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Rogers, Richard B.

Publications and source records attributed to Rogers, Richard B..

Durability of YSZ Coated Ti2AlC in 1300 °C Mach 0.3 Burner Rig Tests

A thermal barrier coating system survived burner rig testing at 1300 °C for 500 h. A 160 µm thick yttria stabilized zirconia (YSZ) coating was applied to a Ti2AlC MAX phase bar sample by plasma spray physical vapor deposition (PS-PVD) and tested face-on in an atmospheric Mach 0.3 jet fuel burner, using 5-h thermal cycles. No thermal barrier coating (TBC) spallation or recession was observed, only a 2.4 mg/cm2 mass gain. The modest weight gain precluded severe volatility losses under high velocity burner conditions. The coating surface exhibited colonies of (111)flourite fiber-textured columns separated by craze patterns, with no visible moisture attack. The metastable tetragonal t' YSZ phase was obtained initially, transitioning to equilibrium teq and cubic YSZ, but with little detrimental monoclinic. The thickness of the alumina TGO was ~21 to 23 μm under the heated YSZ face and ~13 to 15 μm on the uncoated, cooler backside. The backside exhibited removal of initial transient TiO2 nodules and partial etching of the underlying Al2O3 scale by volatile hydroxides formed in high temperature, high velocity water vapor. Aerodynamic forces produced some bending of the cantilevered sample via creep. The test indicated exceptional stability of YSZ coatings on Ti2AlC under turbine conditions, with thermal expansion matching playing a key role. The purpose of this study was to demonstrate long term durability of YSZ/MAX phase system in aggressive high temperature burner rig testing. MAX phases have been keenly studied because of their unique crystal structure and intriguing properties (Refs. 1 and 2). Having Mn+1(Al,Si)(C,N)n general composition, they are defined as ceramics, but possess unusual desirable attributes such as high conductivity, thermal shock resistance, easy machinability, and deformation tolerance. The mechanical properties derive from weak M-(Al,Si) bonding in the basal plane that leads to sliding and kinking in preference to catastrophic crack growth. Like most ceramics they are phase stable at high temperatures, generally up to 1500 °C. High temperature oxidation resistance is excellent for alumina-forming Ti3AlC2, Ti2AlC, and Cr2AlC, as reviewed by Tallman, et al. (Ref. 3). Compatibility with α-Al2O3 scales is further enhanced in cyclic exposures by a close matching of thermal expansion coefficients, (Ref. 4) i.e., (~9.3, 10.2, 11.3×10–6/K for Al2O3, Ti2AlC, and YSZ, to be discussed). Turbine environments generally contain 10 percent water vapor in the combustion gases, therefore moisture effects can be a concern for some materials (Ref. 5). Furnace tests of MAX phases in high temperature steam generally showed little effect on Al2O3 scale growth (Ref. 6). However, high velocity and high pressure gas can influence scale losses by the formation of volatile reaction products, such as TiO(OH)2 and Al(OH)3 (Refs. 7 to 10). This phenomenon had been discussed for 1100 to 1300 °C high pressure burner rig tests of Ti2AlC (Ref. 11). A single cubic growth rate parameter kcubic was measurably lower than comparable furnace TGA data, but it could be matched reasonably well if corrected for a slight volatility term. In general, a two-parameter cubic-linear growth-volatility law was believed to apply. Corresponding scale volatility loss rates, directly measured at 1300 °C on a pre-oxidized sample, were moderate (0.012 mg/cm2/h) and largely attributed to removal of the initial TiO2 transient scale. A related CH4 burner study of high purity Cr2AlC MAX phase demonstrated 1200 °C durability after 500 rapid (5 min. heat and 2 min. cool) thermal shock cycling (29 h hot time) (Ref. 12). Heating and cooling rates were ~1000 and 500 °C per minute, with a gas velocity of 5 m/s, producing a 75 °C/mm gradient. A 7 μm Al2O3 surface scale and a 13 μm Cr7C3 depletion zone formed with no signs of failure. No evidence of scale volatility was evident, although weight change was not provided, the velocity was moderate, and the total hot time was not extensive. The same high gradient BRT was used to produce 1400 °C surface temperatures for a YSZ/Cr2AlC/IN738 system in the first study of MAX phases used as bond coats for thermal barrier coatings (TBC) (Ref. 25). Here TBC failure was reported after 745 cycles, with only a 1.5 μm Al2O3 scale entrained within a porous, Cr7C3 bondcoat depletion phase. YSZ thermal barrier coatings have been considered to be a compatible complement to Al-MAX phases because of thermal expansion matching and extremely low volatility in water vapor. Initial studies showed superior oxidative stability up to 1300 °C, for long times (at least 500 h) for Ti2AlC substrates and less (268 h) for Cr2AlC, while withstanding large alumina TGO scale thickness (~35 to 40 μm) (Refs. 13 and 14). By comparison, typical superalloy systems can only survive 1150 °C maximum interface temperatures for extended periods, with a maximum sustained TGO below 10 μm (Ref. 15). High temperature SiC based systems are known to form slow-growing SiO2 scales. But these are subject to rate enhancement and volatile Si(OH)4 products in the presence of water vapor, as described comprehensively by Opila, et al. (Refs. 5, 16 to 19). Net weight losses are generally observed in high velocity, high pressure burner rig studies (e.g., 0.084 mg/cm2/h at 1300 °C) (Ref. 20). Furthermore, the loss rates have been shown from chemical physics to scale with v1/2 and pH2O 2 (Ref. 16). Low activity, moisture-resistant environmental barrier coatings (EBC), such as rare earth silicates, are needed to prevent substrate recession under turbine conditions (Refs. 21 to 23).

Smialek, James L.↗

Fatigue Life of a NiCr-Coated Powder Metallurgy Disk Superalloy After Varied Processing and Exposures

A protective ductile NiCr coating has shown promise to mitigate oxidation and corrosion attack on superalloy disk alloys. The effects of this coating on fatigue life and failure modes of the disk superalloy are an important concern. The objective of this study was to investigate the fatigue life and failure modes of disk superalloy specimens protected by this coating, using varied pre-coating and post-coating processes. Cylindrical gage fatigue specimens of a powder metallurgy-processed disk superalloy were grit blast or wet blast before being coated with a ductile NiCrY coating, then shot peened at low or medium levels after coating. All were then heat treated, some exposed, and finally all were subjected to fatigue at high temperature. The effects of varied pre-coating treatment, post-coating shot peening, and oxidation plus hot corrosion exposures on fatigue life with the coating were compared.

coating↗

The Effectiveness of a NiCrY-Coating on a Powder Metallurgy Disk Superalloy

Protective ductile coatings could be necessary to mitigate oxidation and corrosion attack on superalloy disks in some turbine engine applications. However, the effects of coatings on fatigue life of the disk during service are an important concern. The objective of this study was to investigate how such a coating could perform after varied post-coating processing. Cylindrical gage fatigue specimens of powder metallurgy-processed disk superalloy LSHR were coated with a NiCrY coating, shot peened, preparation treated, exposed, and then subjected to fatigue at high temperature. The effects of varied shot peening, preparation treatment, and exposures on fatigue life with and without the coating were compared. Each of these variables and several of their interactions significantly influenced fatigue life.

ductile coatings↗

Residual Stresses in a NiCrY-Coated Powder Metallurgy Disk Superalloy

Protective ductile coatings will be necessary to mitigate oxidation and corrosion attack on superalloy disks exposed to increasing operating temperatures in some turbine engine environments. However, such coatings must be resistant to harmful surface cracking during service. The objective of this study was to investigate how residual stresses evolve in such coatings. Cylindrical gage fatigue specimens of powder metallurgy-processed disk superalloy LSHR were coated with a NiCrY coating, shot peened, and then subjected to fatigue in air at room and high temperatures. The effects of shot peening and fatigue cycling on average residual stresses and other aspects of the coating were assessed. Shot peening did induce beneficial compressive residual stresses in the coating and substrate. However, these stresses became more tensile in the coating with subsequent heating and contributed to cracking of the coating in long intervals of cycling at 760 C. Substantial compressive residual stresses remained in the substrate adjacent to the coating, sufficient to suppress fatigue cracking. The coating continued to protect the substrate from hot corrosion pitting, even after fatigue cracks initiated in the coating.

superalloy↗

Influence of Aerogel Morphology and Reinforcement Architecture on Gas Convection in Aerogel Composites

A variety of thermal protection applications require lightweight insulation capable of withstanding temperatures well above 900 C. Aerogels offer extremely low-density thermal insulation due to their mesoporous structure, which inhibits both gas convection and solid conduction. Silica aerogel systems are limited to use temperatures of 600-700 C, above which they sinter. Alumina aerogels maintain a porous structure to higher temperatures than silica, before transforming to -alumina and densifying. We have synthesized aluminosilicate aerogels capable of maintaining higher surface areas at temperatures above 1100 C than an all-alumina aerogel using -Boehmite as the aluminum source and tetraethoxysilane (TEOS) as the silicon source. The pore structure of these aerogels varies with thermal exposure temperature and time, as the aluminosilicate undergoes a variety of phase changes to form transition aluminas. Transformation to -alumina is inhibited by incorporation of silica into the alumina lattice. The aerogels are fragile, but can be reinforced using a large variety of ceramic papers, felts or fabrics. The objective of the current study is to characterize the influence of choice of reinforcement and architecture on gas permeability of the aerogel composites in both the as fabricated condition and following thermal exposure, as well as understand the effects of incorporating hydrophobic treatments in the composites.

aerogels↗

Cyclic Oxidation and Hot Corrosion of NiCrY-Coated Disk Superalloys

Powder metallurgy disk superalloys have been designed for higher engine operating temperatures through improvement of their strength and creep resistance. Yet, increasing disk application temperatures to 704 degrees Centigrade and higher could enhance oxidation and activate hot corrosion in harmful environments. Protective coatings could be necessary to mitigate such attack. Cylindrical coated specimens of disk superalloys LSHR and ME3 were subjected to thermal cycling to produce cyclic oxidation in air at a maximum temperature of 760 degrees Centigrade. The effects of substrate roughness and coating thickness on coating integrity after cyclic oxidation were considered. Selected coated samples that had cyclic oxidation were then subjected to accelerated hot corrosion tests. This cyclic oxidation did not impair the coating's resistance to subsequent hot corrosion pitting attack.

protective coating↗

Exfoliation of Hexagonal Boron Nitride via Ferric Chloride Intercalation

Sodium fluoride (NaF) was used as an activation agent to successfully intercalate ferric chloride (FeCl3) into hexagonal boron nitride (hBN). This reaction caused the hBN mass to increase by approx.100 percent, the lattice parameter c to decrease from 6.6585 to between 6.6565 and 6.6569 Ǻ, the x-ray diffraction (XRD) (002) peak to widen from 0.01deg to 0.05deg of the full width half maximum value, the Fourier transform infrared (FTIR) spectrum's broad band (1277/cm peak) to change shape, and new FTIR bands to emerge at 3700 to 2700 and 1600/cm. This indicates hBN's structural and chemical properties are significantly changed. The intercalated product was hygroscopic and interacted with moisture in the air to cause further structural and chemical changes (from XRD and FTIR). During a 24-h hold at room temperature in air with 100 percent relative humidity, the mass increased another 141 percent. The intercalated product, hydrated or not, can be heated to 750 C in air to cause exfoliation. Exfoliation becomes significant after two intercalation-air heating cycles, when 20-nm nanosheets are commonly found. Structural and chemical changes indicated by XRD and FTIR data were nearly reversed after the product was placed in hydrochloric acid (HCl), resulting in purified, exfoliated, thin hBN products.

Hung, Ching-cheh↗

Compositional Effects on Nickel-Base Superalloy Single Crystal Microstructures

Fourteen nickel-base superalloy single crystals containing 0 to 5 wt% chromium (Cr), 0 to 11 wt% cobalt (Co), 6 to 12 wt% molybdenum (Mo), 0 to 4 wt% rhenium (Re), and fixed amounts of aluminum (Al) and tantalum (Ta) were examined to determine the effect of bulk composition on basic microstructural parameters, including gamma' solvus, gamma' volume fraction, volume fraction of topologically close-packed (TCP) phases, phase chemistries, and gamma - gamma'. lattice mismatch. Regression models were developed to describe the influence of bulk alloy composition on the microstructural parameters and were compared to predictions by a commercially available software tool that used computational thermodynamics. Co produced the largest change in gamma' solvus over the wide compositional range used in this study, and Mo produced the largest effect on the gamma lattice parameter and the gamma - gamma' lattice mismatch over its compositional range, although Re had a very potent influence on all microstructural parameters investigated. Changing the Cr, Co, Mo, and Re contents in the bulk alloy had a significant impact on their concentrations in the gamma matrix and, to a smaller extent, in the gamma' phase. The gamma phase chemistries exhibited strong temperature dependencies that were influenced by the gamma and gamma' volume fractions. A computational thermodynamic modeling tool significantly underpredicted gamma' solvus temperatures and grossly overpredicted the amount of TCP phase at 982 C. Furthermore, the predictions by the software tool for the gamma - gamma' lattice mismatch were typically of the wrong sign and magnitude, but predictions could be improved if TCP formation was suspended within the software program. However, the statistical regression models provided excellent estimations of the microstructural parameters based on bulk alloy composition, thereby demonstrating their usefulness.

MacKay, Rebecca A.↗

Oxide Scales Formed on NiTi and NiPtTi Shape Memory Alloys

Ni-49Ti and Ni-30Pt-50Ti (at.%) shape memory alloys were oxidized isothermally in air over the temperature range of 500 to 900 C. The microstructure, composition, and phase content of the scales were studied by SEM, EDS, XRD, and metallography. Extensive plan view SEM/EDS identified various features of intact or spalled scale surfaces. The outer surface of the scale was a relatively pure TiO2 rutile structure, typified by a distinct highly striated and faceted crystal morphology. Crystal size increased significantly with temperature. Spalled regions exhibited some porosity and less distinct features. More detailed information was obtained by correlation of SEM/EDS studies of 700 C/100 hr cross-sections with XRD analyses of serial or taper-polishing of plan surfaces. Overall, multiple layers exhibited graded mixtures of NiO, TiO2, NiTiO3, Ni(Ti) or Pt(Ni,Ti) metal dispersoids, Ni3Ti or Pt3Ti depletion zones, and substrate, in that order. The NiTi alloy contained a 3 at.% Fe impurity that appeared in embedded localized Fe-Ti-rich oxides, while the NiPtTi alloy contained a 2 v/o dispersion of TiC that appeared in lower layers. The oxidation kinetics of both alloys (in a previous report) indicated parabolic growth and an activation energy (250 kJ/mole) near those reported in other Ti and NiTi studies. This is generally consistent with TiO2 existing as the primary scale constituent, as described here.

Smialek, James L.↗

Detecting Phase Boundaries in Hard-Sphere Suspensions

A special image-data-processing technique has been developed for use in experiments that involve observation, via optical microscopes equipped with electronic cameras, of moving boundaries between the colloidal-solid and colloidal-liquid phases of colloidal suspensions of monodisperse hard spheres. During an experiment, it is necessary to adjust the position of a microscope to keep the phase boundary within view. A boundary typically moves at a speed of the order of microns per hour. Because an experiment can last days or even weeks, it is impractical to require human intervention to keep the phase boundary in view. The present image-data-processing technique yields results within a computation time short enough to enable generation of automated-microscope-positioning commands to track the moving phase boundary

McDowell, Mark↗

An Automatic Phase-Change Detection Technique for Colloidal Hard Sphere Suspensions

Colloidal suspensions of monodisperse spheres are used as physical models of thermodynamic phase transitions and as precursors to photonic band gap materials. However, current image analysis techniques are not able to distinguish between densely packed phases within conventional microscope images, which are mainly characterized by degrees of randomness or order with similar grayscale value properties. Current techniques for identifying the phase boundaries involve manually identifying the phase transitions, which is very tedious and time consuming. We have developed an intelligent machine vision technique that automatically identifies colloidal phase boundaries. The algorithm utilizes intelligent image processing techniques that accurately identify and track phase changes vertically or horizontally for a sequence of colloidal hard sphere suspension images. This technique is readily adaptable to any imaging application where regions of interest are distinguished from the background by differing patterns of motion over time.

McDowell, Mark↗

Microgravity Experiments Being Developed for Microscopic Study of Colloidal Spheres

Microscopic spheres suspended in liquid become highly ordered under the proper conditions. Such collections of particles, called colloidal suspensions or colloids, are the subject of a series of ongoing microgravity experiments at the NASA Lewis Research Center. By studying the way these colloidal suspensions order themselves, scientists can better understand how atoms of a liquid become ordered to form a solid. In addition, highly ordered colloids have special properties that may make them useful in future hightech applications. Work is underway at Lewis to develop an optical microscope to view these colloidal suspensions sphere by sphere in microgravity.

Rogers, Richard B.↗

A preview of a modular surface light scattering instrument with autotracking optics

NASA's Advanced Technology Development (ATD) program is sponsoring the development of a new generation of surface light scattering hardware. This instrument is designed to non-invasively measure the surface response function of liquids over a wide range of operating conditions while automatically compensating for a sloshing surface. The surface response function can be used to compute surface tension, properties of monolayers present, viscosity, surface tension gradient and surface temperature. The instrument uses optical and electronic building blocks developed for the laser light scattering program at NASA Lewis along with several unique surface light scattering components. The emphasis of this paper is the compensation for bulk surface motion (slosh). Some data processing background information is also included.

Meyer, William V.↗

Laser Light Scattering, from an Advanced Technology Development Program to Experiments in a Reduced Gravity Environment

Recent advancements in laser light scattering hardware are described. These include intelligent single card correlators; active quench/active reset avalanche photodiodes; laser diodes; and fiber optics which were used by or developed for a NASA advanced technology development program. A space shuttle experiment which will employ aspects of these hardware developments is previewed.

Meyer, William V.↗