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NASA NTRS1984

Performance of thermal barrier coatings in high heat flux environments

Thermal barrier coatings were exposed to the high temperature and high heat flux produced by a 30 kW plasma torch. Analysis of the specimen heating rates indicates that the temperature drop across the thickness of the 0.038 cm ceramic layer was about 1100 C after 0.5 sec in the flame. An as-sprayed ZrO2-8 percent Y2O3 specimens survived 3000 of the 0.5 sec cycles with falling. Surface spalling was observed when 2.5 sec cycles were employed but this was attributed to uneven heating caused by surface roughness. This surface spalling was prevented by smoothing the surface with silicon carbide paper or by laser glazing. A coated specimen with no surface modification but which was heat treated in argon also did not surface spall. Heat treatment in air led to spalling in as early as 1 cycle from heating stresses. Failures at edges were investigated and shown to be a minor source of concern. Ceramic coatings formed from ZrO2-12 percent Y2O3 or ZrO2-2O percent Y2O3 were shown to be unsuited for use under the high heat flux conditions of this study.

Miller, R. A.↗

NASA NTRS1990

Thermal response of various thermal barrier coatings in a high heat flux rocket engine

Traditional APS ZrO2-Y2O3 thermal barrier coatings (TBCs) formed by air plasma spraying and low pressure and air plasma sprayed ZrO2-Y2O3/NiCrAlY cermet coatings were tested in an H2-O2 rocket engine. The test cycle was approximately 1.2 s at 1400 C in a hydrogen-rich environment. During testing, the maximum metal temperature without a coating was 1310 C. The traditional ZrO2-Y2O3 TBCs with a 100-125 micron thick ceramic layer reduced the maximum metal temperature by approximately 350 C. Increasing the ceramic layer thickness to 200-225 microns resulted in an additional metal temperature reduction of 100 C. However, the cermet coatings, consisting of a ceramic and metal mixture, exhibited a much lower thermal protection capability by reducing the maximum metal temperature by approximately 100 C. It was also found that the surface roughness of the traditional TBCs had little effect on the thermal response.

Nesbitt, J. A.↗

NASA NTRS1998

Thermal Modelling of Various Thermal Barrier Coatings in a High Flux Rocket Engine

A thermal model was developed to predict the thermal response of coated and uncoated tubes tested in a H2/O2 rocket engine. Temperatures were predicted for traditional APS ZrO2-Y2O3 thermal barrier coatings, as well as APS and LPPS ZrO2-Y2O3/NiCrAlY cermet coatings. Good agreement was observed between predicted and measured metal temperatures at locations near the tube surface or at the inner tube wall. The thermal model was also used to quantitatively examine the effect of various coating system parameters on the temperatures in the substrate and coating. Accordingly, the effect of the presence a metallic bond coat and the effect of radiation from the surface of the ceramic layer were examined. In addition, the effect of a variation in the values of the thermal conductivity of the ceramic layer was also investigated. It was shown that a variation in the thermal conductivity of the ceramic layer, on the order of that reported in the literature for plasma sprayed ZrO2-Y2O3 coatings, can result in temperature differences in the substrate greater than 100 C, a much greater effect than that due to the presence of a bond coat or radiation from the ceramic layer. The thermal model was also used to predict the thermal response of a coated rod in order to quantify the difference in the metal temperatures between the two substrate geometries in order to explain the previously-observed increased life of coatings on rods over that on tubes. It was shown that for the short duration testing in the rocket engine, the temperature in a tube could exceed that in a rod by more than 100 C. Lastly, a two-dimensional model was developed to evaluate the effect of tangential heat transfer around the tube and its impact on reducing the stagnation point temperature. It was also shown that tangential heat transfer does not significantly reduce the stagnation point temperature, thus allowing application of a simpler, one-dimensional model for comparing measured and predicted stagnation point temperatures.

Nesbitt, James A.↗

NASA NTRS2003

Creep Resistance of ZrO2 Ceramic Improved by the Addition of a Small Amount of Er2O3

Zirconia (ZrO2) has great technological importance in structural, electrical, and chemical applications. It is the crucial component for state-of-the art thermal barrier coatings and an enabling component as a solid electrolyte for solid-oxide fuel cell systems. Pure ZrO2 is of limited use for industrial applications because of the phase transformations that occur. Upon the addition of stabilizers, cubic (c-ZrO2) and tetragonal (t-ZrO2) forms can be preserved. It is the stabilized and partially stabilized forms of zirconia that function as thermal barrier coatings, solid electrolytes, and oxygen sensors and that have numerous applications in the electrochemical industry. The cubic form of ZrO2 is typically stabilized through Y2O3 additions. However, Y2O3-stabilized zirconia is susceptible to deformation at high temperatures (greater than 900 C) because of the large number of slip systems and the high oxygen diffusion rates, which result in high creep rates at high temperatures. Successful use of ZrO2 at high temperatures requires that new dopant additives be found that will retain or enhance the desirable properties of cubic ZrO2 and yet produce a material with lower creep rates. At the NASA Glenn Research Center, erbium oxide (Er2O3) was identified as a promising dopant for improving the creep resistance of. ZrO2. The selection of Er2O3 was based on the strong interactions of point defects and dislocations. Single crystals of 5 mol% Er2O3- doped ZrO2 rods (4 mm in diameter) and monofilaments (200 to 300 mm in diameter and 30 cm long) were grown using the laser-heated float zone technique, and their creep behavior was measured as a function of temperature. The addition of 5 mol% Er2O3 to single-crystal ZrO2 improved its creep resistance at high temperatures by 2 to 3 orders of magnitude over state-of-the-art Y2O3-doped crystals. Detailed microstructural characterization of ZrO2-Er2O3 single crystals has identified new mechanisms for improving the creep resistance of this class of materials. Adding Er2O3 to ZrO2 results in microstructure of stable and metastable tetragonal precipitates that with thermal treatment evolve to a tweed structure of nanosize tetragonal lamellae. The superior high-temperature creep resistance of Er2O3-doped ZrO2 is attributed to nanoscale precipitation hardening. Doping with Er2O3 will significantly increase the upper-use temperature limit of ZrO2. Potential applications include using Er2O3-doped ZrO2 as a high-temperature fiber for structural applications and adding Er2O3 to reduce the sintering rates of ZrO2 thermal barrier coatings. This work was conducted at Dpto. de F sica de la Materia Condensada, Universidad de Sevilla, Spain, and at NASA Glenn.

Martinez-Fernandez, Julian↗

NASA NTRS2022

Cryogenic Thermal Coatings Final Report

The goals of this project were to produce yttrium oxide- (Y2O3) based tiles and a spray-on coating with minimal solar absorption, to perform exposure testing on these coatings (both rigid and sprayon), and to work towards a manufacturing process whereby these coatings could be made available to the space community. The Key Performance Parameters (threshold values) were to achieve 1% solar absorption for the tiles as measured in a deep space simulator, and 6% solar absorption for the spray-on coating as measured using a reflectance spectrometer. The values achieved were 1.2% (GRC Deep space simulator) and 4% (KSC spectrometer using Spectralon as a reference) for the tiles and spray-on coating, respectively. Exposure testing consisted of measuring tile and spray-on coating degradation due to atomic oxygen, ultraviolet radiation, and electrostatic fields. Atomic oxygen caused some degradation, while ultraviolet exposure caused a significant increase in absorption. However, in-space samples exposed to solar ultraviolet did not show this significant increase. This discrepancy is addressed in this report. As a result of this work, Y2O3 tiles have been manufactured in the Kennedy Space Center (KSC) Applied Chemistry Laboratory (ACL), and the process has been transferred to the Thermal Protection System Facility (TPSF) at KSC. The TPSF manufactures coatings for the space community and is an ideal route by which future users could access Y2O3-based coatings. The spray-on coating has been developed such that it can be applied to a wide range of substrates, substantially lowering absorbed solar power as compared to currently available coatings.

Thermal Control Coatings↗

NASA NTRS1975

Optimization of an oxide dispersion strengthened Ni-Cr-Al alloy for gas turbine engine vanes

The investigation was carried out to determine the optimum alloy within the Ni-16Cr-Al-Y2O3 system for use as a vane material in advanced aircraft gas turbine engines. Six alloys containing nominally 4%, 5% and 6% Al with Y2O3 levels of 0.8% and 1.2% were prepared by mechanical attrition. Six small-scale, rectangular extrusions were produced from each powder lot for property evaluation. The approximate temperatures for incipient melting were found to be 1658 K (2525 F), 1644 K (2500 F) and 1630 K (2475 F) for the 4%, 5% and 6% aluminum levels, respectively. With the exception of longitudinal crystallographic texture, the eight extrusions selected for extensive evaluation either exceeded or were close to mechanical property goals. Major differences between the alloys became apparent during dynamic oxidation testing, and in particular during the 1366 K (2000 F)/500 hour Mach 1 tests carried out by NASA-Lewis. An aluminum level of 4.75% was subsequently judged to be optimum based on considerations of dynamic oxidation resistance, susceptibility to thermal fatigue cracking and melting point.

Klarstrom, D. L.↗

NASA NTRS1977

Application of diffusion barriers to high modulus fibers

Barrier layers were coated onto high-modulus fibers, and nickel and titanium layers were overcoated as simulated matrix materials. The objective was to coat the high-strength fibers with unreactive selected materials without degrading the fibers. The fibers were tungsten, niobium, and single-crystal sapphire, while the materials used as barrier coating layers were Al2O3, Y2O3, TiC, ZrC, WC with 14% Co, and HfO2. An ion-plating technique was used to coat the fibers. The fibers were subjected to high-temperature heat treatments to evaluate the effectiveness of the barrier layer in preventing fiber-metal interactions. Results indicate that Al2O3, Y2O3, and HfO2 can be used as barrier layers to minimize the nickel-tungsten interaction. Further investigation, including thermal cycling tests at 1090 C, revealed that HfO2 is probably the best of the three.

Veltri, R. D.↗

NASA NTRS1978

Pressureless sintered Sialons with low amounts of sintering aid

Two Beta prime - Sialons of composition Si2.6Al0.393y0.007O0.4N3.6 and Si2.6Al0.384Y0.014O0.4N3.6 were pressureless sintered from mixtures of Y2O3 and separately milled Beta -Si3N4, AlN, and SiO2. These Sialons had densities of over 98% of theoretical, four-point bend strengths of 460 and 155 MPa at room temperature and 1400 C, respectively, and 1400 C oxidation rates lower than those reported for hot pressed Si3N4 and for a stronger Sialon with 2.5 weight percentage Y2O3.

Arias, A.↗

NASA NTRS1977

Pressureless sintered beta prime-Si3N4 solid solution: Fabrication, microstructure, and strength

Si3N4, AlN, and Al2O3 were used as basic constituents in a study of the pressureless sintering of beta prime-Si3N4 solid solution as a function of temperature. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 MPa were achieved at moderate temperature (1000 C), but decreased to 228 MPa at 1380 C. This substantial strength loss was attributed to a glassy grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

NASA NTRS1977

Improved performance of silicon nitride-based high temperature ceramics

Results are presented regarding experiments intended for improving the strength and toughness of hot-pressed Si3N4 (HPSN), improving the strength and oxidation resistance of reaction-sintered Si3N4 (RSSN), and improving the strength and oxidation resistance of sinterable Si-Al-O-N compositions. It is shown that the use of ZrO2 instead of MgO as a sintering aid improved the room-temperature and high-temperature flexural strength of HPSN, in addition to enhancing the rupture strength and Charpy impact resistance. The use of crushable energy absorbing layers increased the impact resistance of HPSN. Impregnation of RSSN with solutions that oxidize to Al2O3 or ZrO2 resulted in increased bending strength at room temperature. Beta-prime Si-Al-O-N sintered to full density by means of the sintering aids CeO2, Y2O3, and ZrO2 yielded the greatest strength with Y2O3 and the greatest oxidation resistance with ZrO2.

Ashbrook, R. L.↗

NASA NTRS1977

Pressureless sintered beta-prime-Si3N4 solid solution - Fabrication, microstructure, and strength

Pressureless sintering of beta-prime-Si3N4 solid solution was studied as a function of temperature using Si3N4, A1N, and Al2O3 as basic constituents. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta-prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 M Pa were achieved at moderate temperature (1000 C), but decreased to 228 M Pa at 1380 C. This substantial strength loss was attributed to a 'glassy' grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

NASA NTRS1980

Effect of W and WC on the oxidation resistance of yttria-doped silicon nitride

The effect of W and WC contamination on the oxidation and cracking in air of sintered Si3N4 - 8 w/o Y2O3 ceramics at 500, 750, and 1350 C is examined. A mixture of Si3N4 - 8Y2O3, milled with alumina balls, was divided into four portions. Three portions were doped with 2 w/o WC W, and 4 w/o W respectively, in order to simulate contamination during milling. The fourth portion was undoped and used on a control. The addition of W or WC did not affect the phase relationships in the system, as all bars with or without additions contained melilite as the major Si-Y-O-N phase after sintering. At 750 C, instability (rapid oxidation and cracking) of W-doped bars appears to have occurred as a result of oxidation of the tungsten containing melilite phase. No intermediate temperature instability was observed in bars containing 2 w/o WC or in bars with no additive. Specimens exposed at 1350 C had good oxidation resistance due to the formation of a protective siliceous oxide layer. A specimen containing 4 w/o W which was preoxidized at 1350 C had improved oxidation resistance at 750 C. The tendency towards oxidation and cracking of Si3N4 - 8 Y2O3 at 750 C is concluded to be related to tungsten content of the sintered bars.

Schuon, S.↗

NASA NTRS1980

Performance of two-layer thermal barrier systems on directionally solidified Ni-Al-Mo and comparative effects of alloy thermal expansion on system life

A promising two-layer thermal barrier coating system (TBS), Ni-16.4Cr-5.1A1-0.15Y/ZrO2-6.1Y2O3 (all in weight percent), was identified for directionally solidified Ni-Al-Mo (gamma/gamma' alpha). In cyclic furnace tests at 1095 C this system on gamma/gamma' alpha was better than Ni-16. 4Cr-5.1Al-0.15Y/ZrO2-7.8Y2O3 by about 50 percent. In natural gas - oxygen torch rig tests at 1250 C the ZrO2-6.1Y2O3 coating was better than the ZrO2-7.8Y2O3 coating by 95 percent, on MAR-M509 substrates and by 60 percent on gamma/gamma' alpha substrates. Decreasing the coefficient of thermal expansion of the substrate material from 17-18x10 to the -6 power/C (MAR-M200 + Hf and MAR-M509) to 11x10 to the -6 power/C (gamma/gamma' alpha) also resulted in improved TBS life. For example, in natural gas - oxygen torch rig tests at 1250 C, the life of Ni-16.4Cr-5.1Al-0.15Y/ZrO26.1Y2O3 was about 30 percent better on gamma/gamma' alpha than on MAR-M509 substrates. Thus compositional changes in the bond and thermal barrier coatings were shown to have a greater effect on TBS life than does the coefficient of thermal expansion.

Stecura, S.↗

NASA NTRS1981

Creep and residual mechanical properties of cast superalloys and oxide dispersion strengthened alloys

Tensile, stress-rupture, creep, and residual tensile properties after creep testing were determined for two typical cast superalloys and four advanced oxide dispersion strengthened (ODS) alloys. The superalloys examined included the nickel-base alloy B-1900 and the cobalt-base alloy MAR-M509. The nickel-base ODS MA-757 (Ni-16CR-4Al-0.6Y2O3 and the iron-base ODS alloy MA-956 (Fe-20Cr-5Al-0.8Y2O3) were extensively studied, while limited testing was conducted on the ODS nickel-base alloys STCA (Ni-16Cr-4.5Al-2Y2O3) with a without Ta and YD-NiCrAl (Ni-16Cr-5Al-2Y2O3). Elevated temperature testing was conducted from 114 to 1477 K except for STCA and YD-NiCrAl alloys, which were only tested at 1366 K. The residual tensile properties of B-1900 and MAR-M509 are not reduced by prior creep testing (strains at least up to 1 percent), while the room temperature tensile properties of ODS nickel-base alloys can be reduced by small amounts of prior creep strain (less than 0.5 percent). The iron-base ODS alloy MA-956 does not appear to be susceptible to creep degradation at least up to strains of about 0.25 percent. However, MA-956 exhibits unusual creep behavior which apparently involves crack nucleation and growth.

Whittenberger, J. D.↗

NASA NTRS1981

Microstructure and mechanical properties of bulk yttria-partially-stabilized zirconia

A commercially available bulk 4.5 mole percent yttria-(Y2O3) partially stabilized zirconia (PSZ) was studied by light microscopy, X-ray analysis, microhardness measurement, and fracture toughness testing. The growth of the precipitates and the phase transformations were studied as a function of aging in air at 1500 C. Aging curves were constructed for both the as received and the solution annealed and quenched materials; the curves showed hardness peaks at 1397 and 1517 Kg/sq mm respectively. The rectangular plate shaped tetragonal precipitates were found to have a 110 habit plane. A total of twelve different types of tetragonal precipitates were found. Grinding of the Y2O3 PSZ into powder did not cause a significant amount of metastable tetragonal precipitates to transform into the monoclinc phase, thus indicating that transformation toughening is not a significant mechanism for the material.

Valentine, P. G.↗

NASA NTRS1981

Microstructure and mechanical properties of bulk yttria-partially-stabilized zirconia

A commercially available bulk 4.5 mole percent yttria-Y2O3)-partially-stabilized zirconia (PSZ) was studied by light microscopy, X-ray analysis, microhardness measurement, and fracture toughness testing. The growth of the precipitates and the phase transformations were studied as a function of aging in air at 1500 C. Aging cuves were constructed for both the as-received and the solution-annealed-and-quenched materials; the curves showed hardness peaks at 1397 and 1517 kg/sq mm, respectively. A total of twelve different types of tetragonal precipitates were found. The rectangular plate-shaped tetragonal precipitates were found to have a (110) habit plane. Grinding of the Y2O3 PSZ into powder did not cause a significant amount of metastable tetragonal precipitates to transform into the monoclinic phase, thus indicating that transformation toughening is not a significant mechanism for the material. The fracture toughness of the aged and of the unaged solution-annealed-and-quenched PSZ was found to be between 2 and 3 MN/cu m/2.

Valentine, P. G.↗

NASA NTRS1980

Sintered reaction bonded Si3N4 for the AGT 101 turbine rotor

The sintered reaction reaction bonded Si3N4 (SRBSN) process, with Y2O3 as a sintering aid, was selected for the fabrication of the AGT 101 turbine rotor. Experiments to determine the optimum Y2O3 composition of this system are discussed. The room temperature strength of the optimum material (RM-1) exceeds 700 MPa while the 1200 C strength exceeds 550 MPa. The slip casting fabrication technique employed for the AGT 101 simulated rotor is described. Rotors have been cast, nitrided and sintered. Densities exceeding 97% of theoretical (3.26 g/cc) have been obtained. Problems relating to sintering reproducibility, and the overall quality of the simulated rotors have been identified.

Mangels, J. A.↗

NASA NTRS1983

Improved performance thermal barrier coatings

Thermal barrier coatings offer an attractive approach to improving the durability and efficiency of the hot section of heat engines. The coatings typically consist of an inner alloy bond coating about 0.01 cm thick resistant to oxidation and hot corrosion and an outer ceramic layer, usually a stabilized zirconia, 0.01-0.05 cm thick. Here, the materials, thermomechanical stress, and hot corrosion problems associated with thermal barrier coatings are reviewed along with the capabilities and limitations of current technology. The coatings discussed include ZrO2-Y2O3/NiCrAlY, ZrO2-Y2O3/NiCoCrAlY, ZrO2-MgO/NiCoCrAlY, CaO-SiO2/Co-Cr-Al-Y, and CaO-SiO2/NiCrAlY systems. It is emphasized that the performance of thermal barrier coatings is governed by many complex and interrelated factors, so that optimization of these coatings always involves certain tradeoffs.

Levine, S. R.↗