discussed based on the cyclic test results and are correlated to the sintering, creep, and thermal stress behavior under simulated engine temperature and heat flux conditions.

  2. Cyclic Failure Mechanisms of Thermal and Environmental Barrier Coating Systems Under Thermal Gradient Test Conditions

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

    2002-01-01

    Plasma-sprayed ZrO2-8wt%Y2O3 and mullite+BSAS/Si multilayer thermal and environmental barrier coating (TBC-EBC) systems on SiC/SiC ceramic matrix composite (CMC) substrates were thermally cyclic tested under high thermal gradients using a laser high-heat-flux rig in conjunction with furnace exposure in water-vapor environments. Coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after exposure. Sintering kinetics of the coating systems were also independently characterized using a dilatometer. It was found that the coating failure involved both the time-temperature dependent sintering and the cycle frequency dependent cyclic fatigue processes. The water vapor environments not only facilitated the initial coating conductivity increases due to enhanced sintering and interface reaction, but also promoted later conductivity reductions due to the accelerated coating cracking and delamination. The failure mechanisms of the coating systems are also discussed based on the cyclic test results and are correlated to the sintering and thermal stress behavior under the thermal gradient test conditions.

  3. Pulsed laser deposition of oxide films by multi-kilowatt CO 2 lasers

    NASA Astrophysics Data System (ADS)

    Schultrich, B.; Lenk, A.; Witke, Th.; Borchardt, G.; Fritze, H.

    1997-02-01

    For realizing a high rate pulsed laser deposition (PLD) a pulsed 6 kW-CO2 laser conventionally used for laser machining was adapted by a suitable beam forming system. It allows intensities between 107 and 108 W/cm2 at a minimum pulse length of 100 μs. The targets consist of various compositions in the Al2O3-SiO2 system including the mullite phase. The deposition has been carried out in high vacuum. Even the average power of 200 W of the available 6 kW mostly used in these experiments due to the small sizes of the specially prepared targets yields mean deposition rates up to 100 nm/s. In-situ measurement of mass loss and momentum transfer on the target reveals that most of the material is ablated as microparticle, not as vapour. This corresponds with the cobblestone appearance of the films. Notwithstanding their rather coarse topography, they are dense without any kind of open porosity. This was also proved by mass loss investigations in oxidation experiments and by diffusion of 18O isotopes in combination with SNMS determination of the concentration profiles.

  4. Anti wetting additives for aluminosilicate refractories in molten aluminum contact applications

    NASA Astrophysics Data System (ADS)

    Shukla, Devdutt Pramod

    Aluminosilicate based refractories are widely used in furnace installations for melting aluminum because they are inexpensive, readily available and generally exhibit the properties desired from a refractory material. However, they face severe corrosion and degradation issues due to the extremely reducing nature of molten aluminum alloys. Isothermal static cup testing is widely used as a tool to evaluate the performance of refractories against penetration by molten aluminum alloys. Various testing methods were reviewed and an upgraded static cup test was recommended. Commercially available aluminosilicate refractories were tested using this method and their results were studied in order to understand the corrosion process. Barium sulfate, which is widely used as an anti-wetting additive to improve refractory performance by limiting physical contact between molten metal and the refractory, has proved ineffective at temperatures above 1000°C. A literature review suggested that barium sulfate formed barium celsian at high temperatures and that the celsian was responsible for the non-wetting effect. Wetting angle measurements of molten AL 5083 on synthetic celsian discs revealed that barium celsian and strontium celsian were both not wetted by molten aluminum. Static cup tests were performed on aluminosilicate refractories containing barium carbonate and strontium carbonate. These additives led to the in-situ formation of celsian phases within the refractory matrix that led to improved corrosion resistance at 1300°C. Phase analysis revealed that celsian formation suppressed the formation of mullite within refractories, thereby reducing penetration.

  5. Design and Initial Development of Monolithic Cross-Flow Ceramic Hot-Gas Filters

    SciTech Connect

    Barra, C.; Limaye, S.; Stinton, D.P.; Vaubert, V.M.

    1999-06-06

    Advanced, coal-fueled, power generation systems utilizing pressurized fluidized bed combustion (PFBC) and integrated gasification combined cycle (IGCC) technologies are currently being developed for high-efficiency, low emissions, and low-cost power generation. In spite of the advantages of these promising technologies, the severe operating environment often leads to material degradation and loss of performance in the barrier filters used for particle entrapment. To address this problem, LoTEC Inc., and Oak Ridge National Laboratory are jointly designing and developing a monolithic cross-flow ceramic hot-gas filter. The filter concept involves a truly monolithic cross-flow design that is resistant to delamination, can be easily fabricated, and offers flexibility of geometry and material make-up. During Phase I of the program, a thermo-mechanical analysis was performed to determine how a cross-flow filter would respond both thermally and mechanically to a series of thermal and mechanical loads. The cross-flow filter mold was designed accordingly, and the materials selection was narrowed down to Ca{sub 0.5}Sr{sub 0.5}Zr{sub 4}P{sub 6}O{sub 24} (CS-50) and 2Al{sub 2}O{sub 3}-3SiO{sub 2} (mullite). A fabrication process was developed using gelcasting technology and monolithic cross-flow filters were fabricated. The program focuses on obtaining optimum filter permeability and testing the corrosion resistance of the candidate materials.

  6. Tribological Study on Plasma Electrolytic Oxidation Treatment in Al-Si Alloys for Engine Application

    NASA Astrophysics Data System (ADS)

    Eiliat, Hoda

    Automotive industry strives to reach an optimum level of fuel economy. This can be achieved by overcoming two impacting factors on fuel consumption: weight and friction force. This research contributes to reduce both. The proposed surface treatment can replace cylinder liners of hypoeutectic aluminum silicon alloy engine blocks with a thin layer of ceramic oxide composed of alpha and gamma phases of Al2O3 and mullite. The coatings are achieved in an aqueous electrolytic bath with current densities of 0.1 to 0.2 A/cm2. Coatings produced in silicate based solutions have shown good adaptability to the counter surface with an average 0.12 coefficient of friction. Coatings produced in phosphate and aluminate solution have shown signs of delamination, and excessive porosity and roughness respectively. Coatings produced under Bipolar Pulsed Direct Current mode has up to 12% higher hardness values compared to unipolar coatings. For each increment of 0.2 A/cm2 current density, there is a 30% of increase in coating growth rate. Higher pH values of the solution creates faster growth rate up to 1.5 mu/min. These coatings are 20% more susceptible to wear. Samples treated in MoS2 solution showed 22% lower average roughness values and 37% of reduction in coefficient of friction. Mild wear scars on the piston rings were detected for the optimized coatings.

  7. Recent advances in the development of lightweight CO{sub 2}-resistant well cements

    SciTech Connect

    Kukacka, L.E.; Sugama, T.

    1995-12-31

    Regardless of the properties of the cured material, the practical use of advanced cementitious materials for geothermal well completions depends primarily upon the ability to predictably extend the thickening times for the precursor slurries at elevated temperatures to times sufficient to permit conventional placement. Ongoing work at Brookhaven National Laboratory being conducted with assistance from the geothermal industry, indicates that lightweight calcium phosphate cement slurries being developed as CO{sub 2{minus}} resistant well completion materials, can be conventional pumped at temperatures > 100{degrees}C without the addition of retarding admixtures. These slurries consist of mullite-shelled hollow microspheres, calcium aluminate cements and polybasic sodium phosphate. When cured in hydrothermal environments, the slurries yield high strength, low permeability cements which bond well to steel casing. Two compositional factors that affect the thickening times were identified. One is the calcium aluminate cement species that serve as the base reagent in the slurry formulation, and the other is the rate of hydrothermal reaction between the microspheres and the polybasic sodium phosphate solution.

  8. Anisotropic lattice thermal expansion of PbFeBO4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

    SciTech Connect

    Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

    2014-11-01

    We present the lattice thermal expansion of mullite-type PbFeBO4 in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. Moreover, the unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies of the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO4, FeO6 and BO3 polyhedra as a function of temperature.

  9. Improved ceramic heat exchange material

    NASA Technical Reports Server (NTRS)

    Mccollister, H. L.

    1977-01-01

    Improved corrosion resistant ceramic materials that are suitable for use as regenerative heat exchangers for vehicular gas turbines is reported. Two glass-ceramic materials, C-144 and C-145, have superior durability towards sulfuric acid and sodium sulfate compared to lithium aluminosilicate (LAS) Corning heat exchange material 9455. Material C-144 is a leached LAS material whose major crystalline phase is silica keatite plus mullite, and C-145 is a LAS keatite solid solution (S.S.) material. In comparison to material 9455, material C-144 is two orders of magnitude better in dimensional stability to sulfuric acid at 300 C, and one order of magnitude better in stability to sodium sulfate at 1000 C. Material C-145 is initially two times better in stability to sulfuric acid, and about one order of magnitude better in stability to sodium sulfate. Both C-144 and C-145 have less than 300 ppm delta L/L thermal expansion from ambient to 1000 C, and good dimensional stability of less than approximately 100 ppm delta L/L after exposure to 1000 C for 100 hours. The glass-ceramic fabrication process produced a hexagonal honeycomb matrix having an 85% open frontal area, 50 micrometer wall thickness, and less than 5% porosity.

  10. Spreading of the combustion wave in SiO2-Al systems

    NASA Astrophysics Data System (ADS)

    Maltsev, Vladimir M.; Gafiyatulina, Galina P.; Tavrov, Alexander V.

    1997-11-01

    The process of self-propagating high-temperature synthesis (SHS) has been applied as the new technology for production of construction materials and especial refractories with enhanced strength- and fire-resisting properties. These materials are aimed to be used as synthetic mullits lining refractories in heat units. In the visible light range, the following characteristics of SHS process have been investigated: the localization and the temperature of initiating of SHS process,the propagation of SHS wave on surface- or in volume, velocities of spreading of combustion wave, the number of SHS reaction stages. The visualization with a video-recording of the combustion wave of the SHS process has been performed inside the muffle furnace. The video has been processed with computer card of frame grabber and has been analyzed in multivideo mode, where each frame had been captured in fixed time interval. Thus, several mixtures of SiO2-Al have been studied by variation of: the SiO2 particle size,the stoichiometric coefficient, by the substitution of the SiO2 to ashes and kaolin, and by the adding of supplementary components like Fe2O3. The SHS reactions are processed by the preliminary heating to the temperature of 650-860 degrees C. The local thermal self initiating of the SHS process and its propagation in the volume of a sample have been visualized. The multistage SHS reaction has been identified.

  11. Hot corrosion of ceramic engine materials

    NASA Technical Reports Server (NTRS)

    Fox, Dennis S.; Jacobson, Nathan S.; Smialek, James L.

    1988-01-01

    A number of commercially available SiC and Si3N4 materials were exposed to 1000 C in a high velocity, pressurized burner rig as a simulation of a turbine engine environment. Sodium impurities added to the burner flame resulted in molten Na2SO4 deposition, attack of the SiC and Si4N4 and formation of substantial Na2O-x(SiO2) corrosion product. Room temperature strength of the materials decreased. This was a result of the formation of corrosion pits in SiC, and grain boundary dissolution and pitting in Si3N4. Corrosion regimes for such Si-based ceramics have been predicted using thermodynamics and verified in rig tests of SiO2 coupons. Protective mullite coatings are being investigated as a solution to the corrosion problem for SiC and Si3N4. Limited corrosion occurred to cordierite (Mg2Al4Si5O18) but some cracking of the substrate occurred.

  12. Sliding durability of candidate seal fiber materials in hydrogen from 25 to 900 C

    NASA Technical Reports Server (NTRS)

    Dellacorte, Christopher; Steinetz, Bruce M.

    1992-01-01

    Sliding durability studies of candidate ceramic fibers were conducted in hydrogen to support the high temperature seal development program at NASA LeRC. Pin-on-disk tests were used to measure the friction and durability of a tow or bundle of ceramic fibers in sliding against a superalloy disk. This procedure was used previously to test candidate fibers in an air environment. The fibers based upon mullite (Al2O3-SiO2) chemistry (Nextel 550, 440, and 312) exhibited better durability in hydrogen than in air. HPZ, a complex silicon carboxynitride fiber which showed good durabilty in air, however, showed a significant loss of durability in hot hydrogen. These results are consistent with recent thermodynamic and experimental studies of ceramic compatibility with hydrogen at elevated temperatures. These research results indicate that only oxide fibers display good durability in both air and hydrogen environments. Also, simple, low cost testing in air can provide an adequate data base for initial seal material screening and selection, especially for oxide fiber candidates. The findings of this research provide critical input to the seal design team.

  13. Geochemistry of ultra-fine and nano-compounds in coal gasification ashes: a synoptic view.

    PubMed

    Kronbauer, Marcio A; Izquierdo, Maria; Dai, Shifeng; Waanders, Frans B; Wagner, Nicola J; Mastalerz, Maria; Hower, James C; Oliveira, Marcos L S; Taffarel, Silvio R; Bizani, Delmar; Silva, Luis F O

    2013-07-01

    The nano-mineralogy, petrology, and chemistry of coal gasification products have not been studied as extensively as the products of the more widely used pulverized-coal combustion. The solid residues from the gasification of a low- to medium-sulfur, inertinite-rich, volatile A bituminous coal, and a high sulfur, vitrinite-rich, volatile C bituminous coal were investigated. Multifaceted chemical characterization by XRD, Raman spectroscopy, petrology, FE-SEM/EDS, and HR-TEM/SEAD/FFT/EDS provided an in-depth understanding of coal gasification ash-forming processes. The petrology of the residues generally reflected the rank and maceral composition of the feed coals, with the higher rank, high-inertinite coal having anisotropic carbons and inertinite in the residue, and the lower rank coal-derived residue containing isotropic carbons. The feed coal chemistry determines the mineralogy of the non-glass, non-carbon portions of the residues, with the proportions of CaCO₃ versus Al₂O₃ determining the tendency towards the neoformation of anorthite versus mullite, respectively. Electron beam studies showed the presence of a number of potentially hazardous elements in nanoparticles. Some of the neoformed ultra-fine/nano-minerals found in the coal ashes are the same as those commonly associated with oxidation/transformation of sulfides and sulfates. PMID:23584038

  14. Development, solar test, and evaluation of a high-temperature air receiver for point-focusing parabolic dish applications

    NASA Technical Reports Server (NTRS)

    Hanseth, E. J.

    1981-01-01

    A high temperature solar receiver was fabricated and tested in excess of 1370 C on an 11-meter-diameter test bed concentrator at the Jet Propulsion Laboratory Parabolic Dish Test Site, Edwards, California. The 60-kilowatt thermal receiver design utilizes state-of-the-art silicon carbide honeycomb matrix panels to receive and transfer the solar energy and mullite elements for thermal buffer storage. Solar tests were conducted with indicated air exit temperatures ranging from 885 C (1625 F) to 1427 C (2600 F), mass flow rates of 75 to 105 g/sec (0.16 to 0.23 lbm/sec), and pressures up to 265 kPa absolute (38.4 psia). Estimates of efficiency are 59.7% at 1120 C (2048 F) to 80.6% at 885 C (1625 F) when aperture spillage losses are considered separately. Results are presented which demonstrate the feasibility of this innovative receiver concept for point-focusing parabolic dish applications over a wide temperature range.

  15. Preparation and Characterization of Nano structured Materials from Fly Ash: A Waste from Thermal Power Stations, by High Energy Ball Milling

    PubMed Central

    2007-01-01

    The Class F fly ash has been subjected to high energy ball milling and has been converted into nanostructured material. The nano structured fly ash has been characterized for its particle size by using particle size analyzer, specific surface area with the help of BET surface area apparatus, structure by X-ray diffraction studies and FTIR, SEM and TEM have been used to study particle aggregation and shape of the particles. On ball milling, the particle size got reduced from 60 μm to 148 nm by 405 times and the surface area increased from 0.249 m2/gm to 25.53 m2/gm i.e. by more than 100%. Measurement of surface free energy as well as work of adhesion found that it increased with increased duration of ball milling. The crystallite was reduced from 36.22 nm to 23.01 nm for quartz and from 33.72 nm to 16.38 nm for mullite during ball milling to 60 h. % crystallinity reduced from 35% to 16% during 60 h of ball milling because of destruction of quartz and hematite crystals and the nano structured fly ash is found to be more amorphous. Surface of the nano structured fly ash has become more active as is evident from the FTIR studies. Morphological studies revealed that the surface of the nano structured fly ash is more uneven and rough and shape is irregular, as compared to fresh fly ash which are mostly spherical in shape.

  16. Aluminum-containing intergranular phases in hot-pressed silicon carbide

    SciTech Connect

    Zhang, Xiao Feng; De Jonghe, Lutgard C.

    2003-01-12

    Aluminum-containing intergranular phases, forming intergranular films and secondary phase particles at triple-junctions in SiC hot-pressed with aluminum, boron, and carbon additions, were studied by transmission electron microscopy. Statistical high-resolution electron microscopy study of intergranular films indicated that a large fraction of the vitreous intergranular films in the s-hot-pressed SiC crystallized during postannealing in argon above 1000 C. However, brief heating to 1900 C indeed re-melted 25 percent of the crystallized intergranular films. The structural transitions were reflected in the statistical width distributions of the amorphous grain boundary layers. At triple-junctions, Al2O3, Al2OC-SiC solid solution, and mullite phases were newly identified. These phases,together with others reported before are represented in a quaternary phase diagram for 1900 C. It is proposed that a SiC-Al2OC liquid domain is to be included in this phase diagram.

  17. Elevated-temperature fracture resistances of monolithic and composite ceramics using chevron-notched bend tests

    NASA Technical Reports Server (NTRS)

    Ghosh, Asish; Jenkins, Michael G.; Ferber, Mattison K.; Peussa, Jouko; Salem, Jonathan A.

    1992-01-01

    The quasi-static fracture behaviors of monolithic ceramics (SiC, Si3N4, MgAl2O4), self-reinforced monoliths (acicular grained Si3N4, acicular grained mullite), and ceramic matrix composites (SiC whisker/Al2O3 matrix, TiB2 particulate/SiC matrix, SiC fiber/CVI SiC matrix, Al2O3 fiber/CVI SiC matrix) were measured over the temperature range of 20 to 1400 C. The chevron notched, bend bar test geometry was essential for characterizing the elevated temperature fracture resistances of this wide range of quasi-brittle materials during stable crack growth. Fractography revealed the differences in the fracture behavior of the different materials at the various temperatures. The fracture resistances of the self-reinforced monoliths were comparable to those of the composites and the fracture mechanisms were found to be similar at room temperature. However at elevated temperatures the differences of the fracture behavior became apparent where the superior fracture resistance of the self-reinforced monoliths were attributed to the minor amounts of glassy, intergranular phases which were often more abundant in the composites and affected the fracture behavior when softened by elevated temperatures.

  18. Mineralogy at the magma-hydrothermal system interface in andesite volcanoes, New Zealand

    NASA Astrophysics Data System (ADS)

    Wood, C. Peter

    1994-01-01

    Ejecta from phreatomagmatic eruptions of Ruapehu and White Island andesite volcanoes in New Zealand provide insight into the mineralogical reactions that occur when magma invades a vent-hosted hydrothermal system. At the surface and in ejected blocks from shallow depths, hydrothermal alteration mineralogies are dominated by silica polymorphs, anhydrite, natroalunite, and pyrite. Blocks from greater depths are composed mainly of cristobalite, anhydrite, halite, and magnetite. Where altered material was heated to magmatic temperatures, thermal decomposition reactions produced mullite, wollastonite, and indialite. Some ejected breccias contain osumilite, cordierite, sanidine, and hypersthene, indicative of reactions occurring near the osumilite-cordierite phase boundary at >800 °C and water pressure <0.2 kbar. Hedenbergite, wollastonite, andradite, and magnetite are found in rare skarn fragments, possibly formed by metasomatism of silica-poor, sulfate-rich hydrothermal deposits. High- temperature parageneses of these types have not been reported before in shallow, acidic volcano-hydrothermal systems. However, they may be typical of the magma- hydrothermal contact zone at many andesite volcanoes.

  19. Peraluminous rocks of Bou-Azzer region (Morocco): Geology and firing transformations

    NASA Astrophysics Data System (ADS)

    Hajjaji, M.; Belkabir, A.; Berrada, S. H.

    2008-10-01

    The general geology of the peraluminous rocks of the Bou-Azzer region (Central Anti-Atlas, Morocco) and their firing transformations were investigated by several techniques: optical microscopy, microprobe analysis, X-ray diffraction (XRD), X-ray fluorescence (XRF), thermal analysis, scanning electron microscope (SEM), energy dispersive spectrometry (EDS), and by measuring selected physical properties. The results of the geological study show that these rocks consist mainly of a quartz-pyrophyllite assemblage (70-74 wt.% SiO 2 and 14-17 wt.% Al 2O 3), associated with minor amounts of muscovite and nacrite. They formed from a progressive deformation and hydrothermal alteration of felsic volcanic rocks. The principal mineralogical transformations recorded from rhyodacite to peraluminuous rocks are: K-feldspar → muscovite → pyrophyllite. Regarding the firing transformations, it is found that up to about 1100 °C the rock samples are subjected to expansion associated with the destruction of the pyrophyllite hydroxyl framework. The estimated amount of energy associated with this process is 50.226 kJ/mol. Beyond 1100 °C, a marked shrinkage was observed, due to the formation of a glassy phase, and the precipitation of mullite, cristobalite and K-feldspar. The reaction pathways for these phases are proposed and the evolved heat is determined (-160.928 kJ/mol).

  20. TEM study of PM2.5 emitted from coal and tire combustion in a thermal power station.

    PubMed

    Gieré, Reto; Blackford, Mark; Smith, Katherine

    2006-10-15

    The research presented here was conducted within the scope of an experiment investigating technical feasibility and environmental impacts of tire combustion in a coal-fired power station. Previous work has shown that combustion of a coal+tire blend rather than pure coal increased bulk emissions of various elements (e.g., Zn, As, Sb, Pb). The aim of this study is to characterize the chemical and structural properties of emitted single particles with dimensions <2.5 microm (PM2.5). This transmission electron microscope (TEM)-based study revealed that, in addition to phases typical of coal fly ash (e.g., aluminum-silicate glass, mullite), the emitted PM2.5 contains amorphous selenium particles and three types of crystalline metal sulfates never reported before from stack emissions. Anglesite, PbSO4, is ubiquitous in the PM2.5 derived from both fuels and contains nearly all Pb present in the PM. Gunningite, ZnSO4-H2O, is the main host for Zn and only occurs in the PM derived from the coal+tire blend, whereas yavapaiite, KFe3+(SO4)2, is present only when pure coal was combusted. We conclude that these metal sulfates precipitated from the flue gas, may be globally abundant aerosols, and have, through hydration or dissolution, a major environmental and health impact. PMID:17120547

  1. Theoretical analysis of the microwave-drill near-field localized heating effect

    NASA Astrophysics Data System (ADS)

    Jerby, E.; Aktushev, O.; Dikhtyar, V.

    2005-02-01

    The microwave-drill principle [Jerby et al., Science 298, 587 (2002)] is based on a localized hot-spot effect induced by a near-field coaxial applicator. The microwave drill melts the nonmetallic material locally and penetrates mechanically into it to shape the hole. This paper presents a theoretical analysis of the thermal-runaway effect induced in front of the microwave drill. The model couples the Maxwell's and heat equations including the material's temperature-dependent properties. A finite-difference time-domain algorithm is applied in a two-time-scale numerical model. The simulation is demonstrated for mullite, and benchmarked in simplified cases. The results show a temperature rise of ˜103K/s up to 1300K within a hot spot confined to a ˜4-mm width (˜0.1 wavelength). The input-port response to this near-field effect is modeled by equivalent time-varying lumped-circuit elements. Besides the physical insight, this theoretical study provides computational tools for design and analysis of microwave drills and for their real-time monitoring and adaptive impedance matching.

  2. Development and Testing of a Refractory Millimeter-Wave Absorbent Heat Exchanger

    NASA Technical Reports Server (NTRS)

    Lambot, Thomas; Myrabo, Leik; Murakami, David; Parkin, Kevin

    2014-01-01

    Central to the Millimeter-Wave Thermal Launch System (MTLS) is the millimeter-wave absorbent heat exchanger. We have developed metallic and ceramic variants, with the key challenge being the millimeter-wave absorbent coatings for each. The ceramic heat exchanger came to fruition first, demonstrating for the first time 1800 K peak surface temperatures under illumination by a 110 GHz Gaussian beam. Absorption efficiencies of up to 80 are calculated for mullite heat exchanger tubes and up to 50 are calculated for alumina tubes. These are compared with estimates based on stratified layer and finite element analyses. The problem of how to connect the 1800 K end of the ceramic tubes to a graphite outlet manifold and nozzle is solved by press fitting, or by threading the ends of the ceramic tubes and screwing them into place. The problem of how to connect the ceramic tubes to a metallic or nylon inlet pipe is solved by using soft compliant PTFE and PVC tubes that accommodate thermal deformations of the ceramic tubes during startup and operation. We show the resulting heat exchangers in static tests using argon and helium as propellants.

  3. Asbestos induced diffuse pleural fibrosis: pathology and mineralogy.

    PubMed Central

    Stephens, M; Gibbs, A R; Pooley, F D; Wagner, J C

    1987-01-01

    Lungs from seven cases of diffuse pleural fibrosis with known asbestos exposure were studied to determine the gross and microscopic pathological features and relate these to the analysed mineral fibre content of the lung. All seven individuals had had substantial exposure, ranging from two to 25 years, and chronic chest problems and at necropsy all cases met the criteria for compensatable disease. Macroscopically, all had extensive visceral pleural fibrosis and extensive areas of adhesions, and four also had discrete parietal pleural plaques. The histological features were similar in all the cases--most strikingly the basket weave pattern of the thickened pleura and a dense subpleural parenchymal interstitial fibrosis with fine honeycombing, extending up to 1 cm into the underlying lung. The similar histological appearances raise the possibility that diffuse pleural fibrosis and pleural plaques have a similar pathogenesis. Amphibole asbestos (crocidolite and amosite) counts were high in six of the seven cases and chrysotile counts in four; four cases had high mullite counts, but the importance of this is not known. It is concluded that diffuse pleural fibrosis is a specific asbestos associated entity, of uncertain pathogenesis, with mineral fibre counts falling between those found with plaques and those in minimal asbestosis. Images PMID:3660310

  4. Material and structural characterization of alkali activated low-calcium brown coal fly ash.

    PubMed

    Skvára, Frantisek; Kopecký, Lubomír; Smilauer, Vít; Bittnar, Zdenek

    2009-09-15

    The waste low-calcium Czech brown coal fly ash represents a considerable environmental burden due to the quantities produced and the potentially high content of leachable heavy metals. The heterogeneous microstucture of the geopolymer M(n) [-(Si-O)(z)-Al-O](n).wH(2)O, that forms during the alkaline activation, was examined by means of microcalorimetry, XRD, TGA, DSC, MIP, FTIR, NMR MAS ((29)Si, (27)Al, (23)Na), ESEM, EDS, and EBSD. The leaching of heavy metals and the evolution of compressive strength were also monitored. The analysis of raw fly ash identified a number of different morphologies, unequal distribution of elements, Fe-rich rim, high internal porosity, and minor crystalline phases of mullite and quartz. Microcalorimetry revealed exothermic reactions with dependence on the activator alkalinity. The activation energy of the geopolymerization process was determined as 86.2kJ/mol. The X-ray diffraction analysis revealed no additional crystalline phases associated with geopolymer formation. Over several weeks, the (29)Si NMR spectrum testified a high degree of polymerization and Al penetration into the SiO(4) tetrahedra. The (23)Na NMR MAS spectrum hypothesized that sodium is bound in the form of Na(H(2)O)(n) rather than Na(+), thus causing efflorescence in a moisture-gradient environment. As and Cr(6+) are weakly bonded in the geopolymer matrix, while excellent immobilization of Zn(2+), Cu(2+), Cd(2+), and Cr(3+) are reported. PMID:19303704

  5. Study of Glazes and Their Effects on Properties of Triaxial Electrical Porcelains from Ugandan Minerals

    NASA Astrophysics Data System (ADS)

    Olupot, Peter W.; Jonsson, Stefan; Byaruhanga, Joseph K.

    2010-11-01

    Kaolin, ball clay, feldspar, and sand were collected from deposits in Uganda, milled and sieved to particle sizes of 45, 45, 53, and 25 μm, respectively. Three porcelain bodies and five glazes were formulated from them. The glazes were applied on porcelain specimens and subsequently evaluated for their effects on properties of porcelain samples. The formulated specimens were investigated using dilatometry, Steger test, FEG-SEM, XRD, 4-point bending, dielectric strength, and fracture toughness tests. A porcelain specimen consisting of 68% SiO2, 19% Al2O3, 4.7% K2O, and a glaze RO:0.57Al2O3:4.86SiO2 exhibited MOR of 105 MPa with Weibull modulus of 5.6 and a dielectric strength of 18 kV/mm upon firing at a heating rate of 6 °C/min to 1250 °C and holding for 2 h. The microstructure of the high-strength specimen exhibited round mullite needles, quartz, and glass. Holding samples for 2 h at peak temperature resulted in a 22% increase in MOR compared to 1 h holding. Glazing further improved strength by 67% for the best sample. Compressive stresses in glaze contributed to the strengthening effect. The dielectric and mechanical strength values obtained qualify the formulated sample for application in electrical insulation.

  6. Investigation of the coal fly ashes using IR spectroscopy.

    PubMed

    Mozgawa, W; Król, M; Dyczek, J; Deja, J

    2014-11-11

    The results of FT-IR spectroscopic studies of coal fly ashes, originated from various polish power plants are reported. The results of MIR investigations were compared to the X-ray diffraction (XRD) measurements and chemical analyses. They are mainly composed of silica, alumina and lime. The infrared spectrum in the middle range can be used to describe both the structure of phases present in the fly ash and to identify the characteristic elements of the individual components of ash. The results indicate that the amount of aluminosilicate and its Si/Al ratio induce a shift in the T-O stretching band appearing at 950-1100 cm(-1). Moreover, FWHM of these bands indicates the participation of the crystalline phase relative to amorphous. The presence of carbonate phases generates substantial changes in the 1450-1400 cm(-1) area of the spectra. The presence of such phases as anhydrite, mullite or illite has also been established on the basis of IR spectra. PMID:24935825

  7. Analysis of atmospheric fluidized bed combustion agglomerates. Final report

    SciTech Connect

    Perkins, D. III; Brekke, D.W.; Karner, F.R.

    1984-04-01

    Chemical and textural studies of AFBC agglomerates have revealed detailed information regarding the mechanisms of agglomeration. The formation of agglomerates in a silica sand bed can be described by a four step process: initial ash coatings of quartz grains; thickening of ash coatings and the formation of nodules; cementation of nodules to each other by a sulfated aluminosilicate matrix; and partial or complete melting of eutectic compositions to produce a sticky glass phase between grains and along fractures. Once agglomeration has begun, large scale solidification and restricted flow within the bed will lead to hot spots, wholesale melting and further agglomeration which ultimately forces a shutdown. Standard operating temperatures during normal AFBC runs come quite close to, or may actually exceed, the minimum temperatures for eutectic melting of the silicate phases in the coal and standard bed materials. The partially melted material may be expected to lead to the formation of dense, sticky areas within the bed, and the formation of hot spots which further exacerbate the problem. Ultimately, large scale bed agglomeration will result. Attempts to eliminate agglomeration by removal of sodium via an ion exchange process have yielded encouraging results. A second approach, used to raise melting temperatures within the bed, has been to use bed materials that may react with low-temperature minerals to produce high-temperature refractory phases such as mullite or other alkali and alkali-earth alumino-silicates.

  8. High Temperature Tolerant Ceramic Composites Having Porous Interphases

    DOEpatents

    Kriven, Waltraud M.; Lee, Sang-Jin

    2005-05-03

    In general, this invention relates to a ceramic composite exhibiting enhanced toughness and decreased brittleness, and to a process of preparing the ceramic composite. The ceramic composite comprises a first matrix that includes a first ceramic material, preferably selected from the group including alumina (Al2O3), mullite (3Al2O3.2SiO2), yttrium aluminate garnet (YAG), yttria stabilized zirconia (YSZ), celsian (BaAl2Si2O8) and nickel aluminate (NiAl2O4). The ceramic composite also includes a porous interphase region that includes a substantially non-sinterable material. The non-sinterable material can be selected to include, for example, alumina platelets. The platelets lie in random 3-D orientation and provide a debonding mechanism, which is independent of temperature in chemically compatible matrices. The non-sinterable material induces constrained sintering of a ceramic powder resulting in permanent porosity in the interphase region. For high temperature properties, addition of a sinterable ceramic powder to the non-sinterable material provides sufficiently weak debonding interphases. The ceramic composite can be provided in a variety of forms including a laminate, a fibrous monolith, and a fiber-reinforced ceramic matrix. In the laminated systems, intimate mixing of strong versus tough microstructures were tailored by alternating various matrix-to-interphase thickness ratios to provide the bimodal laminate.

  9. Hollow proppants and a process for their manufacture

    DOEpatents

    Jones, Arfon H.; Cutler, Raymond A.

    1985-01-01

    Hollow, fine-grained ceramic proppants are less expensive and improve fracture control when compared to conventional proppants (dense alumina, mullite, bauxite, zirconia, etc.). Hollow proppants of the present invention have been fabricated by spray drying, followed by sintering in order to obtain a dense case and a hollow core. These proppants generally have high sphericity and roundness (Krumbein sphericity and roundness greater than 0.8), have diameters on average between 2250 and 125 .mu.m, depending on proppant size required, and have strength equal to or greater than that of sand. The hollow core, the size of which can be controlled, permits better fracture control in hydraulic fracturing treatments since the proppant can be transported in lower viscosity fluids. Hollow proppants produced at the same cost/weight as conventional proppants also provide for lower costs, since less weight is required to fill the same volume. The fine-grained (preferably less than 5 .mu.m in diameter) ceramic case provides the strength necessary to withstand closure stresses and prevent crushing.

  10. Component effects on crystallization of RE-containing aluminoborosilicate glass

    NASA Astrophysics Data System (ADS)

    Mohd Fadzil, Syazwani; Hrma, Pavel; Schweiger, Michael J.; Riley, Brian J.

    2016-09-01

    Lanthanide-aluminoborosilicate (LABS) glass is one option for immobilizing rare earth (RE) oxide fission products generated during reprocessing of pyroprocessed fuel. This glass system can accommodate a high loading of RE oxides and has excellent chemical durability. The present study describes efforts to model equilibrium crystallinity as a function of glass composition and temperature as well as liquidus temperature (TL) as a function of glass composition. The experimental method for determining TL was ASTM C1720-11. Typically, three crystalline phases were formed in each glass: Ce-borosilicate (Ce3BSi2O10), mullite (Al10Si2O19), and corundum (Al2O3). Cerianite (CeO2) was a common minor crystalline phase and Nd-silicate (Nd2Si2O7) occurred in some of the glasses. In the composition region studied, TL decreased as SiO2 and B2O3 fractions increased and strongly increased with increasing fractions of RE oxides; Al2O3 had a moderate effect on the TL but, as expected, it strongly affected the precipitation of Al-containing crystals.

  11. The Influence of Interfacial Roughness on Fiber Sliding in Oxide Composites with La-Monazite Interphases

    NASA Technical Reports Server (NTRS)

    Davis, J. B.; Hay, R. S.; Marshall, D. B.; Morgan, P. E. D.; Sayir, A.; Gray, Hugh R. (Technical Monitor); Farmer, Serene C. (Technical Monitor)

    2002-01-01

    Room temperature debonding and sliding of La-Monazite coated fibers is assessed using a composite with a polycrystalline alumina matrix and fibers of several different single crystal (mullite, sapphire) and directionally solidified eutectic (Al2O3/Y3Al5O12 and Al2O3/Y-ZrO2) compositions. These fibers provide a range of residual stresses and interfacial roughnesses. Sliding occurred over a debond crack at the fiber-coating interface when the sliding displacement and surface roughness were relatively small. At large sliding displacements with relatively rough interfaces, the monazite coatings were deformed extensively by fracture, dislocations and occasional twinning, whereas the fibers were undamaged. Dense, fine-grained (10 nm) microstructures suggestive of dynamic recrystallization were also observed in the coatings. Frictional heating during sliding is assessed. The possibility of low temperature recrystallization is discussed in the light of the known resistance of monazite to radiation damage. The ability of La-Monazite to undergo plastic deformation relatively easily at low temperatures may be enabling for its use as a composite interface.

  12. Filter Component Assessment

    SciTech Connect

    Alvin, M.A.; Lippert, T.E.; Diaz, E.S.; Smeltzer, E.E.

    1996-12-31

    Advanced particulate filtration systems are currently being developed at Westinghouse for use in both coal-fired Integrated Gasification Combined Cycle (IGCC) and Pressurized Fluidized Bed Combustion (PFBC) systems. To date, Westinghouse has demonstrated 5855 hours of successful operation of first generation monolithic filter elements in PFBC applications when ash bridging or process thermal transient excursions are avoided. Alternate advanced monolithic and second generation fiber reinforced, filament wound and vacuum infiltrated filters are also being developed which are considered to have enhanced high temperature creep resistance, improved fracture toughness, or enhanced thermal shock characteristics, respectively. Mechanical and component fabrication improvements, as well as degradation mechanisms for each filter element have been identified by Westinghouse during exposure to simulated PFBC operating conditions and alkali-containing steam/air environments. Additional effort is currently being focused on determining the stability of the advanced monolithic high temperature creep resistant clay bonded silicon carbide (SiC) materials, alumina/mullite, and chemically vapor infiltrated (CVI) SiC materials during operation in the Westinghouse Advanced Particulate Filtration (W-APF) system at Foster Wheeler`s pressurized circulating fluidized-bed combustion (PCFBC) test facility in Karhula, Finland. Select advanced filter materials are being defined for additional long-term exposure in integrated gasification combined cycle (IGCC) gas streams. The results of these efforts are summarized in this paper. 6 refs., 7 figs., 11 tabs.

  13. Effects of nitrogen dioxide on algae

    SciTech Connect

    Wodzinski, R.S.; Alexander, M.

    1980-01-01

    Photosynthetic activity of Anabaena flos-aquae in a soil suspension at an initial pH of 4.9 was almost totally eliminated after 3 days of exposure to 5.0 ppm (..mu..l/liter) NO/sub 2/, at which time the pH had fallen to 3.9. In contrast, A. flos-aquae in soil suspensions at an initial pH of 6.0 was not inhibited after 3 days by 5.0 ppm NO/sub 2/, but the activity was reduced by half in the presence of 15.0 ppm NO/sub 2/; the pH was 6.5 and 5.8, respectively, in the NO/sub 2/-treated samples on day 3. Photosynthesis by the green algae Chlamydomonas reinhardtii and Ankistrodesmus falcatus in soil suspensions at an initial pH of approx 4.2 was not appreciably affected by 15.0 ppm of NO/sub 2/ after 3 days, at which time the pH had fallen below 4.0. The high levels of NO/sub 2/ and low pH values required for toxicity suggest that blue-green and green algae probably will not be affected directly by NO/sub 2/ in polluted air.

  14. Effects of nitrogen dioxide on algae

    SciTech Connect

    Wodzinski, R.S.; Alexander, M.

    1980-01-01

    Photosynthetic activity of Anabaena flos-aquae in a soil suspension at an initial pH of 4.9 was almost totally eliminated after 3 days of exposure to 5.0 ppM (..mu..l/liter) NO/sub 2/, at which time the pH had fallen to 3.9. In contrast, A. flos-aquae in soil suspensions at an initial pH of 6.0 was not inhibited after 3 days by 5.0 ppM NO/sub 2/, but the activity was reduced by half in the presence of 15.0 ppM NO/sub 2/; the pH was 6.5 and 5.8, respectively, in the NO/sub 2/-treated samples on day 3. Photosynthesis by the green algae Chlamydomonas reinhardtii and Ankistrodesmus falcatus in soil suspensions at an initial pH of approx. 4.2 was not appreciably affected by 15.0 ppM of NO/sub 2/ after 3 days, at which time the pH had fallen below 4.0. The high levels of NO/sub 2/ and low pH values required for toxicity suggest that blue-green and green algae probably will not be affected directly by NO/sub 2/ in polluted air.

  15. Plasma treatment of heat-resistant materials

    NASA Astrophysics Data System (ADS)

    Vlasov, V. A.; Kosmachev, P. V.; Skripnikova, N. K.; Bezukhov, K. A.

    2015-11-01

    Refractory lining of thermal generating units is exposed to chemical, thermal, and mechanical attacks. The degree of fracture of heat-resistant materials depends on the chemical medium composition, the process temperature and the material porosity. As is known, a shortterm exposure of the surface to low-temperature plasma (LTP) makes possible to create specific coatings that can improve the properties of workpieces. The aim of this work is to produce the protective coating on heat-resistant chamotte products using the LTP technique. Experiments have shown that plasma treatment of chamotte products modifies the surface, and a glass-ceramic coating enriched in mullite is formed providing the improvement of heat resistance. For increasing heat resistance of chamotte refractories, pastes comprising mixtures of Bacor, alumina oxide, and chamot were applied to their surfaces in different ratios. It is proved that the appropriate coating cannot be created if only one of heat-resistant components is used. The required coatings that can be used and recommended for practical applications are obtained only with the introduction of powder chamot. The paste composition of 50% chamot, 25% Bacor, and 25% alumina oxide exposed to plasma treatment, has demonstrated the most uniform surface fusion.

  16. Measurement of activation volume for creep of dry olivine at upper mantle pressure

    NASA Astrophysics Data System (ADS)

    Dixon, N. A.; Durham, W. B.; Suzuki, A. M.; Mei, S.; Kohlstedt, D. L.; Hustoft, J. W.

    2011-12-01

    Olivine is the most abundant and weakest phase in the upper mantle, and thus its rheological properties have a critical role in controlling convective flow in this region. A resilient obstacle to understanding the behavior of olivine in the mantle has been the difficulty of determining activation volume (V*), the influence of hydrostatic pressure on flow strength. The bulk of previous studies examining V* were conducted at low pressure (<300 MPa) and small pressure ranges in gas-medium deformation apparatuses, limiting precision and raising questions about application to relevant geological conditions. For this study, we conducted deformation experiments on dry polycrystalline olivine in the D-DIA apparatus. The development of a new hybrid soft-fired pyrophyllite/mullite sample assembly allowed for a broadened pressure range (2-9 GPa), while stress and strain were measured in-situ with synchrotron x rays. Refinement in diffraction technique has allowed stress resolution of ±0.01 GPa. For the pressure range in this study, we have measured an average activation volume of about 17 cm^3/mol for dry polycrystalline San Carlos olivine. This is a substantial pressure effect, representing a pressure-induced viscosity increase of nearly 7 orders of magnitude from the base of the lithosphere to the bottom of the upper mantle.

  17. TEM study of PM2.5 emitted from coal and tire combustion in a thermal power station

    SciTech Connect

    Reto Giere; Mark Blackford; Katherine Smith

    2006-10-15

    The research presented here was conducted within the scope of an experiment investigating technical feasibility and environmental impacts of tire combustion in a coal-fired power station. Previous work has shown that combustion of a coal + tire blend rather than pure coal increased bulk emissions of various elements (e.g., Zn, As, Sb, Pb). The aim of this study is to characterize the chemical and structural properties of emitted single particles with dimensions <2.5 {mu}m (PM2.5). This transmission electron microscope (TEM)-based study revealed that, in addition to phases typical of coal fly ash (e.g., aluminum-silicate glass, mullite), the emitted PM2.5 contains amorphous selenium particles and three types of crystalline metal sulfates never reported before from stack emissions. Anglesite, PbSO{sub 4}, is ubiquitous in the PM2.5 derived from both fuels and contains nearly all Pb present in the PM. Gunningite, ZnSO{sub 4}H{sub 2}O, is the main host for Zn and only occurs in the PM derived from the coal + tire blend, whereas yavapaiite, KFe{sup 3+}(SO{sub 4}){sub 2}, is present only when pure coal was combusted. It is concluded that these metal sulfates precipitated from the flue gas may be globally abundant aerosols and have, through hydration or dissolution, a major environmental and health impact. 66 refs., 2 figs., 1 tab.

  18. Kinetics and mechanisms of primary and steady state creep in B- and Al-containing alpha silicon carbide

    NASA Astrophysics Data System (ADS)

    Davis, Robert F.; Carter, Calvin H., Jr.

    1989-07-01

    The steady state creep behavior of a number of high temperature structural ceramics has been measured and the results analyzed to determine the controlling mechanism. Pure polycrystalline silicon carbide, devoid of sintering aids, creeps by dislocation motion and climb. Silicon carbide containing B- and Al- sintering aids, creeps by grain boundary sliding controlled by diffusion mechanisms (grain boundary diffusion - Coble creep - below 1920 K; lattice diffusion - Nabarro-Herring creep-above 1920 K). The difference in behavior is attributed to the high concentration of vacancies accompanying impurity substitution in the sintered silicon carbide. Experimental measurements of grain boundary sliding offsets on polycrystalline silicon carbide have shown that the primary, transient, creep stage in this material is primarily due to plastic strain within the grains, and that the secondary, steady state, creep stage is primarily due to grain boundary sliding between the grains. The creep of a single crystal and polycrystalline niobium carbide in the 1570 to 1850 K range is controlled by dislocation glide and climb. The creep of hot pressed silicon nitrate and mullite in the 1470 to 1800 K range is controlled by grain boundary sliding due to the amorphous phase present as a consequence of Y2O3 and Al2O3 sintering aids.

  19. Nanomineralogy in the real world: A perspective on nanoparticles in the environmental impacts of coal fire.

    PubMed

    Sehn, Janaína L; de Leão, Felipe B; da Boit, Kátia; Oliveira, Marcos L S; Hidalgo, Gelsa E; Sampaio, Carlos H; Silva, Luis F O

    2016-03-01

    Detailed geochemistry similarities between the burning coal cleaning rejects (BCCRs) and non-anthropogenic geological environments are outlined here. While no visible flames were detected, this research revealed that auto-combustion existed in the studied area for many years. The occurrence of several amorphous phases, mullite, hematite and many other Al/Fe-minerals formed by high temperature was found. Bad disposal of coal-dump wastes represents significant environmental concerns due to their potential influence on atmosphere, river sediments, soils and as well as on the surface and groundwater in the surroundings of these areas. The present work using multi-analytical techniques were performed to provide an improved understanding of the complex processes related with sulphide-rich coal waste oxidation, spontaneous combustion and newmineral creation. It recording huge numbers of rare minerals with alunite, montmorillonite, szmolnockite, halotrichite, coquimbite and copiapite at the BCCRs. The information presented the presence of abundant amorphous Si-Al-Fe-Ti as (oxy-)hydroxides and Fe-hydro/oxides with goethite and hematite with various degrees of crystallinity, containing potential hazardous elements (PHEs), such as Cu, Cr, Hf, Hg, Mo, Ni, Se, Pb, Th, U, Zr, and others. Most of the nano-particles and ultra-fine particles found in the burned coal-dump wastes are the same as those commonly associated with coal cleaning rejects, in which oxidation of sulphides plays an important impact to environment and subsequently animal and human health. PMID:26774310

  20. Heat flux measurements on ceramics with thin film thermocouples

    NASA Technical Reports Server (NTRS)

    Holanda, Raymond; Anderson, Robert C.; Liebert, Curt H.

    1993-01-01

    Two methods were devised to measure heat flux through a thick ceramic using thin film thermocouples. The thermocouples were deposited on the front and back face of a flat ceramic substrate. The heat flux was applied to the front surface of the ceramic using an arc lamp Heat Flux Calibration Facility. Silicon nitride and mullite ceramics were used; two thicknesses of each material was tested, with ceramic temperatures to 1500 C. Heat flux ranged from 0.05-2.5 MW/m2(sup 2). One method for heat flux determination used an approximation technique to calculate instantaneous values of heat flux vs time; the other method used an extrapolation technique to determine the steady state heat flux from a record of transient data. Neither method measures heat flux in real time but the techniques may easily be adapted for quasi-real time measurement. In cases where a significant portion of the transient heat flux data is available, the calculated transient heat flux is seen to approach the extrapolated steady state heat flux value as expected.

  1. Simultaneous leaching and carbon sequestration in constrained aqueous solutions.

    PubMed

    Moon, Ji-Won; Cho, Kyu-Seong; Moberly, James G; Roh, Yul; Phelps, Tommy J

    2011-12-01

    The behavior of metal ions' leaching and precipitated mineral phases of metal-rich fly ash (FA) was examined in order to evaluate microbial impacts on carbon sequestration and metal immobilization. The leaching solutions consisted of aerobic deionized water (DW) and artificial eutrophic water (AEW) that was anaerobic, organic- and mineral-rich, and higher salinity as is typical of bottom water in eutrophic algae ponds. The Fe- and Ca-rich FAs were predominantly composed of quartz, mullite, portlandite, calcite, hannebachite, maghemite, and hematite. After 86 days, only Fe and Ca contents exhibited a decrease in leaching solutions while other major and trace elements showed increasing or steady trends in preference to the type of FA and leaching solution. Ca-rich FA showed strong carbon sequestration efficiency ranging up to 32.3 g CO(2)/kg FA after 86 days, corresponding to almost 65% of biotic carbon sequestration potential under some conditions. Variations in the properties of FAs such as chemical compositions, mineral constituents as well as the type of leaching solution impacted CO(2) capture. Even though the relative amount of calcite increased sixfold in the AEW and the relative amount of mineral phase reached 37.3 wt% using Ca-rich FA for 86 days, chemical sequestration did not accomplish simultaneous precipitation and sequestration of several heavy metals. PMID:21246259

  2. Crack-resistant Al2O3–SiO2 glasses

    NASA Astrophysics Data System (ADS)

    Rosales-Sosa, Gustavo A.; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

    2016-04-01

    Obtaining “hard” and “crack-resistant” glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3–(100–x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3–SiO2 glasses. In particular, the composition of 60Al2O3•40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses.

  3. Thermal Conductivity and Water Vapor Stability of Ceramic HfO2-Based Coating Materials

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Fox, Dennis S.; Bansal, Narottam P.; Miller, Robert A.

    2004-01-01

    HfO2-Y2O3 and La2Zr2O7 are candidate thermal/environmental barrier coating materials for gas turbine ceramic matrix composite (CMC) combustor liner applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature phase stability of plasma-sprayed coatings and/or hot-pressed HfO2-5mol%Y2O3, HfO2-15mol%Y2O3 and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasma-sprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC Hexoloy or CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications will also be discussed.

  4. Thermal Conductivity and Stability of HfO2-Y2O3 and La2Zr2O7 Evaluated for 1650 Deg C Thermal/Environmental Barrier Coating Applications

    NASA Technical Reports Server (NTRS)

    Zhu, Dong-Ming; Bansal, Narottam P.; Miller, Robert A.

    2003-01-01

    HfO2-Y2O3 and La2Zr2O7 are candidate thermal and environmental barrier coating (T/EBC) materials for gas turbine ceramic matrix composite (CMC) combustor applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature stability of hot-pressed and plasma sprayed specimens with representative partially-stabilized and fully-cubic HfO2-Y2O3 compositions and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasmasprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC hexoloy or SiC/SiC CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications are also discussed.

  5. Thermal Conductivity and Water Vapor Stability of HfO2-based Ceramic Coating Materials

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Fox, Dennis S.; Bansal, Narottam P.; Miller, Robert A.

    2004-01-01

    HfO2-Y2O3 and La2Zr2O7 are candidate thermal/environmental barrier coating materials for gas turbine ceramic matrix composite (CMC) combustor liner applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature phase stability of plasma-sprayed coatings and/or hot-pressed HfO2-5mol%Y2O3, HfO2- 15mol%Y2O3 and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasma-sprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC Hexoloy or CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermaVenvironmenta1 barrier coating applications will also be discussed.

  6. Investigation of Sintering Temperature on Attrition Resistance of Highly Porous Diatomite Based Material

    SciTech Connect

    Garderen, Noemie van; Clemens, Frank J.; Scharf, Dagobert; Graule, Thomas

    2010-05-30

    Highly porous diatomite based granulates with a diameter of 500 mum have been produced by an extrusion method. In order to investigate the relation between microstructure, phase composition and attrition resistance of the final product, the granulates were sintered between 800 and 1300 deg. C. Mean pore size of the granulates was evaluated by Hg-porosimetry. An increase of the pore size is observed in the range of 3.6 nm to 40 mum with increasing sintering temperature. Higher mean pore radii of 1.6 mum and 5.7 mum obtained by sintering at 800 and 1300 deg. C respectively. X-ray diffraction shows that mullite phase appears at 1100 deg. C due to the presence of clay. At 1100 deg. C diatomite (amorphous silicate) started to transform into alpha-cristobalite. Attrition resistance was determined by evaluating the amount of ground material passed through a sieve with a predefined mesh size. It was observed that a material sintered at high temperature leads to an increase of attrition resistance due to the decrease of total porosities and phase transformation. Due to the reason that attrition resistance significantly increased by sintering the granulates at higher temperature, a so called attrition resistance index was determined in order to compare all the different attrition resistance values. This attrition resistance index was determined by using the exponential component of the equation obtained from attrition resistance curves. It permits comparison of the attrition behaviour without a time influence.

  7. Fuel Efficient Diesel Particulate Filter (DPF) Modeling and Development

    SciTech Connect

    Stewart, Mark L.; Gallant, Thomas R.; Kim, Do Heui; Maupin, Gary D.; Zelenyuk, Alla

    2010-08-01

    The project described in this report seeks to promote effective diesel particulate filter technology with minimum fuel penalty by enhancing fundamental understanding of filtration mechanisms through targeted experiments and computer simulations. The overall backpressure of a filtration system depends upon complex interactions of particulate matter and ash with the microscopic pores in filter media. Better characterization of these phenomena is essential for exhaust system optimization. The acicular mullite (ACM) diesel particulate filter substrate is under continuing development by Dow Automotive. ACM is made up of long mullite crystals which intersect to form filter wall framework and protrude from the wall surface into the DPF channels. ACM filters have been demonstrated to effectively remove diesel exhaust particles while maintaining relatively low backpressure. Modeling approaches developed for more conventional ceramic filter materials, such as silicon carbide and cordierite, have been difficult to apply to ACM because of properties arising from its unique microstructure. Penetration of soot into the high-porosity region of projecting crystal structures leads to a somewhat extended depth filtration mode, but with less dramatic increases in pressure drop than are normally observed during depth filtration in cordierite or silicon carbide filters. Another consequence is greater contact between the soot and solid surfaces, which may enhance the action of some catalyst coatings in filter regeneration. The projecting crystals appear to provide a two-fold benefit for maintaining low backpressures during filter loading: they help prevent soot from being forced into the throats of pores in the lower porosity region of the filter wall, and they also tend to support the forming filter cake, resulting in lower average cake density and higher permeability. Other simulations suggest that soot deposits may also tend to form at the tips of projecting crystals due to the axial

  8. C(2)H(4) metabolism in morning glory flowers.

    PubMed

    Beyer, E M; Sundin, O

    1978-06-01

    Flowers of Ipomoea tricolor Cav. (cv. Heavenly Blue) were cut at various stages of development and evaluated for their ability to metabolize ethylene. Freshly cut buds or flowers were treated in glass containers for 8 hours with 6 mul/liter of highly purified (14)C(2)H(4). Following removal of dissolved (14)C(2)H(4), radioactivity was determined for the different flower tissues and trappd CO(2). (14)C(2)H(4) oxidation to (14)CO(2) and tissue incorporation occurred at very low to nondetectable levels 2 to 3 days prior to flower opening. About 1 day prior to full bloom, just at the time when mature buds become responsive to ethylene (Kende and Hanson, Plant Physiol 1976, 57: 523-527), there was a dramatic increase in the capacity of the buds to oxidize (14)C(2)H(4) to (14)CO(2). This activity continued to increase until the flower was fully opened reaching a peak activity of 2,500 dpm per three flowers per 8 hours. It then declined as the flower closed and rapidly senesced. A similar but smaller peak occurred in tissue incorporation and it was followed by a second peak during late flower senescence. This first peak in tissue incorporation and the dramatic peak in ethylene oxidation slightly preceded a large peak of natural ethylene production which accompanied flower senescence. The ethylene metabolism observed was clearly dependent on cellular metabolism and did not involve microorganisms since heat killing destroyed this activity and badly contaminated heat-killed flowers were unable to metabolize ethylene. PMID:16660421

  9. Potential of fly ash for neutralisation of acid mine drainage.

    PubMed

    Qureshi, Asif; Jia, Yu; Maurice, Christian; Öhlander, Björn

    2016-09-01

    Lignite (PK), bituminous (FI) and biomass (SE) fly ashes (FAs) were mineralogically and geochemically characterised, and their element leachability was studied with batch leaching tests. The potential for acid neutralisation (ANP) was quantified by their buffering capacity, reflecting their potential for neutralisation of acid mine drainage. Quartz was the common mineral in FAs detected by XRD with iron oxide, anhydrite, and magnesioferrite in PK, mullite and lime in FI, and calcite and anorthite in SE. All the FAs had high contents of major elements such as Fe, Si, Al and Ca. The Ca content in SE was six and eight times higher compared to PK and FI, respectively. Sulphur content in PK and SE was one magnitude higher than FI. Iron concentrations were higher in PK. The trace element concentrations varied between the FAs. SE had the highest ANP (corresponding to 275 kg CaCO3 tonne(-1)) which was 15 and 10 times higher than PK and FI, respectively. The concentrations of Ca(2+), SO4 (2-), Na(+) and Cl(-) in the leachates were much higher compared to other elements from all FA samples. Iron, Cu and Hg were not detected in any of the FA leachates because of their mild to strong alkaline nature with pH ranging from 9 to 13. Potassium leached in much higher quantity from SE than from the other ashes. Arsenic, Mn and Ni leached from PK only, while Co and Pb from SE only. The concentrations of Zn were higher in the leachates from SE. The FAs used in this study have strong potential for the neutralisation of AMD due to their alkaline nature. However, on the other hand, FAs must be further investigated, with scaled-up experiments before full-scale application, because they might leach pronounced concentrations of elements of concern with decreasing pH while neutralising AMD. PMID:27209637

  10. Evaluation of ceramic and polymeric materials for use in engineered barrier systems

    SciTech Connect

    Fullam, H.T.; Skiens, W.E.

    1980-01-01

    Ceramic materials evaluated in the screening studies were Al/sub 2/O/sub 3/ (99.8%), mullite, vitreous silica, BaTiO/sub 3/, CaTiO/sub 3/, CaZrO/sub 3/, CaTiSiO/sub 5/, TiO/sub 2/, ZrSiO/sub 4/, basalt, Pyroceram 9617, and Marcor code 9658 machinable glass ceramic. One grade of graphite (Toyotanso IB-11) was also evaluated. Demineralized water, a synthetic Hanford groundwater, and a synthetic NaCl brine solution were used in the screening tests. Demineralized water was used in all five of the leach tests, but the other solutions were only used in the static leach tests at 150 and 250/sup 0/C. Based on the results obtained, graphite appears to be the most leach resistant of the materials tested with the two grades of alumina being the best of the ceramic materials. Titanium dioxide and ZrO/sub 2/ are the most leach resistant of the remaining materials. Candidate materials from all three general classes of polymers (thermoplastics, thermosets, and elastomers) were considered in the selection of materials. Selected groups of polymers were tested in the flowing autoclave at 150, 200, and 250/sup 0/C with some polymers being further tested at the next higher temperature. Next, selected samples were exposed to gamma radiation. These samples were then submitted for tensile and elongation measurements. Selected samples which appeared promising from both autoclave and radiation testing were further evaluated by impact tests. The materials that appeared most promising after autoclave testing were the EPDM rubbers, polyphenylene sulfide, poly(ethylene-tetrafluoroethylene) copolymer, and polyfurfuryl alcohol. The radiation dose had little effect on polyfurfuryl alcohol and polyphenylene sulfide samples; very significant decreases in elongation were observed for the fluorocarbon copolymer and the EPDM rubbers. While the polyphenylene sulfide and polyfurfuryl alcohol showed little change in impact strength, poly(ethylene-tetrafluoroethylene) decreased in impact strength.

  11. Potentially toxic elements in lignite and its combustion residues from a power plant.

    PubMed

    Ram, L C; Masto, R E; Srivastava, N K; George, J; Selvi, V A; Das, T B; Pal, S K; Maity, S; Mohanty, D

    2015-01-01

    The presence of potentially toxic elements in lignite and coal is a matter of global concern during energy extraction from them. Accordingly, Barsingsar lignite from Rajasthan (India), a newly identified and currently exploited commercial source of energy, was evaluated for the presence of these elements and their fate during its combustion. Mobility of these elements in Barsingsar lignite and its ashes from a power plant (Bikaner-Nagaur region of Thar Desert, India) is presented in this paper. Kaolinite, quartz, and gypsum are the main minerals in lignite. Both the fly ash and bottom ash of lignite belong to class-F with SiO₂ > Al₂O₃ > CaO > MgO. Both the ashes contain quartz, mullite, anhydrite, and albite. As, In, and Sr have higher concentration in the feed than the ashes. Compared to the feed lignite, Ba, Co, U, Cu, Cd, and Ni are enriched (10-5 times) in fly ash and Co, Pb, Li, Ga, Cd, and U in bottom ash (9-5 times). Earth crust-normalization pattern showed enrichment of Ga, U, B, Ag, Cd, and Se in the lignite; Li, Ba, Ga, B, Cu, Ag, Cd, Hg, Pb, and Se, in fly ash; and Li, Sr, Ga, U, B, Cu, Ag, Cd, Pb, and Se in bottom ash. Hg, Ag, Zn, Ni, Ba, and Se are possibly associated with pyrite. Leaching test by toxicity characteristic leaching procedure (TCLP) showed that except B all the elements are within the safe limits prescribed by Indian Standards. PMID:25446718

  12. Kinetics of ceramic-metal composite formation by reactive metal penetration

    SciTech Connect

    Fahrenholtz, W.G.; Ewsuk, K.G.; Loehman, R.E.; Lu, P.

    1998-10-01

    The rate of composite formation via reactive metal penetration has been determined. The metal penetration depth (i.e., the reaction-layer thickness) was measured from cross sections of partially reacted samples. Samples were fabricated by immersing dense mullite preforms in a bath of molten aluminum at temperatures of 900--1300 C and reacting the combination for up to 250 min. In general, the reaction-layer thickness increased linearly as the time increased. Penetration rates as high as 6.0 mm/h were measured; however, the aluminum penetration rate varied dramatically with time and temperature. The penetration rate increased when the reaction temperature was increased from 900 C to 1100 C, and the reaction-layer thickness increased linearly as the time increased in this temperature range. At temperatures of 1150 C and above, reaction-layer formation slowed or stopped after a relatively short period of rapid linear growth, because of an increase in silicon concentration near the reaction interface. The duration of the rapid linear growth, because of an increase in silicon concentration near the reaction interface. The duration of the rapid linear growth period decreased from 25 min at 1150 C to <1 min at 1250 C. At temperatures of 1300 C and above, no reaction layer was detected by using optical microscopy. Kinetics data and transmission electron microscopy analysis suggest that the reaction was inhibited at higher reaction temperatures and longer times, because of silicon buildup and saturation at the reaction front. Calculations show that, as the reaction temperature increased, the silicon production increased aster than the silicon transport. The two gates were approximately equal at a temperature of 1100 C.

  13. Characterization of the origin and distribution of the minerals and phases in metallurgical cokes

    SciTech Connect

    Sushil Gupta; Maria Dubikova; David French; Veena Sahajwalla

    2007-01-15

    Three industrial metallurgical cokes were examined using X-ray diffraction (XRD) and scanning electron microscopy combined with energy dispersive X-ray analysis (SEM/EDS). The study highlighted the difficulties and implications of identifying the inherent crystalline mineral phases in cokes using XRD such that increasing the ashing temperature led to the formation of anhydrite and destruction of metallic iron: microwave plasma ashing resulted in minimal alteration of the original coke mineralogy apart from the formation of bassanite and possibly jarosite. A preliminary scheme to characterize coke minerals is presented such that, physically, minerals can be classified as fine ({lt}50 {mu}m), coarse (50-100 {mu}m), and agglomerate ({gt}1000 {mu}m); chemically, minerals can be grouped as refractory, semirefractory, and reactive, while on the basis of distribution they can be described as discrete, disseminated, or pore inclusions. Quartz, cristobalite, mullite, and high melting point Al-silicates were found to be the predominant refractory phases while low melting point Al-silicates, e.g., containing high fluxing elements such as K, and Fe were the main semirefractory phases present in all cokes. A variety of iron containing phases including pyrrhotite, troilite, iron oxides, metallic iron, and iron silicates were also invariably present in all cokes while calcium phases were found to occur as sulfide, silicates, and phosphates. In general, iron and calcium phases can be categorized as reactive phases with few exceptions such as oldhamite (CaS). The study highlighted that most of the cokes possess a similar mineralogy, with the main distinction being in their relative abundance, particle size, and nature of distribution in the coke matrix. The study provides a basis to develop a mechanistic understanding of the influence of minerals on coke reactivity and strength at high temperatures. 41 refs., 13 figs., 4 tabs.

  14. PNAS Plus: Very high-temperature impact melt products as evidence for cosmic airbursts and impacts 12,900 years ago

    NASA Astrophysics Data System (ADS)

    Bunch, Ted E.; Hermes, Robert E.; Moore, Andrew M. T.; Kennett, Douglas J.; Weaver, James C.; Wittke, James H.; DeCarli, Paul S.; Bischoff, James L.; Hillman, Gordon C.; Howard, George A.; Kimbel, David R.; Kletetschka, Gunther; Lipo, Carl P.; Sakai, Sachiko; Revay, Zsolt; West, Allen; Firestone, Richard B.; Kennett, James P.

    2012-07-01

    It has been proposed that fragments of an asteroid or comet impacted Earth, deposited silica-and iron-rich microspherules and other proxies across several continents, and triggered the Younger Dryas cooling episode 12,900 years ago. Although many independent groups have confirmed the impact evidence, the hypothesis remains controversial because some groups have failed to do so. We examined sediment sequences from 18 dated Younger Dryas boundary (YDB) sites across three continents (North America, Europe, and Asia), spanning 12,000 km around nearly one-third of the planet. All sites display abundant microspherules in the YDB with none or few above and below. In addition, three sites (Abu Hureyra, Syria; Melrose, Pennsylvania; and Blackville, South Carolina) display vesicular, high-temperature, siliceous scoria-like objects, or SLOs, that match the spherules geochemically. We compared YDB objects with melt products from a known cosmic impact (Meteor Crater, Arizona) and from the 1945 Trinity nuclear airburst in Socorro, New Mexico, and found that all of these high-energy events produced material that is geochemically and morphologically comparable, including: (i) high-temperature, rapidly quenched microspherules and SLOs; (ii) corundum, mullite, and suessite (Fe3Si), a rare meteoritic mineral that forms under high temperatures; (iii) melted SiO2 glass, or lechatelierite, with flow textures (or schlieren) that form at > 2,200 °C; and (iv) particles with features indicative of high-energy interparticle collisions. These results are inconsistent with anthropogenic, volcanic, authigenic, and cosmic materials, yet consistent with cosmic ejecta, supporting the hypothesis of extraterrestrial airbursts/impacts 12,900 years ago. The wide geographic distribution of SLOs is consistent with multiple impactors.

  15. Next generation internet architecture and cyber-assisted energy efficiency in smart grids of buildings

    NASA Astrophysics Data System (ADS)

    Peterson, Robb Alex

    Northern Minnesota's iron mines are the starting point for the majority of the steel that gets produced in the United States. Their taconite processing plants use heat in furnaces to oxidize and indurate iron in the final stage of making a taconite pellet. Facilities can increase efficiencies when refractory service life is maintained. Efficiencies gained include: less fuel used, better quality control, better furnace control, and less mechanical component maintenance. Furnace refractory linings fail when the cracks that develop in them are uncontrolled or too large. These failures allow heat and gases retained by the lining to reach structural or mechanical components. Furnace control and efficiencies are also compromised when heat and gases are allowed to short circuit or escape the system. These failures are primarily the result of thermal of shock and expansion. It is common place to add stainless steel needle reinforcement to a monolithic refractory in an effort to counteract these effects. This study used several standard ASTM testing procedures to test 65% alumina mullite based refractory samples with 304 and 406 grade stainless steel needles. Mechanical property data gathered was used to analyze performance. The study found that adding reinforcement does not increase initial Compression and Cold Modulus of Ruptures strengths, however, after prolonged heat and thermal shock exposure, needles help maintain integrity and mechanical properties of samples. The study also found that corrosion due to oxidation was a major contributing factor to the way needles performed; and concluded that a concentration of 3% 406 "Alfa 1" stainless steel reinforcing needles added to the working lining of a taconite furnace is recommended.

  16. Mineralogy and heavy metal leachability of magnetic fractions separated from some Chinese coal fly ashes.

    PubMed

    Lu, S G; Chen, Y Y; Shan, H D; Bai, S Q

    2009-09-30

    Magnetic fractions (MFs) in fly ashes from eight coal-burning power plants were extracted by magnetic separation procedure. Their mineralogy and potential leachability of heavy metals were analyzed using rock magnetism, X-ray diffraction (XRD), scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy (SEM/EDX) and leaching procedures (toxicity characteristics leaching procedure by the United States Environmental Protection Agency, TCLP, and gastric juice simulation test, GJST). Results show that the MFs in the fly ashes range between 2.2 and 16.3wt%, and are generally composed of magnetite, hematite, quartz and mullite. Thermomagnetic analysis and SEM/EDX indicate that the main magnetic carrier magnetite is substituted with small amounts of impure ions, and its structures are featured by rough, dendritic and granular iron spherules. The MFs are found to be rich in Fe, Mn, Cr, Cu, Cd and Pb. Compared with the non-magnetic fractions (NMFs), the MFs have about 5 times higher iron, and 1.6 times higher Mn, Cr, Cu and Cd concentrations. The TCLP test shows that the TCLP-extractable Cr, Cu, and Pb concentrations in the MFs are higher than those in the NMFs, while the TCLP-extractable Cd concentration in the MFs and NMFs is below the detection limit (<0.1mg/L). The GJST-extractable Cd, Cr, Cu, and Pb concentrations in the MFs are higher those in the NMFs. No significant difference in the leachability ratio of Cr, Cu and Pb with TCLP and GJST is found in the MFs and NMFs. However, the GJST test showed that Pb has higher leachability in MFs than that in NMFs. The leachability ratio of heavy metals has an order of Cu>Cr>Pb>Cd. The heavy metals of fly ashes have a great potential to be released into the environment under acid environment. PMID:19380201

  17. Behavior of sulfur and chlorine in coal during combustion and boiler corrosion. Final technical report, 1 September, 1992--31 August, 1993

    SciTech Connect

    Chou, C.L.; Hackley, K.C.; Cao, J.; Moore, D.M.; Xu, J.; Ruch, R.R.; Pan, W.P.; Upchurch, M.L.; Cao, H.B.

    1993-12-31

    The goals of this project are to investigate the behavior of sulfur and chlorine during pyrolysis and combustion of Illinois coals, the chemistry and mineralogy of boiler deposits, the effects of combustion gases on boiler materials, and remedial measures to reduce the sulfur and chlorine compounds in combustion gases. Replicate determinations of chlorine and sulfur evolution during coal pyrolysis-gas combustion were conducted using a pyrolysis apparatus in conjunction with a quadrupole gas analyzer. HCl is the only gaseous chlorine species measured in combustion gases. Pyrolysis of coal IBC-109 spiked with NaCl solution shows a strong peak of HCl evolution above 700C. The absence of this peak during pyrolysis of Illinois coal indicates that little chlorine in Illinois coal occurs in the NaCl form. Evolution of sulfur during coal pyrolysis was studied; the sulfur evolution profile may be explained by the sulfur forms in coal. To determine the fate of sulfur and chlorine during combustion, a set of six samples of boiler deposits from superheater and reheater tubes of an Illinois power plant was investigated. Scanning electron microscopy shows microscopic calcium sulfate droplets on cenospheres. Superheater deposits are high in mullite, hematite, and cristobalite, whereas a reheater deposit is enriched in anhydrite. The chlorine content is very low, indicating that most of the chlorine in the feed coal is lost as volatile HCl during he combustion process. The profiles of SO{sub 2} released during combustion experiments at 825 C indicate that calcium hydroxide added to the coal has a significant effect on reducing the SO{sub 2} vapors in combustion gases.

  18. Properties and characterization of an oxide/oxide composite filter

    SciTech Connect

    Lane, J.E.; Painter, C.J.; Su, W.F.A.; Radford, K.C.; LeCostaouec, J.F.

    1996-12-31

    Westinghouse, with Techniweave as a major subcontractor, is conducting a three-phase program aimed at providing advanced candle filters for a 1997 pilot scale demonstration in one of the two hot gas filter system at Southern Company Service`s Wilsonville PSD Facility. This program`s objective is to develop an oxide CFCC (continuous fiber ceramic composite) candle filter that is cost competitive with prototype next generation filters through the development of a low cost sol-gel fabrication process and a 3D fiber architecture optimized for high volume filter manufacturing. Phase 1, Filter Material Development and Evaluation, results will be presented. Phase 1 activities included laboratory-scale development, characterization, and testing of a mullite matrix 3D fiber-reinforced (Nextel 550) ceramic composite filter material. Eleven 3D architectures were designed, preforms and ceramic matrix composite (CMC) filter materials were made, tested and evaluated. The CMC fabrication process was optimized for reduced cost and acceptable filter performance. Permeability, 4-pt bend and microstructural evaluation results, previously presented, were used to downselect to one 3D architecture and CMC processing method. The downselected filter material was fabricated and tested via permeability and 4-pt bend; Weibull modulus was determined. High-temperature flow-through corrosion tests and thermal aging tests in static air up to 5,000 h were conducted. SEM and XRD have been used to characterize microstructural and phase changes, if any, from high temperature exposure testing. Weaving feasibility studies for the flange and the closed end of a candle filter have been conducted in order to develop a low cost weaving method to make a single piece candle filter fiber preform. Results and conclusions for the evaluation of the downselected filter material above will be presented and discussed.

  19. Testing of Westinghouse hot gas candle filter at Foster Wheeler Karhula R and D Center

    SciTech Connect

    Eriksson, T.; Sellakumar, K.M.; Lippert, T.; Dennis, R.; Feldmann, H.; Brown, R.

    1996-12-31

    The main objectives of the project are to provide performance and environmental data to the design of a PCFB Demonstration project and evaluate Westinghouse advanced ceramic barrier filter system and candle materials. A total test duration of 1,000 to 1,500 hrs in three segments of 500 hrs each has been planned for evaluating the filter unit. A single cluster Westinghouse hot gas candle filter is being tested. The filter system, which houses 112 ceramic candles in three plenums, takes the full flue gas flow from the PCFB combustor. At full load operation (10 MW load, 10 Bar, 850 C), the nominal filtration velocity is 4.3 cm/s. FWEI and WEC have selected a set of advanced ceramic candle materials based on a state of the art evaluation of the material characteristics in the WEC facilities and earlier test experience at many coal-fired test sites including the 2000 hour testing at the Karhula PCFB pilot plant. The selection comprises the following four types of advanced ceramic candles: Schumacher FT-20; 3M SiCoNeX; Pall 326; and Coors mullite. The ICB has supplied coal and the sorbent. Tests have been in progress since November 1995 and are scheduled for completion by the middle of 1996. The filter unit performance so far has been very satisfactory at the nominal design conditions--10 to 12 bar (150 to 175 psis), 800 to 850 C (1,500 to 1,575 F), and nearly 100% dust removal. There was no visible evidence of any dust carry over into the clean side. This paper describes the performance of the filter including the pulse system and the mechanical package.

  20. Use of ceramic materials in waste-package systems for geologic disposal of nuclear wastes

    SciTech Connect

    Fullam, H.T.

    1980-12-01

    A study to investigate the potential use of ceramic materials as components in the waste package systems was conducted. The initial objective of the study was to screen and compare a large number of ceramic materials and identify the best materials for the proposed application. The principal method used to screen the candidates was to subject samples of each material to a series of leaching tests and to determine their relative resistance to attack by the leach solutions. A total of 14 ceramic materials, plus graphite and basalt were evaluated using three different leach solutions: demineralized water, a synthetic Hanford ground water, and a synthetic WIPP brine solution. The ceramic materials screened were Al/sub 2/O/sub 3/ (99%), Al/sub 2/O/sub 3/ (99.8%), mullite (2Al/sub 2/O/sub 3/.SiO/sub 2/), vitreous silica (SiO/sub 2/), BaTiO/sub 3/, CaTiO/sub 3/, CaTiSiO/sub 5/, TiO/sub 2/, ZrO/sub 2/, ZrSiO/sub 4/, Pyroceram 9617, and Marcor Code 9658 machinable glass-ceramic. Average leach rates for the materials tested were determined from analyses of the leach solutions and/or sample weight loss measurements. Because of the limited scope of the present study, evaluation of the specimens was limited to ceramographic examination. Based on an overall evaluation of the leach rate data, five of the materials tested, namely graphite, TiO/sub 2/, ZrO/sub 2/, and the two grades of alumina, exhibited much greater resistance to leaching than did the other materials tested. Based on all the experimental data obtained, and considering other factors such as cost, availability, fabrication technology, and mechanical and physical properties, graphite and alumina are the preferred candidates for the barrier application. The secondary choices are TiO/sub 2/ and ZrO/sub 2/.

  1. Copper stabilization via spinel formation during the sintering of simulated copper-laden sludge with aluminum-rich ceramic precursors.

    PubMed

    Tang, Yuanyuan; Chui, Stephen Sin-Yin; Shih, Kaimin; Zhang, Lingru

    2011-04-15

    The feasibility of incorporating copper-laden sludge into low-cost ceramic products, such as construction ceramics, was investigated by sintering simulated copper-laden sludge with four aluminum-rich ceramic precursors. The results indicated that all of these precursors (γ-Al(2)O(3), corundum, kaolinite, mullite) could crystallochemically stabilize the hazardous copper in the more durable copper aluminate spinel (CuAl(2)O(4)) structure. To simulate the process of copper transformation into a spinel structure, CuO was mixed with the four aluminum-rich precursors, and fired at 650-1150 °C for 3 h. The products were examined using powder X-ray diffraction (XRD) and scanning electron microscopic techniques. The efficiency of copper transformation among crystalline phases was quantitatively determined through Rietveld refinement analysis of the XRD data. The sintering experiment revealed that the optimal sintering temperature for CuAl(2)O(4) formation was around 1000 °C and that the efficiency of copper incorporation into the crystalline CuAl(2)O(4) structure after 3 h of sintering ranged from 40 to 95%, depending on the type of aluminum precursor used. Prolonged leaching tests were carried out by using acetic acid with an initial pH value of 2.9 to leach CuO and CuAl(2)O(4) samples for 22 d. The sample leachability analysis revealed that the CuAl(2)O(4) spinel structure was more superior to stabilize copper, and suggested a promising and reliable technique for incorporating copper-laden sludge or its incineration ash into usable ceramic products. Such results also demonstrated the potential of a waste-to-resource strategy by using waste materials as part of the raw materials with the attainable temperature range used in the production of ceramics. PMID:21428386

  2. Population Balance Modeling of Polydispersed Bubbly Flow in Continuous-Casting Using Multiple-Size-Group Approach

    NASA Astrophysics Data System (ADS)

    Liu, Zhongqiu; Li, Linmin; Qi, Fengsheng; Li, Baokuan; Jiang, Maofa; Tsukihashi, Fumitaka

    2015-02-01

    A population balance model based on the multiple-size-group (MUSIG) approach has been developed to investigate the polydispersed bubbly flow inside the slab continuous-casting mold and bubble behavior including volume fraction, breakup, coalescence, and size distribution. The Eulerian-Eulerian approach is used to describe the equations of motion of the two-phase flow. All the non-drag forces (lift force, virtual mass force, wall lubrication force, and turbulent dispersion force) and drag force are incorporated in this model. Sato and Sekiguchi model is used to account for the bubble-induced turbulence. Luo and Svendsen model and Prince and Blanch model are used to describe the bubbles breakup and coalescence behavior, respectively. A 1/4th water model of the slab continuous-casting mold was applied to investigate the distribution and size of bubbles by injecting air through a circumferential inlet chamber which was made of the specially-coated samples of mullite porous brick, which is used for the actual upper nozzle. Against experimental data, numerical results showed good agreement for the gas volume fraction and local bubble Sauter mean diameter. The bubble Sauter mean diameter in the upper recirculation zone decreases with increasing water flow rate and increases with increasing gas flow rate. The distribution of bubble Sauter mean diameter along the width direction of the upper mold increases first, and then gradually decreases from the SEN to the narrow wall. Close agreements between the predictions and measurements demonstrate the capability of the MUSIG model in modeling bubbly flow inside the continuous-casting mold.

  3. Steel penetration in sand molds. Final technical report, September 1994--September 1997

    SciTech Connect

    Hayes, K.D.; Owens, M.; Barlow, J.; Stefanescu, D.M.; Lane, A.M.; Piwonka, T.S.

    1997-12-01

    The research program was successful in identifying the major factoirs that influence penetration. This was done first through a case study of penetration samples. The study revealed that both chemical and mechanical penetration were present in carbon and high manganese steels. It also found that only mechanical penetration is found in stainless steel samples. It should be noted that when mechanical penetration does occur, there is a greater risk of chemical reactions with the mold. Therefore, it is common to confuse mechanical penetration with chemical. Sessile drop experiments were run to discover the effect of steel chemistry on the contact angle for different substrates. These experiments revealed the best substrates for each type of metal. Bauxite, magnesite, and mullite were discovered to be the best materials for resisting mechanical penetration. It was also shown that high manganese steels cannot be poured into silica molds and that stainless steel should not be poured in chromite molds. The sessile drop data was used to develop a mechanical penetration model which correctly predicted penetration in sixteen of twenty castings poured at the University of Alabama. Mold/metal atmosphere tests were run to understand the effects of the atmosphere on chemical penetration. It was found that the chemistry affecting penetration has its greatest effect as the casting is just poured. Chemical penetration for low carbon steels cannot be completely eliminated by adding carbon (seacoal) to green sand molds although a marked decrease is obtained in its severity. Extremely high carbon concentrations might be able to totally eliminate the penetration but are not used because of their possible diffusion into the steel causing carburization. A chemical penetration model was produced and its results agree well with the experimental results.

  4. Mechanisms of zinc incorporation in aluminosilicate crystalline structures and the leaching behaviour of product phases.

    PubMed

    Tang, Yuanyuan; Shih, Kaimin

    2015-01-01

    This study quantitatively evaluates a waste-to-resource strategy of blending zinc-laden sludge and clay material for low-cost ceramic products. Using ZnO as the simulated zinc-laden sludge to sinter with kaolinite, both zinc aluminate spinel (ZnAl₂O₄) and willemite (Zn₂SiO₄) phases were formed during the sintering process. To analyse the details of zinc incorporation reactions, γ-Al₂O₃and quartz were further used as precursors to observe ZnAl₂O₄and Zn₂SiO₄formations. By firing the ZnO mixtures and their corresponding precursors at 750-1350°C for 3 h, the efficiency of zinc transformation was determined through Rietveld refinement analyses of X-ray diffraction data. The results also show different incorporation behaviour for kaolinite and mullite precursors during the formation of ZnAl2O₄and Zn2SiO₄in the system. In addition, with a competitive formation between ZnAl₂O₄and Zn₂SiO₄, the ZnAl₂O₄spinel phase is predominant at temperatures higher than 1050°C. This study used a prolonged leaching test modified from the US Environmental Protection Agency's toxicity characteristic leaching procedure to evaluate ZnO, ZnAl₂O₄, and Zn₂SiO₄product phases. The zinc concentrations in ZnO and Zn₂SiO₄leachates were about two orders of magnitude higher than that of ZnAl₂O₄ leachate at the end of the experiment, indicating that ZnAl₂O₄formation is the preferred stabilization mechanism for incorporating zinc in ceramic products. PMID:25399963

  5. The effect of ceramic supports on partial oxidation of hydrocarbons over noble metal coated monoliths

    SciTech Connect

    Bodke, A.S.; Bharadwaj, S.S.; Schmidt, L.D.

    1998-10-01

    Support effects on the production of synthesis gas and olefins by the partial oxidation of light hydrocarbons has been examined on noble metal catalysts at contact times of {approximately}5 ms. The authors consider the effect of the following parameters on selectivities and conversions: adding a washcoat, varying pore size, ceramic support material, and loading of noble metal. In oxidation of methane on rhodium-coated monoliths, maximum hydrogen selectivity improves from 89 to 95% on the addition of a washcoat. It is also a strong function of the catalyst pore size, changing from 83% on a catalyst with 20 ppi (pores per inch) to 93% on a catalyst with 80 ppi. It varies from 86 to 91% on adding a washcoat and changes from 70 to 95% on changing the pore size. In the oxidation of ethane on platinum-coated monoliths, the addition of a washcoat reduces ethylene selectivity from 63 to 35%, while changing the pore size results in minor variations. On different ceramic supports, the ethylene selectivity varies from 60 to 64% with mullite giving the best results. The authors find that washcoat addition, decreasing pore size, and replacement of zirconia for alumina as the support material increase syngas selectivity and reduce olefin selectivity irrespective of the fuel, catalyst, or amount of diluent used. Most of these results can be explained on the basis of differences in mass transfer rates to the catalytic site between catalysts of different support geometries. It is argued that homogeneous reactions play a minor role in these short contact time processes.

  6. -C Refractories

    NASA Astrophysics Data System (ADS)

    Xu, Yibiao; Sang, Shaobai; Li, Yawei; Ren, Bo; Zhao, Lei; Li, Yuanbing; Li, Shujing

    2014-06-01

    Al2O3-C refractories were first fabricated in a coke bed at 1673 K (1400 °C) using tabular corundum, reactive alumina, carbon black, silicon, and microsilica as the starting materials and phenol resin as the binder. Then the alkali attack resistance of those materials was conducted in the powder mixture of carbon black and potassium carbonate (1:1 wt pct) in a graphite crucible at 1273 K (1000 °C) for 10 hours. The correlation between pore size, permeability of Al2O3-C refractories, and their alkali (K2CO3) attack was investigated by means of mercury intrusion porosimetry, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The results showed that the pore structure of Al2O3-C refractories was controlled by the addition of silicon, ultrafine reactive alumina, and microsilica to in-situ form SiC whiskers and mullite in the preparation process. The mean pore size of Al2O3-C refractories was strongly associated with permeability. With the decrease of the mean pore size, the permeability of the Al2O3-C refractories reduced constantly. The alkali attack test also verified that the Al2O3-C refractories with lower permeability had better alkali corrosion resistance, because the penetration of K vapor into the materials could be restricted effectively. The corrosion mechanism of Al2O3-C refractories supposes that (1) K2CO3 was reduced to K vapor and penetrated into the specimen through the open pores and (2) K vapor reacted with SiC, SiO2, and alumina to form KAlSi2O6 and KAlSiO4, which is in agreement with the thermodynamic prediction.

  7. Development of oxidation/corrosion-resistant composite materials and interfaces

    SciTech Connect

    Stinton, D.P.; Besmann, T.M.; Shanmugham, S.

    1995-06-01

    Continuous fiber ceramic composites (CFCCs) are being developed for high temperature structural applications, many of which are in oxidative environments. Such composites are attractive since they are light-weight and possess the desired mechanical properties at elevated temperature and in aggressive environments. The most significant advantage is their toughness and their non-catastrophic failure behavior. The mechanical properties of CFCCs have been characteristically linked with the nature of the interfacial bond between the fibers and the matrix. Weakly bonded fiber-matrix intefaces allow an impinging matrix crack to be deflected such that the fracture process occurs through several stages: Crack deflection, debonding at the interface, fiber slip and pull-out, and ultimately fiber failure. Such a composite will fail in a graceful manner and exhibit substantial fracture toughness. Currently, carbon interface coatings are used to appropriately tailor interface properties, however their poor oxidation resistance has required a search of an appropriate replacement. Generally, metal oxides are inherently stable to oxidation and possess thermal expansion coefficients relatively close to those of Nicalon and SiC. However, the metal oxides must also be chemically compatible with the fiber and matrix. If the fiber/interface/matrix system is chemically compatible, then the interfacial bonding stress is influenced by the thermal residual stresses that are generated as the composite is cooled from processing to room temperature. In the current work, thermomechanical computational results were obtained from a finite element model (FEM) for calculating the thermal residual stresses. This was followed by experimental evaluation of Nicalon/SiC composites with carbon, alumina, and mullite interfacial coatings.

  8. Thermal Cyclic Behavior of Thermal and Environmental Barrier Coatings Investigated Under High-Heat-Flux Conditions

    NASA Technical Reports Server (NTRS)

    Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

    2002-01-01

    Environmental barrier coatings (EBC's) have been developed to protect silicon-carbide- (SiC) based ceramic components in gas turbine engines from high-temperature environmental attack. With continuously increasing demands for significantly higher engine operating temperature, future EBC systems must be designed for both thermal and environmental protection of the engine components in combustion gases. In particular, the thermal barrier functions of EBC's become a necessity for reducing the engine-component thermal loads and chemical reaction rates, thus maintaining the required mechanical properties and durability of these components. Advances in the development of thermal and environmental barrier coatings (TBC's and EBC's, respectively) will directly impact the successful use of ceramic components in advanced engines. To develop high-performance coating systems, researchers must establish advanced test approaches. In this study, a laser high-heat-flux technique was employed to investigate the thermal cyclic behavior of TBC's and EBC's on SiC-reinforced SiC ceramic matrix composite substrates (SiC/SiC) under high thermal gradient and thermal cycling conditions. Because the laser heat flux test approach can monitor the coating's real-time thermal conductivity variations at high temperature, the coating thermal insulation performance, sintering, and delamination can all be obtained during thermal cycling tests. Plasma-sprayed yttria-stabilized zirconia (ZrO2-8 wt% Y2O3) thermal barrier and barium strontium aluminosilicate-based environmental barrier coatings (BSAS/BSAS+mullite/Si) on SiC/SiC ceramic matrix composites were investigated in this study. These coatings were laser tested in air under thermal gradients (the surface and interface temperatures were approximately 1482 and 1300 C, respectively). Some coating specimens were also subject to alternating furnace cycling (in a 90-percent water vapor environment at 1300 C) and laser thermal gradient cycling tests

  9. Identification of Gravity-Related Effects on Crystal Growth From Melts With an Immiscibility Gap

    NASA Technical Reports Server (NTRS)

    Kassemi, M.; Sayir, A.; Farmer, S.

    1999-01-01

    This work involves an experimental-numerical approach to study the effects of natural and Marangoni convections on solidification of single crystals from a silicate melt with a liquid-liquid immiscibility gap. Industrial use of crystals grown from silicate melts is becoming increasingly important in electronic, optical, and high temperature structural applications. Even the simplest silicate systems like Al203-SiO2 have had, and will continue to have, a significant role in the development of traditional and advanced ceramics. A unique feature of crystals grown from the silicate systems is their outstanding linear electro-optic properties. They also exhibit exceptionally high optical rotativity. As a result, these crystals are attractive materials for dielectric, optical, and microwave applications. Experimental work in our laboratory has indicated that directional solidification of a single crystal mullite appears to be preceded by liquid-liquid phase separation in the melt. Disruption of the immiscible state results in crystallization of a two phase structure. There is also evidence that mixing in the melt caused by density-driven convection can significantly affect the stability of the immiscible liquid layers and result in poly-crystalline growth. On earth, the immiscible state has only been observed for small diameter crystals grown in float zone systems where natural convection is almost negligible. Therefore, it is anticipated that growth of large single crystals from silicate melts would benefit from microgravity conditions because of the reduction of the natural convective mixing. The main objective of this research is to determine the effects of transport processes on the phase separation in the melt during growth of a single crystal while addressing the following issues: (1) When do the immiscible layers form and are they real?; (2) What are the main physical characteristics of the immiscible liquids?; and (3) How mixing by natural or Marangoni convection

  10. Very high-temperature impact melt products as evidence for cosmic airbursts and impacts 12,900 years ago

    USGS Publications Warehouse

    Bunch, Ted E.; Hermes, Robert E.; Moore, Andrew M.T.; Kennett, Douglas J.; Weaver, James C.; Wittke, James H.; DeCarli, Paul S.; Bischoff, James L.; Hillman, Gordon C.; Howard, George A.; Kimbel, David R.; Kletetschka, Gunther; Lipo, Carl P.; Sakai, Sachiko; Revay, Zsolt; West, Allen; Firestone, Richard B.; Kennett, James P.

    2012-01-01

    It has been proposed that fragments of an asteroid or comet impacted Earth, deposited silica-and iron-rich microspherules and other proxies across several continents, and triggered the Younger Dryas cooling episode 12,900 years ago. Although many independent groups have confirmed the impact evidence, the hypothesis remains controversial because some groups have failed to do so. We examined sediment sequences from 18 dated Younger Dryas boundary (YDB) sites across three continents (North America, Europe, and Asia), spanning 12,000 km around nearly one-third of the planet. All sites display abundant microspherules in the YDB with none or few above and below. In addition, three sites (Abu Hureyra, Syria; Melrose, Pennsylvania; and Blackville, South Carolina) display vesicular, high-temperature, siliceous scoria-like objects, or SLOs, that match the spherules geochemically. We compared YDB objects with melt products from a known cosmic impact (Meteor Crater, Arizona) and from the 1945 Trinity nuclear airburst in Socorro, New Mexico, and found that all of these high-energy events produced material that is geochemically and morphologically comparable, including: (i) high-temperature, rapidly quenched microspherules and SLOs; (ii) corundum, mullite, and suessite (Fe3,/sup>Si), a rare meteoritic mineral that forms under high temperatures; (iii) melted SiO2 glass, or lechatelierite, with flow textures (or schlieren) that form at > 2,200 °C; and (iv) particles with features indicative of high-energy interparticle collisions. These results are inconsistent with anthropogenic, volcanic, authigenic, and cosmic materials, yet consistent with cosmic ejecta, supporting the hypothesis of extraterrestrial airbursts/impacts 12,900 years ago. The wide geographic distribution of SLOs is consistent with multiple impactors.

  11. Study of Advanced Railgun Hydrogen Pellet Injectors for Fusion Reactor Refueling.

    NASA Astrophysics Data System (ADS)

    King, Tony Levone

    An advanced railgun system has been developed to assess its feasibility as a hypervelocity hydrogen pellet injector for magnetically confined plasmas. It consists of a pellet generator/gas gun assembly for freezing hydrogen pellets and injecting them into the railgun at velocities as high as 1.5 km/s. A plasma armature is formed by ionizing the low-Z propellant gas behind the pellet and firing the railgun. This fuseless operation prevents high-Z impurities from entering the reactor during pellet injection. The railgun system has several features that distinguish it from its predecessors, including: (1) a more compact, versatile pellet generator, (2) a new gas gun configuration that produces significantly higher pellet speeds, (3) a perforated coupling piece between the gas gun and railgun to prevent spurious arcing, and (4) ablation-resistant sidewalls, perforated sidewalls and transaugmentation to reduce inertial and viscous drag, the primary obstacles to achieving hypervelocity. A unique system of sophisticated controls and diagnostics has been assembled to operate the railgun system and assess its performance, including fully automated pellet freezing and gas gun operation, an automatic timing circuit that is immune to mistriggering caused by pellet fragmentation or electromagnetic interference, a streak camera, photostations, light gates, current trans formers, B-dot probes, laser interferometry and optical spectroscopy. Free-arc and hydrogen pellet experiments were conducted to evaluate various railgun designs. Transaugmented and simple railguns 1.2 and 2 m long were tested. The performances of railguns using Mullite, solid Lexan and perforated Lexan sidewalls were compared. The railgun theory of operation and anticipated losses are also examined. The theoretical predictions are found to be in good agreement with the experimental results. The advanced railgun system has set several world records for bare hydrogen pellet velocity, including a 3.3 km/s shot on

  12. Authigenic phyllosilicates in modern acid saline lake sediments and implications for Mars

    NASA Astrophysics Data System (ADS)

    Story, Stacy; Bowen, Brenda Beitler; Benison, Kathleen Counter; Schulze, Darrell G.

    2010-12-01

    Aluminum- and Fe/Mg-phyllosilicates are considered important geochemical indicators in terrestrial and Martian sedimentary systems. Traditionally, Al-phyllosilicates are characterized as forming and remaining stable under conditions of low to moderate pH, while Fe/Mg-phyllosilicates are considered representative of only dilute and moderate to high pH conditions. However, we have observed Al- and Fe/Mg-phyllosilicates in acid saline lake sediments in Western Australia. Phyllosilicate formation mechanisms in these lake systems include direct precipitation from lake waters, early diagenetic precipitation from shallow groundwaters, and deposition/alteration of detrital grains. X-ray diffraction analysis of silt- and clay-size sediments from two acid saline lakes in Western Australia indicates the presence of several complex mineral assemblages with extreme spatial heterogeneity that reflects the complex geochemistry of these lakes. These assemblages include unique combinations of authigenic and/or detrital phyllosilicates (e.g., kaolinite, smectite, and palygorskite-sepiolite), sulfates (e.g., alunite, jarosite, and gypsum), Fe-oxides (e.g., hematite and goethite), and other silicates (e.g., mullite and heulandite-clinoptilolite). Observations of Fe/Mg-phyllosilicates found in acid saline sediments in southern Western Australia suggest their degradation under conditions of low pH (2.5-5.4) is slowed by the high salinity (5-25%) of the lake and shallow groundwaters. The occurrence of both Al- and Fe/Mg-phyllosilicates in these acid saline lake sediments suggests that environmental interpretations based on the occurrence of phyllosilicates require additional consideration of their spatial distribution and association with other minerals. Moreover, the similarity between the diverse mineral assemblages in these terrestrial acid saline systems and those on Mars indicates similar conditions may have existed on Mars.

  13. Thermodynamic effects of calcium and iron oxides on crystal phase formation in synthetic gasifier slags containing from 0 to 27wt.% V2O3

    SciTech Connect

    Nakano, Jinichiro; Duchesne, Marc; Bennett, James; Kwong, Kyei -Sing; Nakano, Anna; Hughes, Robin

    2014-11-15

    Thermodynamic phase equilibria in synthetic slags (Al2O3–CaO–FeO–SiO2–V2O3) were investigated with 0–27 wt.% vanadium oxide corresponding to industrial coal–petroleum coke (petcoke) feedstock blends in a simulated gasifier environment. Samples encompassing coal–petcoke mixed slag compositions were equilibrated at 1500 °C in a 64 vol.% CO/36 vol.% CO2 atmosphere (Po2 ≈ 10–8 atm at 1500 °C) for 72 h, followed by rapid water quench, then analyzed by inductively coupled plasma optical emission spectrometry, X-ray diffractometry, and scanning electron microscopy with wavelength dispersive spectroscopy. With increasing CaO content, FeO content, or both; the slag homogeneity region expanded and a composition range exhibiting crystals was reduced. The mullite (Al6Si2O13) crystalline phase was not present in the slags above 9 wt.% FeO while the karelianite (V2O3) crystalline phase was always present in compositions studied if a sufficient amount of vanadium existed in the slag. Furthermore, based on the present experimental equilibrium evaluation, a set of isothermal phase diagrams showing effects of CaO and FeO on thermodynamic phase stabilities in the vanadium-bearing slags is proposed. Some uses of the diagrams for potential industrial practice are discussed.

  14. Fusion of arkosic sand by intrusive andesite

    USGS Publications Warehouse

    Bailey, Roy A.

    1954-01-01

    An andesite dike in the Valles Mountains of northern New Mexico has intruded and partly fused arkosic sediments for a distance of 50 feet from its contacts. The dike is semi-circular in form, has a maximum width of about 100 feet, and is about 500 feet long. Small associated arcuate dikes are arranged in spiral fashion around the main dike, suggesting that they were intruded along shear fractures similar to those described by Burbank (1941). The fused rocks surrounding the andesite dike are of three general types: 1) partly fused arkosic sand, 2) fused clay, and 3) hybrid rocks. The fused arkosic sand consists of relict detrital grains of quartz, orthoclose, and plagioclase, imbedded in colorless glass containing microlites of tridymite, cordierite, and magnetite. The relict quartz grains are corroded and embayed by glass; the orthoclase is sanidinized and partly fused; and the plagioclase is inverted to the high temperature form and is partly fused. The fused clay, which was originally a mixture of montmorillonite and hydromica, consists primarily of cordierite but also contains needle-like crystals of sillimanite (?) or mullite (?). The hybrid rocks originated in part by intermixing of fused arkosic sediments and andesitic liquid and in part by diffusion of mafic constituents through the fused sediments. They are rich in cordierite and magnetite and also contain hypersthene, augite, and plagioclase. The composition of pigeonite in the andesite indicates that the temperature of the andesite at the time of intrusion probably did not exceed 1200?C. Samples of arkosic sand were fused in the presence of water in a Morey bomb at 1050?C. Stability relations of certain minerals in the fused sand suggest that fusion may have taken place at a lower temperature, however, and the fluxing action of volatiles from the andesite are thought to have made this possible.

  15. Why can tiAicrsiYN-based adaptive coatings deliver exceptional performance under extreme frictional conditions?

    PubMed

    Beake, Ben D; Fox-Rabinovich, German S; Losset, Yannick; Yamamoto, Kenji; Agguire, Myriam H; Veldhuis, Stephen C; Endrino, Jose L; Kovalev, Anatoliy I

    2012-01-01

    Adaptive TiAlCrSiYN-based coatings show promise under the extreme tribological conditions of dry ultra-high-speed (500-700 m min-1) machining of hardened tool steels. During high speed machining, protective sapphire and mullite-like tribo-films form on the surface of TiAlCrSiYN-based coatings resulting in beneficial heat-redistribution in the cutting zone. XRD and HRTEM data show that the tribo-films act as a thermal barrier creating a strong thermal gradient. The data are consistent with the temperature decreasing from approximately 1100-1200 degrees C at the outer surface to approximately 600 degrees C at the tribo-film/coating interface. The mechanical properties of the multilayer TiAICrSiYN/TiA1CrN coating were measured by high temperature nanoindentation. It retains relatively high hardness (21 GPa) at 600 degrees C. The nanomechanical properties of the underlying coating layer provide a stable low wear environment for the tribo-films to form and regenerate so it can sustain high temperatures under operation (600 degrees C). This combination of characteristics explains the high wear resistance of the multilayer TiAlCrSiYN/TiAICrN coating under extreme operating conditions. TiAlCrSiYN and TiAlCrN monolayer coatings have a less effective combination of adaptability and mechanical characteristics and therefore lower tool life. The microstructural reasons for different optimum hardness and plasticity between monolayer and multilayer coatings are discussed. PMID:23285634

  16. Plasma-Sprayed Refractory Oxide Coatings on Silicon-Base Ceramics

    NASA Technical Reports Server (NTRS)

    Tewari, Surendra

    1997-01-01

    Silicon-base ceramics are promising candidate materials for high temperature structural applications such as heat exchangers, gas turbines and advanced internal combustion engines. Composites based on these materials are leading candidates for combustor materials for HSCT gas turbine engines. These materials possess a combination of excellent physical and mechanical properties at high temperatures, for example, high strength, high toughness, high thermal shock resistance, high thermal conductivity, light weight and excellent oxidation resistance. However, environmental durability can be significantly reduced in certain conditions such as when molten salts, H2 or water vapor are present. The oxidation resistance of silicon-base materials is provided by SiO2 protective layer. Molten salt reacts with SiO2 and forms a mixture of SiO2 and liquid silicate at temperatures above 800C. Oxygen diffuses more easily through the chemically altered layer, resulting in a catastrophic degradation of the substrate. SiC and Si3N4 are not stable in pure H2 and decompose to silicon and gaseous species such as CH4, SiH, SiH4, N2, and NH3. Water vapor is known to slightly increase the oxidation rate of SiC and Si3N4. Refractory oxides such as alumina, yttria-stabilized zirconia, yttria and mullite (3Al2O3.2SiO2) possess excellent environmental durability in harsh conditions mentioned above. Therefore, refractory oxide coatings on silicon-base ceramics can substantially improve the environmental durability of these materials by acting as a chemical reaction barrier. These oxide coatings can also serve as a thermal barrier. The purpose of this research program has been to develop refractory oxide chemical/thermal barrier coatings on silicon-base ceramics to provide extended temperature range and lifetime to these materials in harsh environments.

  17. How do the barrier thickness and dielectric material influence the filamentary mode and CO2 conversion in a flowing DBD?

    NASA Astrophysics Data System (ADS)

    Ozkan, A.; Dufour, T.; Bogaerts, A.; Reniers, F.

    2016-08-01

    Dielectric barrier discharges (DBDs) are commonly used to generate cold plasmas at atmospheric pressure. Whatever their configuration (tubular or planar), the presence of a dielectric barrier is mandatory to prevent too much charge build up in the plasma and the formation of a thermal arc. In this article, the role of the barrier thickness (2.0, 2.4 and 2.8 mm) and of the kind of dielectric material (alumina, mullite, pyrex, quartz) is investigated on the filamentary behavior in the plasma and on the CO2 conversion in a tubular flowing DBD, by means of mass spectrometry measurements correlated with electrical characterization and IR imaging. Increasing the barrier thickness decreases the capacitance, while preserving the electrical charge. As a result, the voltage over the dielectric increases and a larger number of microdischarges is generated, which enhances the CO2 conversion. Furthermore, changing the dielectric material of the barrier, while keeping the same geometry and dimensions, also affects the CO2 conversion. The highest CO2 conversion and energy efficiency are obtained for quartz and alumina, thus not following the trend of the relative permittivity. From the electrical characterization, we clearly demonstrate that the most important parameters are the somewhat higher effective plasma voltage (yielding a somewhat higher electric field and electron energy in the plasma) for quartz, as well as the higher plasma current (and thus larger electron density) and the larger number of microdischarge filaments (mainly for alumina, but also for quartz). The latter could be correlated to the higher surface roughness for alumina and to the higher voltage over the dielectric for quartz.

  18. Thermal stabilization of chromium(VI) in kaolin.

    PubMed

    Wei, Yu-Ling; Chiu, Shu-Yuan; Tsai, Hsien-Neng; Yang, Yaw-Wen; Lee, Jyh-Fu

    2002-11-01

    Reduction of Cr(VI) by heating may be a useful detoxification mechanism for thermal immobilization. Using X-ray absorption spectroscopy, the change of speciation of chromium in 105 degrees C dried 3.7% Cr(VI)-sorbed kaolin further heated at 500, 900, or 1100 degrees C was studied. The 105 degrees C dried 3.7% Cr(VI)-sorbed kaolin sample was prepared by mixing 1.5 L of 0.257 M CrO3 solution (pH 0.71) with 0.5 kg of kaolin powder for 48 h, and then the slurry was heated (dried) at 105 degrees C until a constant weight was reached. The toxicity characteristic leaching procedure method was used to determine the percentage of leached chromium from all heated samples. In all 500-900 degrees C heated Cr(VI)-sorbed kaolin samples, Cr2O3 transformed from the hydrated Cr(VI) by a 4-h heat application was identified by the X-ray absorption near edge structure and extended X-ray absorption fine structure (EXAFS) spectroscopy as the key species that is leaching-resistant due to its low solubility. For the 1100 degrees C heated Cr(VI)-sorbed kaolin sample, the Fourier transform of its EXAFS spectrum indicates that the intensity of the peaks at 2.45 (Cr-Cr shell of Cr2O3) and 5.00 A (Cr-Cr and Cr-O shells of Cr2O3) without phase shift correction is either relatively smaller or disappearing, compared with that of the 500-900 degrees C heated Cr(VI)-sorbed kaolin samples. It is suggested that chromium octahedra were bridged to silica tetrahedra and incorporated in minerals formed at 1100 degrees C, such as mullite or sillimanite, since these phases were detected by XRD. Cr of this form is not easily leached. PMID:12433175

  19. Shock-wave compression and release of aluminum/ceramic composites

    SciTech Connect

    Johnson, J.N.; Hixson, R.S.; Gray, G.T. III )

    1994-11-15

    Several composite materials consisting of ceramic particles embedded in a 6061-T6 aluminum matrix have been studied under conditions of shock-wave compression and release, including spallation. The 6061-T6 matrix represents a material for which high-rate shock-wave response has been extremely well characterized for thermoelastic-plastic deformation. The ceramic particles (alumina and mullite) are also well characterized, particularly in the elastic regime. Experimental tests consist of quasistatic, uniaxial-stress compression of both virgin and shock-recovered samples as well as time-resolved velocity interferometer measurements under conditions of flat-plate impact. The latter tests were performed with lithium fluoride windows for transmitted wave studies and free surfaces for spallation measurement. Theoretical analysis of the data is carried out with a pseudodissipation model originated by Barker [J. Composite Mat. [bold 5], 140 (1971)] for application to elastic deformation of layered composites and generalized here to include thermoelastic-plastic properties of the constituents. For a pseudodissipative model to apply to composite material response, significant geometrical randomization must be present in the composite structure; this is something that all commercially produced composites naturally possess. Randomization produces mechanical energy traps, which convert some fraction of regular, directed motion into random elastic vibrations behind the shock front. Within a few microseconds (depending on the pinned dislocation segment density) this macroscale, continuum vibrational energy is converted to heat by means of the anelastic properties of the metal matrix. The use of pseudodissipation as a means of representing dispersive composite material behavior is thus placed on a more secure physical foundation.

  20. Population Balance Modeling of Polydispersed Bubbly Flow in Continuous-Casting Using Multiple-Size-Group Approach

    NASA Astrophysics Data System (ADS)

    Liu, Zhongqiu; Li, Linmin; Qi, Fengsheng; Li, Baokuan; Jiang, Maofa; Tsukihashi, Fumitaka

    2014-09-01

    A population balance model based on the multiple-size-group (MUSIG) approach has been developed to investigate the polydispersed bubbly flow inside the slab continuous-casting mold and bubble behavior including volume fraction, breakup, coalescence, and size distribution. The Eulerian-Eulerian approach is used to describe the equations of motion of the two-phase flow. All the non-drag forces (lift force, virtual mass force, wall lubrication force, and turbulent dispersion force) and drag force are incorporated in this model. Sato and Sekiguchi model is used to account for the bubble-induced turbulence. Luo and Svendsen model and Prince and Blanch model are used to describe the bubbles breakup and coalescence behavior, respectively. A 1/4th water model of the slab continuous-casting mold was applied to investigate the distribution and size of bubbles by injecting air through a circumferential inlet chamber which was made of the specially-coated samples of mullite porous brick, which is used for the actual upper nozzle. Against experimental data, numerical results showed good agreement for the gas volume fraction and local bubble Sauter mean diameter. The bubble Sauter mean diameter in the upper recirculation zone decreases with increasing water flow rate and increases with increasing gas flow rate. The distribution of bubble Sauter mean diameter along the width direction of the upper mold increases first, and then gradually decreases from the SEN to the narrow wall. Close agreements between the predictions and measurements demonstrate the capability of the MUSIG model in modeling bubbly flow inside the continuous-casting mold.

  1. Xenopumice erupted on 15 October 2011 offshore of El Hierro (Canary Islands): a subvolcanic snapshot of magmatic, hydrothermal and pyrometamorphic processes

    NASA Astrophysics Data System (ADS)

    Del Moro, S.; Di Roberto, A.; Meletlidis, S.; Pompilio, M.; Bertagnini, A.; Agostini, S.; Ridolfi, F.; Renzulli, A.

    2015-06-01

    On 15 October 2011, a submarine eruption offshore of El Hierro Island gave rise to floating volcanic products, known as xenopumices, i.e., pumiceous xenoliths partly mingled and coated with the juvenile basanitic magma. Over the last few years, no consensus in the scientific community in explaining the origin of these products has been reached. In order to better understand the formation of xenopumice, we present a textural, mineralogical, and geochemical study of the possible magmatic, hydrothermal, and pyrometamorphic processes, which usually operate in the plumbing systems of active volcanoes. We carried out a comprehensive SEM investigation and Sr-Nd-Pb isotope analyses on some samples representative of three different xenopumice facies. All the data were compared with previous studies, new data for El Hierro extrusives and a literature dataset of Canary Islands igneous and sedimentary rocks. In the investigated xenopumices, we emphasize the presence of restitic magmatic phases as well as crystallization of minerals (mainly olivine + pyroxene + magnetite aggregates) as pseudomorphs after pre-existing mafic phenocrysts, providing evidence of pyrometamorphism induced by the high-T juvenile basanitic magma. In addition, we identify veins consisting of zircon + REE-oxides + mullite associated with Si-rich glass and hydrothermal quartz, which indicate the fundamental role played by hydrothermal fluid circulation in the xenopumice protolith. The petrological data agree with a pre-syneruptive formation of the xenopumice, when El Hierro basanite magma intruded hydrothermally altered trachyandesite to trachyte rocks and triggered local partial melting. Therefore, the El Hierro xenopumice represents a snapshot of the transient processes at the magma-wall rock interface, which normally occurs in the feeding system of active volcanoes.

  2. Silicon-on ceramic process. Silicon sheet growth and device developmentt for the Large-Area Silicon Sheet Task of the Low-Cost Solar Array Project. Quarterly report No. 13, October 1-December 31, 1979

    SciTech Connect

    Chapman, P W; Zook, J D; Grung, B L; McHenry, K; Schuldt, S B

    1980-02-15

    Research on the technical and economic feasibility of producing solar-cell-quality sheet silicon by coating inexpensive ceramic substrates with a thin layer of polycrystalline silicon is reported. The coating methods to be developed are directed toward a minimum-cost process for producing solar cells with a terrestrial conversion efficiency of 11 percent or greater. By applying a graphite coating to one face of a ceramic substrate, molten silicon can be caused to wet only that graphite-coated face and produce uniform thin layers of large-grain polycrystalline silicon; thus, only a minimal quantity of silicon is consumed. A variety of ceramic materials have been dip coated with silicon. The investigation has shown that mullite substrates containing an excess of SiO/sub 2/ best match the thermal expansion coefficient of silicon and hence produce the best SOC layers. With such substrates, smooth and uniform silicon layers 25 cm/sup 2/ in area have been achieved with single-crystal grains as large as 4 mm in width and several cm in length. Crystal length is limited by the length of the substrate. The thickness of the coating and the size of the crystalline grains are controlled by the temperature of the melt and the rate at which the substrate is withdrawn from the melt. The solar-cell potential of this SOC sheet silicon is promising. To date, solar cells with areas from 1 to 10 cm/sup 2/ have been fabricated from material with an as-grown surface. Conversion efficiencies of about 10 percent with antireflection (AR) coating have been achieved. Such cells typically have open-circuit voltage and short-circuit current densities of 0.55V and 23 mA/cm/sup 2/, respectively.

  3. Simplified Reference Electrode for Electrorefining of Spent Nuclear Fuel in High Temperature Molten Salt

    SciTech Connect

    Kim Davies; Shelly X Li

    2007-09-01

    Pyrochemical processing plays an important role in development of proliferation- resistant nuclear fuel cycles. At the Idaho National Laboratory (INL), a pyrochemical process has been implemented for the treatment of spent fuel from the Experimental Breeder Reactor II (EBR-II) in the last decade. Electrorefining in a high temperature molten salt is considered a signature or central technology in pyroprocessing fuel cycles. Separation of actinides from fission products is being demonstrated by electrorefining the spent fuel in a molten UCl3-LiCl-KCl electrolyte in two engineering scale electrorefiners (ERs). The electrorefining process is current controlled. The reference electrode provides process information through monitoring of the voltage difference between the reference and the anode and cathode electrodes. This information is essential for monitoring the reactions occurring at the electrodes, investigating separation efficiency, controlling the process rate, and determining the process end-point. The original reference electrode has provided good life expectancy and signal stability, but is not easily replaceable. The reference electrode used a vycor-glass ion-permeable membrane containing a high purity silver wire with one end positioned in ~2 grams of LiCl/KCl salt electrolyte with a low concentration (~1%) AgCl. It was, however, a complex assembly requiring specialized skill and talent to fabricate. The construction involved multiple small pieces, glass joints, ceramic to glass joints, and ceramic to metal joints all assembled in a high purity inert gas environment. As original electrodes reached end-of-life it was uncertain if the skills and knowledge were readily available to successfully fabricate replacements. Experimental work has been conducted to identify a simpler electrode design while retaining the needed long life and signal stability. This improved design, based on an ion-permeable membrane of mullite has been completed. Use of the silver wire

  4. Characterization of Two Different Clay Materials by Thermogravimetry (TG), Differential Scanning Calorimetry (DSC), Dilatometry (DIL) and Mass Spectrometry (MS) - 12215

    SciTech Connect

    Post, Ekkehard; Henderson, Jack B.

    2012-07-01

    An illitic clay containing higher amounts of organic materials was investigated by dilatometry, thermogravimetry and differential scanning calorimetric. The evolved gases were studied during simultaneous TG-DSC (STA) and dilatometer measurements with simultaneous mass spectrometry in inert gas and oxidizing atmosphere. The dilatometer results were compared with the STA-MS results which confirmed and explained the reactions found during heating of the clay, like dehydration, dehydroxylation, shrinkage, sintering, quartz phase transition, combustion or pyrolysis of organics and the solid state reactions forming meta-kaolinite and mullite. The high amount of organic material effects in inert gas atmosphere most probably a reduction of the oxides which leads to a higher mass loss than in oxidizing atmosphere. Due to this reduction an additional CO{sub 2} emission at around 1000 deg. C was detected which did not occur in oxidizing atmosphere. Furthermore TG-MS results of a clay containing alkali nitrates show that during heating, in addition to water and CO{sub 2}, NO and NO{sub 2} are also evolved, leading to additional mass loss steps. These types of clays showed water loss starting around 100 deg. C or even earlier. This relative small mass loss affects only less shrinkage during the expansion of the sample. The dehydroxylation and the high crystalline quartz content result in considerable shrinkage and expansion of the clay. During the usual solid state reaction where the clay structure collapses, the remaining material finally shrinks down to a so-called clinker. With the help of MS the TG steps can be better interpreted as the evolved gases are identified. With the help of the MS it is possible to distinguish between CO{sub 2} and water (carbonate decomposition, oxidation of organics or dehydration/dehydroxylation). The MS also clearly shows that mass number 44 is found during the TG step of the illitic clay at about 900 deg. C in inert gas, which was interpreted

  5. CaBr{sub 2} hydrolysis for HBr production using a direct sparging contactor.

    SciTech Connect

    Yang, J.; Panchal, C. B.; Doctor, R. D.; Energy Systems

    2009-09-01

    The calcium-bromine cycle being investigated is a novel continuous hybrid cycle for hydrogen production employing both heat and electricity. Calcium bromide (CaBr{sub 2}) hydrolysis generates hydrogen bromide (HBr) which is electrolyzed to produce hydrogen. The CaBr{sub 2} hydrolysis at 1050 K (777 C) is endothermic with the heat of reaction {delta}G{sub T} = 181.5 KJ/mol (43.38 kcal/mol) and the Gibbs free energy change is positive at 99.6 kJ/mol (23.81 kcal/mol). What makes this hydrolysis reaction attractive is both its rate and that well over half the thermodynamic requirements for water-splitting heat of reaction of {delta}G{sub T} = 285.8 KJ/mol (68.32 kcal/mol) are supplied at this stage using heat rather than electricity. Molten-phase calcium bromide reactors may overcome the technical barriers associated with earlier hydrolysis approaches using supported solid-phase calcium bromide studied in the Japanese UT-3 cycle. Before constructing the experiment two design concepts were evaluated using COMSOL{trademark} multi-physics models; (1) the first involved sparging steam into a calcium-bromide melt, while (2) the second considered a 'spray-dryer' contactor spraying molten calcium bromide counter-currently to upward-flowing steam. A recent paper describes this work. These studies indicated that sparging steam into a calcium-bromide melt is more feasible than spraying molten calcium bromide droplets into steam. Hence, an experimental sparging hydrolysis reactor using a mullite tube (ID 70 mm) was constructed capable of holding 0.3-0.5 kg (1.5-2.5 x 10{sup -3} kg mol) CaBr{sub 2} forming a melt with a maximum 0.08 m (8 cm) depth. Sparging steam at a steam rate of 0.02 mol/mol of CaBr{sub 2} per minute (1.2-2.3 x 10{sup -5} kg/s), into this molten bath promptly yielded HBr in a stable operation that converted up to 25% of the calcium bromide. The kinetic constant derived from the experimental data was 2.17 x 10{sup -12} kmol s{sup -1} m{sup -2} MPa{sup -1} for

  6. The properties of the nano-minerals and hazardous elements: Potential environmental impacts of Brazilian coal waste fire.

    PubMed

    Civeira, Matheus S; Pinheiro, Rafael N; Gredilla, Ainara; de Vallejuelo, Silvia Fdez Ortiz; Oliveira, Marcos L S; Ramos, Claudete G; Taffarel, Silvio R; Kautzmann, Rubens M; Madariaga, Juan Manuel; Silva, Luis F O

    2016-02-15

    Brazilian coal area (South Brazil) impacted the environment by means of a large number of coal waste piles emplaced over the old mine sites and the adjacent areas of the Criciúma, Urussanga, and Siderópolis cities. The area studied here was abandoned and after almost 30 years (smokeless visual) some companies use the actual minerals derived from burning coal cleaning rejects (BCCRs) complied in the mentioned area for industry tiles or refractory bricks. Mineralogical and geochemical similarities between the BCCRs and non-anthropogenic geological environments are outlined here. Although no visible flames were observed, this study revealed that auto-combustion existed in the studied area for many years. The presence of amorphous phases, mullite, hematite and other Fe-minerals formed by high temperature was found. There is also pyrite, Fe-sulphates (eg. jarosite) and unburnt coal present, which are useful for comparison purposes. Bad disposal of coal-dump wastes represents significant environmental concerns due to their potential influence on atmosphere, river sediments, soils and as well as on the surface and groundwater in the surroundings of these areas. The present study using advanced analytical techniques were performed to provide an improved understanding of the complex processes related with sulphide-rich coal waste oxidation, spontaneous combustion and mineral formation. It is reporting huge numbers of rare minerals with alunite, montmorillonite, szomolnokite, halotrichite, coquimbite and copiapite at the BCCRs. The data showed the presence of abundant amorphous Si-Al-Fe-Ti as (oxy-)hydroxides and Fe-hydro/oxides with goethite and hematite with various degrees of crystallinity, containing hazardous elements, such as Cu, Cr, Hf, Hg, Mo, Ni, Se, Pb, Th, U, Zr, and others. By Principal Component Analysis (PCA), the mineralogical composition was related with the range of elemental concentration of each sample. Most of the nano-minerals and ultra-fine particles

  7. Surface and bulk characterization of an ultrafine South African coal fly ash with reference to polymer applications

    NASA Astrophysics Data System (ADS)

    van der Merwe, E. M.; Prinsloo, L. C.; Mathebula, C. L.; Swart, H. C.; Coetsee, E.; Doucet, F. J.

    2014-10-01

    South African coal-fired power stations produce about 25 million tons of fly ash per annum, of which only approximately 5% is currently reused. A growing concern about pollution and increasing landfill costs stimulates research into new ways to utilize coal fly ash for economically beneficial applications. Fly ash particles may be used as inorganic filler in polymers, an application which generally requires the modification of their surface properties. In order to design experiments that will result in controlled changes in surface chemistry and morphology, a detailed knowledge of the bulk chemical and mineralogical compositions of untreated fly ash particles, as well as their morphology and surface properties, is needed. In this paper, a combination of complementary bulk and surface techniques was explored to assess the physicochemical properties of a classified, ultrafine coal fly ash sample, and the findings were discussed in the context of polymer application as fillers. The sample was categorized as a Class F fly ash (XRF). Sixty-two percent of the sample was an amorphous glass phase, with mullite and quartz being the main identified crystalline phases (XRD, FTIR). Quantitative carbon and sulfur analysis reported a total bulk carbon and sulfur content of 0.37% and 0.16% respectively. The spatial distribution of the phases was determined by 2D mapping of Raman spectra, while TGA showed a very low weight loss for temperatures ranging between 25 and 1000 °C. Individual fly ash particles were characterized by a monomodal size distribution (PSD) of spherical particles with smooth surfaces (SEM, TEM, AFM), and a mean particle size of 4.6 μm (PSD). The BET active surface area of this sample was 1.52 m2/g and the chemical composition of the fly ash surface (AES, XPS) was significantly different from the bulk composition and varied considerably between spheres. Many properties of the sample (e.g. spherical morphology, small particle size, thermal stability) appeared

  8. Paralava and clinker products of coal combustion, Yellow River, Shanxi Province, China

    NASA Astrophysics Data System (ADS)

    Grapes, Rodney; Zhang, Ke; Peng, Zhuo-lun

    2009-12-01

    Combustion of bituminous coal seams in a Carbonifeorus-Permian sequence of siltstone, quartzose sandstone, sideritic mudstone, kaolinite-rich and sulphide-ankerite rocks exposed on the left bank of the Yellow River, western border of Shanxi Province, China, has resulted in the formation of paralava and glassy clinker. Some paralavas have compositions similar to low alkali basalts and contain anorthite, low Ca-pyroxenes (clinoenstatite, pigeonite), ± minor augite, ± olivine, Fe-Ti oxides and K-bearing siliceous glass. In these paralavas the sequence of pyroxene crystallization was Mg-pigeonite → augite → Fe-pigeonite and Mg-clinoenstatite → borderline Fe-clinoenstatite/pigeonite. More siliceous paralava compositions contain anorthite, clinoenstatite, cordierite, Fe-Ti oxides and glass. Fused clinker consists of cordierite, anorthite, tridymite, mullite, Fe-Ti oxides and K-rich siliceous glass. Paralava liquidus temperatures range between ca. 1230 and 1120 °C and the generalized crystallization sequence in a "basaltic" composition was anorthite, pyroxene (low Ca-clinopyroxene, augite), Ti-magnetite, olivine with quench apatite in glass over a cooling interval of ˜ 345 °C. The liquidus temperature of clinker was ca. 1100 °C. In paralavas and clinker, subsolidus exsolution of hemo-ilmenite from Ti-magnetite occurred under log fO 2 = - 9.0 to - 13.9 at temperatures of 907-756 °C, with formation of almost pure ilmenite at lowest temperatures of 536-567 °C at log fO 2 = - 24.9-21.9. Changes in the texture and habit of pyroxene in paralava adjacent clinker (porphyritic to skeletal/plumose towards clinker) reflect the effects of a cooling front moving into the paralava and changing bulk composition. Paralavas formed by melting of different combinations of siltstone, sideritic mudstone and ankerite-rich rock "end-members", and there was also diffusion of Si, Al, Ti and K into paralava from fused clinker blocks within it.

  9. Disequilibrium between uranium and its progeny in the Lake Issyk-Kul system (Kyrgyzstan) under a combined effect of natural and manmade processes.

    PubMed

    Gavshin, V M; Melgunov, M S; Sukhorukov, F V; Bobrov, V A; Kalugin, I A; Klerkx, J

    2005-01-01

    /(226)Ra ratios 0.28--0.44. The presence of mullite in these sediments indicated that radioactive ash penetrated into the lake in the past. At present, (226)Ra in the ash is buried under a non-radioactive cap. PMID:15935909

  10. NONDESTRUCTIVE EVALUATION OF CERAMIC CANDLE FILTERS

    SciTech Connect

    Roger H.L. Chen, Ph.D.; Alejandro Kiriakidis

    1999-09-01

    Nondestructive evaluation (NDE) techniques have been used to reduce the potential mechanical failures and to improve the reliability of a structure. Failure of a structure is usually initiated at some type of flaw in the material. NDE techniques have been developed to determine the presence of flaws larger than an acceptable size and to estimate the remaining stiffness of a damaged structure (Chen, et. al, 1995). Ceramic candle filters have been tested for use in coal-fueled gas turbine systems. They protect gas turbine components from damage due to erosion. A total of one hundred and one candle filters were nondestructively evaluated in this study. Ninety-eight ceramic candle filters and three ceramic composite filters have been nondestructively inspected using dynamic characterization technique. These ceramic filters include twelve unused Coors alumina/mullite, twenty-four unused and fifteen used Schumacher-Dia-Schumalith TF-20, twenty-five unused and nine used Refractron 326, eight unused and three used Refractron 442T, one new Schumacher-T 10-20, and one used Schumacher-Dia-Schumalith F-40. All filters were subjected to a small excitation and the dynamic response was picked up by a piezoelectric accelerometer. The evaluation of experimental results was processed using digital signal analysis technique including various forms of data transformation. The modal parameters for damage assessment for the unexposed (unused) vs. exposed (used) specimen were based on two vibration parameters: natural frequencies and mode shapes. Finite Element models were built for each specimen type to understand its dynamic response. Linear elastic modal analysis was performed using eight nodes, three-dimensional isotropic solid elements. Conclusions based on our study indicate that dynamic characterization is a feasible NDE technique in studying structural properties of ceramic candle filters. It has been shown that the degradation of the filters due to long working hours (or

  11. Hot corrosion of ceramic-coating materials for industrial/utility gas turbines

    SciTech Connect

    Barkalow, R.H.

    1981-01-01

    Furnace hot corrosion tests of yttria-stabilized zirconia (YSZ) and other candidate ceramic coating materials were run under combinations of temperature, salt deposits, and gaseous environments know to cause severe hot corrosion of state-of-the-art metallic coatings for industrial/utility gas turbines. Specimens were free-standing ceramic coupons and ceramic-coated IN 792. X-ray fluorescence and diffraction data on free-standing YSZ coupons showed surface yttrium loss and cubic-to-monoclinic transformation as a result of exposure to liquid salt and SO/sub 3/. Greater destabilization was observed at the lower of two test temperatures (704 and 982/sup 0/C), and destabilization increased with increasing SO/sub 3/ pressure and V-containing salt deposits. The data suggest that hot corrosion of YSZ can occur by a type of acidic dissolution of Y/sub 2/O/sub 3/ from the ZrO/sub 2/ solid solution. In spite of the greater surface destabilization at 704/sup 0/C, the bond coat and substrate of YSZ-coated IN 792 were not attacked at 704/sup 0/C but severely corroded at 982/sup 0/C. These results show that degradation of ceramic-coated metallic components can be more strongly influenced by the porosity of the microstructure and fluidity of the liquid salt than by the chemical stability of the ceramic coating material in the reactive environment. Other ceramic materials (SiO/sub 2/, Si/sub 3/N/sub 4/, ZrSiO/sub 2/, and mullite), concurrently exposed to the same conditions which produced significant destabilization of YSZ, showed no evidence of reaction at 704/sup 0/C but noticeable corrosion at 982/sup 0/C. Also, the high temperature corrosion was greater in air than in SO/sub 3/-containing gases. These trends suggest that hot corrosion of the silicon-containing ceramics was basic in nature, and such materials have potential for good resistance to chemical decomposition under the acidic conditions characteristics of industrial/utility gas turbines.

  12. Hierarchical zeolites from class F coal fly ash

    NASA Astrophysics Data System (ADS)

    Chitta, Pallavi

    Fly ash, a coal combustion byproduct is classified as types class C and class F. Class C fly ash is traditionally recycled for concrete applications and Class F fly ash often disposed in landfills. Class F poses an environmental hazard due to disposal and leaching of heavy metals into ground water and is important to be recycled in order to mitigate the environmental challenges. A major recycling option is to reuse the fly ash as a low-cost raw material for the production of crystalline zeolites, which serve as catalysts, detergents and adsorbents in the chemical industry. Most of the prior literature of fly ash conversion to zeolites does not focus on creating high zeolite surface area zeolites specifically with hierarchical pore structure, which are very important properties in developing a heterogeneous catalyst for catalysis applications. This research work aids in the development of an economical process for the synthesis of high surface area hierarchical zeolites from class F coal fly ash. In this work, synthesis of zeolites from fly ash using classic hydrothermal treatment approach and fusion pretreatment approach were examined. The fusion pretreatment method led to higher extent of dissolution of silica from quartz and mullite phases, which in turn led to higher surface area and pore size of the zeolite. A qualitative kinetic model developed here attributes the difference in silica content to Si/Al ratio of the beginning fraction of fly ash. At near ambient crystallization temperatures and longer crystallization times, the zeolite formed is a hierarchical faujasite with high surface area of at least 360 m2/g. This work enables the large scale recycling of class F coal fly ash to produce zeolites and mitigate environmental concerns. Design of experiments was used to predict surface area and pore sizes of zeolites - thus obviating the need for intense experimentation. The hierarchical zeolite catalyst supports tested for CO2 conversion, yielded hydrocarbons

  13. Technogenic Magnetic Particles in Alkaline Dusts from Power and Cement Plants.

    PubMed

    Magiera, Tadeusz; Gołuchowska, Beata; Jabłońska, Mariola

    2013-01-01

    During this study, we investigated the mineralogical characterization of technogenic magnetic particles (TMPs) contained in alkaline industrial dust and fly ash emitted by coal burning power plants and cement plants. The reaction of tested dust samples varied between values of pH 8 and pH 12. Their magnetic properties were characterized by measurement of magnetic susceptibility (χ), frequency dependence of magnetic susceptibility (χ(fd)), and temperature dependence of magnetic susceptibility. Mineralogical and geochemical analyses included scanning electron microscopy with energy dispersive spectroscopy, microprobe analysis and X-ray diffraction. The TMPs in fly ash from hard coal combustion have the form of typical magnetic spherules with a smooth or corrugated surface as well as a skeletal morphology, composed of iron oxides (magnetite, maghemite, and magnesioferrite) that occurred in the form of incrustation on the surface of mullite, amorphous silica, or aluminosilicate particles. The TMPs observed in fly ash from lignite combustion have a similar morphological form but a different mineralogical composition. Instead of magnetite and magnesioferrite, maghemite and hematite with lower χ values were the prevailing magnetic minerals, which explains the much lower magnetic susceptibility of this kind of ash in comparison with the ash from hard coal combustion, and probably results from the lower temperature of lignite combustion. Morphology and mineralogical composition of TMPs in cement dust is more diverse. The magnetic fraction of cement dust occurs mostly in the form of angular and octahedral grains of a significantly finer granulation (<20 μm); however, spherules are also present. A very characteristic magnetic form for cement dust is calcium ferrite (CaFe(3)O(5)). The greatest impact on the magnetic susceptibility of cement dust results from iron-bearing additives (often waste materials from other branches of industry), which should be considered the

  14. Chemical and Mineralogical Characterization of Arsenic, Lead, Chromium, and Cadmium in a Metal-contaminated Histosol

    SciTech Connect

    Gao, X.; Schulze, D

    2010-01-01

    The chemical and mineralogical forms of As, Pb, Cr, and Cd were studied in a metal-contaminated organic soil (Histosol) that received runoff and seepage water from a site that was once occupied by a lead smelter. Soil samples were collected from different depth intervals during both wet and dry seasons and analyzed using bulk powder X-ray diffraction (XRD), synchrotron-based micro X-ray diffraction ({mu}-XRD), and micro X-ray fluorescence ({mu}-SXRF) spectroscopy. There was a clear pattern of mineral distribution with depth that indicated the presence of an intense redox gradient. The oxidized reddish brown surface layer (0-10 cm) was dominated by goethite ({alpha}-FeOOH) and poorly crystalline akaganeite ({beta}-FeOOH). Lead and arsenic were highly associated with these Fe oxides, possibly by forming inner-sphere surface complexes. Gypsum (CaSO{sub 4} {center_dot} 2H{sub 2}O) was abundant in the layer as well, particularly for samples collected during dry periods. Fe(II)-containing minerals, such as magnetite (Fe{sub 3}O{sub 4}) and siderite (FeCO{sub 3}), were identified in the intermediate layers (10-30 cm) where the reductive dissolution of Fe(III) oxides occurred. A number of high-temperature minerals, such as mullite (3Al{sub 2}O{sub 3} {center_dot} 2Si{sub 2}O), corundum ({alpha}-Al{sub 2}O{sub 3}), hematite ({alpha}-Fe{sub 2}O{sub 3}), and wustite (FeO) were identified in the subsurface and they probably formed as a result of a burning event. Several sulfide minerals were identified in the most reduced layers at depths > 30 cm. They included realgar (AsS), alacranite (As{sub 4}S{sub 4}), galena (PbS), and sphalerite (Zn, Fe{sup 2+})S, and a series of Fe sulfides, including greigite (Fe{sup 2+}Fe{sub 2}{sup 3+} S{sub 4}), pyrrhotite (Fe{sub 1-x}S), mackinawite (FeS), marcasite (FeS{sub 2}), and pyrite (FeS{sub 2}). Most of these minerals occurred as almost pure phases in sub-millimeter aggregates and appeared to be secondary phases that had precipitated from

  15. Synthesis and characterization of zeolites prepared from industrial fly ash.

    PubMed

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-09-01

    In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination. PMID:24838802

  16. Crystallochemical effects of heat treatment on Fe-dominant tourmalines from Dolní Bory (Czech Republic) and Vlachovo (Slovakia)

    NASA Astrophysics Data System (ADS)

    Bačík, P.; Ozdín, D.; Miglierini, M.; Kardošová, P.; Pentrák, M.; Haloda, J.

    2011-09-01

    Heat treatment was performed on selected Fe-dominant tourmalines to establish the nature of any change in optical properties. Two tourmaline samples from Dolní Bory, Czech Republic (TDB) and Vlachovo, Slovakia (TVL) were heated at 450, 700 and 900°C at 0.1 mPa and ambient oxidation conditions for 8 h. EMPA study shows that tourmaline from Vlachovo has schorlitic composition and tourmaline from Dolní Bory is alkali-depleted schorl to foitite. Although the black colour remained unchanged after heating at 450°C, it changed to brown at 700°C and reddish brown at 900°C. No significant changes of chemical composition were observed during heating. X-ray diffraction, infrared and Mössbauer study showed negligible oxidation of tourmaline heated at 450°C, but a significant change in iron valency state and deprotonization at 700°C. The oxidation of Fe is the main cause of tourmaline colour change, and the substitution vector for oxidation of Fe is Fe3+OFe{-1/2+}(OH)-1. The predicted deprotonization of OH was confirmed by infrared spectroscopy, which documented a decrease in OH groups in both samples, mainly at the V site. The oxidation of Fe is mostly significant in the Y site as documented on the compression of the Y-site octahedra and subsequent decrease in the a lattice parameter. This feature is consistent with lattice dimensions in the transition from schorl and foitite dimensions to those consistent with fluor-buergerite. The Z-site octahedra did not compressed and were not affected by heating-induced Fe oxidation, which indicates only negligible content of Z Fe2+ in original samples. After heating at 900°C, the tourmaline structure collapsed likely due to the thermally induced weakening of bonds in Y and Z octahedra, which results in amorphization of tourmaline. Subsequently, breakdown products including Fe-oxides and mullite replaced alkali-depleted amorphized tourmaline.

  17. Durability of Environmental Barrier Coatings in a Water Vapor/Oxygen Environment

    NASA Technical Reports Server (NTRS)

    Holchin, John E.

    2004-01-01

    Silicon carbide (Sic) and silicon nitride (Si3N4) show potential for application in the hot sections of advanced jet engines. The oxidation behavior of these materials has been studied in great detail. In a pure oxygen environment, a silica (SiO2) layer forms on the surface and provides protection from further oxidation. Initial oxidation is rapid, but slows as silica layer grows; this is known as parabolic oxidation. When exposed to model fuel-lean combustion applications (standard in jet engines), wherein the partial pressure of water vapor is approximately 0.5 atm., these materials exhibit different characteristics. In such an environment, the primary oxidant to form silica is water vapor. At the same time, water vapor reacts with the surface oxide to form gaseous silicon hydroxide (Si(OH)4). The simultaneous formation of both silica and Si(OH)4 -the latter which is lost to the atmosphere- the material continues to recede. Recession rates for uncoated Sic and Si3N4 are unacceptably high, for use in jet engines, - on the order of 1mm/4000h. External coatings have been developed that protect Si-based materials from water vapor attack. One such coating consists of a Ba(0.75)Sr(0.25)Al2Si2O8 (BSAS) topcoat, a mullite/BSAS intermediate layer and a Si bond coat. The key function of the topcoat is to protect the Si-base material from water vapor; therefore it must be fairly stable in water vapor (recession rate of about 1mm/40,000h) and remain crack free. Although BSAS is much more resistant to water vapor attack than pure silica, it exhibits a linear weight loss in 50% H2O - 50% O2 at 1500 C. The objective of my research is to determine the oxidation behavior of a number of alternate hot-pressed monolithic top coat candidates. Potential coatings were exposed at 1500 C to a 50% H2O - 50% O2 gas mixture flowing at 4.4 cm/s . These included rare- earth silicates, barium-strontium aluminosilicates. When weight changes were measured with a continuously recording

  18. Sulfate resistance of high calcium fly ash concrete

    NASA Astrophysics Data System (ADS)

    Dhole, Rajaram

    Sulfate attack is one of the mechanisms which can cause deterioration of concrete. In general, Class C fly ash mixtures are reported to provide poor sulfate resistance. Fly ashes, mainly those belonging to the Class C, were tested as per the ASTM C 1012 procedure to evaluate chemical sulfate resistance. Overall the Class C fly ashes showed poor resistance in the sulfate environment. Different strategies were used in this research work to improve the sulfate resistance of Class C fly ash mixes. The study revealed that some of the strategies such as use of low W/CM (water to cementing materials by mass ratio), silica fume or ultra fine fly ash, high volumes of fly ash and, ternary or quaternary mixes with suitable supplementary cementing materials, can successfully improve the sulfate resistance of the Class C fly ash mixes. Combined sulfate attack, involving physical and chemical action, was studied using sodium sulfate and calcium sulfate solutions. The specimens were subjected to wetting-drying cycles and temperature changes. These conditions were found to accelerate the rate of degradation of concrete placed in a sodium sulfate environment. W/CM was found to be the main governing factor in providing sulfate resistance to mixes. Calcium sulfate did not reveal damage as a result of mainly physical action. Characterization of the selected fly ashes was undertaken by using SEM, XRD and the Rietveld analysis techniques, to determine the relation between the composition of fly ashes and resistance to sulfate attack. The chemical composition of glass represented on the ternary diagram was the main factor which had a significant influence on the sulfate resistance of fly ash mixtures. Mixes prepared with fly ashes containing significant amounts of vulnerable crystalline phases offered poor sulfate resistance. Comparatively, fly ash mixes containing inert crystalline phases such as quartz, mullite and hematite offered good sulfate resistance. The analysis of hydrated lime

  19. AQUEOUS BIPHASE EXTRACTION FOR PROCESSING OF FINE COAL

    SciTech Connect

    K. Osseo-Asare

    2000-06-02

    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 of high-carbon fly ash with the aqueous biphase extraction process.

  20. Characterization and determination of 28 elements in fly ashes collected in a thermal power plant in Argentina using different instrumental techniques

    NASA Astrophysics Data System (ADS)

    Marrero, Julieta; Polla, Griselda; Jiménez Rebagliati, Raúl; Plá, Rita; Gómez, Darío; Smichowski, Patricia

    2007-02-01

    Different techniques were selected for comprehensive characterization of seven samples of fly ashes collected from the electrostatic precipitator of the San Nicolás thermal power plant (Buenos Aires, Argentina). Particle size was measured using laser based particle size analyzer. X-ray diffraction powder (XRD) analysis and scanning electron microscopy (SEM) were used to characterize the mineral phase present in the matrix consisting basically of aluminosilicates and large amounts of amorphous material. The predominant crystalline phases were mullite and quartz. Major and minors elements (Al, Ca, Cl, Fe, K, Mg, Na, S, Si and Ti) were detected by energy dispersive X-ray analysis (EDAX). Trace elements (As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Se, V and Zn) content was quantified by inductively coupled plasma optical emission spectrometry (ICP OES). Different acid mixtures and digestion procedures were compared for subsequent ICP OES measurements of the dissolved samples. The digestion procedures used were: i) a mixture of FH + HNO 3 + HClO 4 (open system digestion); ii) a mixture of FH + HNO 3 (MW-assisted digestion); iii) a mixture of HF and aqua regia (MW-assisted digestion). Instrumental neutron activation analysis (INAA) was employed for the determination of As, Ba, Co, Cr, Ce, Cs, Eu, Fe, Gd, Hf, La, Lu, Rb, Sb, Sc, Sm, Ta, Tb, Th, U and Yb. The validation of the procedure was performed by the analysis of two certified materials namely, i) NIST 1633b, coal fly ash and ii) GBW07105, rock. Mean elements content spanned from 41870 μg g - 1 for Fe to 1.14 μg g - 1 for Lu. The study showed that Fe (41870 μg g - 1 ) ≫ V (1137 μg g - 1 ) > Ni (269 μg g - 1 ) > Mn (169 μg g - 1 ) are the main components. An enrichment, with respect to crustal average, in many elements was observed especially for As, V and Sb that deserve particular interest from the environmental and human health point of view.

  1. Development of Microplasma Thruster

    NASA Astrophysics Data System (ADS)

    Takao, Yoshinori; Ono, Kouichi

    This paper proposes an electrothermal microplasma thruster using azimuthally symmetric microwave-excited plasmas, which consists of a microplasma source and a micronozzle. The microplasma source is made of a 10 mm long dielectric chamber of 2 mm in inner diameter covered with an electrically grounded metal, which produces high temperature plasmas at around atmospheric pressure. The micronozzle has a throat of 0.2 mm in diameter, which converts high thermal energy of plasmas into directional kinetic energy to produce the axial thrust. First, we have developed a numerical model for Ar microplasmas and micronozzle flows to estimate the thruster performance. The model consists of three modules: a volume-averaged global model, an electromagnetic model for microplasma sources, and a fluid model for micronozzle flows. Numerical results indicate that the microwave power absorbed in plasmas increases with microwave frequency f and relative permittivityɛd of the dielectric chamber, to achieve the plasma density in the range 1014-1016 cm-3. A certain combination of the frequency and permittivity significantly increases the power absorption. The micronozzle flow was found to be very lossy because of high viscosity in thick boundary layers, implying that shortening the nozzle length with increasing half-cone angles suppresses the effect of viscous loss and thus enhances the thrust performance. A thrust of 2.5-3.5 mN and a specific impulse of 130-180 s were obtained for a given microwave power range (Pt <10 W), which is applicable to a station-keeping maneuver for microspacecraft less than 10 kg. Moreover, we have developed a microwave-excited microplasma source, which has a dielectric chamber of 10 mm length and 1.5 mm in inner diameter, where off-the-shelf mullite (ɛd ≈ 6) and zirconia (ɛd ≈ 12-25) tubes are employed. Experiments were performed at f = 2 and 4 GHz, Pt < 10 W, an Ar flow rate of 50 sccm, and a microplasma pressure of 10 kPa, where optical emission

  2. Coarse fraction of soils from building rubble (WWII)

    NASA Astrophysics Data System (ADS)

    Mekiffer, Beate; Wessolek, Gerd; Scheytt, Traugott; Bussert, Robert; Nehls, Thomas

    2010-05-01

    oxides of Si (40 - 55%), Al (23-35%), Fe (4-17%), Ca (1-8%), Mg (0,8 - 4,8), K (1,5-4,5%), Na (0,1-3,5), Titane (0,5-1,3%) and S (0,1-2%). Most important minerals are Quarz, Mullite, Illite, Hematite and Magnetite, sometimes Carbonates and Sulphates.

  3. Magma-hydrothermal contact zone of the Stromboli volcano (Italy): evidence from buchite xenoliths

    NASA Astrophysics Data System (ADS)

    Renzulli, A.; Serri, G.; Tribaudino, M.; Santi, P.; Salvioli-Mariani, E.

    2003-04-01

    Large-sized xenoliths (up to 1.5 m) were sampled nearby the summit active craters of Stromboli (Aeolian Islands). The ejecta, erupted during recent eruptions, are spread within an area of ca. 50m2 and consist of fine-grained whitish to light-grey mottled rocks with heterogeneous vesicularity (3--50 vol.%). SEM-EDS and EMP analyses, XRD, TEM investigations and ICP-OES-MS bulk-rock geochemistry were carried out on representative samples. According to petrological and textural data the xenoliths are buchites, i.e. glassy hornfelses produced by high-grade contact metamorphism, up to partial melting. A highly porphyritic shoshonitic basalt generally covers the buchites, both as cm-sized coatings or as thicker spatters. The xenoliths are peraluminous (Al_2O_3 21.4--24.3 wt.%), with SiO_2 62.1--63.6 wt.% and are characterised by fine-grained cordierite (± indialite), plagioclase (An80-95), mullite, orthopyroxene (En74-83), pseudobrookite and rutile. These minerals locally replace, pseudomorphically, mm-sized crystals whose habitus is reminiscent of feldspar and pyroxene phenocrysts. In the xenoliths the glass has a wide range of silica compositions, from 61--66 wt.% (metaluminous) to 69--76 wt.% (peraluminous), going inward from the contact with the basalt coatings. At the xenolith-basalt contact a two mineral xenolith facies often occurs, consisting of a tridymite+clinopyroxene fine-grained glassy hornfels zone up to 5 cm. Cordierites have Mg values 82--91 and contain K_2O up to 1%. TEM and synchrotron powder diffraction examination on cordierites showed the presence of both crystals with fully achieved transformation to the orthorhombic state and euhedra having an hexagonal symmetry (indialites). The presence of different Al-Si ordering state in cordierite, from fully disordered indialite to partially ordered orthorhombic cordierite was observed. This may be due to high K_2O and/or fast cooling of the crystals that inhibited the transformation from hexagonal to

  4. Mechanism of adaptability for the nano-structured TiAlCrSiYN-based hard physical vapor deposition coatings under extreme frictional conditions

    NASA Astrophysics Data System (ADS)

    Fox-Rabinovich, G. S.; Endrino, J. L.; Aguirre, M. H.; Beake, B. D.; Veldhuis, S. C.; Kovalev, A. I.; Gershman, I. S.; Yamamoto, K.; Losset, Y.; Wainstein, D. L.; Rashkovskiy, A.

    2012-03-01

    Recently, a family of hard mono- and multilayer TiAlCrSiYN-based coatings have been introduced that exhibit adaptive behavior under extreme tribological conditions (in particular during dry ultrahigh speed machining of hardened tool steels). The major feature of these coatings is the formation of the tribo-films on the friction surface which possess high protective ability under operating temperatures of 1000 °C and above. These tribo-films are generated as a result of a self-organization process during friction. But the mechanism how these films affect adaptability of the hard coating is still an open question. The major mechanism proposed in this paper is associated with a strong gradient of temperatures within the layer of nano-scaled tribo-films. This trend was outlined by the performed thermodynamic analysis of friction phenomena combined with the developing of a numerical model of heat transfer within cutting zone based on the finite element method. The results of the theoretical studies show that the major physical-chemical processes during cutting are mostly concentrated within a layer of the tribo-films. This nano-tribological phenomenon produces beneficial heat distribution at the chip/tool interface which controls the tool life and wear behavior.Results of x-ray photoelectron spectroscopy studies indicate enhanced formation of protective sapphire- and mullite-like tribo-films on the friction surface of the multilayer TiAlCrSiYN/TiAlCrN coating. Comprehensive investigations of the structure and phase transformation within the coating layer under operation have been performed, using high resolution transmission electron microscopy, synchrotron radiation technique: x-ray absorption near-edge structure and XRD methods.The data obtained show that the tribo-films efficiently perform their thermal barrier functions preventing heat to penetrate into the body of coated cutting tool. Due to this the surface damaging process as well as non-beneficial phase

  5. Osumilite-(Mg): Validation as a mineral species and new data

    NASA Astrophysics Data System (ADS)

    Chukanov, N. V.; Pekov, I. V.; Rastsvetaeva, R. K.; Aksenov, S. M.; Belakovskiy, D. I.; Van, K. V.; Schüller, W.; Ternes, B.

    2013-12-01

    Osumilite-(Mg), the Mg-dominant analogue of osumilite, has been approved by the CNMNC IMA as a new mineral species. The holotype sample has been found at Bellerberg, Eifel volcanic area, Germany. Fluorophlogopite, sanidine, cordierite, mullite, sillimanite, topaz, pseudobrookite and hematite are associated minerals. Osumilite-(Mg) occurs as short prismatic or thick tabular hexagonal crystals reaching 0.5 × 1 mm in size in the cavities in basaltic volcanic glasses at their contact with thermally metamorphosed xenoliths of pelitic rocks. The mineral is brittle, with Mohs' hardness 6.5. Cleavage was not observed. Color is blue to brown. D meas = 2.59(1), D calc = 2.595 g/cm3. No bands corresponding to H2O and OH-groups are in the IR spectrum. Osumilite-(Mg) is uniaxial (+), ω = 1.539(2), ɛ = 1.547(2). The chemical composition (electron microprobe, average of 5 point analyses, wt %) is: 0.08 Na2O, 3.41 K2O, 0.04 CaO, 7.98 MgO, 0.28 MnO, 21.57 Al2O3, 3.59 Fe2O3, 62.33 SiO2, total 99.28. The empirical formula is: (K0.72Na0.03Ca0.01)(Mg1.97Mn0.04)[Al4.21Fe{0.45/3+}Si10.32]O30. The simplified formula is: KMg2Al3(Al2Si10)O10. The crystal structure was refined on a single crystal, R = 0.0294. Osumilite-(Mg) is hexagonal, space group P6/ mcc; a = 10.0959(1), c = 14.3282(2)Å, V = 1264.79(6) Å3, Z = 2. The strongest reflections in the X-ray powder diffraction pattern [ d, Å I %) ( hkl)] are: 7.21 (37) (002), 5.064 (85) (110), 4.137 (45) (112), 3.736 (43) (202), 3.234 (100) (211), 2.932 (42) (114), 2.767 (51) (204). A type specimen is deposited in the Fersman Mineralogical Museum, Russian Academy of Sciences, Moscow, registration number 4174/1.

  6. Peraluminous websterite and granulite xenoliths from the Chyulu Hills volcanic field, Kenya: Plagioclase-rich cumulates re-equilibrated at uppermost mantle and crustal conditions?

    NASA Astrophysics Data System (ADS)

    Ulianov, A.; Kalt, A.; Pettke, T.

    2004-12-01

    Basanites of the Chyulu Hills volcanic field, Kenya, contain a suite of meta-igneous peraluminous spinel-garnet olivine websterite, Mg-Al sapphirine-bearing and Ca-Al hibonite-bearing granulite xenoliths. The websterites are the most mafic and magnesian members of this sequence. The Mg-Al sapphirine-bearing granulites are more Si- and Al-rich and less magnesian. They consist of ortho- and clinopyroxene, corundum, spinel, sapphirine, sillimanite, plagioclase and garnet. The Ca-Al hibonite-bearing granulites are most enriched in Si and Al. They are dominated by clinopyroxene and plagioclase and may contain hibonite closely associated with spinel, mullite, sapphirine and sillimanite. Hibonite, which is very rare in terrestrial rocks, is the earliest mineral in the crystallization sequence. All rocks are poor in REE, HFSE and Cr and enriched in LILE and Ni. They follow a magmatic fractionation trend and form a cumulate sequence finally equilibrated in the range of uppermost mantle (websterites) and crustal (granulites) depths. The websterites could have formed by high-pressure metamorphism of low-pressure troctolite-like cumulates and appear similar to some websteritic lithologies from exhumed high-pressure ultramafic complexes (Kornprobst, 1990; Morishita et al., 2003). The final P-T conditions for most websterites correspond to 920-1000 C / 17-22 kbar, whereas the final equilibration in granulites occurred at ca. 600-740 C / <8 kbar, the pressure limit being defined by the stability field of sillimanite. The geodynamic interpretation of spatially close granulite terranes (Moeller et al., 1998) coupled with the petrological evidence suggest that the studied rocks were metamorphosed and may have formed in the environment of a Pan-African active continental margin. Moeller, A., Mezger, K., Schenk, V. (1998). Journal of Petrology 39, 749-783. Kornprobst, J., Piboule, M., Roden, M., Tabit, A. (1990). Journal of Petrology 31, 717-745. Morishita, T., Arai, S., Gervilla, F

  7. A review of physical, chemical, and biological properties of fly ash and effects on agricultural ecosystems.

    PubMed

    el-Mogazi, D; Lisk, D J; Weinstein, L H

    1988-08-01

    Fly ash is the solid material which is carried away from the power plant boiler in the flue gas during coal combustion. The properties of fly ash may vary considerably according to several factors such as the geographical origin of the source coal, conditions during combustion, and sampling position within the power plant. A typical aggregate of fly ash from the combustion of eastern U.S. coals consists of spherical particles embedded in an amorphous matrix. Most fly ash particles are in the silt-sized range of 2-50 microns. The three major mineralogical matrices identified in fly ash are glass, mullite-quartz, and magnetic spinel. The major elemental constituents of fly ash are Si, Al, Fe, Ca, C, Mg, K, Na, S, Ti, P, and Mn. Nearly all naturally occurring elements can be found in fly ash in trace quantities. Certain trace elements, including As, Mo, Se, Cd, and Zn, are primarily associated with particle surfaces. The solubility of fly ash has been extensively investigated. Results of these investigations are largely dependent on factors specific to the extraction procedure. The most abundant species in fly ash extracts are inorganic ions derived from Ca, Na, Mg, K, Fe, S, and C. Boron is much more soluble than other trace elements in fly ash. The forms of some elements in fly ash extracts have been determined, but the species of most trace elements remain unidentified. Long-term leaching studies predict that fly ash will lose substantial amounts of soluble salts over time, but simulation models predict that the loss of trace elements from fly ash deposits through leaching will be very slow. The constituents of coal fly ash include small amounts of radioisotopes which do not appear to be hazardous. A complex mixture of organic compounds is also associated with fly ash particles. The organic compounds identified in fly ash extracts include known mutagens and carcinogens. Better methods for the extraction of organic compounds from fly ash particles must be developed

  8. Chemical and ceramic methods toward safe storage of actinides using monazite. 1998 annual progress report

    SciTech Connect

    Morgan, P.E.D.; Boatner, L.A.

    1998-06-01

    'The use of ceramic monazite, (La,Ce)PO{sub 4}, for sequestering actinides, especially plutonium, and some other radioactive waste elements (rare earths e.g.) and thus isolating them from the environment has been championed by Lynn Boatner of ORNL. It may be used alone or, as it is compatible with many other minerals in nature, can be used in composite combinations. Natural monazite, which almost invariably contains Th and U, is often formed in hydrothermal pegmatites and is extremely water resistant--examples are known where the mineral has been washed out of rocks (becoming a placer mineral as on the beach sands of India, Australia, Brazil etc.) then reincorporated into new rocks with new crystal overgrowths and then washed out again--being 2.5--3 billion years old. During this demanding water treatment it has retained Th and U. Where very low levels of water attack have been seen (in more siliceous waters), the Th is tied up as new ThSiO{sub 4} and remains immobile. Lest it be thought that rare-earths are rare or expensive, this is not so. In fact, the less common lanthanides such as gadolinium, samarium, europium, and terbium, are necessarily extracted and much used by, e.g., the electronics industry, leaving La and Ce as not-sufficiently-used by-products. The recent development of large scale use of Nd in Nd-B-Fe magnets has further exaggerated this. Large deposits of the parent mineral bastnaesite are present in the USA and in China. (Mineral monazite itself is not preferred due to its thorium content.) In the last 5 years it has become apparent show that monazite (more specifically La-monazite) is an unrecognized/becoming-interesting ceramic material. PuPO4 itself has the monazite structure; the PO{sub 4} 3-unit strongly stabilizes actinides and rare earths in their trivalent state. Monazite melts without decomposition (in a closed system) at 2,074 C and, being compatible with common ceramic oxides such as alumina, mullite, zirconia and YAG, is useful in

  9. Jarosite characteristics and its utilisation potentials.

    PubMed

    Pappu, Asokan; Saxena, Mohini; Asolekar, Shyam R

    2006-04-15

    During metallic zinc extraction from zinc sulphide or sulphide ore, huge quantity of jarosite is being released universally as solid residues. The jarosite mainly contains iron, sulphur, zinc, calcium, lead, cadmium and aluminium. Jarosite released from such industrial process is complex and its quality and quantity make the task more complex for safe disposal. Apart from water contamination, jarosite already accumulated and its increasing annual production is a major source of pollution for surrounding environment including soil, vegetation and aquatic life and hence its disposal leads to major concern because of the stringent environmental protection regulations. An attempt was made to evaluate the characteristics of Indian jarosite with an objectives to understand its potentials for recycling and utilising as raw materials for developing value added products. Sand and Coal Combustion Residues (CCRs) was used as an admixture to attain good workability and detoxify the toxic substance in the jarosite. Result revealed that jarosite is silty clay loam in texture having 63.48% silt sized and 32.35% clay sized particles. The particle size of jarosite (D90=16.21+/-0.20 microm) is finer than the CCRs (D90=19.72+/-0.18 microm). The jarosite is nonuniform in structure and shape as compared to the CCRs having spherical, hollow shaped and some of them are cenosphere in nature. The major mineral phase of jarosite is Potassium Iron Sulphate Hydroxide {KFe3(SO4)2(OH)6}and Iron Sulphate Hydrate {2 Fe2O3SO3 x 5 H2O}. In CCRs the dominant phases are quartz {SiO2}, mullite {3 Al2O3 x 2 SiO2} and hematite {Fe2O3}. The high electrical conductivity of jarosite (13.26+/-0.437 dS/m) indicates that the presence of cations and anions are predominant over CCRs (0.498+/-0.007 dS/m). The major portion of jarosite consists of iron (23.66+/-0.18%), sulphur (12.23+/-0.2%) and zinc (8.243+/-0.075%). But CCRs main constituents are silicon (27.41+/-0.74%), aluminium (15.167+/-0.376%) and iron (4

  10. Mineralogy and the release of trace elements from slag from the Hegeler Zinc smelter, Illinois (USA)

    USGS Publications Warehouse

    Piatak, N.M.; Seal, R.R., II

    2010-01-01

    Slag from the former Hegeler Zn-smelting facility in Illinois (USA) is mainly composed of spinifex Ca-rich plagioclase, fine-grained dendritic or coarse-grained subhedral to anhedral clinopyroxenes, euhedral to subhedral spinels, spherical blebs of Fe sulfides, silicate glass, and less commonly fayalitic olivine. Mullite and quartz were also identified in one sample as representing remnants of the furnace lining. Secondary phases such as goethite, hematite and gypsum are significant in some samples and reflect surficial weathering of the dump piles or represent byproducts of roasting. A relatively rare Zn-rich material contains anhedral willemite, subhedral gahnite, massive zincite, hardystonite and a Zn sulfate (brianyoungite), among other phases, and likely represents the molten content of the smelting furnace before Zn extraction. The bulk major-element chemistry of most slag samples is dominated by SiO2, Al2O3, Fe2O3 and CaO. The bulk composition of the slag suggests a high viscosity of the melt and the mineralogy suggests a high silica content of the melt. Bulk slag trace-element chemistry shows that the dominant metal is Zn with >28.4 wt.% in the Zn-rich material and between 212 and 14,900 mg/kg in the other slags. The concentrations of other trace elements reach the following: 45 mg/kg As, 1170 mg/kg Ba, 191 mg/kg Cd, 242 mg/kg Co, 103 mg/kg Cr, 6360 mg/kg Cu, 107 mg/kg Ni, and 711 mg/kg Pb. Zinc, as the dominant metal in the slags, is likely the most environmentally significant metal in these samples; Cd, Cu, and Pb are also of concern and their concentrations exceed US Environmental Protection Agency preliminary remediation goals for residential soils. Spinel was found to be the dominant concentrator of Zn for samples containing significant Zn (>1 wt.%); the silicate glass also contained relatively high concentrations of Zn compared to other phases. Zinc partitioned into the silicates and oxides in these samples is generally more resistant to weathering

  11. Self-degradable Slag/Class F Fly Ash-Blend Cements

    SciTech Connect

    Sugama, T.; Warren, J.; Butcher, T.; Lance Brothers; Bour, D.

    2011-03-01

    temperature was controlled by the extent of thermal decomposition of CMC, demonstrating that CMC decomposed at higher temperature emitted more gaseous reactants. Hence, such large emission enhanced the evolution of in-situ exothermic heat. In contrast, the excessive formation of geopolymer phase due to more incorporation of Class F fly ash into this cementitious system affected its ability to self-degrade, reflecting that there was no self-degradation. The geopolymer was formed by hydrothermal reactions between sodium hydroxide from sodium silicate and mullite in Class F fly ash. Thus, the major reason why geopolymer-based cementitiuos sealers did not degrade after heated sealers came in contact with water was their lack of free sodium hydroxide.

  12. Natural weathering in dry disposed ash dump: Insight from chemical, mineralogical and geochemical analysis of fresh and unsaturated drilled cores.

    PubMed

    Akinyemi, S A; Akinlua, A; Gitari, W M; Khuse, N; Eze, P; Akinyeye, R O; Petrik, L F

    2012-07-15

    Some existing alternative applications of coal fly ash such as cement manufacturing; road construction; landfill; and concrete and waste stabilisation use fresh ash directly collected from coal-fired power generating stations. Thus, if the rate of usage continues, the demand for fresh ash for various applications will exceed supply and use of weathered dry disposed ash will become necessary alternative. As a result it's imperative to understand the chemistry and pH behaviour of some metals inherent in dry disposed fly ash. The bulk chemical composition as determined by XRF analysis showed that SiO2, Al2O3 and Fe2O3 were the major oxides in fresh ash and unsaturated weathered ashes. The unsaturated weathered ashes are relatively depleted in CaO, Fe2O3, TiO2, SiO2, Na2O and P2O5 due to dissolution and hydrolysis caused by chemical interaction with ingressing CO2 from the atmosphere and infiltrating rain water. Observed accumulations of Fe2O3, TiO2, CaO, K2O, Na2O and SO3 and Zn, Zr, Sr, Pb, Ni, Cr and Co in the lower layers indicate progressive downward movement through the ash dump though at a slow rate. The bulk mineralogy of unsaturated weathered dry disposed ash, as determined by XRD analysis, revealed quartz and mullite as the major crystalline phases; while anorthite, hematite, enstatite, lime, calcite, and mica were present as minor mineral phases. Pore water chemistry revealed a low concentration of readily soluble metals in unsaturated weathered ashes in comparison with fresh ash, which shows high leachability. This suggests that over time the precipitation of transient minor secondary mineral phases; such as calcite and mica might retard residual metal release from unsaturated weathered ash. Chloride and sulphate species of the water soluble extracts of weathered ash are at equilibrium with Na+ and K+; these demonstrate progressive leaching over time and become supersaturated at the base of unsaturated weathered ash. This suggests that the ash dump does not

  13. Improved Materials for High-Temperature Black Liquor Gasification

    SciTech Connect

    Keiser, J.R.; Hemrick, J.G.; Gorog, J.P.; Leary, R.

    2006-06-29

    The laboratory immersion test system built and operated at ORNL was found to successfully screen samples from numerous refractory suppliers, including both commercially available and experimental materials. This system was found to provide an accurate prediction of how these materials would perform in the actual gasifier environment. Test materials included mullites, alumino-silicate bricks, fusion-cast aluminas, alumina-based and chrome-containing mortars, phosphate-bonded mortars, coated samples provided under an MPLUS-funded project, bonded spinels, different fusion-cast magnesia-alumina spinels with magnesia content ranging from 2.5% to about 60%, high-MgO castable and brick materials, spinel castables, and alkali-aluminate materials. This testing identified several candidate material systems that perform well in the New Bern gasifier. Fusion-cast aluminas were found to survive for nearly one year, and magnesia-alumina spinels have operated successfully for 18 months and are expected to survive for two years. Alkali-aluminates and high-MgO-content materials have also been identified for backup lining applications. No other material with a similar structure and chemical composition to that of the fusion-cast magnesium-aluminum spinel brick currently being used for the hot-face lining is commercially available. Other materials used for this application have been found to have inferior service lives, as previously discussed. Further, over 100 laboratory immersion tests have been performed on other materials (both commercial and experimental), but none to date has performed as well as the material currently being used for the hot-face lining. Operating experience accumulated with the high-temperature gasifier at New Bern, North Carolina, has confirmed that the molten alkali salts degrade many types of refractories. Fusion-cast alumina materials were shown to provide a great improvement in lifetime over materials used previously. Further improvement was realized

  14. OPTIMIZATION OF ADVANCED FILTER SYSTEMS

    SciTech Connect

    R.A. Newby; M.A. Alvin; G.J. Bruck; T.E. Lippert; E.E. Smeltzer; M.E. Stampahar

    2002-06-30

    through cold flow and high-temperature testing. The Blasch, mullite-bonded alumina sheet filter element is the only candidate currently approaching qualification for demonstration, although this oxide-based, monolithic sheet filter element may be restricted to operating temperatures of 538 C (1000 F) or less. Many other types of ceramic and intermetallic sheet filter elements could be fabricated. The estimated capital cost of the sheet filter system is comparable to the capital cost of the standard candle filter system, although this cost estimate is very uncertain because the commercial price of sheet filter element manufacturing has not been established. The development of the sheet filter system could result in a higher reliability and availability than the standard candle filter system, but not as high as that of the inverted candle filter system. The sheet filter system has not reached the same level of development as the inverted candle filter system, and it will require more design development, filter element fabrication development, small-scale testing and evaluation before larger-scale testing could be recommended.

  15. Phase transitions of aqueous atmospheric particles: Crystallization of ammonium salts promoted by oxide mineral constituents

    NASA Astrophysics Data System (ADS)

    Han, Jeong-Ho

    2001-09-01

    developed and characterized to generate the internally mixed particles consisting of the soluble and insoluble components. Spray pyrolysis was employed in order to have the control of the size and crystalline phase of the insoluble constituents and combined with the in-line tube furnace to manipulate the coated particles (i.e., internally mixed particles). Employing the stable and well- characterized generation source for the coated particles, the roles of the insoluble constituents (i.e., metal oxides) in heterogeneous nucleation were investigated extensively in terms of their size (i.e., surface area) and crystalline structure as nucleation templates. Ammonium sulfate and ammonium nitrate were selected as the soluble components because they are the most common atmospheric aerosol particles from anthropogenic activities. As for insoluble components, corundum (α-Al2O3), hematite (α- Al2O3), mullite (Al6Si 2O13), silica (am-SiO2), rutile (TiO2), ZrO2, and δ-Al2O3 were selected with the reasoning that some of them represent the abundant crustal components in the atmosphere and that others have interesting chemical compositions and/or crystalline structures.

  16. Integrated acid mine drainage management using fly ash.

    PubMed

    Vadapalli, Viswanath R K; Gitari, Mugera W; Petrik, Leslie F; Etchebers, Olivier; Ellendt, Annabelle

    2012-01-01

    Fly Ash (FA) from a power station in South Africa was investigated to neutralise and remove contaminants from Acid Mine Drainage (AMD). After this primary treatment the insoluble FA residue namely solid residue (SR) was investigated as a suitable mine backfill material by means of strength testing. Moreover, SR was used to synthesise zeolite-P using a two-step synthesis procedure. Furthermore, the zeolite-P was investigated to polish process water from the primary FA-AMD reaction. The main objective of this series of investigations is to achieve zero waste and to propose an integrated AMD management using FA. Fly Ash was mixed with AMD at various predetermined FA-AMD ratios until the mixtures achieved circumneutral pH or higher. The supernatants were then analyzed using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Ion Chromatography (IC) for cations and anions respectively. The physical strength testing of SR was carried out by mixing it with 3% Ordinary Portland Cement (OPC) and curing for 410 days. Synthesis of zeolite-P using SR was carried out by two step synthesis procedure: ageing for 24 hours followed by a mild hydrothermal synthesis at 100°C for 4 days. The polishing of process water from primary AMD treatment using FA was ascertained by mixing the process water with zeolite at a liquid to solid ratio of 100:1 for 1 hour. The results indicated that FA can be successfully used to ameliorate AMD. High removal of major AMD contaminants Fe, Al, Mg, Mn and sulphate was achieved with the ash treatment and trace elements such as Zn, Ni, Cu and Pb were also removed by the FA. Strength testing over 410 days indicated that the material gained strength over the testing period. The maximum unconfined compressive strength and elastic modulus was observed to be approximately 0.3 MPa and 150 Mpa respectively. The X-ray diffraction (XRD) analysis of the synthesized product indicated that SR was successfully converted into zeolite-P with some mullite phase

  17. Development of Cost-Effective Low-Permeability Ceramic and Refractory Components for Aluminum Melting and Casting

    SciTech Connect

    Kadolkar, Puja; Ott, Ronald D

    2006-02-01

    A recent review by the U.S. Advanced Ceramics Association, the Aluminum Association, and the U.S. Department of Energy's Office of Industrial Technologies (DOE/OIT) described the status of advanced ceramics for aluminum processing, including monolithics, composites, and coatings. The report observed that monolithic ceramics (particularly oxides) have attractive properties such as resistance to heat, corrosion, thermal shock, abrasion, and erosion [1]. However, even after the developments of the past 25 years, there are two key barriers to commercialization: reliability and cost-effectiveness. Industry research is therefore focused on eliminating these barriers. Ceramic coatings have likewise undergone significant development and a variety of processes have been demonstrated for applying coatings to substrates. Some processes, such as thermal barrier coatings for gas turbine engines, exhibit sufficient reliability and service life for routine commercial use. Worldwide, aluminum melting and molten metal handling consumes about 506,000 tons of refractory materials annually. Refractory compositions for handling molten aluminum are generally based on dense fused cast silica or mullite. The microstructural texture is extremely important because an interlocking mass of coarser grains must be bonded together by smaller grains in order to achieve adequate strength. At the same time, well-distributed microscopic pores and cracks are needed to deflect cracks and prevent spalling and thermal shock damage [2]. The focus of this project was to develop and validate new classes of cost-effective, low-permeability ceramic and refractory components for handling molten aluminum in both smelting and casting environments. The primary goal was to develop improved coatings and functionally graded materials that will possess superior combinations of properties, including resistance to thermal shock, erosion, corrosion, and wetting. When these materials are successfully deployed in

  18. Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

    NASA Technical Reports Server (NTRS)

    McDaniels, Steven J.

    2004-01-01

    unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the

  19. Radioactive Demonstration Of Mineralized Waste Forms Made From Hanford Low Activity Waste (Tank Farm Blend) By Fluidized Bed Steam Reformation (FBSR)

    SciTech Connect

    Jantzen, C. M.; Crawford, C. L.; Bannochie, C. J.; Burket, P. R.; Cozzi, A. D.; Daniel, W. E.; Hall, H. K.; Miller, D. H.; Missimer, D. M.; Nash, C. A.; Williams, M. F.

    2013-08-01

    -radioactive testing. The granular ESTD and BSR products (radioactive and non-radioactive) were analyzed for total constituents and durability tested as a granular waste form. A subset of the granular material was stabilized in a clay based geopolymer matrix at 42% and 65% FBSR loadings and durability tested as a monolith waste form. The 65 wt% FBSR loaded monolith made with clay (radioactive) was more durable than the 67-68 wt% FBSR loaded monoliths made from fly ash (non-radioactive) based on short term PCT testing. Long term, 90 to 107 day, ASTM C1308 testing (similar to ANSI/ANS 16.1 testing) was only performed on two fly ash geopolymer monoliths at 67-68 wt% FBSR loading and three clay geopolymer monoliths at 42 wt% FBSR loading. More clay geopolymers need to be made and tested at longer times at higher FBSR loadings for comparison to the fly ash monoliths. Monoliths made with metakaolin (heat treated) clay are of a more constant composition and are very reactive as the heat treated clay is amorphous and alkali activated. The monoliths made with fly ash are subject to the inherent compositional variation found in fly ash as it is a waste product from burning coal and it contains unreactive components such as mullite. However, both the fly ash and the clay based monoliths perform well in long term ASTM C1308 testing.