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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

Corrosion of Mullite by Molten Salts

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

Jacobson, Nathan S.↗
NASA NTRS2001

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

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.

Palko, James W.↗
DOE OSTI2025

Additive manufacturing of mullite ceramic by digital light processing

Mullite material was successfully additively manufactured using digital light processing (DLP). The printed geometry involves a one-step process of pyrolysis, de-binding, and sintering under a plain atmosphere to achieve an average of 76 % ceramic yield and linear shrinkage of 12 %. Furthermore, the thermal profile was carefully controlled to obtain consistent phases in which the XRD shows a mullite phase. Here, in addition, the Weibull analysis was conducted on the sintered flexural specimens, showing a Weibull modulus (m) of 13.05 with a characteristic strength (σ 0 ) of 94.96 MPa. Synchrotron microtomography was performed on the sintered specimens, which showed two distinct porosity distributions (small and large). Large porosity (non-spherical elongated) is the primary cause of decreased material strength, while small porosity (spherical) is the sintering product. The measured thermal conductivity of the specimens was in the range of 2.7–3.1 W/m∙k and decreased with an increase in temperature. Lastly, large-scale prototypes were printed concurrently with a fine resolution of 25 μm without any compromise on the predetermined design and structure.

Additive manufacturing↗
DOE OSTI2026

Physicochemical properties of digital light processing 3D-Printed alumina and mullite ceramics

Alumina ceramics fabricated using conventional techniques such as uniaxial pressing or injection molding are popular due to their low density, excellent insulation, and mechanical properties. However, these methods often limit the fabrication of complex geometries with high dimensional accuracy due to tooling constraints and limited design freedom. To overcome these limitations, this study employed Digital Light Processing (DLP) additive manufacturing (AM), which enables the production of precise structures. In addition, the optimization of sintering parameters to enhance the densification and performance of alumina and mullite ceramics was investigated, with a specific focus on how varying sintering temperatures and hold times affect part shrinkage, geometric accuracy, and material integrity. Flexural strength of both alumina and mullite specimens was clearly influenced by the way the layers was stacked. When layers were arranged across the direction of the applied load (Z = 4; XZ), the strength was higher than when they were stacked along the same direction as the load (Z = 3; XY). Weibull analysis based on these results showed high modulus values across all samples, indicating good reliability in the flexural strength measurements. This reliability, combined with the clear influence of sintering parameters, highlights how processing conditions effect the material properties and mechanical performance of parts produced through DLP additive manufacturing. In conclusion, these findings open new avenues for ceramic AM across various applications, enhancing the potential for innovation in fields such as aerospace, biomedical engineering, and energy.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Phase separation in mullite-composition glass

Aluminosilicates (AS) are ubiquitous in ceramics, geology, and planetary science, and their glassy forms underpin vital technologies used in displays, waveguides, and lasers. In spite of this, the nonequilibrium behavior of the prototypical AS compound, mullite (40SiO 2 -60Al 2 O 3 , or AS60), is not well understood. By deeply supercooling mullite-composition liquid via aerodynamic levitation, we observe metastable liquid–liquid unmixing that yields a transparent two-phase glass, comprising a nanoscale mixture of AS7 and AS62. Extrapolations from X-ray scattering measurements show the AS7 phase is similar to vitreous SiO 2 with a few Al species substituted for Si. The AS62 phase is built from a highly polymerized network of 4-, 5-, and 6-coordinated AlO x polyhedra. Polymerization of the AS62 network and the composite morphology provide essential mechanisms for toughening the glass.

36 MATERIALS SCIENCE↗
NASA NTRS1973

An exploratory study of the microstructure of mullite fibers

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

Santoro, G. J.↗
NASA NTRS1973

Environmental testing of REI-Mullite thermal protection system for the space shuttle orbiter

Tests conducted to evaluate performances in the natural environments of salt spray, humidity, rain, vacuum, and cryogenic temperatures have shown the ceramic mullite fiber is completely compatible and that these environments have no adverse effects on subsequent mission performance. Rain erosion testing has indicated a damage threshold that must be accounted for in the final design. Tests conducted to evaluate the performance of ceramic mullite fiber to induced acoustic, re-entry, and structural load environments again have shown complete capability to fulfill mission environments. Although minor cracking of the sidewall coating was seen to occur throughout the induced environment test program, sidewall designs configured to provide increased flexibility have been successfully tested.

Gluck, R.↗
NASA NTRS1974

Development of fine diameter mullite fiber

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

Long, W. G.↗
NASA NTRS1991

Making Mullite Fibers By Airgap Wet Spinning

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

Tucker, Dennis S.↗
NASA NTRS1991

Production of mullite fibers

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

Tucker, Dennis S.↗
NASA NTRS1999

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

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.

Lee, Kang N.↗
NASA NTRS2000

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

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.

Lee, Kang N.↗
NASA NTRS2002

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

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.

Lee, Kang N.↗
DOE OSTI2021

Structural, vibrational, thermal, and magnetic properties of mullite-type NdMnTiO 5 ceramic

Mullite-type $R$Mn 2 O 5 ($R$ = Y, rare-earth element) ceramics are of ongoing research attention because of their interesting crystal-chemical and magnetic properties. We report nuclear and magnetic structures of NdMnTiO 5 together with its spectroscopic, thermogravimetric, and magnetic properties. The polycrystalline sample is prepared by solid-state synthesis and characterized from neutron and X-ray powder diffraction data Rietveld refinements. NdMnTiO 5 crystallizes in the orthorhombic space group $Pbam$ with metric parameter $a$ = 755.20(1) pm, $b$ = 869.91(1) pm, $c$ = 582.42(1) pm, and $V$ = 382.62(1) 10 6 pm 3 . The Mn 3+ and Ti 4+ cations are observed to be located in the octahedral and pyramidal sites, respectively. The vibrational features in these polyhedral sites are characterized by Raman and Fourier transform infrared spectroscopes. The higher decomposition temperature of NdMnTiO 5 , compared to other $R$Mn 2 O 5 phases, is explained in terms of the higher bond strength of Ti-O bonds than those of Mn-O bonds. Temperature-dependent DC magnetic susceptibility suggests a paramagnetic to antiferromagnetic phase transition at 43(1) K. Inverse susceptibility in the paramagnetic region above 120 K follows the Curie-Weiss law, resulting in a magnetic moment of 6.33(1) μ B per formula unit. Neutron diffraction data collected at 7.5 K reveal that the magnetic moments of Nd 3+ and Mn 3+ in NdMnTiO 5 are incommensurately ordered with a propagation vector $k$ = (0, 0.238, 0.117).

36 MATERIALS SCIENCE↗
DOE OSTI2023

High-Entropy Oxides in the Mullite-Type Structure

High-entropy materials (HEMs) represent a new class of solid solutions containing at least five different elements. Their compositional diversity makes them promising as platforms for the development of functional materials. We synthesized new HEMs in a mullite-type structure and present five compounds, i.e., Bi 2 (Al 0.25 Ga 0.25 Fe 0.25 Mn 0.25 ) 4 O 9 and A 2 Mn 4 O 10 with variations of A = Nd, Sm, Y, Er, Eu, Ce, and Bi, demonstrating the vast accessible composition space. By combining scattering, microscopy, and spectroscopy techniques, we show that our materials are mixed solid solutions. Remarkably, when following their crystallization in situ using X-ray diffraction and X-ray absorption spectroscopy, we find that the HEMs form through a metastable amorphous phase without the formation of any crystalline intermediates. We expect that our synthesis is excellently suited to synthesizing diverse HEMs and therefore will have a significant impact on their future exploration.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Anti-reflection coating with mullite and Duroid for large-diameter cryogenic sapphire and alumina optics

We developed a broadband two-layer anti-reflection (AR) coating for use on a sapphire half-wave plate (HWP) and an alumina infrared (IR) filter for the cosmic microwave background (CMB) polarimetry. Measuring the faint CMB B-mode signals requires maximizing the number of photons reaching the detectors and minimizing spurious polarization due to reflection with an off-axis incident angle. Sapphire and alumina have high refractive indices of 3.1 and are highly reflective without an AR coating. This paper presents the design, fabrication, quality control, and measured performance of an AR coating using thermally sprayed mullite and Duroid 5880LZ. This technology enables large optical elements with diameters of 600 mm. We also present a thermography-based nondestructive quality control technique, which is key to assuring good adhesion and preventing delamination when thermal cycling. We demonstrate the average reflectance of about 2.6% (0.9%) for two observing bands centered at 90/150 (220/280) GHz. At room temperature, the average transmittance of a 105 mm square test sample at 220/280 GHz is 83%, and it will increase to 90% at 100 K, attributed to reduced absorption losses. Therefore, our developed layering technique has proved effective for 220/280 GHz applications, particularly in addressing dielectric loss concerns. This AR coating technology has been deployed in the cryogenic HWP and IR filters of the Simons Array and the Simons observatory experiments and applies to future experiments such as CMB-S4.

Sakaguri, Kana (ORCID:0000000156678118)↗
NASA NTRS1973

Processing of Rigidized Rei-mullite Insulative Composites

Systematic development and evaluation of ceramic fiber Mullite are summarized: (1) Major reductions in thermal protection system weight have been achieved by reducing the density and thermal conductivity of the insulation by 20 and 25 percent; (2) already adequate structural margins-of-safety have been greatly enhanced by increasing the tensile strength and strain-to-failure capabilities of the insulation by factors of 3 and 2; (3) cost effectiveness has been increased through the achievement of a high degree of uniformity and reproducibility of properties and through process simplification and binder modifications; and (4) maximization of multimission capability at surface temperatures of 1644 K has been achieved through firing cycle adjustments and the development of a material with high dimensional stability.

Gebhardt, J. J.↗