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NASA NTRS1985

Reliability of void detection in structural ceramics using scanning laser acoustic microscopy

The reliability of scanning laser acoustic microscopy (SLAM) for detecting surface voids in structural ceramic test specimens was statistically evaluated. Specimens of sintered silicon nitride and sintered silicon carbide, seeded with surface voids, were examined by SLAM at an ultrasonic frequency of 100 MHz in the as fired condition and after surface polishing. It was observed that polishing substantially increased void detectability. Voids as small as 100 micrometers in diameter were detected in polished specimens with 0.90 probability at a 0.95 confidence level. In addition, inspection times were reduced up to a factor of 10 after polishing. The applicability of the SLAM technique for detection of naturally occurring flaws of similar dimensions to the seeded voids is discussed. A FORTRAN program listing is given for calculating and plotting flaw detection statistics.

Roth, D. J.↗

NASA NTRS1986

Reliability of void detection in structural ceramics by use of scanning laser acoustic microscopy

Roth, D. J.↗

NASA NTRS1990

Millimeter wave surface resistance of RBa2Cu3O(7-delta) (R=Y,Eu,Dy,Sm,Er) superconductors

The measurements are reported of the millimeter wave surface resistance R(sub s) at 58.6 GHz of bulk samples of RBa2Cu3O(7-delta) (R = Y,Eu,Dy,Sm,Er) and of YBa2Cu3O(7-delta) superconducting films, in the temperature range from 20 to 300 K. The bulk samples were prepared by cold pressing the powders of RBa2Cu3O(7-delta) into one in. disks. The powders were prepared by several sinterings in one atmosphere of oxygen at 925 C, with grindings between sinterings, to obtain the superconducting phase. The thin films were deposited on SrTiO3 and LaGaO3 substrates by pulsed laser ablation. Each sample was measured by replacing the end wall of a gold-plated Te sub 013 circular mode copper cavity with the sample and determining the cavity quality factor . From the difference in the Q-factor of the cavity, with and without the sample, the R(sub s) of the sample was determined.

Miranda, F. A.↗

NASA NTRS2001

Thermal Conductivity of Ceramic Thermal Barrier and Environmental Barrier Coating Materials

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.

Zhu, Dong-Ming↗

NASA NTRS1982

Comparison of NDE techniques for sintered-SiC components

High frequency, bulk-wave ultrasonics detected defects in manufactured SiC components. In addition, gas-turbine blades and vanes were examined by scanning laser acoustic microscopy (SLAM). Comparative results obtained on simple shapes such as disks and bars by microfocus X-ray radiography, ultrasonics, scanning photoacoustic spectroscopy, and SLAM are discussed.

Srinivasan, M.↗

NASA NTRS2003

Therma1 Conductivity and Durability of Advanced Thermal Barrier Coatings

Thermal barrier coatings (TBCs) will play a crucial role in advanced gas turbine engines because of their ability to further increase engine operating temperature and reduce cooling, thus helping to achieve engine emission and efficiency goals. Future TBCs must be designed with increased phase stability, lower thermal conductivity, and improved sintering and thermal stress resistance in order to effectively protect engine hot-section components. Advanced low conductivity TBCs are being developed at NASA by incorporating multi-component oxide dopants into zirconia-yttria or hafnia-yttria to promote the formation of thermodynamically stable defect clusters within the coating structures. This presentation will primarily focus on thermal conductivity and durability of the novel defect cluster thermal barrier coatings for turbine airfoil and combustor applications, determined by a unique CO2 laser heat-flux approach. The laser heat-flux testing approach emphasizes the real-time monitoring and assessment of the coating thermal conductivity under simulated engine temperature and thermal gradient conditions. The conductivity increase due to coating sintering (and/or phase change) and the conductivity decrease due to coating delamination have been determined under steady-state, cyclic, uniform or non-uniform heat-flux conditions. The coating radiation flux resistance has been evaluated by varying coating thermal gradients, and also by using a laser-heated radiative-flux source. Advanced multi-component TBC systems have been shown to have significantly reduced thermal conductivity and improved high temperature stability due to the nano-sized, low mobility defect clusters associated with the paired rare earth dopant additions. The effect of oxide defect cluster dopants on coating thermal conductivity, thermal stability and furnace cyclic durability will also be discussed. The current low conductivity TBC systems have demonstrated long-term cyclic durability at very high temperatures which is far beyond the baseline ZrO2-Y2O3 capabilities.

Zhu, Dong-Ming↗

NASA NTRS1990

Method of making single crystal fibers

Single crystal fibers are made from miniature extruded ceramic feed rods. A decomposable binder is mixed with powders to inform a slurry which is extruded into a small rod which may be sintered, either in air or in vacuum, or it may be used in the extruded and dried condition. A pair of laser beams focuses onto the tip of the rod to melt it thereby forming a liquid portion. A single crystal seed fiber of the same material as the feed rod contacts this liquid portion to establish a zone of liquid material between the feed rod and the single crystal seed fiber. The feed rod and the single crystal feed fiber are moved at a predetermined speed to solidify the molten zone onto the seed fiber while simultaneously melting additional feed rod. In this manner a single crystal fiber is formed from the liquid portion.

Westfall, Leonard J.↗

NASA NTRS1981

InGaAsP/InP laser development for single-mode, high-data-rate communications

Materials studies as well as general and specific device development were carried out in the InGaAsP system. A comparison was made of three standard methods of evaluating substrate quality by means of dislocation studies. A cause of reduced yield of good wafers, the pullover of melt from one bin to the next, has been analyzed. Difficulties with reproducible zinc acceptor doping have been traced to segregation of zinc in the In/Zn alloy used for the doping source. Using EBIC measurments, the pn junction was shown to drift in location depending on factors not always under control. An analysis of contact structures by SIMS showed that the depth to which the sintered Au/Zn contact penetrates into the structure is typically 0.13 microns, or well within the cap layer and out of the p-type cladding and thus not deleterious to laser prformance. The problem of single-mode laser development was investigated and it was shown to be related to the growth habit over four different possible substrate configurations. The fabrication of constricted double heterojunctions, mesa stripe buried heterostructures, and buried heterostructures was discussed, and measurements were presented on the device properties of single-mode buried heterostructure lasers. Results include single spectral line emission at 3 mW and a threshold current of 60 mA.

Ladany, I.↗

NASA NTRS2003

Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier Coatings

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.

Zhu, Dongming↗

NASA NTRS2003

Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier Coatings

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.

Zhu, Dong-Ming↗

NASA NTRS1990

Surface Cracking and Interface Reaction Associated Delamination Failure of Thermal and Environmental Barrier

In this paper, surface cracking and interface reactions of a 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 that 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. The coating design issues will also be discussed based on the observed failure mechanisms under the high-heat-flux test conditions.

Zhu, Dongming↗

NASA NTRS1988

Optical measurements of soot in premixed flames

Two laser diagnostic techniques were used to measure soot volume fractions, number densities and soot particle radii in premixed propane/oxygen flat flames. The two techniques were two wavelength extinction, using 514.5 to 632.8 nm and 457.9 to 632.8 nm wavelength combinations, and extinction/scattering using 514.5 nm light. The flames were fuel rich and had cold gas velocities varying from 3.4 to 5.5 cm/s. Measurements were made at various heights above the sintered bronze, water colored flat flame burner with the equivalence ratio and cold gas velocity fixed. Also, measurements were made at a fixed height above the burner and fixed cold gas velocity while varying the equivalence ratio. Both laser techniques are based on the same underlying assumptions of particle size distribution and soot optical properties. Full Mie theory was used to determine the extinction coefficients and the scattering efficiencies. Temperature measurements in the flame were made using infrared radiometry and fine wire thermocouples. Good agreement between the two techniques in terms of soot particle radii, number density and volume fraction was found for intensity ratios between 0.1 and 0.8.

Lyons, Valerie J.↗

NASA NTRS1987

Application of scanning acoustic microscopy to advanced structural ceramics

A review is presentod of research investigations of several acoustic microscopy techniques for application to structural ceramics for advanced heat engines. Results obtained with scanning acoustic microscopy (SAM), scanning laser acoustic microscopy (SLAM), scanning electron acoustic microscopy (SEAM), and photoacoustic microscopy (PAM) are compared. The techniques were evaluated on research samples of green and sintered monolithic silicon nitrides and silicon carbides in the form of modulus-of-rupture bars containing deliberately introduced flaws. Strengths and limitations of the techniques are described with emphasis on statistics of detectability of flaws that constitute potential fracture origins.

Vary, Alex↗

NASA NTRS2019

Optimization of Aluminum-Tin Ink Composition and Sintering in Atmospheric Conditions

This study will focus on the basics of generating an aluminum-tin ink that can sinter in air and exhibits properties near that of a solid aluminum-tin alloy. Sintering temperatures will also be assessed in this study. Once the optimal aluminum ink composition is determined, the optimal ink thickness for homogeneous sintering must be determined by additional experimentation. Additive manufacturing is a rapidly developing and growing manufacturing process and has proven successful in many different ways. Processes, such as extrusion three-dimensional (3D) printing and selective laser melting (SLM), have proven to work but have limitations, such as material capabilities or density issues. SLM is a revolutionary process for additive manufacturing of metals but cannot be used in outer space due to the need for metallic powder which would diffuse into the atmosphere in a zero-gravity environment. For this reason, metallic ink additive manufacturing is a potential solution. Work is being done on metallic ink additive manufacturing in a vacuum for electrical applications. This project has focused on developing an aluminum-tin metallic ink that can sinter without the need of a vacuum or inert gas-purged atmosphere in order to prevent oxidation of the aluminum by adding flux. Once a potential ink composition has been determined through sintering of small disks and thin layers of ink, the ink may be studied with a multimaterial 3D printer at NASA Marshall Space Flight Center (MSFC) in future experiments. If successful, this aluminum-tin ink will be capable for use on the International Space Station to make replacement parts quickly. Along with its zero-gravity advantages, this ink may also have applications on Earth because it may be extruded on a substrate with precise ceramic tips in a 3D printing process. This would allow the fabrication of precise, complex shapes and may generate a much faster and more efficient printing process as compared with traditional powder bed additive manufacturing processes. The process would not be limited by a small building volume because the system would not require an enclosed chamber.

Courtright, Z. S.↗

NASA NTRS1998

Thermal High- and Low-Cycle Fatigue Behavior of Thick Thermal Barrier Coating Systems

Ceramic thermal barrier coatings have received increasing attention for advanced gas turbine and diesel engine applications because of their ability to provide thermal insulation to engine components. However, the durability of these coatings under the severe thermal cycling conditions encountered in a diesel engine (ref. 1) still remains a major issue. In this research at the NASA Lewis Research Center, a high-power laser was used to investigate the thermal fatigue behavior of a yttria-stabilized zirconia coating system under simulated diesel engine conditions. The mechanisms of fatigue crack initiation and propagation, and of coating failure under complex thermal low-cycle fatigue (LCF, representing stop/start cycles) and thermal high-cycle fatigue (HCF, representing operation at 1300 rpm) are described. Continuous wave and pulse laser modes were used to simulate pure LCF and combined LCF/HCF, respectively (ref. 2). The LCF mechanism was found to be closely related to the coating sintering and creep at high temperatures. These creep strains in the ceramic coating led to a tensile stress state during cooling, thus providing the major driving force for crack growth under LCF conditions. The combined LCF/HCF tests induced more severe coating surface cracking, microspallation, and accelerated crack growth than did the pure LCF test. HCF thermal loads also facilitated lateral crack branching and ceramic/bond coat interface delaminations. HCF is associated with the cyclic stresses originating from the high-frequency temperature fluctuation at the ceramic coating surface. The HCF thermal loads act on the crack by a wedging mechanism (ref. 1), resulting in continuous crack growth at temperature. The HCF stress intensity factor amplitude increases with the interaction depth and temperature swing, and decreases with the crack depth. HCF damage also increases with the thermal expansion coefficient and the Young's modulus of the ceramic coating (refs. 1 and 3).

Miller, Robert A.↗

NASA NTRS1988

Optical measurements of soot and temperature profiles in premixed propane-oxygen flames

Two laser diagnostic techniques were used to measure soot volume fractions, number densities and soot particle radii in premixed propane/oxygen flat flames. The two techniques used were two wavelength extinction, using 514.5 nm to 632.8 nm and 457.9 nm to 632.8 nm wavelength combinations, and extinction/scattering using 514.5 nm light. The flames wre fuel-rich (equivalence ratios from 2.1 to 2.8) and had cold gas velocities varying from 3.4 to 5.5 cm/s. Measurements were made at various heights above the sintered-bronze, water-cooled flat flame burner with the equivalence ratio and cold gas velocity fixed. Also, measurements were made at a fixed height above the burner and fixed cold gas velocity while varying the equivalence ratio. Both laser techniques are based on the same underlying assumptions of particle size distribution and soot optical properties. Full Mie theory was used to determine the extinction coefficients K sub ext, and the scattering efficiencies, Q sub vv. Temperature measurements in the flames were made using infrared radiometry. Good agreement between the two techniques in terms of soot particle radii, number density and volume fraction was found for intensity ratios (I/I sub o) between 0.1 and 0.8. For intensity ratios higher or lower than this range, the differences in extinction coefficients at the wavelengths chosen for the two-wavelength method are too small to give accurate results for comparing particle radii and number densities. However, when comparing only soot volume fractions, the agreement between the two techniques continued to be good for intensity ratios up to 0.95.

Lyons, Valerie J.↗

NASA NTRS1988

Optical measurements of soot and temperature profiles in premixed propane-oxygen flames

Two laser diagnostic techniques were used to measure soot volume fractions, number densities and soot particle radii in premixed propane/oxygen flat flames. The two techniques used were two wavelength extinction, using 514.5 nm to 632.8 nm and 457.9 nm to 632.8 nm wavelength combinations, and extinction/scattering using 514.5 nm light. The flames were fuel-rich (equivalence ratios from 2.1 to 2.8) and had cold gas velocities varying from 3.4 to 5.5 cm/s. Measurements were made at various heights above the sintered-bronze, water-cooled flat flame burner with the equivalence ratio and cold gas velocity fixed. Also, measurements were made at a fixed height above the burner and fixed cold gas velocity while varying the equivalence ratio. Both laser techniques are based on the same underlying assumptions of particle size distribution and soot optical properties. Full Mie theory was used to determine the extinction coefficients K sub ext, and the scattering efficiencies, Q sub vv. Temperature measurements in the flames were made using infrared radiometry. Good agreement between the two techniques in terms of soot particle radii, number density and volume fraction was found for intensity ratios (I/I sub o) between 0.1 and 0.8. For intensity ratios higher or lower than this range, the differences in extinction coefficients at the wavelengths chosen for the two-wavelength method are too small to give accurate results for comparing particle radii and number densities. However, when comparing only soot volume fractions, the agreement between the two techniques continued to be good for intensity ratios up to 0.95.

Lyons, V. J.↗

NASA NTRS2003

Development of Advanced Thermal and Environmental Barrier Coatings Using a High-Heat-Flux Testing Approach

The development of low conductivity, robust thermal and environmental barrier coatings requires advanced testing techniques that can accurately and effectively evaluate coating thermal conductivity and cyclic resistance at very high surface temperatures (up to 1700 C) under large thermal gradients. In this study, a laser high-heat-flux test approach is established for evaluating advanced low conductivity, high temperature capability thermal and environmental barrier coatings under the NASA Ultra Efficient Engine Technology (UEET) program. The test approach emphasizes the real-time monitoring and assessment of the coating thermal conductivity, which initially rises under the steady-state high temperature thermal gradient test due to coating sintering, and later drops under the cyclic thermal gradient test due to coating cracking/delamination. The coating system is then evaluated based on damage accumulation and failure after the combined steady-state and cyclic thermal gradient tests. The lattice and radiation thermal conductivity of advanced ceramic coatings can also be evaluated using laser heat-flux techniques. The external radiation resistance of the coating is assessed based on the measured specimen temperature response under a laser- heated intense radiation-flux source. The coating internal radiation contribution is investigated based on the measured apparent coating conductivity increases with the coating surface test temperature under large thermal gradient test conditions. Since an increased radiation contribution is observed at these very high surface test temperatures, by varying the laser heat-flux and coating average test temperature, the complex relation between the lattice and radiation conductivity as a function of surface and interface test temperature may be derived.

Zhu, Dongming↗