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At least 235 records · Page 13

Chemical and Microstructural Changes in Metallic and Ceramic Materials Exposed to Venusian Surface Conditions

The chemical and microstructural behavior of steels (304, 310, 316, and 1018), nickel-based alloys (beta-NiAl, G30, and 625), gold, coatings (4YSZ, SilcoNert(TradeMark) 1040 (SilcoTek Co.), Dursan(TradeMark) (SilcoTek Co.), and porcelain), and bulk ceramics (alpha-Al2O3, fused quartz, beta-SiC, and alpha-Si3N4) were probed after exposure to supercritical fluid with temperature, pressure, and composition mimicking the Venus lower atmosphere. Exposures were carried out in the Glenn Extreme Environments Rig (GEER) chamber with the Venusian gas mixture (96.5% CO2, 3.5% N2, 30 ppm H2O, 150 ppm SO2, 28 ppm CO, 15 ppm OCS, 3 ppm H2S, 0.5 ppm HCl, and 5 ppb HF) at 92 bar (1330 psi) and 467 C (873 F) for durations of 10 and 42 days. An additional 21-day exposure was done to stainless steel uncoated and coated with SilcoNert(TradeMark) and Dursan(TradeMark). Samples were characterized before and after the experiment by gravimetric analysis, X-ray diffraction, X-ray photoelectron and Auger electron spectroscopies, and cross section electron microscopy analysis. All steels exposed for 10 and 42 days formed double-layered scales consisting mainly of metal (Cr, Fe, Ni) oxides and sulfides showing different chemistry, microstructure, and crystalline phases. The alloys G30 and 625 formed double-layered scales consisting mainly of nickel sulfides. After 10 days, the beta-NiAl exhibited no detectable scale, suggesting only a very thin film was formed. The 304 and 316 stainless steels coated with 4YSZ that were exposed for 10 and 42 days exhibited no significant oxidation. Steel 1018 coated with 4YSZ exhibited a corrosion scale of iron and/or chromium oxide formed at the base of the alloy. The 304 steel coated with porcelain did not exhibit corrosion, although the coating exhibited recession. SilcoNert(TradeMark) exposed for 10 and 42 days exhibited recession, although no oxidation was found to occur at the base of the alloy. Stainless steel 316 coated with Dursan(TradeMark)  exhibited corrosion at the base of the alloy. All ceramics tested showed no clear evidence of reaction. The weight-gain-per-area performance of the materials exposed in the GEER for 10 and 42 days are reported from the lowest to the highest weight gain per area as follows: gold did not exhibit any weight change; nickel-based alloys: beta- NiAl < G30 < 625; steels: 304 < 310 < 316 < 1018; ceramics: considering the experimental uncertainties, no weight change was observed for all ceramics of this work (alpha-Al2O3, Si3N4, SiC, and amorphous SiO2).

Costa, Gustavo C. C.↗

Oxidation-resistant reflective surfaces for solar dynamic power generation in near Earth orbit

Reflective surfaces for space station power generation systems are required to withstand the atomic oxygen-dominated environment of near Earth orbit. Thin films of platinum and rhodium, which are corrosion resistant reflective metals, have been deposited by ion beam sputter deposition onto various substrate materials. Solar reflectances were then measured as a function of time of exposure to a RF-generated air plasma. Similarly, various protective coating materials, including MgF2, SiO2, Al2O3, and Si3N4, were deposited onto silver-coated substrates and then exposed to the plasma. Analysis of the films both before and after exposure by both ESCA and Auger spectroscopy was also performed. The results indicate that Pt and Rh do not suffer any loss in reflectance over the duration of the tests. Also, each of the coating materials survived the plasma environment. The ESCA and Auger analyses are discussed as well.

Gulino, D. A.↗

Progress on Background-Limited Membrane-Isolated TES Bolometers for Far-IR/Submillimeter Spectroscopy

To determine the lowest attainable phonon noise equivalent power (NEP) for membrane-isolation bolometers, we fabricated and measured the thermal conductance of suspended Si3N4 beams with different geometries via a noise thermometry technique. We measured beam cross-sectional areas ranging from 0.35 x 0.5 (micro)m(sup 2) to 135 x 1.0 (micro)m(sup 2) and beam lengths ranging from (micro)m to 8300 (micro)m. The measurements directly imply that membrane-isolation bolometers are capable of reaching a phonon noise equivalent power (NEP) of 4 x 10(sup -20)W/Hz(sup 1)/O . This NEP adequate for the Background-Limited Infrared-Submillimeter Spectrograph (BLISS) proposed for the Japanese SPICA observatory, and adequate for NASA's SAFIR observatory, a 10-meter, 4 K telescope to be deployed at L2. Further, we measured the heat capacity of a suspended Si 3N 4 membrane and show how this result implies that one can make membrane-isolation bolometers with a response time which is fast enough for BLISS.

submillimeter spectrometer↗

Investigation of the fracture mechanics of boride composites

Fracture energies of WC-6Co, Boride 5 (ZrB2+SiC), Boride 8(ZrB2+SiC+C) and Boride 8-M2(ZrB2+SiC+C) were measured by slow bend and impact tests of notched charpy bars. Cobalt bonded tungsten carbide exhibited impact energies of 0.76 ft-lb or 73.9 in-lb/square inch. Boride 5 and the Boride 8 exhibit impact energies one third and one quarter of that observed for WC-6Co comparing favorably with measurements for SiC and Si3N4. Slow bend-notched bar-fracture energies for WC-6Co were near 2.6 in-lb/square inch or 1/20 the impact energies. Slow bend energies for Boride 8-M2, Boride 8 and Boride 5 were 58%, 42% and 25% of the value observed for WC-6Co. Fractograph showed differences for WC-6Co where slow bend testing resulted in smooth transgranular cleavage while samples broken by impact exhibited intergranular failures. By contrast the boride fractures showed no distinction based on testing method. Fabrication studies were conducted to effect alteration of the boride composites by alloying and introduction of graphite cloth.

Kaufman, L.↗

Evaluation of oxidation resistant nonmetallic materials at 1204 C (2200 F) in a Mach 1 burner

Specimens of 23 oxidation resistant, nonmetallic, refractory materials were systematically exposed in a high gas velocity burner to simulate a turbine engine environment. Isothermal and cyclic tests were conducted at a specimen temperature of 2200F which resulted from exposure to Mach 1 or Mach 0.5 hot gas streams. Specimen behavior was judged on the basis of failure mode, appearance, and weight change. SiC and Si3N4 exhibited the most promising behavior surviving all exposures including Mach 1 for 120 cycles (10 hr). Major failure modes identified for other materials were thermal shock, thermal fatigue, and mechanical failure due to gas loading.

Sanders, W. A.↗

High gas velocity burner tests on silicon carbide and silicon nitride at 1200 C

Specimens of silicon carbide and silicon nitride were exposed to a Mach one gas velocity burner simulating a turbine engine environment. Cyclic tests up to 100 hour duration were conducted at specimen temperatures of 1200 C. A specimen geometry was used that develops thermal stresses during thermal cycling in a manner similar to blades and vanes of a gas turbine engine. Materials were compared on a basis of weight change, dimensional reductions, metallography, fluorescent penetrant inspection, X-ray diffraction analyses, failure mode, and general appearance. One hot pressed SiC, one reaction sintered SiC, and three hot pressed Si3N4 specimens survived the program goal of 100 one-hour cycle exposures. Of the materials that failed to meet the program goal, thermal fatigue was identified as the exclusive failure mode.

Sanders, W. A.↗

Directionally solidified composite systems under evaluation

The directionally solidified eutectic in-situ composites being evaluated for use as turbine materials range from ductile-ductile systems, where both matrix and reinforcement are ductile, to brittle-brittle systems, where both phases are brittle. The alloys most likely to be used in gas turbine engines in the near term are the lamellar ductile-semi ductile alloys gamma prime-delta, Ni3Al-Ni3Nb and gamma/gamma prime-delta Ni,Cr,Cb,Al/Ni3Al-Ni3Nb and the fibrous ductile-brittle alloys M-MC CoTaC or NiTaC and M-M7C3(Co,Cr,Al)-(Cr,Co)7C3. The results of tests are given which indicate that gamma prime strengthened NiTaC alloys and a (Co,Cr,Al)7C3 have greater tensile strength than the strongest superalloys at temperatures up to about 600 C. The gamma prime-delta and gamma/gamma prime-delta alloys in the Ni,Al,Nb(Cr) systems have greater tensile strength than the superalloys at temperatures greater than 800 C. At low stresses fibrous carbide reinforced eutectic alloys have longer lives at high temperatures than the strongest superalloys. Lamellar delta, Ni3Nb reinforced eutectic alloys have longer lives at high temperatures than the strongest superalloys at all stresses. The experience currently being gained in designing with the brittle ceramics SiC and Si3N4 may eventually be applied to ceramic matrix eutectic in-situ composites. However, the refractory metal fiber reinforced brittle-ductile systems may find acceptance as turbine materials before the ceramic-ceramic brittle-brittle systems.

Ashbrook, R. L.↗

Process development of beam-lead silicon-gate COS/MOS integrated circuits

Two processes for the fabrication of beam-leaded COS/MOS integrated circuits are described. The first process utilizes a composite gate dielectric of 800 A of silicon dioxide and 450 A of pyrolytically deposited A12O3 as an impurity barrier. The second process utilizes polysilicon gate metallization over which a sealing layer of 1000 A of pyrolytic Si3N4 is deposited. Three beam-lead integrated circuits have been implemented with the first process: (1) CD4000BL - three-input NOR gate; (2) CD4007BL - triple inverter; and (3) CD4013BL - dual D flip flop. An arithmetic and logic unit (ALU) integrated circuit was designed and implemented with the second process. The ALU chip allows addition with four bit accuracy. Processing details, device design and device characterization, circuit performance and life data are presented.

Baptiste, B.↗

Design, processing, and testing of LSI arrays for space station

The development of a beam-leaded low power, high performance metal-oxide-semiconductor (MOS), 256-bit random access memory (RAM) was reported. Previous success with the aluminum-gate current-sense version and a silicon-gate voltage-sense version led to the present effort to make a beam-leaded silicon-gate RAM. Some problems unique to the silicon-on-sapphire beam-lead process development are presented. Beam-leaded SOS TA5388 devices using a Si3N4 passivation layer were shown to have good electrical parameters.

Schneider, W. C.↗

Auger spectroscopy of fracture surfaces of ceramics

Results of Auger electron spectroscopy (AES) studies of fracture surfaces in a series of ceramic materials, including Al2O3, MgO, and Si3N4, which were formed using different processing techniques. AES on the fractured surface of a lunar sample is also discussed. Scanning electron micrograph fractography is used to relate the surface chemistry to the failure mode. Combined argon ion sputtering and AES studies demonstrate the local variations in chemistry near the fracture surface. The problems associated with doing AES in insulators are also discussed, and the experimental techniques directed toward solving them are described.

Marcus, H. L.↗

Sublimation behavior of silicon nitride /Si3N4/ coated silicon germanium /SiGe/ unicouples

For the Multi-Hundred Watt (MHW) Radioisotope Thermoelectric Generator (RTG), the silicon germanium unicouples are coated with silicon nitride to minimize degradation mechanisms which are directly attributable to material sublimation effects. A program is under way to determine the effective vapor suppression of this coating as a function of temperature and gas environment. The results of weight loss experiments, using Si3N4 coated hot shoes (SiMo), operating over a temperature range from 900 C to 1200 C, are analyzed and discussed. These experiments were conducted both in high vacuum and at different pressures of carbon monoxide (CO) to determine its effect on the coating. Although the results show a favorable vapor suppression at all operating temperatures, the pressure of the CO and the thickness of the coating have a decided effect on the useful lifetime of the coating.

Stapfer, G.↗

Effects of Fe2O3 addition on the nitridation of silicon powder

The reaction of silicon powder and nitrogen was studied in the range of 1300-1400 C. When an addition of Fe2O3 was more than 0.8wt%, the reaction was linear and compared to samples with no Fe2O3, the reaction velocity increased 5 to 10 times. The reactions were mediated by the process of peeling and cracking in a thin layer of Si2N4 formed on the silicon particles or on the surface of the Fe-Si melts. As the addition of Fe2O3 increased, the reaction activation energy for highly pure samples decreased. Fe2O3 which exceeded the Si3N4 solubility limits was finally converted to d-Fe.

Hasegawa, Y.↗

Ceramics in gas turbine: Powder and process characterization

Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability are pointed out. The essential features/parameters to characterize a batch of powder are discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. Significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗

Development and evaluation of die and container materials

Commercial high purity ultrafine Si3N4, Al2O3, and SiO2 powders were vacuum dried and stored under nitrogen in sealed containers. Extensive analysis of the chemical, physical, and morphological characteristics of these powders was performed. The interaction of molten silicon with fused quartz was examined in a Knudsen cell using a mass spectrometer. The solubility of oxygen at the melting point of silicon was calculated to be 1.78 times 10 to the 18th power atoms/cu cm, and the activity coefficients of oxygen and silicon monoxide, the major vapor species, were calculated to be 4.83 times 10 to the minus 24th power and 0.0000701, respectively.

Wills, R. R.↗

Effects of pressure and temperature on hot pressing a sialon

Mixed powders (60 m/o Al2O3-40 m/o Si3N4) were hot pressed at temperatures and pressures from 1360 to 1750 C and 3.5 to 27.5 MPa (0.5 to 4.0 ksi). Fully dense sialon bodies are obtainable at temperatures and pressures as low as 1550 C and 0.5 ksi. The fully dense bodies contain Beta prime and x-phase. There is some evidence that plastic deformation has contributed to densification.

Yeh, H. C.↗

Ceramics in gas turbines - Powder and process characterization

The role of powder and process characterization in producing high quality silicon nitride and silicon carbide components, for gas turbine applications, is described. Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability have been pointed out. The essential features/parameters to characterize a batch of powder have been discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. It is inevitable that significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗

High temperature compressive cracking in hot-pressed silicon nitride

Results are presented for high-temperature (1370, 1430, 1540, 1590 C) slow-strain-rate compression tests on cylindrical specimens of hot-pressed Si3N4 of the HS-130 brand under various compressive loads. The results are presented in terms of number of longitudinal cracks, percent increase in diameter, percent decrease in length, and percent loss in weight. Scanning electron micrographs are presented of cylindrical surfaces of compression specimens tested at 1430 C for 640 MN/sq m and at 1590 C for 220 MN/sq m. As compared to results obtained by other investigators, it appears more likely that the cracks resulting from compressive loading are due to subcritical crack growth caused by circumferential tensile stresses acting across grain boundaries that contain a viscous silicate glass phase.

Sanders, W. A.↗

Sialons as high temperature insulators

Sialons were evaluated for application as high temperature electrical insulators in contact with molybdenum and tungsten components in hard vacuum applications. Both D.C. and variable frequency A.C. resistivity data indicate the sialons to have electrical resistivity similar to common oxide in the 1000 C or higher range. Metallographic evaluations indicate good bonding of the type 15R ALN polytype to molybdenum and tungsten. The beta prime or modified silicon nitride phase was unacceptable in terms of vacuum stability. Additives effect on electrical resistivity. Similar resistivity decreases were produced by additions of molybdenum or tungsten to form cermets. The use of hot pressing at 1800 C with ALN, Al2 O3 and Si3N4 starting powders produced a better product than did a combination of SiO2 and AIN staring powders. It was indicated that sialons will be suitable insulators in the 1600K range in contact with molybdenum or tungsten if they are produced as a pure ceramic and subsequently bonded to the metal components at temperatures in the 1600K range.

Phillips, W. M.↗