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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 19 records

Synthesis of Nano-Crystalline Gamma-TiAl Materials

One of the principal problems with nano-crystalline materials is producing them in quantities and sizes large enough for valid mechanical property evaluation. The purpose of this study was to explore an innovative method for producing nano-crystalline gamma-TiAl bulk materials using high energy ball milling and brief secondary processes. Nano-crystalline powder feedstock was produced using a Fritsch P4(TM) vario-planetary ball mill recently installed at NASA-LaRC. The high energy ball milling process employed tungsten carbide tooling (vials and balls) and no process control agents to minimize contamination. In a collaborative effort, two approaches were investigated, namely mechanical alloying of elemental powders and attrition milling of pre-alloyed powders. The objective was to subsequently use RF plasma spray deposition and short cycle vacuum hot pressing in order to effect consolidation while retaining nano-crystalline structure in bulk material. Results and discussion of the work performed to date are presented.

Hales, Stephen J.↗

Development of YAG:Dy Thermographic Phosphor Coatings for Turbine Engine Applications

The selection and development of thermographic phosphor coatings were pursued to meet the objective of demonstrating luminescence-decay-based temperature measurements up to 1300C on the surface of a vane in an operating demonstrator turbine engine. To meet this objective, YAG:Dy was selected based on the desirable luminescence performance observed for YAG:Dy powder: (1) excellent temperature sensitivity and intensity at operating turbine engine temperatures, (2) an emission peak at the relatively short wavelength of 456 nm, where the interference from background blackbody radiation is fairly low, and (3) its nearly single exponential decay which makes for a simple, reliable temperature calibration. However, implementation of YAG:Dy for surface temperature measurements required application of YAG:Dy as a coating onto the surface of a superalloy component with a preexisting yttria-stabilized zirconia (YSZ) thermal barrier coating (TBC). An inherent dilemma in producing a YAG:Dy coating is that coating processing is constrained to be performed at temperatures below (less than 1200C) what is considered safe for the superalloy component, much lower than temperatures used to produce the high quality crystalline powder. Therefore, YAG:Dy coatings tend to exhibit lower luminescence performance compared to well prepared YAG:Dy powder, and the luminescence performance of the coating will depend on the method of coating deposition. In this presentation, the luminescence performance of YAG:Dy coatings prepared by the different methods of (1) application of a binder-based YAG:Dy-containing paint, (2) solution precursor plasma spray (SPPS), and (3) electron-beam physical vapor deposition (EB-PVD) and the effect of post-deposition heat treatments will be discussed.

Eldridge, J. I.↗

Microelectronic components and metallic oxide studies and applications

The project involved work in two basic areas: (1) Evaluation of commercial screen printable thick film conductors, resistors, thermistors and dielectrics as well as alumina substrates used in hybird microelectronics industries. Results of tests made on materials produced by seven companies are presented. (2) Experimental studies on metallic oxides of copper and vanadium, in an effort to determine their electrochemical properties in crystalline, powder mixtures and as screen printable thick films constituted the second phase of the research effort. Oxide investigations were aimed at finding possible applications of these materials as switching devices memory elements and sensors.

Williams, L., Jr.↗

A DSC study on crystalline LaRC TPI powder - A new version with higher initial molecular weight

A new version of crystalline Langley Research Center Thermoplastic Polyimide (LaRC-TPI) imidized powder, which possesses a higher initial molecular weight (MW), has been prepared and characterized. The scheme used for cyclodehydration during the synthesis of this material is described. Evidence of a higher initial MW for the subject LaRC-TPI is supported by both measurements of the inherent viscosity and the DSC thermograms. An initial melting peak at 295 C is noted in the freshly-synthesized sample. The powder can be recrystallized at any elevated temperatures below 340 C, and a single crystalline endothemic peak is always observed after various thermal histories. The heat of fusion for the fresh sample, as represented by the area under the melting peak in the directional scanning calorimeter thermogram, is about 3.9 cal/gm. Comparisons of thermal properties for the subject material are made to those exhibited by the commercial LaRC-TPI powder.

Hou, Tan-Hung↗

Characterization of crystalline LARC-TPI powder

LARC-TPI, a linear aromatic polyimide, developed by NASA Langley Research Center in the late 1970's had thermoplastic character, but its melt-flow properties were much lower than those of conventional thermoplastics. An imidized version of the LARC-TPI molding powder was submitted to NASA-Langley for evaluation. The initial broad melt of this material occurs in the 270 C range and reorders to higher melting forms, depending on the physical and thermal treatments. Rheological characterization of this polymer shows it to have a very low melt viscosity, which increases as the melted specie transforms to other crystalline forms with higher melting temperatures.

Burks, Harold D.↗

A direct process for preparing semi-crystalline polyimides

The invention is a direct process for preparing semi-crystalline polyimides. This process comprises the steps of: providing a polar aprotic solvent, adding a dianhydride and a diamine to the solvent to form a mixture, stirring the mixture at ambient temperature, and adding glacial acetic acid to the mixture to provide a ratio of polar aprotic solvent to glacial acetic acid which ranges from about 90 to 10 to about 75 to 25 by volume to form a solution. The solution was heated to a range from about 110 C to about 140 C to form a polyimide precipitate. The polyimide precipitate was recovered as a semi-crystalline polyimide powder.

Chang, Alice C.↗

Direct process for preparing semi-crystalline polyimides

The invention is a direct process for preparing semi-crystalline polyimides. This process comprises the steps of: providing a polar aprotic solvent, adding a dianhydride and a diamine to the solvent to form a mixture, stirring the mixture at ambient temperature, and adding glacial acetic acid to the mixture to provide a ratio of polar aprotic solvent to glacial acetic acid which ranges from about 90 to 10 to about 75 to 25 by volume to form a solution. The solution was heated to a range from about 110.degree. C. to about 140.degree. C. to form a polyimide precipitate. The polyimide precipitate was recovered as a semi-crystalline polyimide powder.

Chang, Alice C.↗

Experimental studies and applications of vanadium oxides.

The electrical and electrochemical properties of V-5 and V-7 vanadium oxides were investigated. The effects of pressure, temperature and moisture on the bulk resistivity of the oxides in powder, sintered, and crystalline form were determined, and the static and dynamic volt-ampere characteristics were obtained. Sintered samples tested showed better electrical stability than the compressed powder samples. Two types of commercially available vanadium pentoxide were heat-treated to obtain various crystalline oxide forms which were mounted on alumina substrates and terminated by thick-film conductors for making electrical connections. Indications are that these materials could have applications as sensors, critical-temperature resistors, high-speed switches, and temperature-compensation elements in hybrid microelectronic circuits.

Williams, L., Jr.↗

Heats of immersion of titania powders in primer solutions

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Siriwardane, R.↗

Chemically Derived Dense Alumina-Zirconia Composites for Improved Mechanical and Wear Erosion Properties

As a result of this funded project high purity Zirconia-Toughened Alumina (ZTA) ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and rheological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. This improved materials should have enhanced properties such strength, toughness, and wear resistance for advanced structural applications, for example engine components in high technology aerospace applications.

Source record↗

Characterization of the Sol-Gel Transition for Zirconia-Toughened Alumina Precursors

High purity ZTA ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and theological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. In all experimental cases a-alumina and tetragonal zirconia phases were confirmed even in the absence of yttria.

Moeti, I.↗

Solid state polymerization and crystallography of polyimide precursors

Although the production of crystallinity in a polymeric system has historically led to commerically useful properties, the polyimides, prized for their high temperature characteristics, as customarily synthesized by melt or solution casting, are amorphous. It is shown that polymide containing residual crystallinity can be synthesized by isothermal annealing of crystals of the salt of the diisopropyl ester of pyromellitic acid and phenylene diamine. The reaction is topochemical in that the geometry of the polymer product is dependent upon that of the crystalline precursor. Infrared spectroscopy reveals the presence of imide absorption in the polymer, while powder diffractometry suggests residual crystallinity. Single crystal X-ray analysis of the monomer yields a structure of chains of alternating acid and base suggesting that the monomer is amenable to polymerization with a minimum of geometrical disruption.

Wakelyn, N. T.↗

Thermoplastic matrix composites - LARC-TPI, polyimidesulfone and their blends

Composites were fabricated from unidirectional unsized AS-4 carbon fiber and two baseline polyimides: benzophenone dianhydride-3,3'-diaminodiphenylsulfone (PISO2) and benzophenone dianhydride-3,3'-diaminobenzophenone (LARC-TPI). In addition, each polymer solution prior to prepregging was doped with various amounts of crystalline LARC-TPI powder to enhance melt flow during press molding. The 2:1, 1:1, and 1:2 ratios of crystalline to amorphous resin, respectively, were studied in the LARC-TPI system and the 1:2 ratio in the PISO2 system. Matrix characterization, prepreg fabrication/characterization and composite fabrication and physical/mechanical properties are described. The latter include three point short beam shear and flexure, dry and wet, as well as fracture toughness properties in selected compositions.

Johnston, Norman J.↗

Phase transformations in xerogels of mullite composition

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

Hyatt, Mark J.↗

Phase transformations in xerogels of mullite composition

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

Hyatt, Mark J.↗

Evaluation of high temperature structural adhesives for extended service, phase 5

The evaluation of 3 experimental polymers from NASA-Langley and a commercially produced polymer from Mitsui Toatsu Chemicals as high temperature structural adhesives is presented. A polyphenylquinoxaline (PPQ), polyimide (STPI/LaRC-2), and a polyarylene ether (PAE-SO2) were evaluated as metal-to-metal adhesives. Lap shear, crack extension, and climbing drum peel specimens were fabricated from all three polymers and tested after thermal, combined thermal/humidity, and stressed hydraulic fluid (Skydrol) exposure. The fourth polymer, LARC-TPI was evaluated as an adhesive for titanium honeycomb sandwich structure. All three experimental polymers performed well as metal-to-metal adhesives from 219 K (-65 F) to 505 K (450 F), including humidity exposure. Structural adhesive strength was also maintained at 505 K for a minimum of 3000 hours. LaRC-TPI was evaluated as a high temperature (505 K) adhesive for titanium honeycomb sandwich structure. The LaRC-TPI bonding process development concentrated on improving the honeycomb core-to-skin bond. The most promising approach of those evaluated combined a LaRC-TPI polymer solution with a semi-crystalline LaRC-TPI powder for adhesive film fabrication and fillet formation.

Hendricks, C. L.↗

Processing Bi-Pb-Sr-Ca-Cu-O superconductors from amorphous state

Researchers produced superconducting ceramics of the Bi-Pb-Sr-Ca-Cu-O system started from a glass. To form the glass, the mixed oxide powder was melted at 1200 C in air. The liquid was quenched rapidly by pouring it onto an aluminum plate and rapidly pressing with another plate. The quenched compound was in the form of black amorphous solid, whose x-ray powder pattern has no crystalline peaks. After heat treatment at high temperatures, the glass crystallized into a superconductor. The crystalline phases in the superconductor identified using x-ray diffraction patterns. These phases were that associated with the superconducting phases of T(sub c) = 80 K (Bi2Ca1Sr2Cu2Ox) and of T(sub c) = 110 K (Bi2Ca2Sr2Cu3Ox). The dc resistivity and the ac susceptibility of these superconductors were studied.

Chiang, C. K.↗