Reaction-sintered porous mineral-based mullite ceramic membrane supports made from recycled materials.

PubMed

Dong, Yingchao; Zhou, Jian-Er; Lin, Bin; Wang, Yongqing; Wang, Songlin; Miao, Lifeng; Lang, Ying; Liu, Xingqin; Meng, Guangyao

2009-12-15

Bulk porous mullite supports for ceramic membranes were prepared directly using a mixture of industrial waste fly ash and bauxite by dry-pressing, followed by sintering between 1200 and 1550 degrees C. The effects of sintering temperature on the phase composition and shrinkage percent of porous mullite were studied. The XRD results indicate that secondary mullitization reaction took place above 1200 degrees C, and completed at 1450 degrees C. During sintering, the mixture samples first shrunk, then expanded abnormally between 1326 and 1477 degrees C, and finally shrunk again above 1477 degrees C. This unique volume self-expansion is ascribed to the secondary mullitization reaction between bauxite and fly ash. More especially, the micro-structural variations induced by this self-expansion sintering were verified by SEM, porosity, pore size distribution and nitrogen gas permeation flux. During self-expansion sintering, with increasing temperature, an abnormal increase in both open porosity and pore size is observed, which also results in the increase of nitrogen gas flux. The mineral-based mullite supports with increased open porosity were obtained. Furthermore, the sintered porous mullite membrane supports were characterized in terms of thermal expansion co-efficient and mechanical strength.

Characterization of Mullite-Zirconia Composite Processed by Non-Transferred and Transferred Arc Plasma

NASA Astrophysics Data System (ADS)

Yugeswaran, S.; Selvarajan, V.; Lusvarghi, L.; I. Y. Tok, A.; D. Siva Rama, Krishna

2009-04-01

The arc plasma melting technique is a simple method to synthesize high temperature reaction composites. In this study, mullite-zirconia composite was synthesized by transferred and non-transferred arc plasma melting, and the results were compared. A mixture of alumina and zircon powders with a mole ratio of 3: 2 were ball milled for four hours and melted for two minutes in the transferred and non-transferred mode of plasma arcs. Argon and air were used as plasma forming gases. The phase and microstructural formation of melted samples were investigated by X-ray diffraction (XRD) and scanning electron microscope (SEM). The microstructure of the composites was found to be affected by the mode of melting. In transferred arc melting, zirconia flowers with uniform lines along with mullite whiskers were obtained. In the case of non-transferred arc plasma melting, mullite whiskers along with star shape zirconia were formed. Differential thermal analysis (DTA) of the synthesized mullite-zirconia composites provided a deeper understanding of the mechanisms of mullite formation during the two different processes.

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of heating parameters on sintering behaviors and properties of mullite whisker frameworks

NASA Astrophysics Data System (ADS)

Zhang, Y. M.; Zeng, D. J.; Wang, B.; Yang, J. F.

2018-04-01

Mullite whisker frameworks were fabricated by vapor-solid reaction with SiO2, Al2O3 and AlF3 powders as the whisker forming agent at high temperatures. The effects of heating temperature and soaking time on the weight loss, liner shrinkage, porosity, microstructure and compressive strength were investigated. The results showed that with the increasing of the sintering temperature and soaking time, the weight loss and liner shrinkage of the samples increased and the porosities decreased due to the accelerated vapor-solid reaction, resulting in strong bonding and grain growth of the mullite frameworks. The compressive strength of the samples increased with increasing the sintering temperature from 1500 to 1650 °C, and decreased with the soaking time extended to more than 5 h for 1500 °C and 2 h for 1650 °C. A maximum compressive strength of 142 MPa at a porosity of 62.3% was obtained for the mullite whisker framework heated at 1500 °C for 5 h. The enhanced strength was attributed to the strong bonding strength and fine mullite grains resulting from a relative lower heating temperature and a modest soaking time.

Mullite and Mullite/ZrO2-7wt.%Y2O3 Powders for Thermal Spraying of Environmental Barrier Coatings

NASA Astrophysics Data System (ADS)

Garcia, E.; Mesquita-Guimarães, J.; Miranzo, P.; Osendi, M. I.; Wang, Y.; Lima, R. S.; Moreau, C.

2010-01-01

Mullite and mullite/ZrO2-7wt.%Y2O3 coatings could be thought among the main protective layers for environment barrier coatings (EBCs) to protect Si-based substrates in future gas turbine engines. Considering that feedstock of the compound powder is not commercially available, two powder processing routes Spray Drying (SD) and Flame Spheroidization (FS) were implemented for both types of powders. For each method the particle size, the morphology, and microstructure of the powder particles was determined. In addition, the effect of the heat treatment on the powder crystallinity and microstructure of FS powders was also investigated. To evaluate their suitability as feedstock materials, the powders were plasma sprayed and their in-flight particle characteristics monitored for coatings production. The powder morphology was correlated to the in-flight particle characteristics and splat morphology to gain insight about into the influence of powder characteristics on the coating formation.

Phase Transformation of Andalusite-Mullite and Its Roles in the Microstructure and Sinterability of Refractory Ceramic

NASA Astrophysics Data System (ADS)

Li, Bowen; He, Mengsheng; Wang, Huaguang

2017-07-01

Andalusite has been realized as a special mineral for the production of refractory ceramics due to its unique property to automatically decompose into mullite and silica during heating at high temperature. The phase transformation from andalusite to mullite plays a critical role for the effective applications of andalusite. This study investigated the microstructural characteristics and sinterability of andalusite powder during high-temperature decomposition. The andalusite powder was bonded with kaolin and prepared as a cylinder green body at 20 MPa; it was then fired at 1423 K to 1723 K (1150 °C to 1450 °C). The microstructures and mechanical strengths of the sintered ceramics were studied by the compressive test, X-ray diffraction, and scanning electron microscopy. The results showed that newly born mullite appeared as rodlike microcrystals and dispersed around the initial andalusite. At 1423 K (1150 °C), the mullitization of andalusite was started, but the complete mullitization was not found until firing at 1723 K (1450 °C). The compressive strength of the ceramics increased from 93.7 to 294.6 MPa while increasing the fire temperature from 1423 K to 1723 K (1150 °C to 1450 °C). Meanwhile, the bulk density of the ceramics was only slightly changed from 2.15 to 2.19 g/cm3.

Feasible Recycling of Industrial Waste Coal Gangue for Preparation of Mullite Based Ceramic Proppant

NASA Astrophysics Data System (ADS)

Li, Guomin; Ma, Haiqiang; Tian, Yuming; Wang, Kaiyue; Zhou, Yi; Wu, Yaqiao; Zou, Xinwei; Hao, Jianying; Bai, Pinbo

2017-09-01

Industrial waste coal gangue was successfully utilized to prepare the mullite-based ceramic proppants. The experiments involved the pelletizing technology of proppant through intensive mixer and following the sintering process under different temperatures. The crystalline phase, microstructure, density and breakage ratio of the proppants were investigated. The results showed that with the increasing of sintering temperature, the crystalline phases were transformed to rod-like mullite, which formed the cross-linked structure, improving the densification of proppants. Consequently, the breakage ratio under the closure pressure of 35 MPa exhibited declining trend and reached the minimum value of 6.8% at 1450 °C. Owing to the easy preparation, feasible design, low cost and moderate breakage ratio, the mullite-based ceramic proppant prepared by coal gangue and bauxite is promising candidate for fracturing proppants in future applications.

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.

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.

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.

Effects of in situ synthesized mullite whisker on mechanical properties of Al2O3-SiC composite by microwave sintering

NASA Astrophysics Data System (ADS)

Dang, Xudan; Wei, Meng; Fan, Bingbing; Guan, Keke; Zhang, Rui; Long, Weimin; Zhang, Hongsong

2017-06-01

In situ synthesis of mullite whisker was introduced to Al2O3-SiC composite by microwave sintering. The effects of sintering parameters (sintering temperature, holding time and SiC particle size) on thermal shock resistance of Al2O3-SiC composite were also studied in this paper. Original SiC particles coated with SiO2 by a sol-gel method were reacted with Al2O3 particles, resulting in the in situ growth of mullite. The phase composition was identified by x-ray diffraction (XRD). The bridging of mullite whisker between Al2O3 and SiC particles was observed by scanning electron microscopy (SEM) analysis. The thermal shock resistance of samples was investigated through the combination of water quenching and three-point bending methods. The results show that the thermal shock resistance of Al2O3-SiC composite with mullite whisker reinforced remarkably, indicating better mechanical properties than the Al2O3-SiC composite without mullite whisker. Finally, the optimum process parameters (the sintering temperature of 1500 °C, the holding time of 30 min, and the SiC particle size of 5 µm) for toughening Al2O3-SiC composite by in situ synthesized mullite whisker were obtained.

Mullite ceramic membranes for industrial oily wastewater treatment: experimental and neural network modeling.

PubMed

Shokrkar, H; Salahi, A; Kasiri, N; Mohammadi, T

2011-01-01

In this paper, results of an experimental and modeling of separation of oil from industrial oily wastewaters (desalter unit effluent of Seraje, Ghom gas wells, Iran) with mullite ceramic membranes are presented. Mullite microfiltration symmetric membranes were synthesized from kaolin clay and alpha-alumina powder. The results show that the mullite ceramic membrane has a high total organic carbon and chemical oxygen demand rejection (94 and 89%, respectively), a low fouling resistance (30%) and a high final permeation flux (75 L/m2 h). Also, an artificial neural network, a predictive tool for tracking the inputs and outputs of a non-linear problem, is used to model the permeation flux decline during microfiltration of oily wastewater. The aim was to predict the permeation flux as a function of feed temperature, trans-membrane pressure, cross-flow velocity, oil concentration and filtration time, using a feed-forward neural network. Finally the structure of hidden layers and nodes in each layer with minimum error were reported leading to a 4-15 structure which demonstrated good agreement with the experimental measurements with an average error of less than 2%.

X-ray shielding behaviour of kaolin derived mullite-barites ceramic

NASA Astrophysics Data System (ADS)

Ripin, A.; Mohamed, F.; Choo, T. F.; Yusof, M. R.; Hashim, S.; Ghoshal, S. K.

2018-03-01

Mullite-barite ceramic (MBC) is an emergent material for effective shielding of redundant ionizing radiation exposure. The composition dependent mechanical, thermal, and microstructure properties of MBC that makes MBC a high performing novel radiation shielding candidate remained unexplored. This paper examines the possibility of exploiting Malaysian kaolin (AKIM-35) and barite (BaSO4) derived ceramic (MBC) system for X-ray shielding operation. Using conventional pressing and sintering method six ceramic samples are prepared by mixing AKIM-35 with barite at varying contents (0, 10, 20, 30, 40 and 50 wt%). Synthesized pressed mixtures are calcined at 400 °C for 30 min and then sintered to 1300 °C for 120 min at a heating rate of 10 °C/min. Sintered samples are characterized via X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), lead equivalent (LE), uniformity and dose reduction analyses. XRD pattern of prepared ceramics revealed the presence of monoclinic barium alumino-silicate (BAS) and orthorhombic mullite as major shielding phases together with other minor phase of barite and hexagonal quartz (SiO2) structures. Furthermore, FESEM images of ceramics (between 0 and 30 wt%) displayed the existence of compacted monoclinic plate of BAS and acicular mullite morphology (ceramics at 40 and 50 wt%). Radiation tests displayed the capacity of ceramics (at 0 and 10 wt%) to shield the X-ray radiation emanated at tube potential range of 50-120 kV. The highest radiation attenuation is ascertained at 70 kV where the dose is reduced remarkably between 99.11% and 97.42%. Ceramics at 0 and 10 wt% demonstrated the highest lead (Pb) equivalent thickness (LE) of 0.44 mm and 0.34 mm, respectively. It is established that such MBC may contribute towards the development of shielding material against ionizing radiation in diagnostic radiology (X-ray) dose range.

Saturation-resolved-fluorescence spectroscopy of Cr3+:mullite glass ceramic

NASA Astrophysics Data System (ADS)

Liu, Huimin; Knutson, Robert; Yen, W. M.

1990-01-01

We present a saturation-based technique designed to isolate and uncouple individual components of inhomogeneously broadened spectra that are simultaneously coupled to each other through spectral overlap and energy-transfer interactions. We have termed the technique saturation-resolved-fluorescence spectroscopy; we demonstrate its usefulness in deconvoluting the complex spectra of Cr3+:mullite glass ceramic.

Investigation of ZrO/sub 2//mullite solid solution by energy dispersive X-ray spectroscopy and electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinger, T.R.; Krishnam, K.M.; Moya, J.S.

1984-10-01

A mullite/15 vol.%ZrO/sub 2/ composite was analyzed using the techniques of microdiffraction and energy dispersive X-ray spectroscopy (EDXS). The EDXS results indicate that there is a significantly high solid solubility of mullite in zirconia and zirconia in mullite; microdiffraction results suggest that ordering occurs in the ZrO/sub 2/(ss) phase based on the presence of forbidden reflections for the P 2/sub 1//c space group of monoclinic zirconia. The presence of a secondary phase at the grain boundaries, either amorphous or crystalline, has not been generally detected throughout the bulk. The results provide experimental evidence for the hypothesis of Moya and Osendimore » that the increased toughness and flexural strength of these composites are related to solid solution effects rather than to transformation or microcrack toughening mechanisms.« less

Transmission electron microscopy observations on phase transformations during aluminium/mullite composites formation by gas pressure infiltration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pawlyta, M., E-mail: miroslawa.pawlyta@polsl.pl; Tomiczek, B.; Dobrzański, L.A.

The porous ceramic preforms were manufactured using the powder metallurgy technique. First, the start-up material (halloysite with the addition of carbon fibres as the pore-forming agent) was slowly heated to 800 °C and then sintered at 1300 °C. Degradation of the carbon fibres enabled the open canals to form. At the end of the sintering process, the porous ceramic material consisting mainly of two phases (mullite and cristobalite) was formed, without any residual carbon content. During infiltration, the liquid metal filled the empty spaces (pores) effectively and formed the three-dimensional network of metal in the ceramic. The cristobalite was almostmore » entirely decomposed. In the areas of its previous occurrence, there are new pores, only in the ceramic grains. The mullite, which was formed from halloysite during annealing, crystallized in the Pbam orthorhombic space group, with the (3Al{sub 2}O{sub 3}·2SiO{sub 2}) stoichiometric composition. The mullite structure does not change during the infiltration. The composite components are tightly connected. A transition zone between the ceramics and the metal, having the thickness of about 200 nm, was formed. The nanocrystalline zone, identified as γ-Al{sub 2}O{sub 3}, was formed by diffusing the product of the cristobalite decomposition into the aluminium alloy matrix. There is an additional, new phase, identified as (Mg,Si)Al{sub 2}O{sub 4} in the outer parts of the transition zone. - Highlights: • Phase changes after the infiltration of aluminium into porous mullite preforms were observed by TEM. • TEM observations confirm that during infiltration cristobalite was decomposed and the structure of mullite did not change. • Between the ceramic and the metal, a transition zone comprising a layer of γ-Al{sub 2}O{sub 3} and (Mg,Si)Al{sub 2}O{sub 4} was formed.« less

Salt-melt synthesis of B2O3, P2O5 and V2O5 modified high-alumina mullite nanocomposites with promising photoluminescence properties

NASA Astrophysics Data System (ADS)

Kool, Arpan; Thakur, Pradip; Bagchi, Biswajoy; Hoque, Nur Amin; Banerjee, Somtirtha; Das, Sukhen

2017-10-01

High-alumina mullite (Al4.8Si1.2O9.6) nanowhiskers have been prepared by mechano-chemical activation of Al2(SO4)3-Na2SO4 molten salt mixture in the presence of B2O3, P2O5 and V2O5 as additives. Thermal evolution of the precursors has been studied by differential thermal analyzer and thermogravimetric analyzer (DTA-TG). The effect of additives on the phase formation and morphology of mullite is investigated using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and field emission scanning electron microscope (FESEM). Mullite whiskers with submicron sized length and diameter in the nanoscale range were obtained after calcining at 1000 °C. These nanowhiskers decomposed when sintered at 1400 °C with consequent formation of dense alumina platelets. Owing to formation of defect related structures of mullite, UV photoluminescence peaks for mullite reflected at 285, 298, 310, 325, 347, 362 and 379 nm while visible photoluminescence peaks appeared at 407, 424, 436 and 460 nm.

Wetting of single crystal mullite by borosilicate and yttrium-aluminosilicate glasses and wetting phenomena of steels containing aluminum and titanium

NASA Astrophysics Data System (ADS)

Eldred, Benjamin Todd

This dissertation consists of two major sections. The first section concerns the wetting of single crystal mullite by borosilicate and yttrium-aluminosilicate glasses. The borosilicate glass showed poor wetting and interacted only moderately with the substrate. The yttrium-aluminosilicate glass interacted strongly with mullite and showed very good wetting. Balanced chemical equations between each glass and mullite were derived from EDS data. Wetting was found to be dependent on the crystallographic orientation of the substrate, in agreement with previous studies of the surface energy of mullite. The second section concerns the wetting phenomena of steels containing aluminum and titanium. A modified sessile drop technique was used to investigate the wetting of steels containing aluminum and/or titanium as a function of furnace atmosphere. It was found that the steel chemistry and furnace atmosphere had little effect on wetting except in the case of a particular ultra-low carbon steel containing both aluminum and titanium. This steel was found to show significantly lower contact angles than any other steel tested when it was in an atmosphere of pure hydrogen. As nitrogen was added to the atmosphere, the contact angle increased monotonically and irreversibly. The interaction between aluminum, titanium, and nitrogen is explained in terms of first-order interaction coefficients available in thermodynamic literature.

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.

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.

A study on the phytotoxicity of nano mullite and metal-amended nano mullite on mung bean plants.

PubMed

Dey, Anindita; Bagchi, Biswajoy; Das, Sukhen; Basu, Ruma; Nandy, Papiya

2011-06-01

The presence of engineered nanoparticles is continuously increasing in our environment and causing potential risks to the ecosystem. Researchers from various fields report many articles on the effects of different nanoparticles on plants, animals and microorganisms. Here we have studied for the first time the effect of nano mullite (NMu) and their metal- amended derivatives on the growth of mung bean plants. Results shows that the metal- amended NMu exerts adverse effects on the growth and biomass production of plants compared to NMu. For toxicity studies, we measured the germination index and relative root elongation, while leakage of electrolytes and root oxidizability were measured to study the effect of NMu on mung bean seeds and seedling tissues. Translocation and accumulation of NMu within different parts of the plant body were proved by elemental analysis of dried plant samples.

Synthesis of mullite (3Al2O32SiO2) from local kaolin for radiation shielding

NASA Astrophysics Data System (ADS)

Ripin, Azuhar; Mohamed, Faizal; Aman, Asyraf

2018-04-01

Raw kaolin from Kota Tinggi, Johor was used in this study to produce ceramic mullite (3Al2O22SiO2) for radiation shielding materials. In this work, an attempt was made to study the potential of local minerals to be used as a shielding barrier for diagnostic radiology radiation facilities in hospitals and medical centers throughout Malaysia. The conventional ceramic processing route was employed in the study using different pressing strength and sintering time. The obtained samples were characterized using X-ray diffractometer (XRD) for phase identification of each of the samples. The lead equivalent (LE) test was carried out using 15.05 mCi Cobalt-57 with gamma energy of 122 keV to compute the abilities of the mullite ceramic samples to attenuate the radiation. XRD patterns of prepared ceramics revealed the presence of orthorhombic mullite, hexagonal quartz and orthorhombic sillimanite structures. Furthermore, the radiation test displayed the ability of ceramics to shield of 70 % of gamma radiation at the distance of 60 cm from the radiation source. The highest lead equivalent thickness is 1.0 mm Pb and the lowest is about 0.06 mm Pb. From the result, it is shown that the ceramic has the potential to use as a shielding barrier in diagnostic radiology facilities due to the ability of reducing the radiation dose up to 70 % from its initial value.

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.

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.

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.

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. Copyright © 2015 Elsevier Ltd. All rights reserved.

Spectroscopy of disordered low-field sites in Cr3+: Mullite glass ceramic

NASA Astrophysics Data System (ADS)

Knutson, Robert; Liu, Huimin; Yen, W. M.; Morgan, T. V.

1989-09-01

In this article we present results of optical and ESR studies that have allowed us to study the behavior of Cr3+ at disordered low-field sites within a mullite ceramic host. The results indicate that the existence of these low-field ions, which are likely at sites in regions of disorder, accounts for most of the spectroscopic anomalies previously noted in these materials. Furthermore, energy transfer from ordered high-field to disordered low-field ions is observed. The resulting complex spectra are deconvoluted by means of the recently developed technique of saturation-resolved fluorescence spectroscopy.

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.

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. Copyright © 2013 Elsevier Ltd. All rights reserved.

Deformation behavior of migmatites: insights from microstructural analysis of a garnet-sillimanite-mullite-quartz-feldspar-bearing anatectic migmatite at Rampura-Agucha, Aravalli-Delhi Fold Belt, NW India

NASA Astrophysics Data System (ADS)

Prakash, Abhishek; Piazolo, Sandra; Saha, Lopamudra; Bhattacharya, Abhijit; Pal, Durgesh Kumar; Sarkar, Saheli

2018-03-01

In the present study we investigate the microstructural development in mullite, quartz and garnet in an anatectic migmatite hosted within a Grenvillian-age shear zone in the Aravalli-Delhi Fold Belt. The migmatite exhibits three main deformation structures and fabrics (S1, S2, S3). Elongated garnet porphyroblasts are aligned parallel to the metatexite S2 layers and contain crenulation hinges defined by biotite-sillimanite-mullite-quartz (with S1 axial planar foliation). Microstructural evidence and phase equilibrium relations establish the garnet as a peritectic phase of incongruent melting by breakdown of biotite, sillimanite ± mullite and quartz at peak P-T of 8 kbar, 730 °C along a tight-loop, clockwise P-T path. Monazite dating establishes that the partial melting occurred between 1000 and 870 Ma. The absence of subgrains and systematic crystal lattice distortions in these garnets despite their elongation suggests growth pseudomorphing pre-existing 3-D networks of S1 biotite aggregates rather than high-temperature crystal plastic deformation which is noted in the S1 quartz grains that exhibit strong crystallographic preferred orientation (CPO), undulatory extinction and subgrains. Mode-I fractures in these garnet porphyroblasts induced by high melt pressure during late stage of partial melt crystallization are filled by retrograde biotite-sillimanite. Weak CPO and non-systematic crystal lattice distortions in the coarse quartz grains within the S2 leucosome domains indicate these crystallized during melt solidification without later crystal plastic deformation overprint. In the later stages of deformation (D3), strain was mostly accommodated in the mullite-biotite-sillimanite-rich restite domains forming S3 which warps around garnet and leucosome domains; consequently, fine-grained S3 quartz does not exhibit strong CPOs.

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

Thermal conductivity measurements on Mullite and Silica REI for the Space Shuttle - Complementary guarded hot plate and radical outflow measurements. [Reusable External Insulators

NASA Technical Reports Server (NTRS)

Brazel, J. P.; Kennedy, B. S.

1974-01-01

The materials studied are described along with the apparatus and the experimental techniques employed. The results of the measurements involving two REI Silica materials and a Mod 1 B REI Mullite are listed in a table. Measurements were conducted at unusually high temperature differences to detect 'shine-through' radiation transparency. Photographs are presented of the high-temperature guarded hot plate assembly.

Effect of BN coating on the strength of a mullite type fiber

NASA Astrophysics Data System (ADS)

Chawla, K. K.; Xu, Z. R.; Ha, J.-S.; Schmücker, M.; Schneider, H.

1997-09-01

Nextel 480 is a polycrystalline essentially mullite fiber (70 wt.-% Al2O3+28 wt.-% SiO2+2 wt.-% B2O3). Different thicknesses of BN were applied as coatings on this fiber. Optical, scanning electron, and transmission electron microscopy were used to characterize the microstructure of the coatings and fibers. The effects of coating and high temperature exposure on the fiber strength were investigated using two-parameter Weibull distribution. TEM examination showed that the BN coating has a turbostratic structure, with the basal planes lying predominantly parallel to the fiber surface. Such an orientation of coating is desirable for easy crack deflection and subsequent fiber pullout in a composite. The BN coated Nextel 480 fiber showed that Weibull mean strength increased first and then decreased with increasing coating thickness. This was due to the surface flaw healing effect of the coating (up to 0.3 μm) while in the case of thick BN coating (1 μm), the soft nature of the coating material had a more dominant effect and resulted in a decrease of the fiber strength. High temperature exposure of Nextel 480 resulted in grain growth, which led to a strength loss.

The effect of TiO2 concentration on properties of apatite-mullite glass-ceramics for dental use.

PubMed

Fathi, Hawa M; Johnson, Anthony

2016-02-01

The aim of this study was to evaluate the effect of TiO2 concentration on the properties of apatite-mullite glass-ceramics namely strength and the chemical solubility to comply with the ISO standard recommendations for dental ceramics (BS EN ISO 6872-2008). Ten novel glass-ceramic materials were produced based on the general formula (4.5SiO2-3Al2O3-1.5P2O5-3CaO-CaF2-xTiO2) where x varied from 0.5 to 5 wt%. Glass with no TiO2 added (HG1T0.0) was used as a reference. Discs of 12 mm diameter and 1.6 mm (±0.2 mm) thickness were prepared for both biaxial flexural strength (BFS) and chemical solubility testing, in accordance with the BS EN ISO 6872-2008 for dental ceramics. All produced materials were investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Energy dispersive X-ray analysis (EDS) was also carried out on some samples to identify the element composition of samples. Increasing the concentration of TiO2 from 0.5 wt% to 2 wt% significantly (P<0.05) increased the chemical solubility of the material. With the material containing 2.5 wt% of TiO2, the solubility significantly reduced (P<0.05) and resulted in a solubility value of 228.3 μm/cm(2) and BFS value of 197.9 MPa. Increasing the TiO2 concentration more than 2.5 wt%, led to a significant (P<0.05) increase in solubility and a reduction in BFS. TiO2 is an effective agent for improving the durability and the mechanical properties of an apatite-mullite glass-ceramic only up to 2.5 wt% concentration. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Role of Y2O3, CaO, MgO additives on structural and microstructural behavior of zirconia/mullite aggregates

NASA Astrophysics Data System (ADS)

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

2012-07-01

Zirconia mullite (MUZ), Y2O3-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 Y2O3, CaO, MgO added MUZ composites. The Y2O3, 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.

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.

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.

Tuning electronic and magnetic properties of Mn-mullite oxide sub-nanoclusters via MnOn polyhedron units.

PubMed

Li, Hui; Cho, Kyeongjae; Li, Shunfang; Wang, Weichao

2018-06-13

Ternary oxide nano-clusters compared to unary metallic and binary ones potentially exhibit more remarkable properties due to their higher stoichiometric flexibility in addition to cluster size variations. Herein, by combining with the structural searching scheme CALYPSO, we have built a series of Mn-mullite oxide clusters (SmxMnyOz)n {(xyz) = (125); (115); n = 1-4, 8} prior to investigation of their geometric and electronic structures via first-principles calculations. In small size regime (n < 4), (SmxMnyOz)n prefer nonstoichiometric (Sm1Mn1O5)n phases composed of nonmagnetic MnO4 tetrahedrons. When n ≧ 4, the clusters tend to develop as stoichiometric (Sm1Mn2O5)n species, including magnetic MnOn polyhedrons and Mn-Mn dimers, which contribute 3d-orbitals (dz2 and/or dx2-y2) around the Fermi levels. The different magnetic behaviors of nonstoichiometric and stoichiometric species originate from the distinct couplings of MnOn polyhedronal units, wherein Mn atoms experience different ligand fields and thus display different spin states. Such findings enable the tuning of electronic properties and potential applications in heterogeneous catalysis, electrochemical catalysis, and the related fields via engineering cluster size and stoichiometry.

Optimisation of the enamelling of an apatite-mullite glass-ceramic coating on Ti6Al4V.

PubMed

O'Flynn, Kevin P; Stanton, Kenneth T

2011-09-01

Apatite-mullite glass-ceramics (AMGCs) are under investigation as a potential alternative to hydroxyapatite (HA) as a coating for cementless fixation of orthopaedic implants. These materials have tailorable mechanical and chemical properties that make them attractive for use as bioactive coatings. Here, AMGC coatings on Ti(6)Al(4)V were investigated to determine an improved heat treatment regime using a systematic examination of the different inputs: composition of glass, nucleation hold and crystallisation hold. An upper limit to the heat treatment temperature was determined by the α + β --> β of Ti(6)Al(4)V at 970°C. The glass composition was modified to produce different crystallisation temperatures and sintering characteristics. A glass was found that is fully crystalline below 970°C and has good sinterability. The effects of different heat treatment time and temperature combinations on the coating and substrate morphologies were examined and the most suitable combination determined. This sample was further investigated and was found to have qualitatively good adhesion and evidence of an interfacial reaction region between the coating and substrate indicating that a chemical reaction had occurred. Oxygen infiltration into the substrate was quantified and the new route was shown to result in a 63% reduction in penetration depth.

Mullite and Mullite Ceramics

DTIC Science & Technology

1994-01-01

possible. The here reported measurements were carried out with synchrotron radiation from the electron storage ring ELSA of the Bonn University. All...Physikalisches Institut der Universitdt Bonn , Bonn , Germany Measurements of X-ray absorption spectra near the absorption edge of a selected element (XANES

Study of the interfacial reactions between a bioactive apatite-mullite glass-ceramic coating and titanium substrates using high angle annular dark field transmission electron microscopy.

PubMed

Stanton, Kenneth T; O'Flynn, Kevin P; Nakahara, Shohei; Vanhumbeeck, Jean-François; Delucca, John M; Hooghan, Bobby

2009-04-01

Glass of generic composition SiO(2) . Al(2)O(3) . P(2)O(5) . CaO . CaF(2) will crystallise predominantly to apatite and mullite upon heat-treatment. Such ceramics are bioactive, osseoconductive, and have a high resistance to fracture. As a result, they are under investigation for use as biomedical device coatings, and in particular for orthopaedic implants. Previous work has shown that the material can be successfully enamelled to titanium with an interfacial reaction zone produced during heat treatment. The present study uses high angle annular dark field transmission electron microscopy (HAADF-TEM) to conduct a detailed examination of this region. Results show evidence of complex interfacial reactions following the diffusion of titanium into an intermediate layer and the production of titanium silicides and titanium phosphides. These results confirm previously hypothesised mechanisms for the bonding of silicate bioceramics with titanium alloys.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Debnath, Tapas, E-mail: debnath@du.ac.bd; Ullah, Ahamed; Rüscher, Claus H.

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 indicatingmore » 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.« less

The effect of aqueous media on the mechanical properties of fluorapatite-mullite glass-ceramics.

PubMed

Mollazadeh, S; Ajalli, Siamak; Kashi, Tahereh S Jafarzadeh; Yekta, Bijan Eftekhai; Javadpour, Jafar; Jafari, S; Youssefi, Abbas; Fazel, Akbar

2015-11-01

To verify the effects of alternating thermal changes in aqueous media and chemical composition on mechanical properties of apatite-mullite glass-ceramics and to investigate concentration of ions eluted from glass-ceramics in aqueous media. The glass compositions were from SiO2Al2O3P2O5CaOTiO2BaOZrO2CaF2 system. Glass-ceramics were prepared by heat-treating at 1100°C for 3h samples alternately immersed in water at 5 and 60°C. The 3-point bending strength (n=10) were determined using 3×4×25mm/bar and a universal testing machine, at a cross-head speed of 0.1mm/min. Vickers micro hardness were evaluated by applying a total of 15-20 indentations under a 100g load for 30s. Concentrations of ions eluted from glass-ceramics immersed in 60±5°C double distilled water were determined by ion chromatography. The toxicity of glass-ceramics was assessed by seeding the osteosarcoma cells (MG63) on powder for different days and their cell proliferation assessment was investigated by MTT assay. The data were analyzed using one way analysis of variance and the means were compared by Tukey's test (5% significance level). The highest flexural strength and hardness values after thermal changes belonged to TiO2 and ZrO2 containing glass-ceramics which contained lower amount of released ions. BaO containing glass-ceramic and sample with extra amount of silica showed the highest amount of reduction in their mechanical strength values. These additives enhanced the concentration of eluted ions in aqueous media. MTT results showed that glass-ceramics were almost equivalent concerning their in-vitro biological behavior. Thermal changes and chemical compositions had significant effects on flexural strength and Vickers micro-hardness values. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

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.

Multilayer article having stabilized zirconia outer layer and chemical barrier layer

NASA Technical Reports Server (NTRS)

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

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.

Oily wastewater treatment by adsorption-membrane filtration hybrid process using powdered activated carbon, natural zeolite powder and low cost ceramic membranes.

PubMed

Rasouli, Yaser; Abbasi, Mohsen; Hashemifard, Seyed Abdollatif

2017-08-01

In this research, four types of low cost and high performance ceramic microfiltration (MF) membranes have been employed in an in-line adsorption-MF process for oily wastewater treatment. Mullite, mullite-alumina, mullite-alumina-zeolite and mullite-zeolite membranes were fabricated as ceramic MF membranes by low cost kaolin clay, natural zeolite and α-alumina powder. Powdered activated carbon (PAC) and natural zeolite powder in concentrations of 100-800 mg L -1 were used as adsorbent agent in the in-line adsorption-MF process. Performance of the hybrid adsorption-MF process for each concentration of PAC and natural zeolite powder was investigated by comparing quantity of permeation flux (PF) and total organic carbon (TOC) rejection during oily wastewater treatment. Results showed that by application of 400 mg L -1 PAC in the adsorption-MF process with mullite and mullite-alumina membranes, TOC rejection was enhanced up to 99.5% in comparison to the MF only process. An increasing trend was observed in PF by application of 100-800 mg L -1 PAC. Also, results demonstrated that the adsorption-MF process with natural zeolite powder has higher performance in comparison to the MF process for all membranes except mullite-alumina membranes in terms of PF. In fact, significant enhancement of PF and TOC rejection up to 99.9% were achieved by employing natural zeolite powder in the in-line adsorption-MF hybrid process.

Formation, stability and crystal structure of mullite-type Al{sub 6−x}B{sub x}O{sub 9}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffmann, K., E-mail: Kristin.Hoffmann@uni-bremen.de; Institut für Anorganische Chemie und Kristallographie, FB02, Leobener Straße/NW2, Universität Bremen, D-28359 Bremen; Hooper, T.J.N.

2016-11-15

Mullite-type Al{sub 6−x}B{sub x}O{sub 9} compounds were studied by means of powder diffraction and spectroscopic methods. The backbones of this structure are chains of edge-connected AlO{sub 6} octahedra crosslinked by AlO- and BO-polyhedra. Rietveld refinements show that the a and b lattice parameters can be well resolved, thus representing an orthorhombic metric. A continuous decrease of the lattice parameters most pronounced in c-direction indicates a solid solution for Al{sub 6−x}B{sub x}O{sub 9} with 1.09≤x≤2. A preference of boron in 3-fold coordination is confirmed by {sup 11}B MAS NMR spectroscopy and Fourier calculations based on neutron diffraction data collected at 4more » K. Distance Least Squares modeling was performed to simulate a local geometry avoiding long B-O distances linking two octahedral chains by planar BO{sub 3} groups yielding split positions for the oxygen atoms and a strong distortion in the octahedral chains. The lattice thermal expansion was calculated using the Grüneisen first-order equation of state Debye-Einstein-Anharmonicity model. - Graphical abstract: Local distortion induced by boron linking the octahedral chains. - Highlights: • Decreasing lattice parameters indicate a solid solution for Al{sub 6−x}B{sub x}O{sub 9} (1.09≤x≤2). • B-atoms induce a local distortion of neighboring AlO{sub 6} octahedra. • A preference of boron in BO{sub 3} coordination is confirmed by {sup 11}B MAS NMR spectroscopy. • An optimized structural model for Al{sub 6−x}B{sub x}O{sub 9} is presented.« less

Glass formation and crystallization in the alumina-silica-lanthanum phosphate system for ceramics composites

NASA Astrophysics Data System (ADS)

Guo, Shuling

The formation, structure, and dynamics of glasses in the alumina-silica-lanthanum phosphate system and their crystallization were investigated as a function of composition. These are of interest because of their potential as precursors for synthesizing ceramic-matrix-composites via co-crystallization of lanthanum monazite and either mullite or alumina into finely mixed microstructures. The glasses were characterized by X-Ray Diffraction (XRD), Raman spectroscopy, Differential Scanning Calorimetry (DSC), Nuclear Magnetic Resonance (NMR), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Electron Energy Loss Spectrometry (EELS). Glass formation from rapidly quenched liquids was easiest and most consistent for compositions containing silica, such as for mullitemonazite compositions, and more difficult for alumina-monazite compositions. For mullite-monazite glasses, the glass transition temperatures increased linearly from 845°C to 906°C with increasing mullite content. An analysis of the glass structure indicated a network consisting of corner-linked aluminate, silicate and phosphate tetrahedra where aluminum played a central role of separating silicon and phosphorous. It was hypothesized that the glass network consisted of domains of aluminum silicate network edged by phosphate tetrahedra. A maximum in the crystallization temperature was attributed to the complexity of the glass network. At relatively mullite-rich compositions, simultaneous and cooperative crystallization of lanthanum phosphate and mullite correlated with the highest crystallization temperatures, and the lowest activation energies of crystallization. This was preceded by amorphous phase segregation in the glass at lower temperatures. An intermediate phase of lanthanum phosphate was discovered with an orthorhombic unit cell. For compositions of high phosphate contents, lanthanum phosphate precipitated first at about 900°C leaving an essentially pure mullite glass

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.

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.

Radiant Heat Transfer in Reusable Surface Insulation

NASA Technical Reports Server (NTRS)

Hughes, T. A.; Linford, R. M. F.; Chmitt, R. J.; Christensen, H. E.

1973-01-01

During radiant testing of mullite panels, temperatures in the insulation and support structure exceeded those predicted on the basis of guarded hot plate thermal conductivity tests. Similar results were obtained during arc tunnel tests of mullite specimens. The differences between effective conductivity and guarded hot plate values suggested that radiant transfer through the mullite was occurring. To study the radiant transport, measurements were made of the infrared transmission through various insulating materials and fibers of interest to the shuttle program, using black body sources over the range of 780 to 2000 K. Experimental data were analyzed and scattering coefficients were derived for a variety of materials, fiber diameters, and source temperature.

Growth and development of the pink bollworm, Pectinophora gossypiella (Lepidoptera: Gelechiidae), on bolls of cotton grown in enriched carbon dioxide atmospheres

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akey, D.H.; Kimball, B.A.; Mauney, J.R.

1988-06-01

The pink bollworm, Pectinophora gossypiella (Saunders), was reared on the bolls of cotton plants grown in CO/sub 2/-enriched (649 ..mu..l/liter) and ambient CO/sub 2/ (371 ..mu..l/liter) chambers and in two open field plots, one with free-air CO/sub 2/ enrichment (522 ..mu..l/liter) and one without enrichment (ambient CO/sub 2/, 360 ..mu..l/liter). The effects of increased CO/sub 2/ levels on growth and development were examined. There was no difference in pupal weights of pink bollworm raised on CO/sub 2/-enriched cotton compared with those raised on ambient CO/sub 2/ cotton (26.80 versus 26.64 mg, respectively). Also, there was no difference in developmental timemore » (21-27 d). Analysis of percent seed damage by larvae showed no differences between CO/sub 2/-enriched and ambient CO/sub 2/ cotton. These results were attributed to the nutritional qualities of the seed remaining the same (specifically the carbon/nitrogen ratio) despite CO/sub 2/ and photosynthetic changes in the plant.« less

Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single

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.

A study of processing parameters in thermal-sprayed alumina and zircon mixtures

NASA Astrophysics Data System (ADS)

Li, Y.; Khor, K. A.

2002-06-01

A method of plasma spraying of alumina and zircon mixtures to form ZrO2-mullite composites has been proposed and developed. The feedstock is prepared by a combination of mechanical alloying, which allows formation of fine-grained, homogeneous solid-solution mixtures, followed by plasma spheroidization that yields rapid solidified microstructures and enhanced compositional homogeneity. The effects of ball-milling duration and milling media were studied. It was found that zirconia is a more efficient milling media and that increasing milling duration enhanced the dissociation of zircon. Flame spray and plasma spray processes were used to spheroidize the spray-dried powders. The temperature of the flame spray was found to be insufficient to melt the powders completely. The processing parameters of the plasma spray played an important role in zircon decomposition and mullite formation. Increasing the arc current or reducing secondary gas pressure caused more zircon to decompose and more mullite to form after heat treatment at 1200 °C for 3 h. Dissociation of zircon and the amount of mullite for med can be enhanced significantly when using the more efficient, computerized plasma-spraying system and increasing the ball-milling duration from 4 to 8 h.

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.

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.

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.

Crystallization of lanthanum and yttrium aluminosilicate glasses

NASA Astrophysics Data System (ADS)

Sadiki, Najim; Coutures, Jean Pierre; Fillet, Catherine; Dussossoy, Jean Luc

2006-01-01

The crystallization behaviour of aluminosilicate glasses of lanthanum (LAS) and yttrium (YAS) containing 2-8 mol% of Ln 2O 3 (Ln = La or Y), 12-30 mol% of Al 2O 3, and 64-80 mol% of SiO 2 has been studied by DTA, XRD and SEM-EDX analysis. X-ray diffraction results indicate the presence of the mullite phase and La 2Si 2O 7 in the monoclinic high-temperature G form (group space P2 1/c) for the LAS glasses, and mullite y-Y 2Si 2O 7 in the monoclinic structure (group space C2/m) and a small amount of β-Y 2Si 2O 7 in the orthorhombic structure (space group Pna2) for the YAS. For both cases, very little tridymite phase is observed. The results also show that the values of Tg for YAS are higher than those for LAS glasses. The crystallization of LAS glasses is more difficult than that of YAS. For all samples, we observed only one kind of mullite (Al/Si = 3.14).

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

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

PubMed

Pasternak, Grzegorz; Greenman, John; Ieropoulos, Ioannis

2016-01-08

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. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of low cost/high temperature insulation, July 1974 - June 1975

NASA Technical Reports Server (NTRS)

Strauss, E. L.

1975-01-01

Six fiber products and six insulation blankets comprising silica, alumina, zirconia, mullite, and mixed ceramic systems were subjected to furnace exposures up to 500 hours at temperatures of 1000 to 1600 C and evaluated for chemical and dimensional stability and for changes in thermal conductivity. Alumina, zirconia, and mullite fibers were fabricated into reusable surface insulation (RSI) tile by water-felting and reimpregnation with ethyl silicate. Specimens were exposed to 25 thermal cycles at 1200 C and 1400 C and a pressure of 10 and 32 torr, respectively. Production costs for 930 sq m (10,000 sq ft) of blanket insulation and of alumina RSI tile were developed.

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.

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.

The influence of crystallography and kinetics on phengite breakdown reactions in a low-pressure metamorphic aureole

NASA Astrophysics Data System (ADS)

Worden, R. H.; Droop, G. T. R.; Champness, P. E.

1992-04-01

A natural example of phengite that had undergone partial thermal decomposition at a pressure of about 0.5 kbar and a temperature of about 680° C in a contact aureole was exmined in the transmission electron microscope (TEM). Partially pseudomorphed phengites were found to consist of combinations of phengite, biotite, K-feldspar, mullite, sillimanite, spinel and cordierite. Different areas within individual, partially pseudomorphed, phengite grains show various degrees of reaction and different reaction products; the cores are the least reacted and the margins have reacted most. In the cores the assemblage Al-, Mg-enriched phengite+biotite +K-feldspar+mullite±spinel has formed, whereas the assemblage K-feldspar+mullite+sillimanite+spinel +biotite+cordierite has formed at the edges. According to our thermodynamic calculations, the breakdown of phengite should have produced cordierite+spinel +corundum+K-feldspar in regions isolated from the influx of SiO2 and cordierite+andalusite+quartz+K-feldspar in regions near the edge of the grains that were essentially saturated with SiO2. Chemical equilibrium was not achieved in any part of the partially pseudomorphed phengites on a micron scale or larger. Breakdown theoretically should have been complete by about 550° C; the reaction temperature was overstepped by at least 130° C for 20 25 years. The variations in the degree and type of reaction are probably due partly to the availability of suitable nucleation sites in different regions, partly to the need to remove H2O from reaction sites and partly to the influence of SiO2, which diffused into the grains during metamorphism. The presence of SiO2 lowers the equilibrium temperatures. Thus there is a higher driving force for breakdown near the grain boundaries than in the cores. Most of the products show an orientation relationship with the parent phengite and have consistent habit planes; they have their closest-packed planes and closest-packed directions parallel to one

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.

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.

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.

Cyclic arc plasma tests of RSI materials using a preheater

NASA Technical Reports Server (NTRS)

Stewart, D. A.

1973-01-01

The results of a test program are reported in which a preheater was used with an arc plasma stream to study the thermal response of samples of candidate reusable surface insulation materials for the space shuttle. The preheater simulated the shuttle temperature history during the first and last portions of the test cycle, which could not be simulated by the air arc plasma flow. Pre- and post-test data taken for each of the materials included magnified views, optical properties, and chemical analyses. The test results indicate that the mullite base samples experience higher surface temperatures than the other materials at heating rates greater than 225 kw/sq m. The ceramic fibrous mullite and silica coatings show noncatalytic wall behavior. Internal temperature response data for the materials are compared and correlated with analytical predictions.

The Final Proceedings for Mullite and Mullite Ceramics Held in Irsee, Germany on 7-9 September 1994

DTIC Science & Technology

1996-01-01

10 Rue Vauquelin, Department of Mechanical Engineering, Fairey Tecramics Ltd, F-75231 Paris C~dex, France Worcester Polytechnic Institute, Mount ...through an evacu- ated beam path. The sample solution was mounted in a glass capillary 3 mm in diameter so* C and 8 p/m in thickness. Intensity measurements...thickness round the Cr atoms. The second peak is assumed product of about 2 in the region just after the - edge were mounted on Scotch Tape. The spectra

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.

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.

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.

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.

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.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

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 tomore » 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.« less

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

2013-08-06

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.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jie Li; Mei-Fang Du; Zhong-Xiao Zhang

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 limestonemore » 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.« less

Thermoelectric Properties and Morphology of Si/SiC Thin-Film Multilayers Grown by Ion Beam Sputtering

DOE PAGES

Cramer, Corson; Farnell, Casey; Farnell, Cody; ...

2018-03-19

Multilayers (MLs) of 31 bi-layers and a 10-nm layer thickness each of Si/SiC were deposited on silicon, quartz and mullite substrates using a high-speed, ion-beam sputter deposition process. The samples deposited on the silicon substrates were used for imaging purposes and structural verification as they did not allow for accurate electrical measurement of the material. The Seebeck coefficient and the electrical resistivity on the mullite and the quartz substrates were reported as a function of temperature and used to compare the film performance. The thermal conductivity measurement was performed for ML samples grown on Si, and an average value ofmore » the thermal conductivity was used to find the figure of merit, zT, for all samples tested. X-ray diffraction (XRD) spectra showed an amorphous nature of the thin films. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to study the film morphology and verify the nature of the crystallinity. The mobility of the multilayer films was measured to be only 0.039 to 1.0 cm 2/Vs at room temperature. The samples were tested three times in the temperature range of 300 K to 900 K to document the changes in the films with temperature cycling. The highest Seebeck coefficient is measured for a Si/SiC multilayer system on quartz and mullite substrates and were observed at 870 K to be roughly -2600 μV/K due to a strain-induced redistribution of the states’ effect. The highest figure of merit, zT, calculated for the multilayers in this study was 0.08 at 870 K.« less

Thermoelectric Properties and Morphology of Si/SiC Thin-Film Multilayers Grown by Ion Beam Sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cramer, Corson; Farnell, Casey; Farnell, Cody

Multilayers (MLs) of 31 bi-layers and a 10-nm layer thickness each of Si/SiC were deposited on silicon, quartz and mullite substrates using a high-speed, ion-beam sputter deposition process. The samples deposited on the silicon substrates were used for imaging purposes and structural verification as they did not allow for accurate electrical measurement of the material. The Seebeck coefficient and the electrical resistivity on the mullite and the quartz substrates were reported as a function of temperature and used to compare the film performance. The thermal conductivity measurement was performed for ML samples grown on Si, and an average value ofmore » the thermal conductivity was used to find the figure of merit, zT, for all samples tested. X-ray diffraction (XRD) spectra showed an amorphous nature of the thin films. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to study the film morphology and verify the nature of the crystallinity. The mobility of the multilayer films was measured to be only 0.039 to 1.0 cm 2/Vs at room temperature. The samples were tested three times in the temperature range of 300 K to 900 K to document the changes in the films with temperature cycling. The highest Seebeck coefficient is measured for a Si/SiC multilayer system on quartz and mullite substrates and were observed at 870 K to be roughly -2600 μV/K due to a strain-induced redistribution of the states’ effect. The highest figure of merit, zT, calculated for the multilayers in this study was 0.08 at 870 K.« less

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.

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.

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.

The internal microstructure and fibrous mineralogy of fly ash from coal-burning power stations.

PubMed

Brown, Patrick; Jones, Tim; BéruBé, Kelly

2011-12-01

Coal fly ash (CFA) is a significant environmental pollutant that presents a respiratory hazard when airborne. Although previous studies have identified the mineral components of CFA, there is a paucity of information on the structural habits of these minerals. Samples from UK, Polish and Chinese power stations were studied to further our understanding of the factors that affect CFA geochemistry and mineralogy. ICP-MS, FE-SEM/EDX, XRD, and laser diffraction were used to study physicochemical characteristics. Analysis revealed important differences in the elemental compositions and particle size distributions of samples between sites. Microscopy of HF acid-etched CFA revealed the mullite present possesses a fibrous habit; fibres ranged in length between 1 and 10 μm. Respirable particles (<10 μm) were frequently observed to contain fibrous mullite. We propose that the biopersistence of these refractory fibres in the lung environment could be contributing towards chronic lung diseases seen in communities and individuals continually exposed to high levels of CFA. Copyright © 2011 Elsevier Ltd. All rights reserved.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 highmore » 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.« less

Ceramic-Ceramic Composites Meeting in Belgium.

DTIC Science & Technology

1987-08-04

the liquid phase Vidrio , Madrid, Spain) described the use should disappear during the heat treat- of SIC grains as a dispersed phase to ment. The...SiC fiber-reinforced SiO2 glass ma- trix, mullite-zirconia-A120 3-SiC, C-fi- used elastic wave measurements at high ber-reinforced reaction-bonded SiC

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.

Single-crystal diffraction at the Extreme Conditions beamline P02.2: procedure for collecting and analyzing high-pressure single-crystal data.

PubMed

Rothkirch, André; Gatta, G Diego; Meyer, Mathias; Merkel, Sébastien; Merlini, Marco; Liermann, Hanns Peter

2013-09-01

Fast detectors employed at third-generation synchrotrons have reduced collection times significantly and require the optimization of commercial as well as customized software packages for data reduction and analysis. In this paper a procedure to collect, process and analyze single-crystal data sets collected at high pressure at the Extreme Conditions beamline (P02.2) at PETRA III, DESY, is presented. A new data image format called `Esperanto' is introduced that is supported by the commercial software package CrysAlis(Pro) (Agilent Technologies UK Ltd). The new format acts as a vehicle to transform the most common area-detector data formats via a translator software. Such a conversion tool has been developed and converts tiff data collected on a Perkin Elmer detector, as well as data collected on a MAR345/555, to be imported into the CrysAlis(Pro) software. In order to demonstrate the validity of the new approach, a complete structure refinement of boron-mullite (Al5BO9) collected at a pressure of 19.4 (2) GPa is presented. Details pertaining to the data collections and refinements of B-mullite are presented.

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.

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.

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.

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

Processing of a Mullite Matrix, Molybdenum Disilicide Reinforced Composite

DTIC Science & Technology

1991-01-01

at high temperatures (best of the silicides and almost as good as SiC) is due to the formation of protective SiO2 layers on the surface of the MoSi 2...of the precipitation preparation process) consisted largely of sodium . Previous work 52 showed that the particle size was 160 A (TEM analysis) not...M.K. Brun, L.E. Szala, "Kinetics of Oxidation of Carbide and Silicide Dispersed Phases in Oxide Matrices," Adv. Ceram. Mat., 3 [5] 491-497 (1988). 5

New Measurements of Activation Volume in Olvine Under Anhydrous Conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Durham, W.; Mei, S; Kohlstedt, D

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 bymore » 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.« less

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.

Filtration Efficiency of Functionalized Ceramic Foam Filters for Aluminum Melt Filtration

NASA Astrophysics Data System (ADS)

Voigt, Claudia; Jäckel, Eva; Taina, Fabio; Zienert, Tilo; Salomon, Anton; Wolf, Gotthard; Aneziris, Christos G.; Le Brun, Pierre

2017-02-01

The influence of filter surface chemistry on the filtration efficiency of cast aluminum alloys was evaluated for four different filter coating compositions (Al2O3—alumina, MgAl2O4—spinel, 3Al2O3·2SiO2—mullite, and TiO2—rutile). The tests were conducted on a laboratory scale with a filtration pilot plant, which facilitates long-term filtration tests (40 to 76 minutes). This test set-up allows the simultaneous use of two LiMCAs (before and after the filter) for the determination of the efficiency of inclusion removal. The four tested filter surface chemistries exhibited good thermal stability and mechanical robustness after 750 kg of molten aluminum had been cast. All four filter types exhibited a mean filtration efficiency of at least 80 pct. However, differences were also observed. The highest filtration efficiencies were obtained with alumina- and spinel-coated filter surfaces (>90 pct), and the complete removal of the largest inclusions (>90 µm) was observed. The efficiency was slightly lower with mullite- and rutile-coated filter surfaces, in particular for large inclusions. These observations are discussed in relation to the properties of the filters, in particular in terms of, for example, the surface roughness.

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.

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.

Thermoluminescence and X-ray diffraction studies on sliced ancient porcelain samples

NASA Astrophysics Data System (ADS)

Leung, P. L.; Yang, B.

1999-09-01

The thermal activation characteristics (TACs) of the sensitivity of the '110°C' peak in 14 sliced ancient Chinese porcelain samples are studied. Comparing with the TACs of natural quartz and synthetic mullite, the relation between the TACs and the composition of the sample is discussed with reference to the X-ray diffraction (XRD) spectra. It is suggested that in some cases, contribution of the porcelain components other than quartz to the TACs is not negligible.

Chemical Processing of Structural Ceramics and Composites

DTIC Science & Technology

1988-09-01

aluminum isopropoxide (Eq. 2). Silicon alkoxide was purchased (Alfa Products) since it is relatively stable. Mg + 2C2 H 5OH ---> Mg(OC 2H5 )2 + 1/2H 2...hydrolysis of mullite precursor mixed alkoxides (TEOS and aluminum isopropoxide ) were studied. The effect of pH on hydrolysis was significant due to the...followed by IR measurements. A stoichiometric amount of TEOS was added to aluminum isopropoxide , refluxed for 48 hours, then the excess isopropyl

Effect of Environment on Creep Behavior of an Oxide/Oxide CFCC with 45 deg. Fiber Orientation

DTIC Science & Technology

2006-06-01

MPa, the elastic modulus (E) was 45 GPa, and failure strain was 0.265%. The creep -rupture results showed a decrease in creep life with increasing...failure and increased creep life . A qualitative spectral analysis provided evidence of silicon species migration from the mullite phase of the...N720/AS in 0/90˚ and ±45˚ orientation at 1100°C. Shows that high creep rates generally correspond to a short creep life .................... 17

[Volatile ashes and their biological effect. 2. Fibrogenic effect of volatile ashes].

PubMed

Woźniak, H; Wiecek, E; Lao, I; Wojtczak, J

1989-01-01

In experiments on white Wistar rats fibrogenic effects of 6 samples of fly-ashes collected from electric precipitators in power engineering plants have been evaluated. The coal came from different national deposits. All the ashes have been found to contain: quartz and mullite, 3 ashes contained additionally orthoclase, whereas 1, apart from quartz and mullite, contained kaolinite; naturally radioactive elements (Ra226, K40, Th228) and trace elements (As, Ba, Be, Cd, Ce, Cu, Fe, Pa, Mo, Ni, Pb, Se, U Zu). Experimental pneumoconiosis was induced through intratracheal administration of single doses of 50 mg of dust; the experiment was carried out at 3 time intervals of 3, 6 and 9 months. The fibrogenic activity was evaluated both qualitatively (histopathological methods) and quantitatively (lung weight, hydroxyproline content in lungs, dust elimination from lungs); control groups consisted of animals which obtained NaCl solution and quartz sands. Fly-ashes were found to exhibit different fibrogenic effects, yet, their fibrogenic activity was weaker, compared to quartz sands. No clear correlation was found between fibrogenic effects of ashes and test physico-chemical properties, such as the content of SiO2, trace elements or naturally radioactive elements. Analysis of occupational diseases (for the period section): (1979-1983) demonstrated occupational diseases of dust-related aetiology among power engineering workers, pneumoconioses, constituting 7.8% of 127 cases of occupational diseases.

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.

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.

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.

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.

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.

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.

Microstructure, Tensile Adhesion Strength and Thermal Shock Resistance of TBCs with Different Flame-Sprayed Bond Coat Materials Onto BMI Polyimide Matrix Composite

NASA Astrophysics Data System (ADS)

Abedi, H. R.; Salehi, M.; Shafyei, A.

2017-10-01

In this study, thermal barrier coatings (TBCs) composed of different bond coats (Zn, Al, Cu-8Al and Cu-6Sn) with mullite top coats were flame-sprayed and air-plasma-sprayed, respectively, onto bismaleimide matrix composites. These polyimide matrix composites are of interest to replace PMR-15, due to concerns about the toxicity of the MDA monomer from which PMR-15 is made. The results showed that pores and cracks appeared at the bond coat/substrate interface for the Al-bonded TBC because of its high thermal conductivity and diffusivity resulting in transferring of high heat flux and temperature to the polymeric substrate during top coat deposition. The other TBC systems due to the lower conductivity and diffusivity of bonding layers could decrease the adverse thermal effect on the polymer substrate during top coat deposition and exhibited adhesive bond coat/substrate interfaces. The tensile adhesion test showed that the adhesion strength of the coatings to the substrate is inversely proportional to the level of residual stress in the coatings. However, the adhesion strength of Al bond-coated sample decreased strongly after mullite top coat deposition due to thermal damage at the bond coat/substrate interface. TBC system with the Cu-6Sn bond coat exhibited the best thermal shock resistance, while Al-bonded TBC showed the lowest. It was inferred that thermal mismatch stresses and oxidation of the bond coats were the main factors causing failure in the thermal shock test.

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.

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.

Metal stabilization mechanism of incorporating lead-bearing sludge in kaolinite-based ceramics.

PubMed

Lu, Xingwen; Shih, Kaimin

2012-02-01

The feasibility and mechanism of incorporating simulated lead-laden sludge into low-cost ceramic products was investigated by observing the reaction of lead with two kaolinite-based precursors under sintering conditions. To investigate the phase transformation process of lead, lead oxide (PbO) mixed with a kaolinite or mullite precursor were fired at 500-950°C for 3h. Detailed X-ray diffraction analysis of sintered products revealed that both precursors had crystallochemically incorporated lead into the lead feldspar (PbAl(2)Si(2)O(8)) crystalline structure. By mixing lead oxide with kaolinite, lead feldspar begins to crystallize at 700°C; maximum incorporation of lead into this structure occurred at 950°C. However, two intermediate phases, Pb(4)Al(4)Si(3)O(16) and a polymorph of lead feldspar, were detected at temperatures between 700 and 900°C. By sintering lead oxide with the mullite precursor, lead feldspar was detected at temperatures above 750°C, and an intermediate phase of Pb(4)Al(4)Si(3)O(16) was observed in the temperature range of 750-900°C. This study compared the lead leachabilities of PbO and lead feldspar using a prolonged leaching test (at pH 2.9 for 23d) modified from the toxicity characteristic leaching procedure. The results indicate the superiority of lead feldspar in stabilizing lead and suggest a promising and reliable strategy to stabilize lead in ceramic products. Copyright © 2011 Elsevier Ltd. All rights reserved.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ari-Wahjoedi, Bambang, E-mail: bambang-ariwahjoedi@petronas.com.my; Centre for Intelligent Signal and Imaging Research, Universiti Teknologi PETRONAS, Bandar Seri Iskandar; Ginta, Turnad Lenggo

2014-10-24

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

The high temperature creep behavior of oxides and oxide fibers

NASA Technical Reports Server (NTRS)

Jones, Linda E.; Tressler, Richard E.

1991-01-01

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

Zr doped anatase supported reticulated ceramic foams for photocatalytic water purification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plesch, G., E-mail: plesch@fns.uniba.sk; Vargová, M.; Vogt, U.F.

2012-07-15

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

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.

Determination of anisotropy and multimorphology in fly ash based geopolymers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, M. Irfan, E-mail: mirfanwazir@gmail.com; Azizli, Khairun, E-mail: khairun-azizli@petronas.com.my; Sufian, Suriati, E-mail: suriati@petronas.com.my

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.

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.

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.

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

The study of the thermal behavior of solid mixtures of metakaolin and sodium hydroxide by isoconversional model-free analyzes

NASA Astrophysics Data System (ADS)

Gordina, Natalya E.; Prokof'ev, Valery Yu; Smirnov, Nikolay N.; Khramtsova, Alexandra P.

2017-11-01

Interactions in solid mixtures of 6Al2Si2O7: 12NaOH and 6Al2Si2O7: 12NaOH: 2Al2O3 under thermal treatment were studied. Ultrasonic pre-treatment of suspensions with a frequency of 22 kHz was applied. X-ray phase analysis, scanning electron microscopy, and synchronous thermal analysis were used in this research. It was shown that after evaporation of the suspensions, the hydrated LTA zeolite and sodium hydroaluminate are synthesized. During thermal treatment up to 500 °C, the adsorption water is removed first and then the dehydration of the zeolite and hydroaluminate occurs. Calcination at temperatures above 500° C leads to the synthesis of Na6Al4Si4O17 and Na8Al4Si4O18 by the interaction of metakaolin and zeolite with sodium hydroxide. At temperatures above 700 °C, the formation of mullite and nepheline occurs in the temperature range of 500-800 °C. The kinetic parameters have been calculated using Friedman analysis (differential method), Kissinger-Akahira-Sunose and Ozawa-Flynn-Wall analyzes (integral methods). It was shown that all analyzes give similar dependences of the apparent activation energy vs the conversion extent and the values of E are in the range of 70-350 kJ mol-1. It was established that ultrasonic pre-treatment allows to reduce the values of the apparent activation energy. It was discovered that the Al2O3 excess over the stoichiometry of the LTA zeolite synthesis is an inhibitor of the mullite and nepheline formation reactions.

Numerical Study of Suspension HVOF Spray and Particle Behavior Near Flat and Cylindrical Substrates

NASA Astrophysics Data System (ADS)

Jadidi, M.; Yeganeh, A. Zabihi; Dolatabadi, A.

2018-01-01

In thermal spray processes, it is demonstrated that substrate shape and location have significant effects on particle in-flight behavior and coatings quality. In the present work, the suspension high-velocity oxygen fuel (HVOF) spraying process is modeled using a three-dimensional two-way coupled Eulerian-Lagrangian approach. Flat and cylindrical substrates are placed at different standoff distances, and particles characteristics near the substrates and upon impact are studied. Suspension is a mixture of ethanol, ethylene glycol, and mullite solid powder (3Al2O3·2SiO2) in this study. Suspension droplets with predefined size distribution are injected into the combustion chamber, and the droplet breakup phenomenon is simulated using Taylor analogy breakup model. Furthermore, the eddy dissipation model is used to model the premixed combustion of oxygen-propylene, and non-premixed combustion of oxygen-ethanol and oxygen-ethylene glycol. To simulate the gas phase turbulence, the realizable k-ɛ model is applied. In addition, as soon as the breakup and combustion phenomena are completed, the solid/molten mullite particles are tracked through the domain. It is shown that as the standoff distance increases the particle temperature and velocity decrease and the particle trajectory deviation becomes more significant. The effect of stagnation region on the particle velocity and temperature is also discussed in detail. The catch rate, which is defined as the ratio of the mass of landed particles to injected particles, is calculated for different substrate shapes and standoff distances in this study. The numerical results presented here is consistent with the experimental data in the literature for the same operating conditions.

Water Adsorption Isotherms on Fly Ash from Several Sources.

PubMed

Navea, Juan G; Richmond, Emily; Stortini, Talia; Greenspan, Jillian

2017-10-03

In this study, horizontal attenuated total reflection (HATR) Fourier-transform infrared (FT-IR) spectroscopy was combined with quartz crystal microbalance (QCM) gravimetry to investigate the adsorption isotherms of water on fly ash, a byproduct of coal combustion in power plants. Because of composition variability with the source region, water uptake was studied at room temperature as a function of relative humidity (RH) on fly ash from several regions: United States, India, The Netherlands, and Germany. The FT-IR spectra show water features growth as a function of RH, with water absorbing on the particle surface in both an ordered (ice-like) and a disordered (liquid-like) structure. The QCM data was modeled using the Brunauer, Emmett, and Teller (BET) adsorption isotherm model. The BET model was found to describe the data well over the entire range of RH, showing that water uptake on fly ash takes place mostly on the surface of the particle, even for poorly combusted samples. In addition, the source region and power-plant efficiency play important roles in the water uptake and ice nucleation (IN) ability of fly ash. The difference in the observed water uptake and IN behavior between the four samples and mullite (3Al 2 O 3 ·2SiO 2 ), the aluminosilicate main component of fly ash, is attributed to differences in composition and the density of OH binding sites on the surface of each sample. A discussion is presented on the RH required to reach monolayer coverage on each sample as well as a comparison between surface sites of fly ash samples and enthalpies of adsorption of water between the samples and mullite.

Spectroscopic determination of the distribution of Cr3+ sites in mullite ceramics

NASA Astrophysics Data System (ADS)

Liu, Huimin; Knutson, Robert; Jia, Weiyi; Strauss, Eugen; Yen, W. M.

1990-06-01

Excitation spectra and lifetime measurements were used to distinguish high-field-site (HFS) and low-field-site (LFS) Cr3+-ion behaviors. A theoretical analysis of site distribution gives an adequate fit to the luminescent spectra. The residual content of LFS in the glass ceramic was found to depend on the extent of the heat treatment.

Interface Analyses Between a Case-Hardened Ingot Casting Steel and Carbon-Containing and Carbon-Free Refractories

NASA Astrophysics Data System (ADS)

Fruhstorfer, Jens; Dudczig, Steffen; Rudolph, Martin; Schmidt, Gert; Brachhold, Nora; Schöttler, Leandro; Rafaja, David; Aneziris, Christos G.

2018-06-01

Corrosion tests of carbon-free and carbon-containing refractories were performed. The carbon-free crucibles corroded, whereas the carbon-containing crucibles were negligibly attacked. On them, inclusions were attached. This study investigates melt oxygen contents, interface properties, and steel compositions with their non-metallic inclusions in order to explore the inclusion formation and deposition mechanisms. The carbon-free crucibles were based on alumina, mullite, and zirconia- and titania-doped alumina (AZT). The carbon-containing (-C) ones were alumina-C and AZT-C. Furthermore, nanoscaled carbon and alumina additives (-n) were applied in an AZT-C-n material. In the crucibles, the case-hardened steel 17CrNiMo7-6 was remelted at 1580 °C. It was observed that the melt and steel oxygen contents were higher for the tests in the carbon-free crucibles. Into these crucibles, the deoxidizing alloying elements Mn and Si diffused. Reducing contents of deoxidizing elements resulted in higher steel oxygen levels and less inclusions, mainly of the inclusion group SiO2-core-MnS-shell (2.5 to 8 μ m). These developed from smaller SiO2 nuclei. The inclusion amount in the steel was highest after remelting in AZT-C-n for 30 minutes but decreased strongly with increasing remelting time (60 minutes) due to inclusions' deposition on the refractory surface. The Ti from the AZT and the nanoadditives supported inclusion growth and deposition. Other inclusion groups were alumina and calcium aluminate inclusions. Their contents were high after remelting in carbon- or AZT-containing crucibles but generally decreased during remelting. On the AZT-C-n crucible, a dense layer formed from vitreous compositions including Al, Ca, Mg, Si, and Ti. To summarize, for reducing forming inclusion amounts, mullite is recommended as refractory material. For capturing formed inclusions, AZT-C-n showed a high potential.

Structure and performance of polymer-derived bulk ceramics determined by method of filler incorporation

NASA Astrophysics Data System (ADS)

Konegger, T.; Schneider, P.; Bauer, V.; Amsüss, A.; Liersch, A.

2013-12-01

The effect of four distinct methods of incorporating fillers into a preceramic polymer matrix was investigated with respect to the structural and mechanical properties of the resulting materials. Investigations were conducted with a polysiloxane/Al2O3/ZrO2 model system used as a precursor for mullite/ZrO2 composites. A quantitative evaluation of the uniformity of filler distribution was obtained by employing a novel image analysis. While solvent-free mixing led to a heterogeneous distribution of constituents resulting in limited mechanical property values, a strong improvement of material homogeneity and properties was obtained by using solvent-assisted methods. The results demonstrate the importance of the processing route on final characteristics of polymer-derived ceramics.

Environmental Barrier Coatings (EBC) for Ceramic Matrix Composite (CMC) Materials

NASA Technical Reports Server (NTRS)

Lee,Kang

2001-01-01

The upper use temperature of current Environmental Barrier Coatings (EBC's) based on mullite and BSAS (EPM EBC's) is limited to -255 F due to silica volatility, chemical reactions, and high thermal conductivity. Therefore, new EBC s having low CTE, good chemical compatibility, and high melting point (greater than 2700 F ) are being investigated. Sinter-resistant, low thermal conductivity EBC s are strongly desired to achieve the UEET EBC goal of 270 F EBC surface temperature and 30 F AT over long exposures (greater than 1000 hr). Key areas affecting the upper temperature limit of current EBC s as well as the ongoing efforts to develop next generation EBC s in the UEET Program will be discussed.

Adsorption of chromium ions from aqueous solution by using activated carbo-aluminosilicate material from oil shale.

PubMed

Shawabkeh, Reyad Awwad

2006-07-15

A novel activated carbo-aluminosilicate material was prepared from oil shale by chemical activation. The chemicals used in the activation process were 95 wt% sulfuric and 5 wt% nitric acids. The produced material combines the sorption properties and the mechanical strength of both activated carbon and zeolite. An X-ray diffraction analysis shows the formation of zeolite Y, Na-X, and A-types, sodalite, sodium silicate, mullite, and cancrinite. FT-IR spectrum shows the presence of carboxylic, phenolic, and lactonic groups on the surface of this material. The zero point of charge estimated at different mass to solution ratio ranged from 7.9 to 8.3. Chromium removal by this material showed sorption capacity of 92 mg/g.

Fundamental studies on the nature and properties of ceramic fiber insulation

NASA Technical Reports Server (NTRS)

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

1975-01-01

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

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.

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.

Sensors for ceramic components in advanced propulsion systems

NASA Technical Reports Server (NTRS)

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

1995-01-01

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

Silver-hafnium braze alloy

DOEpatents

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

2003-12-16

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

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

DOE PAGES

Shen, Tengming; Ye, Liyang; Li, Pei

2016-07-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Tengming; Ye, Liyang; Li, Pei

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

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.

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.

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.

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.

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

PubMed

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

2015-03-05

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

Gehlenite and anorthite formation from fluid fly ash

NASA Astrophysics Data System (ADS)

Perná, Ivana; Šupová, Monika; Hanzlíček, Tomáš

2018-04-01

Fluid fly ash could be considered a waste, but, when well treated, it may also become a useful secondary source material. Its rather high content of calcium-containing phases along with thermally treated alumino-silicate residues resulting from coal combustion can lead to the formation of a stable system with newly formatted phases. The high temperature destroys the clay lattice and activates a new configuration of aluminum ions, changing their coordination to oxygen. The effect is accompanied by changes in charge in the surroundings, which are compensated for by calcium ions. The higher the temperature of the fluid ash treatment, the more pronounced the appearance of gehlenite and anorthite in the final mass. Both are natural materials and, together with mullite and anhydrite, they could ensure safety and protection even if exposed to open fire of up to 1150 °C.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kirby, Brent W.

The crucibles used currently for microwave melting of U-Mo alloy at the Y-12 Complex contain silicon carbide (SiC) in a mullite (3Al 2O 3-2SiO 2) matrix with an erbia coating in contact with the melt. Due to observed silicon contamination, Pacific Northwest National Laboratory has investigated alternative crucible materials that are susceptible to microwave radiation and are chemically compatible with molten U-Mo at 1400 1500C. Recommended crucibles for further testing are: 1) high-purity alumina (Al 2O 3); 2) yttria-stabilized zirconia (ZrO 2); 3) a composite of alumina and yttria-stabilized zirconia; 4) aluminum nitride (AlN). Only AlN does not require anmore » erbia coating. The recommended secondary susceptor, for heating at low temperature, is SiC in a “picket fence” arrangement.« less

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.

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.

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.

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.

Silicon carbide whisker reinforced ceramic composites and method for making same

DOEpatents

Wei, George 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 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.

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

PubMed Central

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

2015-01-01

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

Dynamic Compressibility of High-Porosity Dampers of Thermal and Shock Loadings:. Modeling and Experiment

NASA Astrophysics Data System (ADS)

Bragov, Anatoly; Konstantinov, Alexander; Lomunov, Andrey; Sadyrin, Anatoly; Sergeichev, Ivan; Kruszka, Leopold

High-porosity materials, such as chamotte and mullite, possess a heat of fusion. Owing to their properties, these materials can be used with success as damping materials in containers for airplane, automobile, etc. transportation of radioactive or highly toxic materials. Experimental studies of the dynamic properties have been executed with using some original modifications of the Kolsky method. These modified experiments have allowed studying the dynamic compressibility of high-porosity chamotte at deformations up to 80% and amplitudes up to 50 MPa. The equations of the mathematical model describing shock compacting of chamotte as a highly porous, fragile, collapsing material are presented. Deformation of high-porous materials at non-stationary loadings is usually accompanied by fragile destruction of interpore partitions as observed in other porous ceramic materials. Comparison of numerical and experimental results has shown their good conformity.

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.

Dilithium dialuminium trisilicate Crystalline Phase Prepared from Coal Fly Ash

NASA Astrophysics Data System (ADS)

Yao, Zhitong; Xia, Meisheng; Ye, Ying

2012-06-01

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

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

NASA Technical Reports Server (NTRS)

Tewari, S.N.

1995-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2010-01-01

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

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.

Ceramic thermal barrier coating for rapid thermal cycling applications

DOEpatents

Scharman, Alan J.; Yonushonis, Thomas M.

1994-01-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 ofmore » 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.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

2009-07-01

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

Anthropogenic- and natural sources of dust in peatland during the Anthropocene

NASA Astrophysics Data System (ADS)

Fiałkiewicz-Kozieł, B.; Smieja-Król, B.; Frontasyeva, M.; Słowiński, M.; Marcisz, K.; Lapshina, E.; Gilbert, D.; Buttler, A.; Jassey, V. E. J.; Kaliszan, K.; Laggoun-Défarge, F.; Kołaczek, P.; Lamentowicz, M.

2016-12-01

As human impact have been increasing strongly over the last decades, it is crucial to distinguish human-induced dust sources from natural ones in order to define the boundary of a newly proposed epoch - the Anthropocene. Here, we track anthropogenic signatures and natural geochemical anomalies in the Mukhrino peatland, Western Siberia. Human activity was recorded there from cal AD 1958 (±6). Anthropogenic spheroidal aluminosilicates clearly identify the beginning of industrial development and are proposed as a new indicator of the Anthropocene. In cal AD 1963 (±5), greatly elevated dust deposition and an increase in REE serve to show that the geochemistry of elements in the peat can be evidence of nuclear weapon testing; such constituted an enormous force blowing soil dust into the atmosphere. Among the natural dust sources, minor signals of dryness and of the Tunguska cosmic body (TCB) impact were noted. The TCB impact was indirectly confirmed by an unusual occurrence of mullite in the peat.

Determining and analyzing the strength and impact resistance of high modulus glass

NASA Technical Reports Server (NTRS)

Bacon, J. F.

1972-01-01

A number of new glass compositions have been prepared with increased emphasis on compositions without beryllia. Glass preparations have been much more broadly based and have included the eutectic glass fields, and the mullite-rare earth glass systems. Of the new glasses, the best non-toxic composition is UARL 472 with a bulk modulus of only 18.20 million psi. A second experimental glass, UARL 417, was chosen for research in making large quantities of fiber in monofilament form. Tests of these UARL 417 epoxy resin samples in comparison to similar composites made with the DuPont organic fiber, PRD-49-1, show that the UARL composites have a compressive strength 41/2 times higher and a specific compressive strength at least 21/2 times greater. Much of the research effort attempted to answer the question of why a given glass should have an impact strength superior to other glasses. No definitive answer to the question was found.

Anthropogenic- and natural sources of dust in peatland during the Anthropocene

PubMed Central

Fiałkiewicz-Kozieł, B.; Smieja-Król, B.; Frontasyeva, M.; Słowiński, M.; Marcisz, K.; Lapshina, E.; Gilbert, D.; Buttler, A.; Jassey, V. E. J.; Kaliszan, K.; Laggoun-Défarge, F.; Kołaczek, P.; Lamentowicz, M.

2016-01-01

As human impact have been increasing strongly over the last decades, it is crucial to distinguish human-induced dust sources from natural ones in order to define the boundary of a newly proposed epoch - the Anthropocene. Here, we track anthropogenic signatures and natural geochemical anomalies in the Mukhrino peatland, Western Siberia. Human activity was recorded there from cal AD 1958 (±6). Anthropogenic spheroidal aluminosilicates clearly identify the beginning of industrial development and are proposed as a new indicator of the Anthropocene. In cal AD 1963 (±5), greatly elevated dust deposition and an increase in REE serve to show that the geochemistry of elements in the peat can be evidence of nuclear weapon testing; such constituted an enormous force blowing soil dust into the atmosphere. Among the natural dust sources, minor signals of dryness and of the Tunguska cosmic body (TCB) impact were noted. The TCB impact was indirectly confirmed by an unusual occurrence of mullite in the peat. PMID:27995953

Influences of powder granularity on crystallizing characteristics in mica-contained glass ceramic

NASA Astrophysics Data System (ADS)

Xu, L. N.; Kong, D. Y.; Tian, Q. B.; Lv, Z. J.

2017-09-01

A machinable mica-contained glass ceramic in the SiO2-Al2O3-MgO-F glassy system was prepared by ball milling and hot pressed sintering. Three kinds of powder sizes of base glass were chosen and the effects of the glass powder sizes on the crystallization were explored by x-ray diffraction and scanning electron microscopy techniques. The results indicate that mica crystal as a major phase and KFeSi2O6 and mullite as minor phases are crystallized. Applying pressure at 670°C has little influences on the types of crystal precipitated and the preferential growth of crystal. The powder sizes, however, have obvious effects on the morphology of precipitated mica crystals. In the glass sample with a powder size of d50=16.4 µm, the plate-shaped mica phase is precipitated. As the powder size decrease to 9.9 µm and 3.3 µm, however, the particle-shaped mica is formed instead of the plate-shaped crystals.

Mineralogy of ash of some American coals: variations with temperature and source

USGS Publications Warehouse

Mitchell, R.S.; Gluskoter, H.J.

1976-01-01

Ten samples of mineral-matter residue were obtained by the radio-frequency low-temperature ashing of subbituminous and bituminous coals. The low-temperature ash samples were then heated progressively from 400 ??C to 1400 ??C at 100 ??C intervals. Mineral phases present at each temperature interval were determined by X-ray diffraction analyses. The minerals originally present in the coals (quartz, kaolinite, illite, pyrite, calcite, gypsum, dolomite, and sphalerite) were all altered to higher temperature phases. Several of these phases, including kaolinite, metakaolinite, mullite, anhydrite, and anorthite, were found only in limited temperature ranges. Therefore the temperature of formation of the ashes in which they occur may be determined. Mineralogical differences were observed between coal samples from the Rocky Mountain Province, the Illinois Basin, and the Appalachians; and as a result of these mineralogical differences, different high-temperature phases resulted as the samples were heated. However, regional generalizations cannot be made until a greater number of samples have been studied. ?? 1976.

Hot corrosion of ceramic engine materials

NASA Technical Reports Server (NTRS)

Fox, Dennis S.; Jacobson, Nathan S.; Smialek, James L.

1988-01-01

A number of commercially available SiC and Si3N4 materials were exposed to 1000 C in a high velocity, pressurized burner rig as a simulation of a turbine engine environment. Sodium impurities added to the burner flame resulted in molten Na2SO4 deposition, attack of the SiC and Si4N4 and formation of substantial Na2O-x(SiO2) corrosion product. Room temperature strength of the materials decreased. This was a result of the formation of corrosion pits in SiC, and grain boundary dissolution and pitting in Si3N4. Corrosion regimes for such Si-based ceramics have been predicted using thermodynamics and verified in rig tests of SiO2 coupons. Protective mullite coatings are being investigated as a solution to the corrosion problem for SiC and Si3N4. Limited corrosion occurred to cordierite (Mg2Al4Si5O18) but some cracking of the substrate occurred.

The Leaching of Aluminium In Spanish Clays, Coal Mining Wastes and Coal Fly Ashes by Sulphuric Acid.

NASA Astrophysics Data System (ADS)

Fernández, A. M.; Ibáñez, J. L.; Llavona, M. A.; Zapico, R.

The acid leaching of aluminium from several non traditional ores, bayerite, kaolinite, different clays, coal mining wastes and coal fly ashes, and the kinetic of their dissolution are described. The effects of time, temperature, acid concentration, sample calcination, particle size were examined. The leaching of aluminium is dependent on acid concentration and strongly on temperature. Generally, the time to reach a fixed percentage of dissolution decreases with increasing acid concentration in the range 6% to 40% acid by weight. On clays and coal mining wastes a good relation between Al removal and ratio kaolinite/illite was also observed at all temperatures and acid concentration tested. Coal fly ashes are particles that were heated at very high temperatures in the power station and Al compounds were transformed into mullite and so Al recovery was minor. Several rate equations describing the kinetics of the leach reaction were discussed and Kinetic parameters and activation energy values of samples are presented.

Development, solar test, and evaluation of a high-temperature air receiver for point-focusing parabolic dish applications

NASA Technical Reports Server (NTRS)

Hanseth, E. J.

1981-01-01

A high temperature solar receiver was fabricated and tested in excess of 1370 C on an 11-meter-diameter test bed concentrator at the Jet Propulsion Laboratory Parabolic Dish Test Site, Edwards, California. The 60-kilowatt thermal receiver design utilizes state-of-the-art silicon carbide honeycomb matrix panels to receive and transfer the solar energy and mullite elements for thermal buffer storage. Solar tests were conducted with indicated air exit temperatures ranging from 885 C (1625 F) to 1427 C (2600 F), mass flow rates of 75 to 105 g/sec (0.16 to 0.23 lbm/sec), and pressures up to 265 kPa absolute (38.4 psia). Estimates of efficiency are 59.7% at 1120 C (2048 F) to 80.6% at 885 C (1625 F) when aperture spillage losses are considered separately. Results are presented which demonstrate the feasibility of this innovative receiver concept for point-focusing parabolic dish applications over a wide temperature range.

Alumosilicate ceramic proppants based on natural refractory raw materials

NASA Astrophysics Data System (ADS)

Vakalova, T. V.; Devyashina, L. P.; Burihina, M. A.; Kisner, A. S.; Pashenko, N. V.

2017-12-01

The sintering-strengthening effect of the additions of the highly ferrous bauxite (with Fe2O3 content of 20-25 % in the calcined state) in the compositions with refractory clays was established. It was found that in the temperature range 1350-1500°C the additions of bauxite in amounts of 10-40% have a fluxing effect due to the iron oxide introduced with bauxite in compositions with clay. An increasing the bauxite additive in the amount of 50-70% ensures its strengthening effect by increasing the total content of the mullite of the prismatic habit in the firing products of composites with clay. Preliminary clay and bauxite calcination at 900 °C and an increase in the content of bauxite additive up to 50-70% in compositions with clay allow to produce aluminosilicate proppants with a bulk density of 1.62-1.65 g/cm3 and compressive strength up to 52 MPa.

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.

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1990-01-01

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

The plasma electrolytic oxidation micro-discharge channel model and its microstructure characteristic based on Ti tracer

NASA Astrophysics Data System (ADS)

Gao, Fangyuan; Hao, Li; Li, Guang; Xia, Yuan

2018-02-01

This study focuses on the individual discharge channel of ceramic coating prepared by plasma electrolytic oxidation (PEO), and attempts to reveal the mechanism of breakdown discharge at low voltage. Titanium (Ti) was employed as a substrate with the layer of aluminum deposited on it (aluminized Ti). The shape and microstructure of the discharge channels in PEO coatings were investigated using transmission electron microscope (TEM) and scanning electron microscopy (SEM). A schematic model of the individual discharge channel was proposed based on Ti tracer method. The shape of the discharge channel was mainly cylinder-shaped in the compact coating, with a groove-like oxidation region existed at the coating/substrate interface. In the groove-like oxidation region, the phase composition mainly composed of amorphous and mixed polycrystalline (aluminum titanate and mullite). β-Al2O3 was found in the ceramic coating. TEM morphology showed that nanometer sized micro channels existed in the ceramic coatings.

Anthropogenic- and natural sources of dust in peatland during the Anthropocene.

PubMed

Fiałkiewicz-Kozieł, B; Smieja-Król, B; Frontasyeva, M; Słowiński, M; Marcisz, K; Lapshina, E; Gilbert, D; Buttler, A; Jassey, V E J; Kaliszan, K; Laggoun-Défarge, F; Kołaczek, P; Lamentowicz, M

2016-12-20

As human impact have been increasing strongly over the last decades, it is crucial to distinguish human-induced dust sources from natural ones in order to define the boundary of a newly proposed epoch - the Anthropocene. Here, we track anthropogenic signatures and natural geochemical anomalies in the Mukhrino peatland, Western Siberia. Human activity was recorded there from cal AD 1958 (±6). Anthropogenic spheroidal aluminosilicates clearly identify the beginning of industrial development and are proposed as a new indicator of the Anthropocene. In cal AD 1963 (±5), greatly elevated dust deposition and an increase in REE serve to show that the geochemistry of elements in the peat can be evidence of nuclear weapon testing; such constituted an enormous force blowing soil dust into the atmosphere. Among the natural dust sources, minor signals of dryness and of the Tunguska cosmic body (TCB) impact were noted. The TCB impact was indirectly confirmed by an unusual occurrence of mullite in the peat.

Phase transformations and residual stresses in environmental barrier coatings

NASA Astrophysics Data System (ADS)

Harder, Bryan J.

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

Effects of Environment on Creep Behavior of Nextel 720/Alumina-Mullite Ceramic Composite at 1200 deg C

DTIC Science & Technology

2008-03-01

creep life . This degradation increased with increasing temperatures. At 1000°, all specimens achieved creep run-out, defined as...strain measurement 29 Table 4. Summary of N720/AM creep data. Sample Environment Thermal Strain (%) E (GPa) Creep Stress (MPa) Creep Life (h...Material Creep Stress(MPa) Creep Life (h) Creep Strain (%) Secondary Creep Rate (s-1) N720/A 80 >100 0.798 1.5E-08 N720/A 100 41 1.520

Sliding durability of candidate seal fiber materials in hydrogen from 25 to 900 C

NASA Technical Reports Server (NTRS)

Dellacorte, Christopher; Steinetz, Bruce M.

1992-01-01

Sliding durability studies of candidate ceramic fibers were conducted in hydrogen to support the high temperature seal development program at NASA LeRC. Pin-on-disk tests were used to measure the friction and durability of a tow or bundle of ceramic fibers in sliding against a superalloy disk. This procedure was used previously to test candidate fibers in an air environment. The fibers based upon mullite (Al2O3-SiO2) chemistry (Nextel 550, 440, and 312) exhibited better durability in hydrogen than in air. HPZ, a complex silicon carboxynitride fiber which showed good durabilty in air, however, showed a significant loss of durability in hot hydrogen. These results are consistent with recent thermodynamic and experimental studies of ceramic compatibility with hydrogen at elevated temperatures. These research results indicate that only oxide fibers display good durability in both air and hydrogen environments. Also, simple, low cost testing in air can provide an adequate data base for initial seal material screening and selection, especially for oxide fiber candidates. The findings of this research provide critical input to the seal design team.

Heat flux measurements on ceramics with thin film thermocouples

NASA Technical Reports Server (NTRS)

Holanda, Raymond; Anderson, Robert C.; Liebert, Curt H.

1993-01-01

Two methods were devised to measure heat flux through a thick ceramic using thin film thermocouples. The thermocouples were deposited on the front and back face of a flat ceramic substrate. The heat flux was applied to the front surface of the ceramic using an arc lamp Heat Flux Calibration Facility. Silicon nitride and mullite ceramics were used; two thicknesses of each material was tested, with ceramic temperatures to 1500 C. Heat flux ranged from 0.05-2.5 MW/m2(sup 2). One method for heat flux determination used an approximation technique to calculate instantaneous values of heat flux vs time; the other method used an extrapolation technique to determine the steady state heat flux from a record of transient data. Neither method measures heat flux in real time but the techniques may easily be adapted for quasi-real time measurement. In cases where a significant portion of the transient heat flux data is available, the calculated transient heat flux is seen to approach the extrapolated steady state heat flux value as expected.

Transformation toughened ceramics for the heavy duty diesel engine technology program

NASA Technical Reports Server (NTRS)

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

1984-01-01

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

The Influence of Interfacial Roughness on Fiber Sliding in Oxide Composites with La-Monazite Interphases

NASA Technical Reports Server (NTRS)

Davis, J. B.; Hay, R. S.; Marshall, D. B.; Morgan, P. E. D.; Sayir, A.; Gray, Hugh R. (Technical Monitor); Farmer, Serene C. (Technical Monitor)

2002-01-01

Room temperature debonding and sliding of La-Monazite coated fibers is assessed using a composite with a polycrystalline alumina matrix and fibers of several different single crystal (mullite, sapphire) and directionally solidified eutectic (Al2O3/Y3Al5O12 and Al2O3/Y-ZrO2) compositions. These fibers provide a range of residual stresses and interfacial roughnesses. Sliding occurred over a debond crack at the fiber-coating interface when the sliding displacement and surface roughness were relatively small. At large sliding displacements with relatively rough interfaces, the monazite coatings were deformed extensively by fracture, dislocations and occasional twinning, whereas the fibers were undamaged. Dense, fine-grained (10 nm) microstructures suggestive of dynamic recrystallization were also observed in the coatings. Frictional heating during sliding is assessed. The possibility of low temperature recrystallization is discussed in the light of the known resistance of monazite to radiation damage. The ability of La-Monazite to undergo plastic deformation relatively easily at low temperatures may be enabling for its use as a composite interface.

Spinel formation for stabilizing simulated nickel-laden sludge with aluminum-rich ceramic precursors.

PubMed

Shih, Kaimin; White, Tim; Leckie, James O

2006-08-15

The feasibility of stabilizing nickel-laden sludge from commonly available Al-rich ceramic precursors was investigated and accomplished with high nickel incorporation efficiency. To simulate the process, nickel oxide was mixed alternatively with gamma-alumina, corundum, kaolinite, and mullite and was sintered from 800 to 1480 degrees C. The nickel aluminate spinel (NiAl2O4) was confirmed as the stabilization phase for nickel and crystallized with efficiencies greater than 90% for all precursors above 1250 degrees C and 3-h sintering. The nickel-incorporation reaction pathways with these precursors were identified, and the microstructure and spinel yield were investigated as a function of sintering temperature with fixed sintering time. This study has demonstrated a promising process for forming nickel spinel to stabilize nickel-laden sludge from a wide range of inexpensive ceramic precursors, which may provide an avenue for economically blending waste metal sludges via the building industry processes to reduce the environmental hazards of toxic metals. The correlation of product textures and nickel incorporation efficiencies through selection of different precursors also provides the option of tailoring property-specific products.

Component effects on crystallization of RE-containing aluminoborosilicate glass

NASA Astrophysics Data System (ADS)

Mohd Fadzil, Syazwani; Hrma, Pavel; Schweiger, Michael J.; Riley, Brian J.

2016-09-01

Lanthanide-aluminoborosilicate (LABS) glass is one option for immobilizing rare earth (RE) oxide fission products generated during reprocessing of pyroprocessed fuel. This glass system can accommodate a high loading of RE oxides and has excellent chemical durability. The present study describes efforts to model equilibrium crystallinity as a function of glass composition and temperature as well as liquidus temperature (TL) as a function of glass composition. The experimental method for determining TL was ASTM C1720-11. Typically, three crystalline phases were formed in each glass: Ce-borosilicate (Ce3BSi2O10), mullite (Al10Si2O19), and corundum (Al2O3). Cerianite (CeO2) was a common minor crystalline phase and Nd-silicate (Nd2Si2O7) occurred in some of the glasses. In the composition region studied, TL decreased as SiO2 and B2O3 fractions increased and strongly increased with increasing fractions of RE oxides; Al2O3 had a moderate effect on the TL but, as expected, it strongly affected the precipitation of Al-containing crystals.

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

NASA Technical Reports Server (NTRS)

Pearson, A.

1975-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2005-01-01

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

Hollow proppants and a process for their manufacture

DOEpatents

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

1985-10-15

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

Competitive adsorption of Pb2+ and Zn2+ ions from aqueous solutions by modified coal fly ash

NASA Astrophysics Data System (ADS)

Astuti, Widi; Martiani, Wulan; Any Ismawati Khair, N.

2017-03-01

Coal fly ash (CFA), which is a solid waste generated in large amounts worldwide, is mainly composed of some oxides having high crystallinity, including quartz (SiO2) and mullite (3Al2O3 2SiO2), and unburned carbon as a mesopore material that enables it to act as a dual site adsorbent. To decrease the crystallinity, CFA was modified by sodium hydroxide treatment. The modified fly ash (MFA) contains lower amount of Si and Al and has a higher specific surface area than the untreated fly ash (CFA). The objective of this study is to investigate the competitive adsorption of Pb2+ and Zn2+ from aqueous solutions by CFA and MFA. The effect of pH, contact time and initial concentration was investigated. Effective pH for Pb2+ and Zn2+ removal was 4. A greater percentage of Pb2+ and Zn2+ was removed with a decrease in the initial concentration of Pb2+ and Zn2+. Quasi-equilibrium reached in 240 min.

Crack-resistant Al2O3–SiO2 glasses

PubMed Central

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

2016-01-01

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

Crack-resistant Al2O3-SiO2 glasses.

PubMed

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

2016-04-07

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

Hollow proppants and a process for their manufacture

DOEpatents

Jones, Arfon H.; Cutler, Raymond A.

1985-01-01

Hollow, fine-grained ceramic proppants are less expensive and improve fracture control when compared to conventional proppants (dense alumina, mullite, bauxite, zirconia, etc.). Hollow proppants of the present invention have been fabricated by spray drying, followed by sintering in order to obtain a dense case and a hollow core. These proppants generally have high sphericity and roundness (Krumbein sphericity and roundness greater than 0.8), have diameters on average between 2250 and 125 .mu.m, depending on proppant size required, and have strength equal to or greater than that of sand. The hollow core, the size of which can be controlled, permits better fracture control in hydraulic fracturing treatments since the proppant can be transported in lower viscosity fluids. Hollow proppants produced at the same cost/weight as conventional proppants also provide for lower costs, since less weight is required to fill the same volume. The fine-grained (preferably less than 5 .mu.m in diameter) ceramic case provides the strength necessary to withstand closure stresses and prevent crushing.

Crack-resistant Al2O3-SiO2 glasses

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

Continuous coating of silicon-on-ceramic

NASA Technical Reports Server (NTRS)

Heaps, J. D.; Schuldt, S. B.; Grung, B. L.; Zook, J. D.; Butter, C. D.

1980-01-01

Growth of sheet silicon on low-cost substrates has been demonstrated by the silicon coating with inverted meniscus (SCIM) technique. A mullite-based ceramic substrate is coated with carbon and then passed over a trough of molten silicon with a raised meniscus. Solidification occurs at the trailing edge of the downstream meniscus, producing a silicon-on-ceramic (SOC) layer. Meniscus shape and stability are controlled by varying the level of molten silicon in a reservoir connected to the trough. The thermal conditions for growth and the crystallographic texture of the SOC layers are similar to those produced by dip-coating, the original technique of meniscus-controlled growth. The thermal conditions for growth have been analyzed in some detail. The analysis correctly predicts the velocity-thickness relationship and the liquid-solid interface shape for dip-coating, and appears to be equally applicable to SCIM-coating. Solar cells made from dip-coated SOC material have demonstrated efficiencies of 10% on 4-sq cm cells and 9.9% on 10-sq cm cells.

Thermal Conductivity and Water Vapor Stability of Ceramic HfO2-Based Coating Materials

NASA Technical Reports Server (NTRS)

Zhu, Dong-Ming; Fox, Dennis S.; Bansal, Narottam P.; Miller, Robert A.

2004-01-01

HfO2-Y2O3 and La2Zr2O7 are candidate thermal/environmental barrier coating materials for gas turbine ceramic matrix composite (CMC) combustor liner applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature phase stability of plasma-sprayed coatings and/or hot-pressed HfO2-5mol%Y2O3, HfO2-15mol%Y2O3 and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasma-sprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC Hexoloy or CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications will also be discussed.

Thermal Conductivity and Stability of HfO2-Y2O3 and La2Zr2O7 Evaluated for 1650 Deg C Thermal/Environmental Barrier Coating Applications

NASA Technical Reports Server (NTRS)

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

2003-01-01

HfO2-Y2O3 and La2Zr2O7 are candidate thermal and environmental barrier coating (T/EBC) materials for gas turbine ceramic matrix composite (CMC) combustor applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature stability of hot-pressed and plasma sprayed specimens with representative partially-stabilized and fully-cubic HfO2-Y2O3 compositions and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasmasprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC hexoloy or SiC/SiC CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications are also discussed.

Effect of Steam Environment on Creep Behavior of Nextel720/Alumina-Mullite Ceramic Matrix Composite at Elevated Temperature

DTIC Science & Technology

2009-03-01

specimens achieving creep run-out of 100 h. Presence of v steam caused larger creep strains and the higher stress levels decreased the creep life ...tested at the same stress levels in other environments. He reported that environment did not appear to have a significant influence on the creep life of...MPa) Elastic Modulus (GPa) Creep Strain (%) Creep Life (h) 6* Air 1100 65.2 109 0.2 >100 7* Air 1100 64.7 131 0.23 >100 8 Steam 1100 62.9

Environmental Barrier Coatings for Ceramic Matrix Composites - An Overview

NASA Technical Reports Server (NTRS)

Lee, Kang; Zhu, Dongming; Wiesner, Valerie Lynn; van Roode, Mark; Kashyap, Tania; Zhu, Dongming; Wiesner, Valerie

2016-01-01

Ceramic Matrix Composites (CMCs) are increasingly being considered as structural materials for advanced power generation equipment. Broadly speaking the two classes of materials are oxide-based CMCs and non-oxide based CMCs. The non-oxide CMCs are primarily silicon-based. Under conditions prevalent in the gas turbine hot section the water vapor formed in the combustion of gaseous or liquid hydrocarbons reacts with the surface-SiO2 to form volatile products. Progressive surface recession of the SiC-SiC CMC component, strength loss as a result of wall thinning and chemical changes in the component occur, which leads to the loss of structural integrity and mechanical strength and becomes life limiting to the equipment in service. The solutions pursued to improve the life of SiC-SiC CMCs include the incorporation of an external barrier coating to provide surface protection to the CMC substrate. The coating system has become known as an Environmental Barrier Coating (EBC). The relevant early coatings work was focused on coatings for corrosion protection of silicon-based monolithic ceramics operating under severely corrosive conditions. The development of EBCs for gas turbine hot section components was built on the early work for silicon-based monolithics. The first generation EBC is a three-layer coating, which in its simplest configuration consists of a silicon (Si) base coat applied on top of the CMC, a barium-strontium-aluminosilicate (BSAS) surface coat resistant to water vapor attack, and a mullite-based intermediate coating layer between the Si base coat and BSAS top coat. This system can be represented as Si-Mullite-BSAS. While this baseline EBC presented a significant improvement over the uncoated SiC-SiC CMC, for the very long durations of 3-4 years or more expected for industrial operation further improvements in coating durability are desirable. Also, for very demanding applications with higher component temperatures but shorter service lives more rugged EBCs

High-Temperature Erosive Behavior of Plasma Sprayed Cr3C2-NiCr/Cenosphere Coating

NASA Astrophysics Data System (ADS)

Mathapati, Mahantayya; Doddamani, Mrityunjay; Ramesh, M. R.

2018-02-01

This research examines the deposition of Cr3C2-NiCr/cenosphere and Cr3C2-NiCr coatings on MDN 321 steel through the process of plasma spray. In this process, the solid particle erosion test is established at 200, 400, 600 °C with 30° and 90° impact angles. Alumina erodent is adopted to investigate the erosive behavior of the coating at higher temperatures. The properties of the Cr3C2-NiCr/cenosphere coating are established based on the microhardness, the adhesive strength, the fracture toughness, and the ductility. To quantify volume loss as a result of erosion, an optical profilometer is used. At higher temperature, decrease in the erosion volume loss of Cr3C2-NiCr/cenosphere and Cr3C2-NiCr coatings is observed. The erosion-resistive property of Cr3C2-NiCr/cenosphere coating is higher than that of MDN 321 steel by 76%. This property is influenced by high-temperature stability of mullite, alumina, and protective oxide layer that is formed at elevated temperatures. The morphology of eroded coating discloses a brittle mode of material removal.

Cyclic Failure Mechanisms of Thermal and Environmental Barrier Coating Systems Under Thermal Gradient Test Conditions

NASA Technical Reports Server (NTRS)

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

2002-01-01

Plasma-sprayed ZrO2-8wt%Y2O3 and mullite+BSAS/Si multilayer thermal and environmental barrier coating (TBC-EBC) systems on SiC/SiC ceramic matrix composite (CMC) substrates were thermally cyclic tested under high thermal gradients using a laser high-heat-flux rig in conjunction with furnace exposure in water-vapor environments. Coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after exposure. Sintering kinetics of the coating systems were also independently characterized using a dilatometer. It was found that the coating failure involved both the time-temperature dependent sintering and the cycle frequency dependent cyclic fatigue processes. The water vapor environments not only facilitated the initial coating conductivity increases due to enhanced sintering and interface reaction, but also promoted later conductivity reductions due to the accelerated coating cracking and delamination. The failure mechanisms of the coating systems are also discussed based on the cyclic test results and are correlated to the sintering and thermal stress behavior under the thermal gradient test conditions.

Current Issues with Environmental Barrier Coatings for Ceramics and Ceramic Composites

NASA Technical Reports Server (NTRS)

Lee, Kang N.

2004-01-01

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohd Fadzil, Syazwani; Hrma, Pavel; Schweiger, Michael J.

Lanthanide-aluminoborosilicate (LABS) glass is one option for immobilizing rare earth (RE) oxide fission products generated during reprocessing of pyroprocessed fuel. This glass system can accommodate a high loading of RE oxides and has excellent chemical durability. The present study describes efforts to model equilibrium crystallinity as a function of glass composition and temperature as well as liquidus temperature (TL) as a function of glass composition. The experimental method for determining TL was ASTM C1720-11. Typically, three crystalline phases were formed in each glass: Ce-borosilicate (Ce 3BSi 2O 10), mullite (Al 10Si 2O 19), and corundum (Al 2O 3). Cerianite (CeOmore » 2) was a common minor crystalline phase and Nd-silicate (Nd 2Si 2O 7) occurred in some of the glasses. In the composition region studied, TL decreased as SiO 2 and B 2O 3 fractions increased and strongly increased with increasing fractions of RE oxides; Al 2O 3 had a moderate effect on the TL but, as expected, it strongly affected the precipitation of Alcontaining crystals.« less

Development and Testing of a Refractory Millimeter-Wave Absorbent Heat Exchanger

NASA Technical Reports Server (NTRS)

Lambot, Thomas; Myrabo, Leik; Murakami, David; Parkin, Kevin

2014-01-01

Central to the Millimeter-Wave Thermal Launch System (MTLS) is the millimeter-wave absorbent heat exchanger. We have developed metallic and ceramic variants, with the key challenge being the millimeter-wave absorbent coatings for each. The ceramic heat exchanger came to fruition first, demonstrating for the first time 1800 K peak surface temperatures under illumination by a 110 GHz Gaussian beam. Absorption efficiencies of up to 80 are calculated for mullite heat exchanger tubes and up to 50 are calculated for alumina tubes. These are compared with estimates based on stratified layer and finite element analyses. The problem of how to connect the 1800 K end of the ceramic tubes to a graphite outlet manifold and nozzle is solved by press fitting, or by threading the ends of the ceramic tubes and screwing them into place. The problem of how to connect the ceramic tubes to a metallic or nylon inlet pipe is solved by using soft compliant PTFE and PVC tubes that accommodate thermal deformations of the ceramic tubes during startup and operation. We show the resulting heat exchangers in static tests using argon and helium as propellants.

Elevated-temperature fracture resistances of monolithic and composite ceramics using chevron-notched bend tests

NASA Technical Reports Server (NTRS)

Ghosh, Asish; Jenkins, Michael G.; Ferber, Mattison K.; Peussa, Jouko; Salem, Jonathan A.

1992-01-01

The quasi-static fracture behaviors of monolithic ceramics (SiC, Si3N4, MgAl2O4), self-reinforced monoliths (acicular grained Si3N4, acicular grained mullite), and ceramic matrix composites (SiC whisker/Al2O3 matrix, TiB2 particulate/SiC matrix, SiC fiber/CVI SiC matrix, Al2O3 fiber/CVI SiC matrix) were measured over the temperature range of 20 to 1400 C. The chevron notched, bend bar test geometry was essential for characterizing the elevated temperature fracture resistances of this wide range of quasi-brittle materials during stable crack growth. Fractography revealed the differences in the fracture behavior of the different materials at the various temperatures. The fracture resistances of the self-reinforced monoliths were comparable to those of the composites and the fracture mechanisms were found to be similar at room temperature. However at elevated temperatures the differences of the fracture behavior became apparent where the superior fracture resistance of the self-reinforced monoliths were attributed to the minor amounts of glassy, intergranular phases which were often more abundant in the composites and affected the fracture behavior when softened by elevated temperatures.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaneko, Gen-yo; Kitagawa, Hiroyuki; Hasezaki, Kazuhiro

2008-02-15

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

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Correlation between thermal behavior of clays and their chemical and mineralogical composition: a review

NASA Astrophysics Data System (ADS)

Dwi Yanti, Evi; Pratiwi, I.

2018-02-01

Clay's abundance has been widely used as industrial raw materials, especially ceramic and tile industries. Utilization of these minerals needs a thermal process for producing ceramic products. Two studies conducted by Septawander et al. and Chin C et al., showed the relationship between thermal behavior of clays and their chemical and mineralogical composition. Clays are characterized by XRD analysis and thermal analysis, ranging from 1100°C to 1200°C room temperature. Specimen of raw materials of clay which is used for the thermal treatment is taken from different geological conditions and formation. In raw material, Quartz is almost present in all samples. Halloysite, montmorillonite, and feldspar are present in Tanjung Morawa raw clay. KC and MC similar kaolinite and illite are present in the samples. The research illustrates the interrelationships of clay minerals and chemical composition with their heat behavior. As the temperature of combustion increases, the sample reduces a significant weight. The minerals which have undergone a transformation phase became mullite, cristobalite or illite and quartz. Under SEM analysis, the microstructures of the samples showed irregularity in shape; changes occurred due the increase of heat.

Anisotropic lattice thermal expansion of PbFeBO 4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

DOE PAGES

Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; ...

2014-11-01

We present the lattice thermal expansion of mullite-type PbFeBO 4 in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. Moreover, the unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequenciesmore » of the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO4, FeO6 and BO3 polyhedra as a function of temperature.« less

Characterization of solid airborne particles deposited in snow in the vicinity of urban fossil fuel thermal power plant (Western Siberia).

PubMed

Talovskaya, A V; Yazikov, E G; Filimonenko, E A; Lata, J-C; Kim, J; Shakhova, T S

2017-07-20

Recognition and detailed characterization of solid particles emitted from thermal power plants into the environment is highly important due to their potential detrimental effects on human health. Snow cover is used for the identification of anthropogenic emissions in the environment. However, little is known about types, physical and chemical properties of solid airborne particles (SAP) deposited in snow around thermal power plants. The purpose of this study is to quantify and characterize in detail the traceable SAP deposited in snow near fossil fuel thermal power plant in order to identify its emissions into the environment. Applying the scanning electron microscopy-energy dispersive spectroscopy, and X-ray diffraction, mineral and anthropogenic phase groups in SAP deposited in snow near the plant and in fly ash were observed. We identified quartz, albite and mullite as most abundant mineral phases and carbonaceous matter, slag and spherical particles as dominate anthropogenic phases. This is the first study reporting that zircon and anthropogenic sulphide-bearing, metal oxide-bearing, intermetallic compound-bearing and rare-earth element-bearing particles were detected in snow deposits near thermal power plant. The identified mineral and anthropogenic phases can be used as tracers for fossil fuel combustion emissions, especially with regard to their possible effect on human health.

Development of Thin Film Thermocouples on Ceramic Materials for Advanced Propulsion System Applications

NASA Technical Reports Server (NTRS)

Holanda, R.

1992-01-01

Thin film thermocouples have been developed for use on metal parts in jet engines to 1000 c. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose of this work is to develop thin film thermocouples for use on ceramic materials. The new thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials tested are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high heating rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hours or more up to temperature of 1500 C depending on the stability of the particular ceramic substrate.

Thin film thermocouples for high temperature measurement on ceramic materials

NASA Technical Reports Server (NTRS)

Holanda, Raymond

1992-01-01

Thin film thermocouples have been developed for use on metal parts in jet engines to 1000 C. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose of this work is to develop thin film thermocouples for use on ceramic materials. The thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high-heating-rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hours or more up to temperatures of 1500 C depending on the stability of the particular ceramic substrate.

Development of thin film thermocouples on ceramic materials for advanced propulsion system applications

NASA Technical Reports Server (NTRS)

Holanda, Raymond

1993-01-01

Thin film thermocouples were developed for use on metal parts in jet engines to 1000 C. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose is to develop thin film thermocouples for use on ceramic materials. The new thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials tested are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high heating rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hr or more up to temperatures of 1500 C depending on the stability of the particular ceramic substrate.

Tribological and Corrosion Properties of Coatings Produced by Plasma Electrolytic Oxidation on the ZA27 Alloy

NASA Astrophysics Data System (ADS)

Li, Guangyin; Mao, Yifan; Li, Zhijian; Wang, Linlin; DaCosta, Herbert

2018-05-01

In this paper, a continuous and dense coating was deposited on samples of the ZA27 alloy through the plasma electrolytic oxidation (PEO) process to improve its wear and corrosion performance. A nontoxic and environmentally friendly inorganic salt, Na2SiO3, is chosen as electrolytes with different concentrations. The effect of the concentration of Na2SiO3 aqueous solutions on the coating performances was investigated. The coatings with 3Al2O3·2SiO2 (mullite), Zn2SiO4 and Al2O3 (either crystal phase or with some amorphous SiO2 phases) were formed by the PEO processes. It was found that the coating thickness increased with the increase in electrolyte concentration. However, the wear and corrosion resistance performance of the coatings did not improve as the coating's thickness increased. This was due to the fact that the coating produced with electrolytes of 10 g/L has a porous structure with large pore size. Among all the samples, coating produced by 15 g/L Na2SiO3 has the best wear and corrosion resistance, which is attributed to its continuous and dense structure with thickness of about 47 μm.

Optical and Mechanical Properties of Glass Blown In Vacuo

NASA Technical Reports Server (NTRS)

Manning, andrew; Tucker, Dennis; Mooney, Theodore; Herren, Kenneth; Gregory, Don A.

2006-01-01

Theoretically, the strength of glass processed in vacuum should be higher due to outgassing of contaminants normally present in the glass, such as bulk water in the form of OH bonds that tends to weaken the glass structure. In this research, small discs of a few types of glass have been subjected to various temperatures for extended periods of time in vacuum. Their strength was then tested using a standard flexure technique, facilitated by a custom-designed test fixture, and the results were compared to glass tested in air using the same fixture. The purpose of the glass blowing investigation was to prove the basic feasibility of a high-level concept for in-space manufacture of optical elements. The central requirement was that the glass bubble had to be blown into a support structure such that the bubble could be handled by manipulation of the structure. The blown bubble attached itself to a mullite ring geometrically and mechanically, as a demonstration in the initial experiments described here, by expanding through and around it. The vacuum system used was custom made, as were most of the components of the system, such as the heating element, the glass and ring support structure, and the gas inlet system that provided the pressure needed to blow the glass.

Improved ceramic heat exchange material

NASA Technical Reports Server (NTRS)

Mccollister, H. L.

1977-01-01

Improved corrosion resistant ceramic materials that are suitable for use as regenerative heat exchangers for vehicular gas turbines is reported. Two glass-ceramic materials, C-144 and C-145, have superior durability towards sulfuric acid and sodium sulfate compared to lithium aluminosilicate (LAS) Corning heat exchange material 9455. Material C-144 is a leached LAS material whose major crystalline phase is silica keatite plus mullite, and C-145 is a LAS keatite solid solution (S.S.) material. In comparison to material 9455, material C-144 is two orders of magnitude better in dimensional stability to sulfuric acid at 300 C, and one order of magnitude better in stability to sodium sulfate at 1000 C. Material C-145 is initially two times better in stability to sulfuric acid, and about one order of magnitude better in stability to sodium sulfate. Both C-144 and C-145 have less than 300 ppm delta L/L thermal expansion from ambient to 1000 C, and good dimensional stability of less than approximately 100 ppm delta L/L after exposure to 1000 C for 100 hours. The glass-ceramic fabrication process produced a hexagonal honeycomb matrix having an 85% open frontal area, 50 micrometer wall thickness, and less than 5% porosity.

The characterization of ceramic alumina prepared by using additive glass beads

NASA Astrophysics Data System (ADS)

Suprapedi; Muljadi; Sardjono, Priyo

2018-01-01

The ceramic alumina has been made by using additive glass bead (5 and 10 % wt.). There are two kinds of materials, such as : gamma Alumina and glass bead. Synthesis of alumina was done by ball milling for 24 hours, then the mixed powder was dried in drying oven at 100 °C for 6 hours. Furthermore, the dried powder was mixed by using 2 % of PVA and continued with compacted to form a pellet with pressure of 50 MPA. The next step is sintering process with variation temperature of 1150, 1200, 1250, 1300 and 1400 °C and holding time for 2 hours. The characterization conducted are consist of test density, hardness, shrinkage, and microstructure. The results show that ceramic alumina with addition of 10 % wt. glass bead has the higher value of density, hardness and shrinkage than addition of 5% wt. glass bead. The highest characterization of ceramic alumina with addition 10 % glass bead was achieved at sintering temperature of 1400 °C with density 3.68 g/cm3, hardness vickers 780.40 Hv and shrinkage 15.23 %. The XRD results show that it was founds a corrundum (alpha Alumina) as dominant phase and mullite as minor phase.

Investigation of aluminosilicate as a solid oxide fuel cell refractory

NASA Astrophysics Data System (ADS)

Gentile, Paul S.; Sofie, Stephen W.

2011-05-01

Aluminosilicate represents a potential low cost alternative to alumina for solid oxide fuel cell (SOFC) refractory applications. The objectives of this investigation are to study: (1) changes of aluminosilicate chemistry and morphology under SOFC conditions, (2) deposition of aluminosilicate vapors on yttria stabilized zirconia (YSZ) and nickel, and (3) effects of aluminosilicate vapors on SOFC electrochemical performance. Thermal treatment of aluminosilicate under high temperature SOFC conditions is shown to result in increased mullite concentrations at the surface due to diffusion of silicon from the bulk. Water vapor accelerates the rate of surface diffusion resulting in a more uniform distribution of silicon. The high temperature condensation of volatile gases released from aluminosilicate preferentially deposit on YSZ rather than nickel. Silicon vapor deposited on YSZ consists primarily of aluminum rich clusters enclosed in an amorphous siliceous layer. Increased concentrations of silicon are observed in enlarged grain boundaries indicating separation of YSZ grains by insulating glassy phase. The presence of aluminosilicate powder in the hot zone of a fuel line supplying humidified hydrogen to an SOFC anode impeded peak performance and accelerated degradation. Energy dispersive X-ray spectroscopy detected concentrations of silicon at the interface between the electrolyte and anode interlayer above impurity levels.

Comparative study of the microstructural and magnetic properties of fly ashes obtained from different thermal power plants in West Bengal, India.

PubMed

Bhattacharjee, Ashis; Mandal, Haradhan; Roy, Madhusudan; Kusz, Joachim; Hofmeister, Wolfgang

2013-10-01

This paper deals with the physical nature of the fly ashes obtained from two thermal power plants, situated in West Bengal, India. The fly ash samples are characterized by using comprehensive techniques with an emphasis on their ultrafine nature. The particle sizes of the samples are estimated using scanning electron microcopy (SEM) and found to lie within 0.18-5.90 μm. For morphology and compositional analysis, we also use SEM coupled with energy dispersive X-ray spectrometry. From X-ray study of the fly ashes the nature of conglomeration is seen to be crystalline, and the major components are mullite (Al6Si2O13) and quartz (SiO2). The magnetic measurement of the fly ash samples was carried out by SQUID magnetometer. (57)Fe Mössbauer spectra are obtained using a conventional constant-acceleration spectrometer with a (57)Co/Rh Mössbauer source. The hyperfine parameters obtained, in general, support the findings as made from XRD analysis and provide a quantitative measure of different iron ions present in the samples. The paper presents experimental data on the physical aspects of the fly ash samples of the thermal power plants which comprise coarse, fine, and ultrafine magnetic particulate materials and attempts to provide an exhaustive analysis.

Performance of Nitrogen and Phosphorus Removal in Petrochemical Wastewater by Zeolited Fly Ash

NASA Astrophysics Data System (ADS)

Li, Zheng; Gu, Guizhou; Ji, Shenghao

2018-05-01

The zeolitized fly ash was synthesized by alkali melt hydrothermal method. The cation exchange capacity of zeolitized fly ash was far greater than the raw material fly ash. The main component was NaP1 zeolite (Na6Al6Si10O32·12H2O), followed by mullite, and a small amount of heterozygous crystals. The effect of synthetic zeolite dosage, pH value, adsorption time and reaction temperature on the effect of nitrogen and phosphorus removal in petrochemical wastewater were investigated. The results showed that when the zeolitized fly ash dosage was 9 g/L, the petrochemical wastewater pH value was 6∼8, adsorption time was 30 min and the reaction temperature was 30°C, the synthetic zeolite had the best effect on the removal of TN and TP in petrochemical wastewater, and the removal was 65.5%, 91.4% respectively. Besides, the concentrations of TN and TP in the effluent were 11.04 mg/L, 0.31 mg/L respectively. The concentrations met the sewage discharge standard in petrochemical industry of "Liaoning sewage comprehensive discharge standard" (DB21 1627-2008). This study was to realize the comprehensive utilization of solid waste and achieve the purpose of waste and waste.

Structure of high alumina content Al2O3-SiO2 composition glasses.

PubMed

Weber, Richard; Sen, Sabyasachi; Youngman, Randall E; Hart, Robert T; Benmore, Chris J

2008-12-25

The structure of binary aluminosilicate glasses containing 60-67 mol % Al2O3 were investigated using high-resolution 27Al NMR and X-ray and neutron diffraction. The glasses were made by aerodynamic levitation of molten oxides. The 67% alumina composition required a cooling rate of approximately 1600 degrees C s(1-) to form glass from submillimeter sized samples. NMR results show that the glasses contain aluminum in 4-, 5-, and 6-fold coordination in the approximate ratio 4:5:1. The average Al coordination increases from 4.57 to 4.73 as the fraction of octahedral Al increases with alumina content. The diffraction results on the 67% composition are consistent with a disordered Al framework with Al ions in a range of coordination environments that are substantially different from those found in the equilibrium crystalline phases. Analysis of the neutron and X-ray structure factors yields an average bond angle of 125 +/- 4 degrees between an Al ion and the adjoining cation via a bridging oxygen. We propose that the structure of the glass is a "transition state" between the alumina-rich liquid and the equilibrium mullite phase that are dominated by 4- and 6-coordinated aluminum ions, respectively.

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Hyatt, Mark J.

1989-01-01

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

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Hyatt, Mark J.

1988-01-01

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

Tribological and Corrosion Properties of Coatings Produced by Plasma Electrolytic Oxidation on the ZA27 Alloy

NASA Astrophysics Data System (ADS)

Li, Guangyin; Mao, Yifan; Li, Zhijian; Wang, Linlin; DaCosta, Herbert

2018-04-01

In this paper, a continuous and dense coating was deposited on samples of the ZA27 alloy through the plasma electrolytic oxidation (PEO) process to improve its wear and corrosion performance. A nontoxic and environmentally friendly inorganic salt, Na2SiO3, is chosen as electrolytes with different concentrations. The effect of the concentration of Na2SiO3 aqueous solutions on the coating performances was investigated. The coatings with 3Al2O3·2SiO2 (mullite), Zn2SiO4 and Al2O3 (either crystal phase or with some amorphous SiO2 phases) were formed by the PEO processes. It was found that the coating thickness increased with the increase in electrolyte concentration. However, the wear and corrosion resistance performance of the coatings did not improve as the coating's thickness increased. This was due to the fact that the coating produced with electrolytes of 10 g/L has a porous structure with large pore size. Among all the samples, coating produced by 15 g/L Na2SiO3 has the best wear and corrosion resistance, which is attributed to its continuous and dense structure with thickness of about 47 μm.

Effects of Environment On Creep Behavior of Nextel720/Alumina-Mullite Ceramic Composite With 45 Deg. Fiber Orientation at 1200 Deg. C

DTIC Science & Technology

2009-03-01

iv AFIT/GSS/ENY/09-M05 Abstract Aerospace components require structural materials that have superior long-term mechanical properties ...Page 1. Physical properties of the N720/AM CMC test panel provided by COI…………...….9 2...tensile data…………………………………….………………………..22 5. Summary of creep data………………………………………………………...…......23 6. Summary of retained properties for specimens

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

PubMed

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

2015-06-01

Tailings are solid waste arising from mineral processing. This type of waste can cause severe damage to the environment during stockpiling as a result of the leaching of something harmful into the ecosystem. Gold deposit of ductile shear zone type is an important type of gold deposit, and the recycling of its tailings has been challenging researchers for a long time. In this article, the characteristics of this type of tailings were systematically studied by using modern technical means. Considering the characteristics of the tailings, clay was selected to make up for the shortcomings of the tailings and improve their performance. Water and raw materials were mixed to produce green bodies, which are subsequently sintered into ceramic bodies at 980 °C~1020 °C (sintering temperature). The results showed that some new kinds of mineral phases, such as mullite, anorthite and orthoclase, appear in ceramic bodies. Furthermore, the ceramic bodies have a surface hardness of 5 to 6 (Mohs scale), and their water absorption and modulus of rupture can meet some technical requirements of ceramic materials described in ISO 13006-2012 and GB 5001-1985. These gold mine tailings can be made into ceramic tiles, domestic ceramic bodies, and other kinds of ceramic bodies for commercial and industrial purposes after further improvements. © The Author(s) 2015.

TEM study of PM2.5 emitted from coal and tire combustion in a thermal power station.

PubMed

Gieré, Reto; Blackford, Mark; Smith, Katherine

2006-10-15

The research presented here was conducted within the scope of an experiment investigating technical feasibility and environmental impacts of tire combustion in a coal-fired power station. Previous work has shown that combustion of a coal+tire blend rather than pure coal increased bulk emissions of various elements (e.g., Zn, As, Sb, Pb). The aim of this study is to characterize the chemical and structural properties of emitted single particles with dimensions <2.5 microm (PM2.5). This transmission electron microscope (TEM)-based study revealed that, in addition to phases typical of coal fly ash (e.g., aluminum-silicate glass, mullite), the emitted PM2.5 contains amorphous selenium particles and three types of crystalline metal sulfates never reported before from stack emissions. Anglesite, PbSO4, is ubiquitous in the PM2.5 derived from both fuels and contains nearly all Pb present in the PM. Gunningite, ZnSO4-H2O, is the main host for Zn and only occurs in the PM derived from the coal+tire blend, whereas yavapaiite, KFe3+(SO4)2, is present only when pure coal was combusted. We conclude that these metal sulfates precipitated from the flue gas, may be globally abundant aerosols, and have, through hydration or dissolution, a major environmental and health impact.

Thermodynamic effects of calcium and iron oxides on crystal phase formation in synthetic gasifier slags containing from 0 to 27wt.% V 2O 3

DOE PAGES

Nakano, Jinichiro; Duchesne, Marc; Bennett, James; ...

2014-11-15

Thermodynamic phase equilibria in synthetic slags (Al 2O 3–CaO–FeO–SiO 2–V 2O 3) were investigated with 0–27 wt.% vanadium oxide corresponding to industrial coal–petroleum coke (petcoke) feedstock blends in a simulated gasifier environment. Samples encompassing coal–petcoke mixed slag compositions were equilibrated at 1500 °C in a 64 vol.% CO/36 vol.% CO 2 atmosphere (Po 2 ≈ 10 –8 atm at 1500 °C) for 72 h, followed by rapid water quench, then analyzed by inductively coupled plasma optical emission spectrometry, X-ray diffractometry, and scanning electron microscopy with wavelength dispersive spectroscopy. With increasing CaO content, FeO content, or both; the slag homogeneity regionmore » expanded and a composition range exhibiting crystals was reduced. The mullite (Al 6Si 2O 13) crystalline phase was not present in the slags above 9 wt.% FeO while the karelianite (V 2O 3) crystalline phase was always present in compositions studied if a sufficient amount of vanadium existed in the slag. Furthermore, based on the present experimental equilibrium evaluation, a set of isothermal phase diagrams showing effects of CaO and FeO on thermodynamic phase stabilities in the vanadium-bearing slags is proposed. Some uses of the diagrams for potential industrial practice are discussed.« less

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

NASA Technical Reports Server (NTRS)

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

1998-01-01

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

Numerical Modeling of Suspension HVOF Spray

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phelps, Tommy Joe; Moon, Ji Won; Roh, Yul

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

The Effect of Thermal and Mechanical Treatments on Kaolinite: Characterization by XPS and IEP Measurements.

PubMed

Torres Sánchez RM; Basaldella; Marco

1999-07-15

The surface transformations induced on kaolinite by different thermal and mechanical treatments have been investigated by means of X-ray photoelectron spectroscopy (XPS), Bremsstrahlung induced Auger spectroscopy, and isoelectric point (IEP) measurements. Heating the kaolinite at temperatures between 500 and 750 degrees C results in the change of a substantial fraction of surface Al from octahedral to tetrahedral coordination, which we associate with the dehydroxylation of kaolinite. Heating at 900 and 980 degrees C brings about the development of an octahedral Al fraction which is associated with the formation of gamma-Al(2)O(3). The development of an Al tetrahedral component in the Al KLL spectra of the mechanically treated (ground) samples has been also observed. The Si/Al atomic ratio obtained by XPS in the thermally treated samples is the same as that shown by the original kaolinite. However, the XPS data show a clear reduction of the Si/Al atomic ratio in the mechanically treated samples, which suggests that the mechanical treatment has induced an Al enrichment of the kaolinite surface. The IEP values indicated a thermal transformation to metakaolinite and mullite with the increase of temperature (750 to 980 degrees C). The IEP change for the milled samples can be only explained by assuming a 30% kaolinite coating by the Al oxide neoformed by grinding. Copyright 1999 Academic Press.

A study of surface tension driven segregation in monotectic alloy systems

NASA Technical Reports Server (NTRS)

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

1988-01-01

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

High Temperature Tolerant Ceramic Composites Having Porous Interphases

DOEpatents

Kriven, Waltraud M.; Lee, Sang-Jin

2005-05-03

In general, this invention relates to a ceramic composite exhibiting enhanced toughness and decreased brittleness, and to a process of preparing the ceramic composite. The ceramic composite comprises a first matrix that includes a first ceramic material, preferably selected from the group including alumina (Al2O3), mullite (3Al2O3.2SiO2), yttrium aluminate garnet (YAG), yttria stabilized zirconia (YSZ), celsian (BaAl2Si2O8) and nickel aluminate (NiAl2O4). The ceramic composite also includes a porous interphase region that includes a substantially non-sinterable material. The non-sinterable material can be selected to include, for example, alumina platelets. The platelets lie in random 3-D orientation and provide a debonding mechanism, which is independent of temperature in chemically compatible matrices. The non-sinterable material induces constrained sintering of a ceramic powder resulting in permanent porosity in the interphase region. For high temperature properties, addition of a sinterable ceramic powder to the non-sinterable material provides sufficiently weak debonding interphases. The ceramic composite can be provided in a variety of forms including a laminate, a fibrous monolith, and a fiber-reinforced ceramic matrix. In the laminated systems, intimate mixing of strong versus tough microstructures were tailored by alternating various matrix-to-interphase thickness ratios to provide the bimodal laminate.

Thermal Gradient Cyclic Behavior of a Thermal/Environmental Barrier Coating System on SiC/SiC Ceramic Matrix Composites

NASA Technical Reports Server (NTRS)

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

2002-01-01

Thermal barrier and environmental barrier coatings (TBCs and EBCs) will play a crucial role in future advanced gas turbine engines because of their ability to significantly extend the temperature capability of the ceramic matrix composite (CMC) engine components in harsh combustion environments. In order to develop high performance, robust coating systems for effective thermal and environmental protection of the engine components, appropriate test approaches for evaluating the critical coating properties must be established. In this paper, a laser high-heat-flux, thermal gradient approach for testing the coatings will be described. Thermal cyclic behavior of plasma-sprayed coating systems, consisting of ZrO2-8wt%Y2O3 thermal barrier and NASA Enabling Propulsion Materials (EPM) Program developed mullite+BSAS/Si type environmental barrier coatings on SiC/SiC ceramic matrix composites, was investigated under thermal gradients using the laser heat-flux rig in conjunction with the furnace thermal cyclic tests in water-vapor environments. The coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after the tests. The coating failure mechanisms are discussed based on the cyclic test results and are correlated to the sintering, creep, and thermal stress behavior under simulated engine temperature and heat flux conditions.

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

PubMed

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

2015-04-28

In order to reduce environment risk of zinc, a spinel-based porous membrane support was prepared by the high-temperature reaction of zinc and bauxite mineral. The phase evolution process, shrinkage, porosity, mechanical property, pore size distribution, gas permeation flux and microstructure were systematically studied. The XRD results, based on a Zn/Al stoichiometric composition of 1/2, show a formation of ZnAl2O4 structure starting from 1000°C and then accomplished at 1300°C. For spinel-based composite membrane, shrinkage and porosity are mainly influenced by a combination of an expansion induced by ZnAl2O4 formation and a general densification due to amorphous liquid SiO2. The highest porosity, as high as 44%, is observed in ZnAl4 membrane support among all the investigated compositions. Compared with pure bauxite (Al), ZnAl4 composite membrane support is reinforced by ZnAl2O4 phase and inter-locked mullite crystals, which is proved by the empirical strength-porosity relationships. Also, an increase in average pore diameter and gas flux can be observed in ZnAl4. A prolonged leaching experiment reveals the zinc can be successfully incorporated into ceramic membrane support via formation of ZnAl2O4, which has substantially better resistance toward acidic attack. Copyright © 2015 Elsevier B.V. All rights reserved.

Environmental Barrier Coatings for Ceramics and Ceramic Composites

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Fuel Efficient Diesel Particulate Filter (DPF) Modeling and Development

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stewart, Mark L.; Gallant, Thomas R.; Kim, Do Heui

The project described in this report seeks to promote effective diesel particulate filter technology with minimum fuel penalty by enhancing fundamental understanding of filtration mechanisms through targeted experiments and computer simulations. The overall backpressure of a filtration system depends upon complex interactions of particulate matter and ash with the microscopic pores in filter media. Better characterization of these phenomena is essential for exhaust system optimization. The acicular mullite (ACM) diesel particulate filter substrate is under continuing development by Dow Automotive. ACM is made up of long mullite crystals which intersect to form filter wall framework and protrude from the wallmore » surface into the DPF channels. ACM filters have been demonstrated to effectively remove diesel exhaust particles while maintaining relatively low backpressure. Modeling approaches developed for more conventional ceramic filter materials, such as silicon carbide and cordierite, have been difficult to apply to ACM because of properties arising from its unique microstructure. Penetration of soot into the high-porosity region of projecting crystal structures leads to a somewhat extended depth filtration mode, but with less dramatic increases in pressure drop than are normally observed during depth filtration in cordierite or silicon carbide filters. Another consequence is greater contact between the soot and solid surfaces, which may enhance the action of some catalyst coatings in filter regeneration. The projecting crystals appear to provide a two-fold benefit for maintaining low backpressures during filter loading: they help prevent soot from being forced into the throats of pores in the lower porosity region of the filter wall, and they also tend to support the forming filter cake, resulting in lower average cake density and higher permeability. Other simulations suggest that soot deposits may also tend to form at the tips of projecting crystals due to

Nanomineralogy in the real world: A perspective on nanoparticles in the environmental impacts of coal fire.

PubMed

Sehn, Janaína L; de Leão, Felipe B; da Boit, Kátia; Oliveira, Marcos L S; Hidalgo, Gelsa E; Sampaio, Carlos H; Silva, Luis F O

2016-03-01

Detailed geochemistry similarities between the burning coal cleaning rejects (BCCRs) and non-anthropogenic geological environments are outlined here. While no visible flames were detected, this research revealed that auto-combustion existed in the studied area for many years. The occurrence of several amorphous phases, mullite, hematite and many other Al/Fe-minerals formed by high temperature was found. Bad disposal of coal-dump wastes represents significant environmental concerns due to their potential influence on atmosphere, river sediments, soils and as well as on the surface and groundwater in the surroundings of these areas. The present work using multi-analytical techniques were performed to provide an improved understanding of the complex processes related with sulphide-rich coal waste oxidation, spontaneous combustion and newmineral creation. It recording huge numbers of rare minerals with alunite, montmorillonite, szmolnockite, halotrichite, coquimbite and copiapite at the BCCRs. The information presented the presence of abundant amorphous Si-Al-Fe-Ti as (oxy-)hydroxides and Fe-hydro/oxides with goethite and hematite with various degrees of crystallinity, containing potential hazardous elements (PHEs), such as Cu, Cr, Hf, Hg, Mo, Ni, Se, Pb, Th, U, Zr, and others. Most of the nano-particles and ultra-fine particles found in the burned coal-dump wastes are the same as those commonly associated with coal cleaning rejects, in which oxidation of sulphides plays an important impact to environment and subsequently animal and human health. Copyright © 2015 Elsevier Ltd. All rights reserved.

Material and structural characterization of alkali activated low-calcium brown coal fly ash.

PubMed

Skvára, Frantisek; Kopecký, Lubomír; Smilauer, Vít; Bittnar, Zdenek

2009-09-15

The waste low-calcium Czech brown coal fly ash represents a considerable environmental burden due to the quantities produced and the potentially high content of leachable heavy metals. The heterogeneous microstucture of the geopolymer M(n) [-(Si-O)(z)-Al-O](n).wH(2)O, that forms during the alkaline activation, was examined by means of microcalorimetry, XRD, TGA, DSC, MIP, FTIR, NMR MAS ((29)Si, (27)Al, (23)Na), ESEM, EDS, and EBSD. The leaching of heavy metals and the evolution of compressive strength were also monitored. The analysis of raw fly ash identified a number of different morphologies, unequal distribution of elements, Fe-rich rim, high internal porosity, and minor crystalline phases of mullite and quartz. Microcalorimetry revealed exothermic reactions with dependence on the activator alkalinity. The activation energy of the geopolymerization process was determined as 86.2kJ/mol. The X-ray diffraction analysis revealed no additional crystalline phases associated with geopolymer formation. Over several weeks, the (29)Si NMR spectrum testified a high degree of polymerization and Al penetration into the SiO(4) tetrahedra. The (23)Na NMR MAS spectrum hypothesized that sodium is bound in the form of Na(H(2)O)(n) rather than Na(+), thus causing efflorescence in a moisture-gradient environment. As and Cr(6+) are weakly bonded in the geopolymer matrix, while excellent immobilization of Zn(2+), Cu(2+), Cd(2+), and Cr(3+) are reported.

Discovery and Characterization of a Pourbaix-Stable, 1.8 eV Direct Gap Bismuth Manganate Photoanode

DOE PAGES

Newhouse, Paul F.; Reyes-Lillo, Sebastian E.; Li, Guo; ...

2017-11-13

Solar-driven oxygen evolution is a critical technology for renewably synthesizing hydrogen- and carbon-containing fuels in solar fuel generators. New photoanode materials are needed to meet efficiency and stability requirements, motivating materials explorations for semiconductors with (i) band-gap energy in the visible spectrum and (ii) stable operation in aqueous electrolyte at the electrochemical potential needed to evolve oxygen from water. Motivated by the oxygen evolution competency of many Mn-based oxides, the existence of several Bi-containing ternary oxide photoanode materials, and the variety of known oxide materials combining these elements with Sm, we explore the Bi-Mn-Sm oxide system for new photoanodes. Throughmore » the use of a ferri/ferrocyanide redox couple in high-throughput screening, BiMn 2O 5 and its alloy with Sm are identified as photoanode materials with a near-ideal optical band gap of 1.8 eV. Using density functional theory-based calculations of the mullite Bi 3+ Mn 3+ Mn 4+O 5 phase, we identify electronic analogues to the well-known BiVO 4 photoanode and demonstrate excellent Pourbaix stability above the oxygen evolution Nernstian potential from pH 4.5 to 15. Lastly, our suite of experimental and computational characterization indicates that BiMn 2O 5 is a complex oxide with the necessary optical and chemical properties to be an efficient, stable solar fuel photoanode.« less

Influence of Alkali Resistant (Ar) Fibreglass in Porcelain Clay for Manufacturing Vitrified Clay Pipes

NASA Astrophysics Data System (ADS)

Ikhmal Hanapi, Muhammad; Ahmad, Sufizar; Taib, Hariati; Ismail, Al Emran; Nasrull Abdol Rahman, Mohd; Salleh, Salihatun Md; Sadikin, Azmahani; Mahzan, Shahruddin

2017-10-01

The aim of this work is to determine the characteristics of porcelain ceramic with influence of milled Alkali Resistant (AR) fiberglass for manufacturing vitrified clay pipes. In this study, raw materials consist of porcelain clay and AR fiberglass were refined into powders less than 90μm. Subsequently, these samples were compacted into cylindrical pellet for chemical analysis using X-Ray Fluorescence (XRF). The ceramic sample was produced by mixing different weight percentage of AR glass to porcelain ceramic with 3 wt%, 6 wt%, 9 wt% and 12 wt%. Subsequently, the sample was compacted with 3 ton of pressure load and sintered at 900 °C, 1000 °C, 1100 °C and 1200 °C. The phase identification by using X-Ray Diffraction (XRD) and microstructural analysis were performed for the sintered sample. Chemical analysis revealed that the significant element for all raw material are SiO2, Al2O3, Na2O and K2O. Phase identification analysis shown that sample sintered at 1000 °C produces quartz (SiO2), berlinite (AlPO4), albite (NaAlSi3O8) and calcium-magnesium-aluminum-silicate (CaMgAlSiO). The formation of primary mullite was observed in sample sintered at 1100 °C. The image of microstructural morphology denoted that the formation of glassy phase with decreasing amount of void when sintering temperature and addition of AR glass were increased, which correspond well to phase identification analysis.

Discovery and Characterization of a Pourbaix-Stable, 1.8 eV Direct Gap Bismuth Manganate Photoanode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Newhouse, Paul F.; Reyes-Lillo, Sebastian E.; Li, Guo

Solar-driven oxygen evolution is a critical technology for renewably synthesizing hydrogen- and carbon-containing fuels in solar fuel generators. New photoanode materials are needed to meet efficiency and stability requirements, motivating materials explorations for semiconductors with (i) band-gap energy in the visible spectrum and (ii) stable operation in aqueous electrolyte at the electrochemical potential needed to evolve oxygen from water. Motivated by the oxygen evolution competency of many Mn-based oxides, the existence of several Bi-containing ternary oxide photoanode materials, and the variety of known oxide materials combining these elements with Sm, we explore the Bi-Mn-Sm oxide system for new photoanodes. Throughmore » the use of a ferri/ferrocyanide redox couple in high-throughput screening, BiMn 2O 5 and its alloy with Sm are identified as photoanode materials with a near-ideal optical band gap of 1.8 eV. Using density functional theory-based calculations of the mullite Bi 3+ Mn 3+ Mn 4+O 5 phase, we identify electronic analogues to the well-known BiVO 4 photoanode and demonstrate excellent Pourbaix stability above the oxygen evolution Nernstian potential from pH 4.5 to 15. Lastly, our suite of experimental and computational characterization indicates that BiMn 2O 5 is a complex oxide with the necessary optical and chemical properties to be an efficient, stable solar fuel photoanode.« less

Investigation of Sintering Temperature on Attrition Resistance of Highly Porous Diatomite Based Material

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garderen, Noemie van; Clemens, Frank J.; Scharf, Dagobert

2010-05-30

Highly porous diatomite based granulates with a diameter of 500 mum have been produced by an extrusion method. In order to investigate the relation between microstructure, phase composition and attrition resistance of the final product, the granulates were sintered between 800 and 1300 deg. C. Mean pore size of the granulates was evaluated by Hg-porosimetry. An increase of the pore size is observed in the range of 3.6 nm to 40 mum with increasing sintering temperature. Higher mean pore radii of 1.6 mum and 5.7 mum obtained by sintering at 800 and 1300 deg. C respectively. X-ray diffraction shows thatmore » mullite phase appears at 1100 deg. C due to the presence of clay. At 1100 deg. C diatomite (amorphous silicate) started to transform into alpha-cristobalite. Attrition resistance was determined by evaluating the amount of ground material passed through a sieve with a predefined mesh size. It was observed that a material sintered at high temperature leads to an increase of attrition resistance due to the decrease of total porosities and phase transformation. Due to the reason that attrition resistance significantly increased by sintering the granulates at higher temperature, a so called attrition resistance index was determined in order to compare all the different attrition resistance values. This attrition resistance index was determined by using the exponential component of the equation obtained from attrition resistance curves. It permits comparison of the attrition behaviour without a time influence.« less

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

PubMed

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

2016-07-15

Microstructure of expandable lightweight aggregates (LWAs), which was composed of phosphate waste (PW), cement kiln dust (CKD) and raw clay (RC) was investigated, and the effects of processing factors (temperature, waste content, soaking time) on their physical properties were quantified by using response surface methodology (RSM). The potential use of LWAs as a phosphorus source was assessed through the use of seeds of alfalfa. It was found that the main minerals of the waste, namely carbonates and fluorapatite, were involved in the formation of labradorite/anorthite and melt respectively. Stability of mullite- the main constituent of CKD- was sensitive to the melt content. The assemblage of the identified phases was discussed based on the CaO-SiO2-Al2O3 phase diagram. The results of RSM showed that the change of compressive strength, firing shrinkage and water absorption of LWAs versus processing factors was well described with a polynomial model and the weights of the effects of the factors increased in the following order: sintering temperature > waste content (in the case of PW-RC) > soaking time. On the other hand, it was found that due to the release of phosphorus by soil-embedded pellets, the growth of alfalfa plants improved, and the rate enhanced in this order: PW-RC > PW-CKD > PW-CKD-RC. The absorbed quantity of phosphorus (0.12%) was still lower than the common uptake amount. Copyright © 2016 Elsevier Ltd. All rights reserved.

Theoretical prediction of energy release rate for interface crack initiation by thermal stress in environmental barrier coatings for ceramics

NASA Astrophysics Data System (ADS)

Kawai, E.; Umeno, Y.

2017-05-01

As weight reduction of turbines for aircraft engines is demanded to improve fuel consumption and curb emission of carbon dioxide, silicon carbide (SiC) fiber reinforced SiC matrix composites (SiC/SiC) are drawing enormous attention as high-pressure turbine materials. For preventing degradation of SiC/SiC, environmental barrier coatings (EBC) for ceramics are deposited on the composites. The purpose of this study is to establish theoretical guidelines for structural design which ensures the mechanical reliability of EBC. We conducted finite element method (FEM) analysis to calculate energy release rates (ERRs) for interface crack initiation due to thermal stress in EBC consisting of Si-based bond coat, Mullite and Ytterbium (Yb)-silicate layers on a SiC/SiC substrate. In the FEM analysis, the thickness of one EBC layer was changed from 25 μm to 200 μm while the thicknesses of the other layers were fixed at 25 μm, 50 μm and 100 μm. We compared ERRs obtained by the FEM analysis and a simple theory for interface crack in a single-layered structure where ERR is estimated as nominal strain energy in the coating layers multiplied by a constant factor (independent of layer thicknesses). We found that, unlike the case of single-layered structures, the multiplication factor is no longer a constant but is determined by the combination of consisting coating layer thicknesses.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

High temperature range recuperator. Phase I: materials selection, design optimization, evaluation and thermal testing. Final report, April 1977-May 1978

DOE Office of Scientific and Technical Information (OSTI.GOV)

Power, D V

1978-06-01

Initial efforts to develop, test, and evaluate counterflow recuperator designs are reported for the High Temperature Range Recuperator project. Potential materials to withstand glass furnace exhaust environments at temperatures up to 2800/sup 0/F were evaluated on the bases of material properties, fabrication capability, and relative performance in the flue environment of a day tank glass furnace. Polycrystalline alumina (Vistal), reaction sintered silicon carbide (KT and NC 430), chemically vapor deposited silicon carbide (CVD) and sintered alpha silicon carbide proved most satisfactory in the material temperature range of 2300/sup 0/F to 2800/sup 0/F. Relatively pure alumina (AD 998 and AD 94),more » mullite and cordierite were most satisfactory in the material temperature range of 1700/sup 0/F to 2300/sup 0/F. Recuperator designs were evaluated on the bases of cold air flow tests on laboratory models, fabricability, and calculated thermomechanical stress under expected operating conditions. Material strengths are shown to be greater than expected stresses by factors ranging from 2.6 for KT silicon carbide to 16 for cordierite. Recuperator test sections were fabricated from KT silicon carbide and subjected to thermal stress conditions in excess of twice the expected operating conditions with no deterioration or failure evident. A test section was subjected to the thermal shock of instant transfer between room temperature and a 2000/sup 0/F furnace without damage. Economic analysis based on calculated heat transfer indicates a recuperator system of this design and using currently available materials would have a payback period of 2.3 years.« less

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

USGS Publications Warehouse

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

2001-01-01

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

Assessment and comparison of three high-aluminum fly ash utilization scenarios in Inner Mongolia, China using an eco-efficiency indicator.

PubMed

Yang, Shuo; Lin, Ling; Li, Shao Peng; Li, Qiang; Wang, Xiu Teng; Sun, Liang

2017-05-01

Utilization of fly ash is of great importance in China in the context of resource and environmental crises. Different fly ash utilization processes are proposed, and some have been practically applied. However, none of these fly ash utilization pathways has been evaluated comprehensively by integrating both environmental and economic perspectives. In this study, three high-aluminum fly ash utilization methods in Mongolia were assessed and compared based on the concept of eco-efficiency. The environmental assessment was conducted in accordance with life-cycle assessment principles, and a monetization-weighting approach was applied to obtain social willingness-to-pay as a reflection of environmental impact. The environmental assessment results revealed that the reuse of fly ash had significant advantage for saving primary resource, while solid waste, depletion of water, and global warming were the three highest environmental impacts from the life cycle perspective. The economic performance assessment showed positive net profits for fly ash utilization, but high value-added products were not necessarily indicative of better economic performance due to the relatively high operation cost. Comparison of the eco-efficiency indicators (EEIs) implied that the process of scenario 1#, which produced mullite ceramic and active calcium silicate, was the most recommended out of the three scenarios on the present scale. This judgment was consistent with the evaluation of the resource utilization rate. The present study showed that the EEI could be used to compare different fly ash utilization processes in a comprehensive and objective manner, thus providing definitive and insightful suggestions for decision-making and technical improvement.

Very high-temperature impact melt products as evidence for cosmic airbursts and impacts 12,900 years ago.

PubMed

Bunch, Ted E; Hermes, Robert E; Moore, Andrew M T; Kennett, Douglas J; Weaver, James C; Wittke, James H; DeCarli, Paul S; Bischoff, James L; Hillman, Gordon C; Howard, George A; Kimbel, David R; Kletetschka, Gunther; Lipo, Carl P; Sakai, Sachiko; Revay, Zsolt; West, Allen; Firestone, Richard B; Kennett, James P

2012-07-10

It has been proposed that fragments of an asteroid or comet impacted Earth, deposited silica- and iron-rich microspherules and other proxies across several continents, and triggered the Younger Dryas cooling episode 12,900 years ago. Although many independent groups have confirmed the impact evidence, the hypothesis remains controversial because some groups have failed to do so. We examined sediment sequences from 18 dated Younger Dryas boundary (YDB) sites across three continents (North America, Europe, and Asia), spanning 12,000 km around nearly one-third of the planet. All sites display abundant microspherules in the YDB with none or few above and below. In addition, three sites (Abu Hureyra, Syria; Melrose, Pennsylvania; and Blackville, South Carolina) display vesicular, high-temperature, siliceous scoria-like objects, or SLOs, that match the spherules geochemically. We compared YDB objects with melt products from a known cosmic impact (Meteor Crater, Arizona) and from the 1945 Trinity nuclear airburst in Socorro, New Mexico, and found that all of these high-energy events produced material that is geochemically and morphologically comparable, including: (i) high-temperature, rapidly quenched microspherules and SLOs; (ii) corundum, mullite, and suessite (Fe(3)Si), a rare meteoritic mineral that forms under high temperatures; (iii) melted SiO(2) glass, or lechatelierite, with flow textures (or schlieren) that form at > 2,200 °C; and (iv) particles with features indicative of high-energy interparticle collisions. These results are inconsistent with anthropogenic, volcanic, authigenic, and cosmic materials, yet consistent with cosmic ejecta, supporting the hypothesis of extraterrestrial airbursts/impacts 12,900 years ago. The wide geographic distribution of SLOs is consistent with multiple impactors.

Geochemistry and mineralogy of fly-ash from the Mae Moh lignite deposit, Thailand

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hart, B.R.; Powell, M.A.; Fyfe, W.S.

The concentration of 21 elements in fly ash from three boilers (75 MW, 150 MW, and 300 MW) at the EGAT power plant, Mae Moh, Thailand, were determined by INAA. The concentration of 10 major elements was determined by XRF. As, Co, Cr, Ni, Mo, and Sb generally increase in concentration going from bottom ash (BA) through the sequence of electrostatic precipitator ashes (ESPA) and reach maxima of As (352 ppm), Co (45 ppm), Cr (105 ppm), Mo (32 ppm), Ni (106 ppm), and Sb (15 ppm) in the ESPA. Ce, Cs, Fe, Hf, La, Sc, Ta, Tb, and Ybmore » did not exhibit concentration trends or are variable except in the case of one boiler, which showed an increase going from BA to ESPA. Only Br decreased in composition going from BA to ESPA. Rb, Sm, U, and Th showed marked variation in trends. The major elements identified by EDS were Al, Si, S, K, Ca, Fe, and Ba, with minor amounts of Mg, Na, Ti, Mn, and Sr. Al, Si, K, and Ca occur together and are present in most of the fly-ash particles. Ba was found as a major component with Ca, Al, and Si. Fe and Ca are usually associated with sulfur. Some small spheres (< 5 {mu}m) are comprised almost entirely of Fe (probably as oxide). Symplectite textures are noted in high-Fe phases. All elements except Br are significantly enriched in the fly ash relative to the coal, which contains 35% ash. Particle chemistry is consistent with the major mineral phases identified by XRD, which include: quartz, magnetite, mullite, gehlenite, anorthite, hematite, anhydrite, and clinopyroxene.« less

Fracture resistance measurement of advanced ceramics at elevated-temperatures using Chevron-notched specimens and other novel techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jenkins, M.G.

1995-12-31

The quasi-static fracture behavior of advanced ceramics was assessed in the temperature range of 20{degrees} to 1400{degrees}C. Chevron-notched, three-point flexure specimens and a laser-based CMOD measurement systems were used in testing. Types of materials characterized included monolithic ceramics (SiC, Si{sub 3}N{sub 4}, MgAl{sub 2}O{sub 4}), self-reinforced monoliths (acicular-grained Si{sub 3}N{sub 4}, acicular grained mullite), and ceramic matrix composites (SiC whisker/Al{sub 2}O{sub 3} matrix, TiB{sub 2} particulate/SiC matrix, SiC fibre/CVI SiC matrix, Al{sub 2}O{sub 3} fibre/CVI SiC matrix). Fracture resistance behaviour of the materials was quantified as three distinct regimes of the fracture histories. At crack initiation, the apparent fracture toughnessmore » was evaluated as the critical stress intensity factor, K{sub IC}. During stable crack propagation, the crack growth resistance was characterized by the instantaneous strain energy release rate, G{sub R} using a compliance method assuming linear-elastic unloading to calculate the effective crack lengths. At final fracture, the complete fracture process was quantified using the work-of-fracture, WOF, which can be equated to the fracture surface energy for linearelastic materials. Results indicate that the chevron-notched, three-point flexure specimen facilitates the study of fracture behavior in a wide range of brittle and quasi-brittle materials at elevated temperatures. The unique features of the chevron geometry, which are automatic, in-situ crack initiation and inherent stable crack growth, are crucial to the successful evaluation of the fracture tests.« less

Xenopumice erupted on 15 October 2011 offshore of El Hierro (Canary Islands): a subvolcanic snapshot of magmatic, hydrothermal and pyrometamorphic processes

NASA Astrophysics Data System (ADS)

Del Moro, S.; Di Roberto, A.; Meletlidis, S.; Pompilio, M.; Bertagnini, A.; Agostini, S.; Ridolfi, F.; Renzulli, A.

2015-06-01

On 15 October 2011, a submarine eruption offshore of El Hierro Island gave rise to floating volcanic products, known as xenopumices, i.e., pumiceous xenoliths partly mingled and coated with the juvenile basanitic magma. Over the last few years, no consensus in the scientific community in explaining the origin of these products has been reached. In order to better understand the formation of xenopumice, we present a textural, mineralogical, and geochemical study of the possible magmatic, hydrothermal, and pyrometamorphic processes, which usually operate in the plumbing systems of active volcanoes. We carried out a comprehensive SEM investigation and Sr-Nd-Pb isotope analyses on some samples representative of three different xenopumice facies. All the data were compared with previous studies, new data for El Hierro extrusives and a literature dataset of Canary Islands igneous and sedimentary rocks. In the investigated xenopumices, we emphasize the presence of restitic magmatic phases as well as crystallization of minerals (mainly olivine + pyroxene + magnetite aggregates) as pseudomorphs after pre-existing mafic phenocrysts, providing evidence of pyrometamorphism induced by the high-T juvenile basanitic magma. In addition, we identify veins consisting of zircon + REE-oxides + mullite associated with Si-rich glass and hydrothermal quartz, which indicate the fundamental role played by hydrothermal fluid circulation in the xenopumice protolith. The petrological data agree with a pre-syneruptive formation of the xenopumice, when El Hierro basanite magma intruded hydrothermally altered trachyandesite to trachyte rocks and triggered local partial melting. Therefore, the El Hierro xenopumice represents a snapshot of the transient processes at the magma-wall rock interface, which normally occurs in the feeding system of active volcanoes.

Characterization, partitioning, and potential ecological risk quantification of trace elements in coal fly ash.

PubMed

Usmani, Zeba; Kumar, Vipin

2017-06-01

Coal-based thermal power plants are the major source of power generation in India. Combustion of coal gives rise to by-products such as fly ash (FA) in huge quantities. The current study focuses on physico-chemical and mineralogical characterization and risk evaluation of FA, generated from five thermal power plants (TPPs) of India. The coal, and corresponding FA and bottom ash (BA) were further analyzed for trace elements in order to observe the enrichment and partitioning behavior of elements. The environmental risk assessment of trace elements in FA was performed in accordance with geoaccumulation index (I geo ) and potential ecological risk index (PERI). The results demonstrated that FA was enriched predominantly in SiO 2 , Al 2 O 3 , and Fe 2 O 3 along with small concentrations of CaO and MgO. The mineral phases identified in FA were quartz, mullite, hematite, and magnetite. Elemental characterization indicated that the metals were more enriched in FA as compared to coal and BA. The concentrations of trace elements, Cr, Pb, Hg, and As in FA (TPPs), varied from 12.59-24.28, 22.68-43.19, <0.0001-2.29, and 0.08-3.39 mg/kg, respectively. Maximum enrichment ratio (ER) was observed for Pb (5.21) in TPP3 FA. Hg in TPP1 showed the highest partition ratio (PR) value. I geo values for metals were mostly below zero. The PERI values indicated moderate risk from TPP4 FA and low risk from TPP1, TPP2, TPP3, and TPP5 FA to the environment, according to the threshold values provided.

Next generation internet architecture and cyber-assisted energy efficiency in smart grids of buildings

NASA Astrophysics Data System (ADS)

Peterson, Robb Alex

Northern Minnesota's iron mines are the starting point for the majority of the steel that gets produced in the United States. Their taconite processing plants use heat in furnaces to oxidize and indurate iron in the final stage of making a taconite pellet. Facilities can increase efficiencies when refractory service life is maintained. Efficiencies gained include: less fuel used, better quality control, better furnace control, and less mechanical component maintenance. Furnace refractory linings fail when the cracks that develop in them are uncontrolled or too large. These failures allow heat and gases retained by the lining to reach structural or mechanical components. Furnace control and efficiencies are also compromised when heat and gases are allowed to short circuit or escape the system. These failures are primarily the result of thermal of shock and expansion. It is common place to add stainless steel needle reinforcement to a monolithic refractory in an effort to counteract these effects. This study used several standard ASTM testing procedures to test 65% alumina mullite based refractory samples with 304 and 406 grade stainless steel needles. Mechanical property data gathered was used to analyze performance. The study found that adding reinforcement does not increase initial Compression and Cold Modulus of Ruptures strengths, however, after prolonged heat and thermal shock exposure, needles help maintain integrity and mechanical properties of samples. The study also found that corrosion due to oxidation was a major contributing factor to the way needles performed; and concluded that a concentration of 3% 406 "Alfa 1" stainless steel reinforcing needles added to the working lining of a taconite furnace is recommended.

Very high-temperature impact melt products as evidence for cosmic airbursts and impacts 12,900 years ago

USGS Publications Warehouse

Bunch, Ted E.; Hermes, Robert E.; Moore, Andrew M.T.; Kennett, Douglas J.; Weaver, James C.; Wittke, James H.; DeCarli, Paul S.; Bischoff, James L.; Hillman, Gordon C.; Howard, George A.; Kimbel, David R.; Kletetschka, Gunther; Lipo, Carl P.; Sakai, Sachiko; Revay, Zsolt; West, Allen; Firestone, Richard B.; Kennett, James P.

2012-01-01

It has been proposed that fragments of an asteroid or comet impacted Earth, deposited silica-and iron-rich microspherules and other proxies across several continents, and triggered the Younger Dryas cooling episode 12,900 years ago. Although many independent groups have confirmed the impact evidence, the hypothesis remains controversial because some groups have failed to do so. We examined sediment sequences from 18 dated Younger Dryas boundary (YDB) sites across three continents (North America, Europe, and Asia), spanning 12,000 km around nearly one-third of the planet. All sites display abundant microspherules in the YDB with none or few above and below. In addition, three sites (Abu Hureyra, Syria; Melrose, Pennsylvania; and Blackville, South Carolina) display vesicular, high-temperature, siliceous scoria-like objects, or SLOs, that match the spherules geochemically. We compared YDB objects with melt products from a known cosmic impact (Meteor Crater, Arizona) and from the 1945 Trinity nuclear airburst in Socorro, New Mexico, and found that all of these high-energy events produced material that is geochemically and morphologically comparable, including: (i) high-temperature, rapidly quenched microspherules and SLOs; (ii) corundum, mullite, and suessite (Fe3,/sup>Si), a rare meteoritic mineral that forms under high temperatures; (iii) melted SiO2 glass, or lechatelierite, with flow textures (or schlieren) that form at > 2,200 °C; and (iv) particles with features indicative of high-energy interparticle collisions. These results are inconsistent with anthropogenic, volcanic, authigenic, and cosmic materials, yet consistent with cosmic ejecta, supporting the hypothesis of extraterrestrial airbursts/impacts 12,900 years ago. The wide geographic distribution of SLOs is consistent with multiple impactors.

Characterization of Rare Earth Element Minerals in Coal Utilization Byproducts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Montross, Scott N.; Verba, Circe A.; Collins, Keith

realizing the occurrence of REE mineral phases in CUB and allowed us to calculate structural and volumetric estimates of REE. Collectively, the rock and coal ash samples contained minerals such as quartz, kaolinite, muscovite/illite, iron oxide (as hematite or magnetite), mullite, and clinochlore. Trace minerals included pyrite, zircon, siderite, rutile, diopside, foresterite, gypsum, and barite. We identified REE phosphate minerals monazite (Ce,La,Nd,Th)(PO 4,SiO 4), xenotime (YPO 4,SiO 4), and apatite (Ca 5(PO 4) 3(F,Cl,OH) via SEM and electron microprobe analysis: these materials generally occurred as 1-10 μm-long crystals in the rock and ash samples. As has been shown in other studies, amorphous material-aluminosilicate glass or iron oxyhydroxide-are the major components of coal fly and bottom ash. Trace amounts of amorphous calcium oxide and mixed element (e.g., Al-Si-Ca-Fe) slag are also present. Quartz, mullite, hematite, and magnetite are the crystalline phases present. We found that REEs are present as monomineralic grains dispersed within the ash, as well as fused to or encapsulated by amorphous aluminosilicate glass particles. Monazite and xenotime have relatively high melting points (>1800 °C) compared to typical combustion temperatures; our observations indicate that the REE-phosphates, which presumably contribute a large percentage of REE to the bulk ash REE pool, as measured by mass spectroscopy, are largely unaltered by the combustion. Our study shows that conventional coal combustion processes sequester REE minerals into aluminosilicate glass phases, which presents a new engineering challenge for extracting REE from coal ash. The characterization work summarized in this report provides a semi-quantitative assessments of REE in coal-containing rock and CUB. The data we obtained from 2- and 3-D imaging, elemental mapping, volumetric estimates, and advanced high-resolution pixel classification successfully identified the different mineral phases present in

Copper stabilization via spinel formation during the sintering of simulated copper-laden sludge with aluminum-rich ceramic precursors.

PubMed

Tang, Yuanyuan; Chui, Stephen Sin-Yin; Shih, Kaimin; Zhang, Lingru

2011-04-15

The feasibility of incorporating copper-laden sludge into low-cost ceramic products, such as construction ceramics, was investigated by sintering simulated copper-laden sludge with four aluminum-rich ceramic precursors. The results indicated that all of these precursors (γ-Al(2)O(3), corundum, kaolinite, mullite) could crystallochemically stabilize the hazardous copper in the more durable copper aluminate spinel (CuAl(2)O(4)) structure. To simulate the process of copper transformation into a spinel structure, CuO was mixed with the four aluminum-rich precursors, and fired at 650-1150 °C for 3 h. The products were examined using powder X-ray diffraction (XRD) and scanning electron microscopic techniques. The efficiency of copper transformation among crystalline phases was quantitatively determined through Rietveld refinement analysis of the XRD data. The sintering experiment revealed that the optimal sintering temperature for CuAl(2)O(4) formation was around 1000 °C and that the efficiency of copper incorporation into the crystalline CuAl(2)O(4) structure after 3 h of sintering ranged from 40 to 95%, depending on the type of aluminum precursor used. Prolonged leaching tests were carried out by using acetic acid with an initial pH value of 2.9 to leach CuO and CuAl(2)O(4) samples for 22 d. The sample leachability analysis revealed that the CuAl(2)O(4) spinel structure was more superior to stabilize copper, and suggested a promising and reliable technique for incorporating copper-laden sludge or its incineration ash into usable ceramic products. Such results also demonstrated the potential of a waste-to-resource strategy by using waste materials as part of the raw materials with the attainable temperature range used in the production of ceramics.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ethridge, F.G.; Saracino, A.M.; Burns, L.K.

The encompassing sandstones, siltstones, shales and thin conglomerates of the gasified G Coal seam at the North Knobs SDB-UCG site were deposited mainly in fluvial and poorly-drained swamp environments. These beds dip at 65/sup 0/ at the North Knobs site. Thin section and SEM analyses of the sandstones and coarse siltstones show that they are sublithic to subarkosic arenites cemented with clay minerals, calcite hematite, siderite and silica. The sandstones of Unit D directly above the coal seam have the highest concentration of calcite cement, the lowest mean grain size, and are best sorted in terms of quartz grain sizemore » variations; however, they are the worst sorted in terms of sieve size variations. Clay minerals in the sandstones are dominantly kaolinite and smectite with lesser amounts of illite and chlorite. These clays are of secondary origin. Heat alteration is present only in coals and overburden rock from cores that penetrated the cavity. Thermally altered rocks including hornfels, buchite, paralava rock and paralava breccia were found in the bottom of the dipping cavity near the injection well. The high temperature minerals of tridymite, cristobalite, mullite, cordierite, monoclinic pyroxene and high temperature plagioclase indicate that temperatures of at least 1200/sup 0/C to 1400/sup 0/C were attained in the lower part of the burn cavity. The mechanical test on the unaltered and altered overburden rock show that the most important lithologic property controlling rock strength and seismic wave velocity is the amount and type of cement in the rock. Other parameters measured were grain size, amount of clay cement, and porosity; sorting had a secondary effect on the rock strength and seismic wave velocity. There is a non-linear and direct relationship between mechanical strength and ultrasonic wave velocities for the rock tests. 30 references.« less

Fusion of arkosic sand by intrusive andesite

USGS Publications Warehouse

Bailey, Roy A.

1954-01-01

An andesite dike in the Valles Mountains of northern New Mexico has intruded and partly fused arkosic sediments for a distance of 50 feet from its contacts. The dike is semi-circular in form, has a maximum width of about 100 feet, and is about 500 feet long. Small associated arcuate dikes are arranged in spiral fashion around the main dike, suggesting that they were intruded along shear fractures similar to those described by Burbank (1941). The fused rocks surrounding the andesite dike are of three general types: 1) partly fused arkosic sand, 2) fused clay, and 3) hybrid rocks. The fused arkosic sand consists of relict detrital grains of quartz, orthoclose, and plagioclase, imbedded in colorless glass containing microlites of tridymite, cordierite, and magnetite. The relict quartz grains are corroded and embayed by glass; the orthoclase is sanidinized and partly fused; and the plagioclase is inverted to the high temperature form and is partly fused. The fused clay, which was originally a mixture of montmorillonite and hydromica, consists primarily of cordierite but also contains needle-like crystals of sillimanite (?) or mullite (?). The hybrid rocks originated in part by intermixing of fused arkosic sediments and andesitic liquid and in part by diffusion of mafic constituents through the fused sediments. They are rich in cordierite and magnetite and also contain hypersthene, augite, and plagioclase. The composition of pigeonite in the andesite indicates that the temperature of the andesite at the time of intrusion probably did not exceed 1200?C. Samples of arkosic sand were fused in the presence of water in a Morey bomb at 1050?C. Stability relations of certain minerals in the fused sand suggest that fusion may have taken place at a lower temperature, however, and the fluxing action of volatiles from the andesite are thought to have made this possible.

Potential of fly ash for neutralisation of acid mine drainage.

PubMed

Qureshi, Asif; Jia, Yu; Maurice, Christian; Öhlander, Björn

2016-09-01

Lignite (PK), bituminous (FI) and biomass (SE) fly ashes (FAs) were mineralogically and geochemically characterised, and their element leachability was studied with batch leaching tests. The potential for acid neutralisation (ANP) was quantified by their buffering capacity, reflecting their potential for neutralisation of acid mine drainage. Quartz was the common mineral in FAs detected by XRD with iron oxide, anhydrite, and magnesioferrite in PK, mullite and lime in FI, and calcite and anorthite in SE. All the FAs had high contents of major elements such as Fe, Si, Al and Ca. The Ca content in SE was six and eight times higher compared to PK and FI, respectively. Sulphur content in PK and SE was one magnitude higher than FI. Iron concentrations were higher in PK. The trace element concentrations varied between the FAs. SE had the highest ANP (corresponding to 275 kg CaCO3 tonne(-1)) which was 15 and 10 times higher than PK and FI, respectively. The concentrations of Ca(2+), SO4 (2-), Na(+) and Cl(-) in the leachates were much higher compared to other elements from all FA samples. Iron, Cu and Hg were not detected in any of the FA leachates because of their mild to strong alkaline nature with pH ranging from 9 to 13. Potassium leached in much higher quantity from SE than from the other ashes. Arsenic, Mn and Ni leached from PK only, while Co and Pb from SE only. The concentrations of Zn were higher in the leachates from SE. The FAs used in this study have strong potential for the neutralisation of AMD due to their alkaline nature. However, on the other hand, FAs must be further investigated, with scaled-up experiments before full-scale application, because they might leach pronounced concentrations of elements of concern with decreasing pH while neutralising AMD.

Identification of Gravity-Related Effects on Crystal Growth From Melts With an Immiscibility Gap

NASA Technical Reports Server (NTRS)

Kassemi, M.; Sayir, A.; Farmer, S.

1999-01-01

This work involves an experimental-numerical approach to study the effects of natural and Marangoni convections on solidification of single crystals from a silicate melt with a liquid-liquid immiscibility gap. Industrial use of crystals grown from silicate melts is becoming increasingly important in electronic, optical, and high temperature structural applications. Even the simplest silicate systems like Al203-SiO2 have had, and will continue to have, a significant role in the development of traditional and advanced ceramics. A unique feature of crystals grown from the silicate systems is their outstanding linear electro-optic properties. They also exhibit exceptionally high optical rotativity. As a result, these crystals are attractive materials for dielectric, optical, and microwave applications. Experimental work in our laboratory has indicated that directional solidification of a single crystal mullite appears to be preceded by liquid-liquid phase separation in the melt. Disruption of the immiscible state results in crystallization of a two phase structure. There is also evidence that mixing in the melt caused by density-driven convection can significantly affect the stability of the immiscible liquid layers and result in poly-crystalline growth. On earth, the immiscible state has only been observed for small diameter crystals grown in float zone systems where natural convection is almost negligible. Therefore, it is anticipated that growth of large single crystals from silicate melts would benefit from microgravity conditions because of the reduction of the natural convective mixing. The main objective of this research is to determine the effects of transport processes on the phase separation in the melt during growth of a single crystal while addressing the following issues: (1) When do the immiscible layers form and are they real?; (2) What are the main physical characteristics of the immiscible liquids?; and (3) How mixing by natural or Marangoni convection

Plasma-Sprayed Refractory Oxide Coatings on Silicon-Base Ceramics

NASA Technical Reports Server (NTRS)

Tewari, Surendra

1997-01-01

Silicon-base ceramics are promising candidate materials for high temperature structural applications such as heat exchangers, gas turbines and advanced internal combustion engines. Composites based on these materials are leading candidates for combustor materials for HSCT gas turbine engines. These materials possess a combination of excellent physical and mechanical properties at high temperatures, for example, high strength, high toughness, high thermal shock resistance, high thermal conductivity, light weight and excellent oxidation resistance. However, environmental durability can be significantly reduced in certain conditions such as when molten salts, H2 or water vapor are present. The oxidation resistance of silicon-base materials is provided by SiO2 protective layer. Molten salt reacts with SiO2 and forms a mixture of SiO2 and liquid silicate at temperatures above 800C. Oxygen diffuses more easily through the chemically altered layer, resulting in a catastrophic degradation of the substrate. SiC and Si3N4 are not stable in pure H2 and decompose to silicon and gaseous species such as CH4, SiH, SiH4, N2, and NH3. Water vapor is known to slightly increase the oxidation rate of SiC and Si3N4. Refractory oxides such as alumina, yttria-stabilized zirconia, yttria and mullite (3Al2O3.2SiO2) possess excellent environmental durability in harsh conditions mentioned above. Therefore, refractory oxide coatings on silicon-base ceramics can substantially improve the environmental durability of these materials by acting as a chemical reaction barrier. These oxide coatings can also serve as a thermal barrier. The purpose of this research program has been to develop refractory oxide chemical/thermal barrier coatings on silicon-base ceramics to provide extended temperature range and lifetime to these materials in harsh environments.

Osumilite-(Mg): Validation as a mineral species and new data

NASA Astrophysics Data System (ADS)

Chukanov, N. V.; Pekov, I. V.; Rastsvetaeva, R. K.; Aksenov, S. M.; Belakovskiy, D. I.; Van, K. V.; Schüller, W.; Ternes, B.

2013-12-01

Osumilite-(Mg), the Mg-dominant analogue of osumilite, has been approved by the CNMNC IMA as a new mineral species. The holotype sample has been found at Bellerberg, Eifel volcanic area, Germany. Fluorophlogopite, sanidine, cordierite, mullite, sillimanite, topaz, pseudobrookite and hematite are associated minerals. Osumilite-(Mg) occurs as short prismatic or thick tabular hexagonal crystals reaching 0.5 × 1 mm in size in the cavities in basaltic volcanic glasses at their contact with thermally metamorphosed xenoliths of pelitic rocks. The mineral is brittle, with Mohs' hardness 6.5. Cleavage was not observed. Color is blue to brown. D meas = 2.59(1), D calc = 2.595 g/cm3. No bands corresponding to H2O and OH-groups are in the IR spectrum. Osumilite-(Mg) is uniaxial (+), ω = 1.539(2), ɛ = 1.547(2). The chemical composition (electron microprobe, average of 5 point analyses, wt %) is: 0.08 Na2O, 3.41 K2O, 0.04 CaO, 7.98 MgO, 0.28 MnO, 21.57 Al2O3, 3.59 Fe2O3, 62.33 SiO2, total 99.28. The empirical formula is: (K0.72Na0.03Ca0.01)(Mg1.97Mn0.04)[Al4.21Fe{0.45/3+}Si10.32]O30. The simplified formula is: KMg2Al3(Al2Si10)O10. The crystal structure was refined on a single crystal, R = 0.0294. Osumilite-(Mg) is hexagonal, space group P6/ mcc; a = 10.0959(1), c = 14.3282(2)Å, V = 1264.79(6) Å3, Z = 2. The strongest reflections in the X-ray powder diffraction pattern [ d, Å I %) ( hkl)] are: 7.21 (37) (002), 5.064 (85) (110), 4.137 (45) (112), 3.736 (43) (202), 3.234 (100) (211), 2.932 (42) (114), 2.767 (51) (204). A type specimen is deposited in the Fersman Mineralogical Museum, Russian Academy of Sciences, Moscow, registration number 4174/1.

Deciphering mineralogical changes and carbonation development during hydration and ageing of a consolidated ternary blended cement paste

PubMed Central

Grangeon, Sylvain; De Nolf, Wout; Harker, Nicholas; Boulahya, Faiza; Bourbon, Xavier

2018-01-01

To understand the main properties of cement, a ubiquitous material, a sound description of its chemistry and mineralogy, including its reactivity in aggressive environments and its mechanical properties, is vital. In particular, the porosity distribution and associated sample carbonation, both of which affect cement’s properties and durability, should be quantified accurately, and their kinetics and mechanisms of formation known both in detail and in situ. However, traditional methods of cement mineralogy analysis (e.g. chemical mapping) involve sample preparation (e.g. slicing) that can be destructive and/or expose cement to the atmosphere, leading to preparation artefacts (e.g. dehydration). In addition, the kinetics of mineralogical development during hydration, and associated porosity development, cannot be examined. To circumvent these issues, X-ray diffraction computed tomography (XRD-CT) has been used. This allowed the mineralogy of ternary blended cement composed of clinker, fly ash and blast furnace slag to be deciphered. Consistent with previous results obtained for both powdered samples and dilute systems, it was possible, using a consolidated cement paste (with a water-to-solid ratio akin to that used in civil engineering), to determine that the mineralogy consists of alite (only detected in the in situ hydration experiment), calcite, calcium silicate hydrates (C-S-H), ettringite, mullite, portlandite, and an amorphous fraction of unreacted slag and fly ash. Mineralogical evolution during the first hydration steps indicated fast ferrite reactivity. Insights were also gained into how the cement porosity evolves over time and into associated spatially and time-resolved carbonation mechanisms. It was observed that macroporosity developed in less than 30 h of hydration, with pore sizes reaching about 100–150 µm in width. Carbonation was not observed for this time scale, but was found to affect the first 100 µm of cement located around macropores

Characterization and determination of 28 elements in fly ashes collected in a thermal power plant in Argentina using different instrumental techniques

NASA Astrophysics Data System (ADS)

Marrero, Julieta; Polla, Griselda; Jiménez Rebagliati, Raúl; Plá, Rita; Gómez, Darío; Smichowski, Patricia

2007-02-01

Different techniques were selected for comprehensive characterization of seven samples of fly ashes collected from the electrostatic precipitator of the San Nicolás thermal power plant (Buenos Aires, Argentina). Particle size was measured using laser based particle size analyzer. X-ray diffraction powder (XRD) analysis and scanning electron microscopy (SEM) were used to characterize the mineral phase present in the matrix consisting basically of aluminosilicates and large amounts of amorphous material. The predominant crystalline phases were mullite and quartz. Major and minors elements (Al, Ca, Cl, Fe, K, Mg, Na, S, Si and Ti) were detected by energy dispersive X-ray analysis (EDAX). Trace elements (As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Se, V and Zn) content was quantified by inductively coupled plasma optical emission spectrometry (ICP OES). Different acid mixtures and digestion procedures were compared for subsequent ICP OES measurements of the dissolved samples. The digestion procedures used were: i) a mixture of FH + HNO 3 + HClO 4 (open system digestion); ii) a mixture of FH + HNO 3 (MW-assisted digestion); iii) a mixture of HF and aqua regia (MW-assisted digestion). Instrumental neutron activation analysis (INAA) was employed for the determination of As, Ba, Co, Cr, Ce, Cs, Eu, Fe, Gd, Hf, La, Lu, Rb, Sb, Sc, Sm, Ta, Tb, Th, U and Yb. The validation of the procedure was performed by the analysis of two certified materials namely, i) NIST 1633b, coal fly ash and ii) GBW07105, rock. Mean elements content spanned from 41870 μg g - 1 for Fe to 1.14 μg g - 1 for Lu. The study showed that Fe (41870 μg g - 1 ) ≫ V (1137 μg g - 1 ) > Ni (269 μg g - 1 ) > Mn (169 μg g - 1 ) are the main components. An enrichment, with respect to crustal average, in many elements was observed especially for As, V and Sb that deserve particular interest from the environmental and human health point of view.

Thermal Cyclic Behavior of Thermal and Environmental Barrier Coatings Investigated Under High-Heat-Flux Conditions

NASA Technical Reports Server (NTRS)

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

2002-01-01

Environmental barrier coatings (EBC's) have been developed to protect silicon-carbide- (SiC) based ceramic components in gas turbine engines from high-temperature environmental attack. With continuously increasing demands for significantly higher engine operating temperature, future EBC systems must be designed for both thermal and environmental protection of the engine components in combustion gases. In particular, the thermal barrier functions of EBC's become a necessity for reducing the engine-component thermal loads and chemical reaction rates, thus maintaining the required mechanical properties and durability of these components. Advances in the development of thermal and environmental barrier coatings (TBC's and EBC's, respectively) will directly impact the successful use of ceramic components in advanced engines. To develop high-performance coating systems, researchers must establish advanced test approaches. In this study, a laser high-heat-flux technique was employed to investigate the thermal cyclic behavior of TBC's and EBC's on SiC-reinforced SiC ceramic matrix composite substrates (SiC/SiC) under high thermal gradient and thermal cycling conditions. Because the laser heat flux test approach can monitor the coating's real-time thermal conductivity variations at high temperature, the coating thermal insulation performance, sintering, and delamination can all be obtained during thermal cycling tests. Plasma-sprayed yttria-stabilized zirconia (ZrO2-8 wt% Y2O3) thermal barrier and barium strontium aluminosilicate-based environmental barrier coatings (BSAS/BSAS+mullite/Si) on SiC/SiC ceramic matrix composites were investigated in this study. These coatings were laser tested in air under thermal gradients (the surface and interface temperatures were approximately 1482 and 1300 C, respectively). Some coating specimens were also subject to alternating furnace cycling (in a 90-percent water vapor environment at 1300 C) and laser thermal gradient cycling tests

Synthesis and characterization of zeolites prepared from industrial fly ash.

PubMed

Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

2014-09-01

In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

Nanocrystalline coating design for extreme applications based on the concept of complex adaptive behavior

NASA Astrophysics Data System (ADS)

Fox-Rabinovich, G. S.; Veldhuis, S. C.; Dosbaeva, G. K.; Yamamoto, K.; Kovalev, A. I.; Wainstein, D. L.; Gershman, I. S.; Shuster, L. S.; Beake, B. D.

2008-04-01

The development of effective hard coatings for high performance dry machining, which is associated with high stress/temperatures during friction, is a major challenge. Newly developed synergistically alloyed nanocrystalline adaptive Ti0.2Al0.55Cr0.2Si0.03Y0.02N plasma vapor deposited hard coatings exhibit excellent tool life under conditions of high performance dry machining of hardened steel, especially under severe and extreme cutting conditions. The coating is capable of sustaining cutting speeds as high as 600 m/min. Comprehensive investigation of the microstructure and properties of the coating was performed. The structure of the coating before and after service has been characterized by high resolution transmission electron microscopy. Micromechanical characteristics of the coating have been investigated at elevated temperatures. Oxidation resistance of the coating has been studied by using thermogravimetry within a temperature range of 25-1100 °C in air. The coefficient of friction of the coatings was studied within a temperature range of 25-1200 °C. To determine the causes of excellent tool life and improved wear behavior of the TiAlCrSiYN coatings, its surface structure characteristics after service have been investigated by using x-ray photoelectron spectroscopy and extended energy-loss fine spectroscopy. One of the major features of this coating is the dynamic formation of the protective tribo-oxide films (dissipative structures) on the surface during friction with a sapphire and mullite crystal structure. Aluminum- and silicon-rich tribofilms with dangling bonds form on the surface as well. These tribofilms act in synergy and protect the surface so efficiently that it is able to sustain extreme operating conditions. Moreover, the Ti0.2Al0.55Cr0.2Si0.03Y0.02N coating possesses some features of a complex adaptive behavior because it has a number of improved characteristics (tribological adaptability, ultrafine nanocrystalline structure, hot hardness and

The properties of the nano-minerals and hazardous elements: Potential environmental impacts of Brazilian coal waste fire.

PubMed

Civeira, Matheus S; Pinheiro, Rafael N; Gredilla, Ainara; de Vallejuelo, Silvia Fdez Ortiz; Oliveira, Marcos L S; Ramos, Claudete G; Taffarel, Silvio R; Kautzmann, Rubens M; Madariaga, Juan Manuel; Silva, Luis F O

2016-02-15

Brazilian coal area (South Brazil) impacted the environment by means of a large number of coal waste piles emplaced over the old mine sites and the adjacent areas of the Criciúma, Urussanga, and Siderópolis cities. The area studied here was abandoned and after almost 30 years (smokeless visual) some companies use the actual minerals derived from burning coal cleaning rejects (BCCRs) complied in the mentioned area for industry tiles or refractory bricks. Mineralogical and geochemical similarities between the BCCRs and non-anthropogenic geological environments are outlined here. Although no visible flames were observed, this study revealed that auto-combustion existed in the studied area for many years. The presence of amorphous phases, mullite, hematite and other Fe-minerals formed by high temperature was found. There is also pyrite, Fe-sulphates (eg. jarosite) and unburnt coal present, which are useful for comparison purposes. Bad disposal of coal-dump wastes represents significant environmental concerns due to their potential influence on atmosphere, river sediments, soils and as well as on the surface and groundwater in the surroundings of these areas. The present study using advanced analytical techniques were performed to provide an improved understanding of the complex processes related with sulphide-rich coal waste oxidation, spontaneous combustion and mineral formation. It is reporting huge numbers of rare minerals with alunite, montmorillonite, szomolnokite, halotrichite, coquimbite and copiapite at the BCCRs. The data showed the presence of abundant amorphous Si-Al-Fe-Ti as (oxy-)hydroxides and Fe-hydro/oxides with goethite and hematite with various degrees of crystallinity, containing hazardous elements, such as Cu, Cr, Hf, Hg, Mo, Ni, Se, Pb, Th, U, Zr, and others. By Principal Component Analysis (PCA), the mineralogical composition was related with the range of elemental concentration of each sample. Most of the nano-minerals and ultra-fine particles

Characterization of feed coal and coal combustion products from power plants in Indiana and Kentucky

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brownfield, M.E.; Affolter, R.H.; Cathcart, J.D.

1999-07-01

The US Geological Survey, Kentucky Geological Survey, and the University of Kentucky Center for Applied Energy Research are collaborating with Indiana and Kentucky utilities to determine the physical and chemical properties of feed coal and coal combustion products (CCP) from three coal-fired power plants. These three plants are designated as Units K1, K2, and I1 and burn high-, moderate-, and low-sulfur coals, respectively. Over 200 samples of feed coal and CCP were analyzed by various chemical and mineralogical methods to determine mode of occurrence and distribution of trace elements in the CCP. Generally, feed coals from all 3 Units containmore » mostly well-crystallized kaolinite and quartz. Comparatively, Unit K1 feed coals have higher amounts of carbonates, pyrite and sphalerite. Unit K2 feed coals contain higher kaolinite and illite/muscovite when compared to Unit K1 coals. Unit I1 feed coals contain beta-form quartz and alumino-phosphates with minor amounts of calcite, micas, anatase, and zircon when compared to K1 and K2 feed coals. Mineralogy of feed coals indicate that the coal sources for Units K1 and K2 are highly variable, with Unit K1 displaying the greatest mineralogic variability; Unit I1 feed coal however, displayed little mineralogic variation supporting a single source. Similarly, element contents of Units K1 and K2 feed coals show more variability than those of Unit I1. Fly ash samples from Units K1 and K2 consist mostly of glass, mullite, quartz, and spines group minerals. Minor amounts of illite/muscovite, sulfates, hematite, and corundum are also present. Spinel group minerals identified include magnetite, franklinite, magnesioferrite, trevorite, jacobisite, and zincochromite. Scanning Electron Microscope analysis reveals that most of the spinel minerals are dendritic intergrowths within aluminum silicate glass. Unit I1 fly ash samples contain glass, quartz, perovskite, lime, gehlenite, and apatite with minor amounts of periclase

Effect of sintering temperature on flexural properties of alumina fiber-reinforced, alumina-based ceramics prepared by tape casting technique.

PubMed

Tanimoto, Yasuhiro; Nemoto, Kimiya

2006-01-01

-alumina transformed to mullite. There were significant differences in the flexural properties between the alumina-fiber/alumina composite sintered at the four temperatures. This indicates that the choice of optimum sintering temperature is an important factor for successful dental applications of alumina-fiber/alumina composite developed by the tape casting system.

Hierarchical zeolites from class F coal fly ash

NASA Astrophysics Data System (ADS)

Chitta, Pallavi

Fly ash, a coal combustion byproduct is classified as types class C and class F. Class C fly ash is traditionally recycled for concrete applications and Class F fly ash often disposed in landfills. Class F poses an environmental hazard due to disposal and leaching of heavy metals into ground water and is important to be recycled in order to mitigate the environmental challenges. A major recycling option is to reuse the fly ash as a low-cost raw material for the production of crystalline zeolites, which serve as catalysts, detergents and adsorbents in the chemical industry. Most of the prior literature of fly ash conversion to zeolites does not focus on creating high zeolite surface area zeolites specifically with hierarchical pore structure, which are very important properties in developing a heterogeneous catalyst for catalysis applications. This research work aids in the development of an economical process for the synthesis of high surface area hierarchical zeolites from class F coal fly ash. In this work, synthesis of zeolites from fly ash using classic hydrothermal treatment approach and fusion pretreatment approach were examined. The fusion pretreatment method led to higher extent of dissolution of silica from quartz and mullite phases, which in turn led to higher surface area and pore size of the zeolite. A qualitative kinetic model developed here attributes the difference in silica content to Si/Al ratio of the beginning fraction of fly ash. At near ambient crystallization temperatures and longer crystallization times, the zeolite formed is a hierarchical faujasite with high surface area of at least 360 m2/g. This work enables the large scale recycling of class F coal fly ash to produce zeolites and mitigate environmental concerns. Design of experiments was used to predict surface area and pore sizes of zeolites - thus obviating the need for intense experimentation. The hierarchical zeolite catalyst supports tested for CO2 conversion, yielded hydrocarbons

The aluminum ordering in aluminosilicates: a dipolar 27Al NMR spectroscopy study.

PubMed

Gee, Becky A

2004-01-01

The spatial ordering of aluminum atoms in CsAl(SiO3)2 and 3Al2O3.2SiO2 was probed by 27Al dipolar solid-state NMR spectroscopy. The 27Al response to a Hahn spin-echo pulse sequence in a series of aluminum-containing model crystalline compounds demonstrates that quantitative 27Al homonuclear dipolar second moments can be obtained to within +/-20% of the theoretical values, if evaluation of the spin-echo response curve is limited to short evolution periods (2t1 < or = 0.10 ms). Additionally, selective excitation of the central transition m = 1/2 --> -1/2 is necessary in order to ensure quantitative results. Restriction of spin exchange affecting the dephasing of the magnetization may decelerate the spin-echo decay at longer evolution periods. Considering these restraints, the method was used to probe the spatial distribution of aluminum atoms among the tetrahedral sites in two aluminosilicate materials. Experimental 27Al spin-echo response data for the aluminosilicates CsAl(SiO3)2 (synthetic pollucite) and 3Al2O3.2SiO2 (mullite) are compared with theoretical data based on (I) various degrees of aluminum-oxygen-aluminum bond formation among tetrahedrally coordinated aluminum atoms (Al(T(d) )-O-Al(T(d) )) and (II) the maximum avoidance of Al(T(d) )-O-Al(T(d) ) bonding. Analysis of the second moment values and resulting echo decay responses suggests that partial suppression of spin exchange among aluminum atoms in crystallographically distinct sites may contribute to the 27Al spin echo decay in 3Al2O3.2SiO2, thus complicating quantitative analysis of the data. Silicon-29 and aluminum-27 magic angle spinning (MAS) NMR spectra of 3Al2O3.2SiO2 are consistent with those previously reported. The experimental 27Al spin-echo response behavior of CsAl(SiO3)2 differs from the theoretical response behavior based on the maximum avoidance of Al-O-Al bonding between tetrahedral aluminum sites in CsAl(SiO3)2. A single unresolved resonance is observed in both the silicon-29 and

Durability of Environmental Barrier Coatings in a Water Vapor/Oxygen Environment

NASA Technical Reports Server (NTRS)

Holchin, John E.

2004-01-01

Silicon carbide (Sic) and silicon nitride (Si3N4) show potential for application in the hot sections of advanced jet engines. The oxidation behavior of these materials has been studied in great detail. In a pure oxygen environment, a silica (SiO2) layer forms on the surface and provides protection from further oxidation. Initial oxidation is rapid, but slows as silica layer grows; this is known as parabolic oxidation. When exposed to model fuel-lean combustion applications (standard in jet engines), wherein the partial pressure of water vapor is approximately 0.5 atm., these materials exhibit different characteristics. In such an environment, the primary oxidant to form silica is water vapor. At the same time, water vapor reacts with the surface oxide to form gaseous silicon hydroxide (Si(OH)4). The simultaneous formation of both silica and Si(OH)4 -the latter which is lost to the atmosphere- the material continues to recede. Recession rates for uncoated Sic and Si3N4 are unacceptably high, for use in jet engines, - on the order of 1mm/4000h. External coatings have been developed that protect Si-based materials from water vapor attack. One such coating consists of a Ba(0.75)Sr(0.25)Al2Si2O8 (BSAS) topcoat, a mullite/BSAS intermediate layer and a Si bond coat. The key function of the topcoat is to protect the Si-base material from water vapor; therefore it must be fairly stable in water vapor (recession rate of about 1mm/40,000h) and remain crack free. Although BSAS is much more resistant to water vapor attack than pure silica, it exhibits a linear weight loss in 50% H2O - 50% O2 at 1500 C. The objective of my research is to determine the oxidation behavior of a number of alternate hot-pressed monolithic top coat candidates. Potential coatings were exposed at 1500 C to a 50% H2O - 50% O2 gas mixture flowing at 4.4 cm/s . These included rare- earth silicates, barium-strontium aluminosilicates. When weight changes were measured with a continuously recording

Chemical and Mineralogical Characterization of Arsenic, Lead, Chromium, and Cadmium in a Metal-contaminated Histosol

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, X.; Schulze, D

2010-01-01

The chemical and mineralogical forms of As, Pb, Cr, and Cd were studied in a metal-contaminated organic soil (Histosol) that received runoff and seepage water from a site that was once occupied by a lead smelter. Soil samples were collected from different depth intervals during both wet and dry seasons and analyzed using bulk powder X-ray diffraction (XRD), synchrotron-based micro X-ray diffraction ({mu}-XRD), and micro X-ray fluorescence ({mu}-SXRF) spectroscopy. There was a clear pattern of mineral distribution with depth that indicated the presence of an intense redox gradient. The oxidized reddish brown surface layer (0-10 cm) was dominated by goethitemore » ({alpha}-FeOOH) and poorly crystalline akaganeite ({beta}-FeOOH). Lead and arsenic were highly associated with these Fe oxides, possibly by forming inner-sphere surface complexes. Gypsum (CaSO{sub 4} {center_dot} 2H{sub 2}O) was abundant in the layer as well, particularly for samples collected during dry periods. Fe(II)-containing minerals, such as magnetite (Fe{sub 3}O{sub 4}) and siderite (FeCO{sub 3}), were identified in the intermediate layers (10-30 cm) where the reductive dissolution of Fe(III) oxides occurred. A number of high-temperature minerals, such as mullite (3Al{sub 2}O{sub 3} {center_dot} 2Si{sub 2}O), corundum ({alpha}-Al{sub 2}O{sub 3}), hematite ({alpha}-Fe{sub 2}O{sub 3}), and wustite (FeO) were identified in the subsurface and they probably formed as a result of a burning event. Several sulfide minerals were identified in the most reduced layers at depths > 30 cm. They included realgar (AsS), alacranite (As{sub 4}S{sub 4}), galena (PbS), and sphalerite (Zn, Fe{sup 2+})S, and a series of Fe sulfides, including greigite (Fe{sup 2+}Fe{sub 2}{sup 3+} S{sub 4}), pyrrhotite (Fe{sub 1-x}S), mackinawite (FeS), marcasite (FeS{sub 2}), and pyrite (FeS{sub 2}). Most of these minerals occurred as almost pure phases in sub-millimeter aggregates and appeared to be secondary phases that had

Mechanism of adaptability for the nano-structured TiAlCrSiYN-based hard physical vapor deposition coatings under extreme frictional conditions

NASA Astrophysics Data System (ADS)

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

2012-03-01

Recently, a family of hard mono- and multilayer TiAlCrSiYN-based coatings have been introduced that exhibit adaptive behavior under extreme tribological conditions (in particular during dry ultrahigh speed machining of hardened tool steels). The major feature of these coatings is the formation of the tribo-films on the friction surface which possess high protective ability under operating temperatures of 1000 °C and above. These tribo-films are generated as a result of a self-organization process during friction. But the mechanism how these films affect adaptability of the hard coating is still an open question. The major mechanism proposed in this paper is associated with a strong gradient of temperatures within the layer of nano-scaled tribo-films. This trend was outlined by the performed thermodynamic analysis of friction phenomena combined with the developing of a numerical model of heat transfer within cutting zone based on the finite element method. The results of the theoretical studies show that the major physical-chemical processes during cutting are mostly concentrated within a layer of the tribo-films. This nano-tribological phenomenon produces beneficial heat distribution at the chip/tool interface which controls the tool life and wear behavior.Results of x-ray photoelectron spectroscopy studies indicate enhanced formation of protective sapphire- and mullite-like tribo-films on the friction surface of the multilayer TiAlCrSiYN/TiAlCrN coating. Comprehensive investigations of the structure and phase transformation within the coating layer under operation have been performed, using high resolution transmission electron microscopy, synchrotron radiation technique: x-ray absorption near-edge structure and XRD methods.The data obtained show that the tribo-films efficiently perform their thermal barrier functions preventing heat to penetrate into the body of coated cutting tool. Due to this the surface damaging process as well as non-beneficial phase

Sulfate resistance of high calcium fly ash concrete

NASA Astrophysics Data System (ADS)

Dhole, Rajaram

Sulfate attack is one of the mechanisms which can cause deterioration of concrete. In general, Class C fly ash mixtures are reported to provide poor sulfate resistance. Fly ashes, mainly those belonging to the Class C, were tested as per the ASTM C 1012 procedure to evaluate chemical sulfate resistance. Overall the Class C fly ashes showed poor resistance in the sulfate environment. Different strategies were used in this research work to improve the sulfate resistance of Class C fly ash mixes. The study revealed that some of the strategies such as use of low W/CM (water to cementing materials by mass ratio), silica fume or ultra fine fly ash, high volumes of fly ash and, ternary or quaternary mixes with suitable supplementary cementing materials, can successfully improve the sulfate resistance of the Class C fly ash mixes. Combined sulfate attack, involving physical and chemical action, was studied using sodium sulfate and calcium sulfate solutions. The specimens were subjected to wetting-drying cycles and temperature changes. These conditions were found to accelerate the rate of degradation of concrete placed in a sodium sulfate environment. W/CM was found to be the main governing factor in providing sulfate resistance to mixes. Calcium sulfate did not reveal damage as a result of mainly physical action. Characterization of the selected fly ashes was undertaken by using SEM, XRD and the Rietveld analysis techniques, to determine the relation between the composition of fly ashes and resistance to sulfate attack. The chemical composition of glass represented on the ternary diagram was the main factor which had a significant influence on the sulfate resistance of fly ash mixtures. Mixes prepared with fly ashes containing significant amounts of vulnerable crystalline phases offered poor sulfate resistance. Comparatively, fly ash mixes containing inert crystalline phases such as quartz, mullite and hematite offered good sulfate resistance. The analysis of hydrated lime

Integrated acid mine drainage management using fly ash.

PubMed

Vadapalli, Viswanath R K; Gitari, Mugera W; Petrik, Leslie F; Etchebers, Olivier; Ellendt, Annabelle

2012-01-01

Fly Ash (FA) from a power station in South Africa was investigated to neutralise and remove contaminants from Acid Mine Drainage (AMD). After this primary treatment the insoluble FA residue namely solid residue (SR) was investigated as a suitable mine backfill material by means of strength testing. Moreover, SR was used to synthesise zeolite-P using a two-step synthesis procedure. Furthermore, the zeolite-P was investigated to polish process water from the primary FA-AMD reaction. The main objective of this series of investigations is to achieve zero waste and to propose an integrated AMD management using FA. Fly Ash was mixed with AMD at various predetermined FA-AMD ratios until the mixtures achieved circumneutral pH or higher. The supernatants were then analyzed using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Ion Chromatography (IC) for cations and anions respectively. The physical strength testing of SR was carried out by mixing it with 3% Ordinary Portland Cement (OPC) and curing for 410 days. Synthesis of zeolite-P using SR was carried out by two step synthesis procedure: ageing for 24 hours followed by a mild hydrothermal synthesis at 100°C for 4 days. The polishing of process water from primary AMD treatment using FA was ascertained by mixing the process water with zeolite at a liquid to solid ratio of 100:1 for 1 hour. The results indicated that FA can be successfully used to ameliorate AMD. High removal of major AMD contaminants Fe, Al, Mg, Mn and sulphate was achieved with the ash treatment and trace elements such as Zn, Ni, Cu and Pb were also removed by the FA. Strength testing over 410 days indicated that the material gained strength over the testing period. The maximum unconfined compressive strength and elastic modulus was observed to be approximately 0.3 MPa and 150 Mpa respectively. The X-ray diffraction (XRD) analysis of the synthesized product indicated that SR was successfully converted into zeolite-P with some mullite phase

Self-degradable Slag/Class F Fly Ash-Blend Cements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sugama, T.; Warren, J.; Butcher, T.

2011-03-01

exothermic temperature was controlled by the extent of thermal decomposition of CMC, demonstrating that CMC decomposed at higher temperature emitted more gaseous reactants. Hence, such large emission enhanced the evolution of in-situ exothermic heat. In contrast, the excessive formation of geopolymer phase due to more incorporation of Class F fly ash into this cementitious system affected its ability to self-degrade, reflecting that there was no self-degradation. The geopolymer was formed by hydrothermal reactions between sodium hydroxide from sodium silicate and mullite in Class F fly ash. Thus, the major reason why geopolymer-based cementitiuos sealers did not degrade after heated sealers came in contact with water was their lack of free sodium hydroxide.« less

Mineralogy and the release of trace elements from slag from the Hegeler Zinc smelter, Illinois (USA)

USGS Publications Warehouse

Piatak, Nadine M.; Seal, Robert R.

2010-01-01

Slag from the former Hegeler Zn-smelting facility in Illinois (USA) is mainly composed of spinifex Ca-rich plagioclase, fine-grained dendritic or coarse-grained subhedral to anhedral clinopyroxenes, euhedral to subhedral spinels, spherical blebs of Fe sulfides, silicate glass, and less commonly fayalitic olivine. Mullite and quartz were also identified in one sample as representing remnants of the furnace lining. Secondary phases such as goethite, hematite and gypsum are significant in some samples and reflect surficial weathering of the dump piles or represent byproducts of roasting. A relatively rare Zn-rich material contains anhedral willemite, subhedral gahnite, massive zincite, hardystonite and a Zn sulfate (brianyoungite), among other phases, and likely represents the molten content of the smelting furnace before Zn extraction. The bulk major-element chemistry of most slag samples is dominated by SiO2, Al2O3, Fe2O3 and CaO. The bulk composition of the slag suggests a high viscosity of the melt and the mineralogy suggests a high silica content of the melt. Bulk slag trace-element chemistry shows that the dominant metal is Zn with >28.4 wt.% in the Zn-rich material and between 212 and 14,900 mg/kg in the other slags. The concentrations of other trace elements reach the following: 45 mg/kg As, 1170 mg/kg Ba, 191 mg/kg Cd, 242 mg/kg Co, 103 mg/kg Cr, 6360 mg/kg Cu, 107 mg/kg Ni, and 711 mg/kg Pb.Zinc, as the dominant metal in the slags, is likely the most environmentally significant metal in these samples; Cd, Cu, and Pb are also of concern and their concentrations exceed US Environmental Protection Agency preliminary remediation goals for residential soils. Spinel was found to be the dominant concentrator of Zn for samples containing significant Zn (>1 wt.%); the silicate glass also contained relatively high concentrations of Zn compared to other phases. Zinc partitioned into the silicates and oxides in these samples is generally more resistant to

Natural weathering in dry disposed ash dump: Insight from chemical, mineralogical and geochemical analysis of fresh and unsaturated drilled cores.

PubMed

Akinyemi, S A; Akinlua, A; Gitari, W M; Khuse, N; Eze, P; Akinyeye, R O; Petrik, L F

2012-07-15

Some existing alternative applications of coal fly ash such as cement manufacturing; road construction; landfill; and concrete and waste stabilisation use fresh ash directly collected from coal-fired power generating stations. Thus, if the rate of usage continues, the demand for fresh ash for various applications will exceed supply and use of weathered dry disposed ash will become necessary alternative. As a result it's imperative to understand the chemistry and pH behaviour of some metals inherent in dry disposed fly ash. The bulk chemical composition as determined by XRF analysis showed that SiO2, Al2O3 and Fe2O3 were the major oxides in fresh ash and unsaturated weathered ashes. The unsaturated weathered ashes are relatively depleted in CaO, Fe2O3, TiO2, SiO2, Na2O and P2O5 due to dissolution and hydrolysis caused by chemical interaction with ingressing CO2 from the atmosphere and infiltrating rain water. Observed accumulations of Fe2O3, TiO2, CaO, K2O, Na2O and SO3 and Zn, Zr, Sr, Pb, Ni, Cr and Co in the lower layers indicate progressive downward movement through the ash dump though at a slow rate. The bulk mineralogy of unsaturated weathered dry disposed ash, as determined by XRD analysis, revealed quartz and mullite as the major crystalline phases; while anorthite, hematite, enstatite, lime, calcite, and mica were present as minor mineral phases. Pore water chemistry revealed a low concentration of readily soluble metals in unsaturated weathered ashes in comparison with fresh ash, which shows high leachability. This suggests that over time the precipitation of transient minor secondary mineral phases; such as calcite and mica might retard residual metal release from unsaturated weathered ash. Chloride and sulphate species of the water soluble extracts of weathered ash are at equilibrium with Na+ and K+; these demonstrate progressive leaching over time and become supersaturated at the base of unsaturated weathered ash. This suggests that the ash dump does not

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the

Ceramic Proppant Design for In-situ Microbially Enhanced Methane Recovery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sparks, Taylor D.; Mclennan, John; Fuertez, John

an initial pH value of 5.5, at 30 °C, and at a NaCl concentration 3.7 mg/cm 3 (i.e., 145,165 ppm). Task 3) To create the lightweight ceramic proppant, the kaolinite and iron oxide (Fe 2O 3) mixture were sintered under reducing atmosphere varying partial pressures of oxygen from 1.7×10 -13 atm to 1.8×10-11 atm. The Fe 2O 3 reduces to FeO and reacts with kaolinite decomposed to mullite to form Fe 2SiO 4, FeSiO 3, and FeAl 2O 4. As a result the proppant develops large pores (~100 µm), giving it a low bulk density (1.43 g/cm 3), and high porosity (45.2 vol%) at P_(O_2 )of 1.8×10 -11 atm. The proppant sintered at P_(O_2 )of 1.7×10 -13 atm is characterized by smaller pores (26 µm), higher density (1.72 g/cm3) and lower porosity (37.5 vol%). Crush resistance testing at 9,000 psi yields 6.8 wt% fine particles increasing to 17.7 wt% in porous samples. Acid solubility varies from 5.5 wt% loss increasing to 12.9 wt% in porous samples. Task 4 and 5) The microbial consortia obtained from the optimized condition and lightweight proppant were encapsulated by calcium-alginate polymer. The encapsulation system, including microbes and a proppant, was stored at 20°C and 36°C. The sample stored at 36°C generated 7.1×[10] 3 ppm of methane at 670 h, whereas the sample incubated at 20°C generated 1.1×[10] 3 ppm of methane. Benchtop lab-scale bioreactors were constructed and showed with real-time measurements that, as the microbes produced methane, the pH decreased, and hydrogen and carbon dioxide gases were consumed. A calcium ion-selective sensor revealed the release mechanism of the microbes from encapsulation. The calcium ions interconnecting the alginate monomers were disassociated by counter cations such as protons and potassium ions. The counter cations bound to the carboxyl group on the alginate monomer, which thus lost its ionic interactions with the calcium ions, resulting in decomposition of the hydrogel structure. Furthermore, the conductivity was increased to ~700

Radioactive Demonstration Of Mineralized Waste Forms Made From Hanford Low Activity Waste (Tank Farm Blend) By Fluidized Bed Steam Reformation (FBSR)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jantzen, C. M.; Crawford, C. L.; Bannochie, C. J.

-radioactive testing. The granular ESTD and BSR products (radioactive and non-radioactive) were analyzed for total constituents and durability tested as a granular waste form. A subset of the granular material was stabilized in a clay based geopolymer matrix at 42% and 65% FBSR loadings and durability tested as a monolith waste form. The 65 wt% FBSR loaded monolith made with clay (radioactive) was more durable than the 67-68 wt% FBSR loaded monoliths made from fly ash (non-radioactive) based on short term PCT testing. Long term, 90 to 107 day, ASTM C1308 testing (similar to ANSI/ANS 16.1 testing) was only performed on two fly ash geopolymer monoliths at 67-68 wt% FBSR loading and three clay geopolymer monoliths at 42 wt% FBSR loading. More clay geopolymers need to be made and tested at longer times at higher FBSR loadings for comparison to the fly ash monoliths. Monoliths made with metakaolin (heat treated) clay are of a more constant composition and are very reactive as the heat treated clay is amorphous and alkali activated. The monoliths made with fly ash are subject to the inherent compositional variation found in fly ash as it is a waste product from burning coal and it contains unreactive components such as mullite. However, both the fly ash and the clay based monoliths perform well in long term ASTM C1308 testing.« less