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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Dielectric Performance of a High Purity HTCC Alumina at High Temperatures - a Comparison Study with Other Polycrystalline Alumina

A very high purity (99.99+%) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this alumina material for co-firing processing. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96% polycrystalline alumina (96% Al2O3), where 96% alumina was used as the benchmark. A prototype packaging system based on regular 96% alumina with Au thickfilm metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500 C. In order to evaluate this new high purity HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96% alumina and a previously tested LTCC alumina from room temperature to 550 C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96% alumina and a selected LTCC alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

Electronic packaging↗
NASA NTRS2012

Dielectric Performance of High Purity HTCC Alumina at High Temperatures - A Comparison Study with Other Polycrystalline Alumina

A very high purity (99.99+) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this co-fired material. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96 polycrystalline alumina (96 Al2O3), where 96 alumina was used as the benchmark. A prototype packaging system based on regular 96 alumina with Au thick-film metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500C. In order to evaluate this new HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96 alumina and a LTCC alumina from room temperature to 550C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96 alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

High temperature↗
NASA NTRS1975

Edge-defined film-fed growth of beta-alumina and Mg-substituted beta-alumina

High Na vapor pressure, peritectic decomposition, and high reactivity of the melt complicate the growth of beta-alumina crystals. These difficulties were overcome by using a high-pressure (300 psig) growth chamber, Na2O-rich melts, and Ir for all surfaces in contact with the melt. These procedures were combined with the edge-defined film-fed growth technique to produce single-crystal beta-alumina tubes and ribbons.

Morrison, A. D.↗
NASA NTRS1978

Interaction of hydrogen chloride with alumina

The influence of temperature, pressure, and outgas conditions on the absorption of hydrogen chloride and water vapor on both alpha and gamma alumina was studied. Characterization of the adsorbents was performed using X-ray powder diffraction, scanning electron microscopy (SEM), low temperature nitrogen adsorption desorption measurements, BET nitrogen surface area measurements and electron spectroscopy for chemical analysis (ESCA). Water vapor adsorption isotherms at 30, 40, and 50 C were measured on alpha and gamma alumina after outgassing at 80, 200, and 400 C. Both outgas temperature and adsorption temperature influenced the adsorption of water vapor on the aluminas. The water vapor adsorption was completely reversible. Alpha alumina absorbed more water per unit area than gamma alumina. Differences in the adsorption capacity for water vapor of the two aluminas were explained on the basis of ideal surface models of alpha and gamma alumina. Isosteric heats of adsorption for water vapor on the aluminas were determined over a limited range of surface coverage.

Bailey, R. R.↗
NASA NTRS2007

Process for High-Rate Fabrication of Alumina Nanotemplates

An anodizing process, at an early stage of development at the time of reporting the information for this article, has shown promise as a means of fabricating alumina nanotemplates integrated with silicon wafers. Alumina nanotemplates are basically layers of alumina, typically several microns thick, in which are formed approximately regular hexagonal arrays of holes having typical diameters of the order of 10 to 100 nm. Interest in alumina nanotemplates has grown in recent years because they have been found to be useful as templates in the fabrication of nanoscale magnetic, electronic, optoelectronic, and other devices. The present anodizing process is attractive for the fabrication of alumina nanotemplates integrated with silicon wafers in two respects: (1) the process involves self-ordering of the holes; that is, the holes as formed by the process are spontaneously arranged in approximately regular hexagonal arrays; and (2) the rates of growth (that is, elongation) of the holes are high enough to make the process compatible with other processes used in the mass production of integrated circuits. In preparation for fabrication of alumina nanotemplates in this process, one first uses electron-beam evaporation to deposit thin films of titanium, followed by thin films of aluminum, on silicon wafers. Then the alumina nanotemplates are formed by anodizing the aluminum layers, as described below. In experiments in which the process was partially developed, the titanium films were 200 A thick and the aluminum films were 5 m thick. The aluminum films were oxidized to alumina, and the arrays of holes were formed by anodizing the aluminum in aqueous solutions of sulfuric and/or oxalic acid at room temperature (see figure). The diameters, spacings, and rates of growth of the holes were found to depend, variously, on the composition of the anodizing solution, the applied current, or the applied potential, as follows: In galvanostatically controlled anodizing, regardless of the chemical composition of the solution, relatively high current densities (50 to 100 mA/cm2) resulted in arrays of holes that were more nearly regular than were those formed at lower current densities. . The rates of elongation of the holes were found to depend linearly on the applied current density: the observed factor of proportionality was 1.2 (m/h)/(mA/cm2). For a given fixed current density and room temperature, the hole diameters were found to depend mainly on the chemical compositions of the anodizing solutions. The holes produced in sulfuric acid solutions were smaller than those produced in oxalic acid solutions. The arrays of holes produced in sulfuric acid were more ordered than were those produced in oxalic acid. . The breakdown voltage was found to decrease logarithmically with increasing concentration of sulfuric acid. The breakdown voltage was also found to decrease with temperature and to be accompanied by a decrease in hole diameter. The hole diameter was found to vary linearly with applied potential, with a slope of 2.1 nm/V. This slope differs from slopes (2.2 and 2.77 nm/V) reported for similar prior measurements on nanotemplates made from bulk aluminum. The differences among these slopes may be attributable to differences among impurities and defects in bulk and electron-beam-evaporated aluminum specimens.

Myung, Nosang↗
NASA NTRS1987

Zirconia toughened SiC whisker reinforced alumina composites small business innovation research

The objective of this phase 1 project was to develop a ceramic composite with superior fracture toughness and high strength, based on combining two toughness inducing materials: zirconia for transformation toughening and SiC whiskers for reinforcement, in a controlled microstructure alumina matrix. The controlled matrix microstructure is obtained by controlling the nucleation frequency of the alumina gel with seeds (submicron alpha-alumina). The results demonstrate the technical feasibility of producing superior binary composites (Al2O3-ZrO2) and tertiary composites (Al2O3-ZrO2-SiC). Thirty-two composites were prepared, consolidated, and fracture toughness tested. Statistical analysis of the results showed that: (1) the SiC type is the key statistically significant factor for increased toughness; (2) sol-gel processing with a-alumina seed had a statistically significant effect on increasing toughness of the binary and tertiary composites compared to the corresponding mixed powder processing; and (3) ZrO2 content within the range investigated had a minor effect. Binary composites with an average critical fracture toughness of 6.6MPam sup 1/2, were obtained. Tertiary composites with critical fracture toughness in the range of 9.3 to 10.1 MPam sup 1/2 were obtained. Results indicate that these composites are superior to zirconia toughened alumina and SiC whisker reinforced alumina ceramic composites produced by conventional techniques with similar composition from published data.

Loutfy, R. O.↗
NASA NTRS1998

Effects of Ambient High Temperature Exposure on Alumina-Titania High Emittance Surfaces for Solar Dynamic Systems

Solar dynamic (SD) space power systems require durable, high emittance surfaces on a number of critical components, such as heat receiver interior surfaces and parasitic load radiator (PLR) elements. To enhance surface characteristics, an alumina-titania coating has been applied to 500 heat receiver thermal energy containment canisters and the PLR of NASA Lewis Research Center's (LeRC) 2 kW SD ground test demonstrator (GTD). The alumina-titania coating was chosen because it had been found to maintain its high emittance under vacuum (less than or equal to 10(exp -6) torr) at high temperatures (1457 F (827 C)) for an extended period (approximately 2,700 hours). However, preflight verification of SD systems components, such as the PLR require operation at ambient pressure and high temperatures. Therefore, the purpose of this research was to evaluate the durability of the alumina-titania coating at high temperature in air. Fifteen of sixteen alumina-titania coated Incoloy samples were exposed to high temperatures (600 F (316 C) to l500 F (816 C)) for various durations (2 to 32 hours). Samples, were characterized prior to and after heat treatment for reflectance, solar absorptance, room temperature emittance and emittance at 1,200 F (649 C). Samples were also examined to detect physical defects and to determine surface chemistry using optical microscopy, scanning electron microscopy operated with an energy dispersive spectroscopy (EDS) system, and x ray photoelectron spectroscopy (XPS). Visual examination of the heat-treated samples showed a whitening of samples exposed to temperatures of 1,000 F (538 C) and above. Correspondingly, the optical properties of these samples had degraded. A sample exposed to 1,500 F (816 C) for 24 hours had whitened and the thermal emittance at 1,200 F (649 C) had decreased from the non-heat treated value of 0.94 to 0.62. The coating on this sample had become embrittled with spalling off the substrate noticeable at several locations. Based on this research it is recommended that preflight testing of SD components with alumina-titania coatings be restricted to temperatures no greater than 600 F (316 C) in air to avoid optical degradation. Moreover, components with the alumina-titania coating are likely to experience optical property degradation with direct atomic oxygen exposure in space.

deGroh, Kim K.↗
NASA NTRS1993

Tribological characteristics of sputtered Au/Cr films on alumina substrates at elevated temperatures

Research to evaluate the tribological properties of alumina pins sliding against thin sputtered gold films deposited on alumina disk substrates is described. A 250 A thick chromium interlayer was first deposited onto the alumina test disks to enhance adhesion and high temperature wetting of the gold films. The Au/Cr films were tribotested in pure sliding in a pin-on-disk tribometer under a 4.9 N load at 1m/s. The test atmosphere was room air at temperatures of 25, 500, and 800 C and the test duration varied from 60 to 540 min. The use of the Au/Cr films reduced friction by about a factor of two compared to the unlubricated alumina sliding couple. The coatings prevented wear of the alumina substrate disks and reduced pin wear by one to two orders of magnitude. In addition, wear lives in excess of 200,000 sliding passes (9 hr) were observed during sliding at 800 C. The results suggest that these films show promise for the practical lubrication of many high temperature sliding components.

Benoy, P. A.↗
NASA NTRS2003

Thermal Conductivity of Alumina-Toughened Zirconia Composites

10-mol% yttria-stabilized zirconia (10YSZ)-alumina composites containing 0 to 30 mol% alumina were fabricated by hot pressing at 1500 C in vacuum. Thermal conductivity of the composites, determined at various temperatures using a steady-state laser heat flux technique, increased with increase in alumina content. Composites containing 0, 5, and 10-mol% alumina did not show any change in thermal conductivity with temperature. However, those containing 20 and 30-mol% alumina showed a decrease in thermal conductivity with increase in temperature. The measured values of thermal conductivity were in good agreement with those calculated from simple rule of mixtures.

Bansal, Narottam P.↗
NASA NTRS2005

Thermal Conductivity of Alumina-reinforced Zirconia Composites

10-mol% yttria-stabilized zirconia (10SZ) - alumina composites containing 0-30 mol% alumina were fabricated by hot pressing at 1500 C in vacuum. Thermal conductivity was determined at various temperatures using a steady-state laser heat flux technique. Thermal conductivity of the composites increased with increase in alumina content. Composites containing 0, 5, and 10-mol% alumina did not show any change in thermal conductivity with temperature. However, those containing 20 and 30-mol% alumina showed a decrease in thermal conductivity with increase in temperature. The measured values of thermal conductivity were in good agreement with those calculated from the Maxwell-Eucken model where one phase is uniformly dispersed within a second major continuous phase.

Bansal, Narottam P.↗
NASA NTRS2012

Fischer-Tropsch Cobalt Catalyst Improvements with the Presence of TiO2, La2O3, and ZrO2 on an Alumina Support

The objective of this study was to evaluate the effect of titanium oxide, lanthanum oxide, and zirconium oxide on alumina supported cobalt catalysts. The hypothesis was that the presence of lanthanum oxide, titanium oxide, and zirconium oxide would reduce the interaction between cobalt and the alumina support. This was of interest because an optimized weakened interaction could lead to the most advantageous cobalt dispersion, particle size, and reducibility. The presence of these oxides on the support were investigated using a wide range of characterization techniques such as SEM, nitrogen adsorption, x-ray diffraction (XRD), temperature programmed reduction (TPR), temperature programmed reduction after reduction (TPR-AR), and hydrogen chemisorptions/pulse reoxidation. Results indicated that both La2O3 and TiO2 doped supports facilitated the reduction of cobalt oxide species in reference to pure alumina supported cobalt catalysts, however further investigation is needed to determine the effect of ZrO2 on the reduction profile. Results showed an increased corrected cluster size for all three doped supported catalysts in comparison to their reference catalysts. The increase in reduction and an increase in the cluster size led to the conclusion that the support-metal interaction weakened by the addition of TiO2 and La2O3. It is also likely that the interaction decreased upon presence of ZrO2 on the alumina, but further research is necessary. Preliminary results have indicated that the alumina-supported catalysts with titanium oxide and lanthanum oxide present are of interest because of the weakened cobalt support interaction. These catalysts showed an increased extent of reduction, therefore more metallic cobalt is present on the support. However, whether or not there is more cobalt available to participate in the Fischer-Tropsch synthesis reaction (cobalt surface atoms) depends also on the cluster size. On one hand, increasing cluster size alone tends to decrease the active site density; on the other hand, by increasing the size of the cobalt clusters, there is less likelihood of forming oxidized cobalt complexes (cobalt aluminate) during Fischer-Tropsch synthesis. Thus, from the standpoint of stability, improving the extent of reduction while increasing the particle size slightly may be beneficial for maintaining the sites, even if there is a slight decrease in overall initial active site density.

Klettlinger, Jennifer Lindsey Suder↗
NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.

High temperature↗
NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.

electronic packaging↗
NASA NTRS1973

Electromotive force measurements on cells involving beta-alumina solid electrolyte

Open circuit emf measurements have been made to demonstrate that a two-phase, polycrystalline mixture of beta- alumina and alpha-alumina could be used as a solid electrolyte in galvanic cells with reversible electrodes fixing oxygen or aluminum chemical potentials. These measurements indicate that such a two phase solid electrolyte can be used to monitor oxygen chemical potentials as low as that corresponding to Al, Al2O3 coexistence. The activity of Na2O in beta-alumina in coexistence with alpha-alumina was also determined by emf measurements.

Choudhury, N.↗
NASA NTRS1973

Electromotive force measurements on cells involving beta-alumina solid electrolyte

Open-circuit emf measurements have been made to demonstrate that a two-phase, polycrystalline mixture of beta-alumina and alpha-alumina could be used as a solid electrolyte in galvanic cells with reversible electrodes fixing oxygen or aluminum chemical potentials. These measurements indicate that such a two-phase solid electrolyte may be used to monitor oxygen chemical potentials as low as that corresponding to Al and Al2O3 coexistence (potentials of about 10 to the minus 47th power atm at 1000 K). The activity of Na2O in beta-alumina in coexistence with alpha-alumina was also determined by emf measurements.

Choudhury, N. S.↗
NASA NTRS1984

Surface chloride salt formation on Space Shuttle exhaust alumina

Aluminum oxide samples from the exhaust of Space Shuttle launches STS-1, STS-4, STS-5, and STS-6 were collected from surfaces on or around the launch pad complex and chemically analyzed. The results indicate that the particulate solid-propellant rocket motor (SRM) alumina was heavily chlorided. Concentrations of water-soluble aluminum (III) ion were large, suggesting that the surface of the SRM alumina particles was rendered soluble by prior reactions with HCl and H2O in the SRM exhaust cloud. These results suggest that Space Shuttle exhaust alumina particles are good sites for nucleation and condensation of atmospheric water. Laboratory experiments conducted at 220 C suggest that partial surface chloriding of alumina may occur in hot Space Shuttle exhaust plumes.

Cofer, W. R., III↗
NASA NTRS2003

Processing of Alumina-Toughened Zirconia Composites

Dense and crack-free 10-mol%-yttria-stabilized zirconia (10YSZ)-alumina composites, containing 0 to 30 mol% of alumina, have been fabricated by hot pressing. Release of pressure before onset of cooling was crucial in obtaining crack-free material. Hot pressing at 1600 C resulted in the formation of ZrC by reaction of zirconia with grafoil. However, no such reaction was observed at 1500 C. Cubic zirconia and -alumina were the only phases detected from x-ray diffraction indicating no chemical reaction between the composite constituents during hot pressing. Microstructure of the composites was analyzed by scanning electron microscopy and transmission electron microscopy. Density and elastic modulus of the composites followed the rule-of-mixtures. Addition of alumina to 10YSZ resulted in lighter, stronger, and stiffer composites by decreasing density and increasing strength and elastic modulus.

Bansal, Narottam P.↗
NASA NTRS2003

Alumina Volatility in Water Vapor at Elevated Temperatures: Application to Combustion Environments

The volatility of alumina in high temperature water vapor was determined by measuring weight loss of sapphire coupons at temperatures between 1250 and 1500 C, water vapor partial pressures between 0.15 and 0.68 atm in oxygen, at one atmosphere total pressure, and a gas velocity of 4.4 centimeters per second. The variation of the volatility with water vapor partial pressure was consistent with Al(OH)3(g) formation. The enthalpy of reaction to form Al(OH)3(g) from alumina and water vapor was found to be 210 plus or minus 20 kJ/mol. Surface rearrangement of ground sapphire surfaces increased with water vapor partial pressure, temperature and volatility rate. Recession rates of alumina due to volatility were determined as a function of water vapor partial pressure and temperature to evaluate limits for use of alumina in long term applications in combustion environments.

Opila, Elizabeth J.↗