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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. 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.

  10. 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.

  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. 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.

  5. 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.

  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 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.

  19. 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.

  20. 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.

  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. 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.

  15. 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.

  16. 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.

  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. 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.

  20. 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.

  1. 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

  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. 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.

  4. 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.

  5. 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.

  6. 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.

  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. 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

  11. 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.

  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. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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

  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. 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

  2. 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

  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. 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.

  16. 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.

  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. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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

  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. 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.

  7. 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.

  8. 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.

  9. 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

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  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. 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.

  4. 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.

  5. 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.

  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.; 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  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. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. 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.

  11. 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

  12. 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

  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. 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

  16. 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.

  17. 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

  18. 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

  19. 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.

  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. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  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. 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

  15. 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.

  16. 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.

  17. 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.

  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. 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

  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. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.