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All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Windows(Registered Trademark)-Based Software Models Cyclic Oxidation Behavior

Oxidation of high-temperature aerospace materials is a universal issue for combustion-path components in turbine or rocket engines. In addition to the question of the consumption of material due to growth of protective scale at use temperatures, there is also the question of cyclic effects and spallation of scale on cooldown. The spallation results in the removal of part of the protective oxide in a discontinuous step and thereby opens the way for more rapid oxidation upon reheating. In experiments, cyclic oxidation behavior is most commonly characterized by measuring changes in weight during extended time intervals that include hundreds or thousands of heating and cooling cycles. Weight gains occurring during isothermal scale-growth processes have been well characterized as being parabolic or nearly parabolic functions of time because diffusion controls reaction rates. In contrast, the net weight change in cyclic oxidation is the sum of the effects of the growth and spallation of scale. Typically, the net weight gain in cyclic oxidation is determined only empirically (that is, by measurement), with no unique or straightforward mathematical connection to either the rate of growth or the amount of metal consumed. Thus, there is a need for mathematical modeling to infer spallation mechanisms. COSP is a computer program that models the growth and spallation processes of cyclic oxidation on the basis of a few elementary assumptions that were discussed in COSP: A Computer Model of Cyclic Oxidation, Oxidation of Metals, vol. 36, numbers 1 and 2, 1991, pages 81-112. Inputs to the model include the selection of an oxidation-growth law and a spalling geometry, plus oxide-phase, growth-rate, cycle-duration, and spall-constant parameters. (The spalling fraction is often shown to be a constant factor times the existing amount of scale.) The output of COSP includes the net change in weight, the amounts of retained and spalled oxide, the total amounts of oxygen and metal consumed, and the terminal rates of weight loss and metal consumption.

Smialek, J. L.↗
NASA NTRS1992

Nonequilibrium synthesis of NbAl3 and Nb-Al-V alloys by laser cladding. II - Oxidation behavior

Isothermal oxidation behaviors of NbAl3 alloy synthesized by laser cladding were investigated at temperatures between 800 and 1400 C, and the effect of vanadium microalloying on the oxidation of the laser-clad alloy was examined. The oxidation kinetics of the two alloys were monitored using thermal gravimetric weight gain data, and the bulk and surface chemistries were analyzed using XRD and XPS, respectively. It was found that NbAl3 did not form an exclusive layer of protective Al2O3. The oxidation products at 800 C were found to be a mixture of Nb2O5 and Al2O3. At 1200 C, a mixture of NbAlO4, Nb2O5, and Al2O3 formed; and at 1400 C, a mixture of NbAlO4, Al2O3, NbO2, NbO(2.432), and Nb2O5 formed. The addition of V led to a dramatic increase of the oxidation rate, which may be related to the formation of (Nb, V)2O5 and VO2, which grows in preference to protective Al2O3.

Haasch, R. T.↗
NASA NTRS1976

COREST: A FORTRAN computer program to analyze paralinear oxidation behavior and its application to chromic oxide forming alloys

A FORTRAN computer program (COREST) was developed to analyze the high-temperature paralinear oxidation behavior of metals. It is based on a mass-balance approach and uses typical gravimetric input data. COREST was applied to predominantly Cr2O3-forming alloys tested isothermally for long times. These alloys behaved paralinearly above 1100 C as a result of simultaneous scale formation and scale vaporization. Output includes the pertinent formation and vaporization constants and kinetic values of interest. COREST also estimates specific sample weight and specific scale weight as a function of time. Most importantly, from a corrosion standpoint, it estimates specific metal loss.

Barrett, C. E.↗
NASA NTRS1985

Oxidation Behavior of Glassy Alloys

The oxidation behavior of high temperature glassy alloys produced by rapid solidification processing is investigated and the effects of processing and composition on oxidation behavior is studied. Glassy Ta-44.5at%Ir, Ta-40at%Ir-10at%B and Nb-45at%Ir oxidized rapidly at 700 to 800 C at an oxygen partial pressure of .001 atm. The alloys were embrittled during the oxidation process. No apparent oxidation or embrittlement of the Ta-Ir alloy occurred after oxidation for 4h at 500 C at an oxygen partial pressure of .001 atm. Embrittlement occurred, however, after 100h of exposure under the latter conditions. Alloy embrittlement is associated with the partial or full conversion of the metallic glass to a mixture of crystalline beta-Ta2O5 and metallic iridium. Hot compaction of glassy alloys of this type must be limited to relatively low temperatures (approx. 500 C) and short times at the low temperatures unless extremely low oxygen partial pressures can be achieved during the compaction process.

Yurek, G.↗
NASA NTRS1975

Dynamic oxidation behavior of TD-NiCr alloy with different surface pretreatments

Oxidation tests of TD-NiCr alloy with different surface pretreatments were conducted in a Mach-5 arc-jet at 1200 C and 0.002 lb/sec flowing air environment. The mechanisms responsible for the observed oxidation behavior are examined. The presence of atomic oxygen in the air stream plays a significant role in determining the oxidation characteristic of the alloy. The rate of Cr2O3 vaporization by formation of volatile CrO3 is greatly enhanced by the flowing conditions. The typical microstructure of oxides formed in the dynamic tests consists of an external layer of NiO with a porous mushroom-type morphology, an intermediate layer of NiO and Cr2O3 oxide mixture, and a continuous inner layer of Cr2O3 in contact with the Cr-depleted alloy substrate. Three basic processes underlying the formation of mushroom-type NiO are identified and discussed. The oxidation rate is determined by the rate of vaporization of NiO. Surface pretreatment has a significant effect on the oxidation behavior of the alloy in the early stage of oxidation, but becomes less important as exposure time increases. Mechanical polishing induces surface recrystallization, but promotes the concurrence of external growth of NiO and internal oxidation of the alloy in the dynamic atmosphere.

Young, C. T.↗
DOE OSTI2025

Influence of temperature, oxygen partial pressure, and microstructure on the high-temperature oxidation behavior of the SiC Layer of TRISO particles

Tristructural isotropic (TRISO)-coated fuel particles are designed for use in high-temperature gas-cooled nuclear reactors, featuring a structural SiC layer that may be exposed to oxygen-rich environments over 1000 °C. Surrogate TRISO particles were tested in 0.2–20 kPa O 2 atmospheres to observe the differences in oxidation behavior. Oxide growth mechanisms remained consistent from 1200–1600 °C for each P O$_2$ , with activation energies of 228 ± 7 kJ/mol for 20 kPa O 2 and 188 ± 8 kJ/mol for 0.2 kPa O 2 . At 1600 °C, kinetic analysis revealed a change in oxide growth mechanisms between 0.2 and 6 kPa O2. In 0.2 kPa O 2 , oxidation produced raised oxide nodules on pockets with nanocrystalline SiC. Oxidation mechanisms were determined using Atom probe tomography. Active SiC oxidation occurred in C-rich grain boundaries with low P O$_2$ , leading to SiO 2 buildup in porous nodules. Here, this phenomenon was not observed at any temperature in 20 kPa O 2 environments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1975

Effect of magnesium oxide content on oxidation behavior of some superalloy-base cermets

The effect of increasing magnesium oxide (MgO) content on the cyclic oxidation resistance of hot-pressed cermets of MgO in NiCrAlY, MgO in Hoskins-875, MgO in Inconel-702, and MgO in Hastelloy-X was investigated. The cermets with magnesium oxide levels of 5, 10, 20, and 40 vol percent were examined. The cyclic oxidation behavior of these cermets at 1100 and 1200 C in still air was determined by a thermogravimetric method supplemented by X-ray diffraction analysis and light and electron microscopy. In all instances, MgO prevented grain growth in the metallic phase. No evidence of oxidation along interphase boundaries was detected. Cermets of MgO in NiCrAlY and MgO in Hoskins-875 were superior to cermets of MgO in Inconel-702 and MgO in Hastelloy-X. Their oxidation resistance was degraded only when the MgO content was 40 vol percent. The oxidation behavior of MgO-in-Inconel-702 powder cermets containing 5- and 10-vol percent MgO was approximately similar to that of pure Inconel-702 compacts. The 20- and 40-vol percent MgO content reduced the oxidation resistance of MgO-in-Inconel-702 powder cermets relative to that of pure Inconel-702.

Zaplatynsky, I.↗
NASA NTRS1974

Oxidation behavior of TD-NiCr in a dynamic high temperature environment

The oxidation behavior of TD-NiCr has been studied in static and high-speed flowing air environments at 1100 and 1200 C. It has been found that the stable oxide morphologies formed on the specimens exposed to the static and dynamic environments were markedly different. The faceted crystal morphology characteristic of static oxidation was found to be unstable under high-temperature, high-speed flow conditions and was quickly replaced by a porous NiO 'mushroom' type structure. Also, it was found that the rate of formation of CrO3 from Cr2O3 was greatly enhanced by high gas velocity conditions. The stability of Cr2-O3 was found to be greatly improved by the presence of an outer NiO layer, even though the NiO layer was very porous. An oxidation model is proposed to explain the observed microstructures and overall oxidation behavior of TD-NiCr alloys.

Tenney, D. R.↗
NASA NTRS1999

10 000-hr Cyclic Oxidation Behavior of 68 High-Temperature Co-, Fe-, and Ni- Base Alloys Evaluated at 982 deg. C (1800 deg. F)

Power systems with operating temperatures in the range of 815 to 982 C (1500 to 1800 F) frequently require alloys that can operate for long times at these temperatures. A critical requirement is that these alloys have adequate oxidation resistance. The alloys used in these power systems require thousands of hours of operating life with intermittent shutdown to room temperature. Intermittent power plant shutdowns, however, offer the possibility that the protective scale will tend to spall (i.e., crack and flake off) upon cooling, increasing the rate of oxidative attack in subsequent heating cycles. Thus, it is critical that candidate alloys be evaluated for cyclic oxidation behavior. It was determined that exposing test alloys to ten 1000-hr cycles in static air at 982 10 000-hr Cyclic Oxidation Behavior of 68 High-Temperature Co-, Fe-, and Ni-Base Alloys Evaluated at 982 C (1800 F) could give a reasonable simulation of long-time power plant operation. Iron- (Fe-), nickel- (Ni-), and cobalt- (Co-) based high-temperature alloys with sufficient chromium (Cr) and/or aluminum (Al) content can exhibit excellent oxidation resistance. The protective oxides formed by these classes of alloys are typically Cr2O3 and/or Al2O3, and are usually influenced by their Cr, or Cr and Al, content. Sixty-eight Co-, Fe-, and Ni-base high-temperature alloys, typical of those used at this temperature or higher, were used in this study. At the NASA Lewis Research Center, the alloys were tested and compared on the basis of their weight change as a function of time, x-ray diffraction of the protective scale composition, and the physical appearance of the exposed samples. Although final appearance and x-ray diffraction of the final scale products were two factors used to evaluate the oxidation resistance of each alloy, the main criterion was the oxidation kinetics inferred from the specific weight change versus time data. These data indicated a range of oxidation behavior including parabolic (typical of isothermal oxidation), paralinear, linear, and mixed-linear kinetics.

Barrett, Charles A.↗
NASA NTRS1974

Investigation of the oxidation behavior of dispersion stabilized alloys when exposed to a dynamic high temperature environment

The oxidation behavior of TD-NiCr and TD-NiCrAlY alloys have been studied at 2000 and 2200 F in static and high speed flowing air environments. The TD-NiCrAlY alloys preoxidized to produce an Al2O3 scale on the surface showed good oxidation resistance in both types of environments. The TD-NiCr alloy which had a Cr2O3 oxide scale after preoxidation was found to oxidize more than an order of magnitude faster under the dynamic test conditions than at comparable static test conditions. Although Cr2O3 normally provides good oxidation protection, it was rapidly lost due to formation of volatile CrO3 when exposed to the high speed air stream. The preferred oxide arrangement for the dynamic test consisted of an external layer of NiO with a porous mushroom type morphology, an intermediate duplex layer of NiO and Cr2O3, and a continuous inner layer of Cr2O3 in contact with the alloy substrate. An oxidation model has been developed to explain the observed microstructure and overall oxidation behavior of all alloys.

Tenney, D. R.↗
NASA NTRS1988

The effect of 0.1 atomic percent zirconium on the cyclic oxidation behavior of beta-NiAl for 300 hours at 1200 C

The long time effect of 0.1 at percent Zr (0.2 wt percent Zr) on the cyclic oxidation behavior of hipped beta-NiAl was studied. Oxidation testing was performed in static air at 1200 C for up to 3000 one-hour exposure cycles. Specific weight change versus time data was modeled with the COSP computer program to analyze cyclic oxidation behavior. The Zr-free stoichiometric alloy oxidized and spalled randomly to bare metal between cycles at a rate high enough to deplete Al to a low enough level that oxidation breakaway took place as nonprotective NiO replaced the alpha-Al2O3/NiAl2O4 scale as the controlling oxide. The Zr minimized this severe type of spalling maintaining the protective alpha-Al2O3 scale even out to 3000 hours for the stoichiometric alloy with no significant Al depletion. A third beta-NiAl alloy containing 0.1 at percent Zr but with 10 percent less Al than the stoichiometric alloy was also tested and showed some depletion of Al, but the protective Al2O3/NiAl2O4 was still maintained to close to 2700 hours.

Barrett, C. A.↗
NASA NTRS1989

The effect of 0.1 atomic percent zirconium on the cyclic oxidation behavior of beta-NiAl for 3000 hours at 1200 C

The long time effect of 0.1 at percent Zr (0.2 wt percent Zr) on the cyclic oxidation behavior of hipped beta-NiAl was studied. Oxidation testing was performed in static air at 1200 C for up to 3000 one-hour exposure cycles. Specific weight change versus time data was modeled with the COSP computer program to analyze cyclic oxidation behavior. The Zr-free stoichiometric alloy oxidized and spalled randomly to bare metal between cycles at a rate high enough to deplete Al to a low enough level that oxidation breakaway took place as nonprotective NiO replaced the alpha-Al203/NiAl204 scale as the controlling oxide. The Zr minimized this severe type of spalling maintaining the protective alpha-Al203 scale even out to 3000 hours for the stoichiometric alloy with no significant Al depletion. A third beta-NiAl alloy containing 0.1 at percent Zr but with 10 percent less Al than the stoichiometric alloy was also tested and showed some depletion of Al, but the protective Al203/NiAl204 was still maintained to close to 2700 hours.

Barrett, C. A.↗
NASA NTRS1988

Oxidation behavior of FeAl+Hf,Zr,B

The oxidation behavior of Fe-40Al-1Hf, Fe-40Al-1Hf-0.4B, and Fe-40Al-0.1Zr-0.4B (at. percent) alloys was characterized after 900, 1000, and 100 C exposures. Isothermal tests revealed parabolic kinetics after a period of transitional theta-alumina scale growth. The parabolic growth rates for the subsequent alpha-alumina scales were about five times higher than those for NiAl+0.1Zr alloys. The isothermally grown scales showed a propensity toward massive scale spallation due to both extensive rumpling from growth stresses and to an inner layer of HfO2. Cyclic oxidation for 200 1-hr cycles produced little degradation at 900 or 1000 C, but caused significant spallation at 1100 C in the form of small segments of the outer scale. The major difference in the cyclic oxidation of the three FeAl alloys was increased initial spallation for FeAl+Zr,B. Although these FeAl alloys showed many similarities to NiAl alloys, they were generally less oxidation resistant. It is believed that this resulted from nonoptimal levels of dopants and larger thermal expansion mismatch stresses.

Smialek, James L.↗
NASA NTRS1989

Oxidation behavior of FeAl+Hf,Zr,B

The oxidation behavior of Fe-40Al-1Hf, Fe-40Al-1Hf-0.4B, and Fe-40Al-0.1Zr-0.4B (at. percent) alloys was characterized after 900, 1000, and 100 C exposures. Isothermal tests revealed parabolic kinetics after a period of transitional theta-alumina scale growth. The parabolic growth rates for the subsequent alpha-alumina scales were about five times higher than those for NiAl+0.1Zr alloys. The isothermally grown scales showed a propensity toward massive scale spallation due to both extensive rumpling from growth stresses and to an inner layer of Hf02. Cyclic oxidation for 200 1-hr cycles produced little degradation at 900 or 1000 C, but caused significant spallation at 1100 C in the form of small segments of the outer scale. The major difference in the cyclic oxidation of the three FeAl alloys was increased initial spallation for FeAl+Zr,B. Although these FeAl alloys showed many similarities to NiAl alloys, they were generally less oxidation resistant. It is believed that this resulted from nonoptimal levels of dopants and larger thermal expansion mismatch stresses.

Smialek, James L.↗
NASA NTRS1977

Paralinear oxidation behavior

Program analyzes paralinear oxidation with emphasis on long-time behavior. Program is also used to analyze cyclic oxidation where oxide growth and spalling between heating cycles approximates paralinear behavior.

Barrett, C. A.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17%Cr and Cu-17%Cr-5%Al: Oxidation Kinetics - Part 1

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. These observations reveal that Cu- 17%Cr-5%Al oxidizes at significantly slower rates than Cu-17%Cr. The rate constants for the alloys were determined from generalized analyses of the data without an a priori assumption of the nature of the oxidation kinetics. Detailed analyses of the isothermal thermogravimetric weight change data revealed that Cu-17%Cr exhibited parabolic oxidation kinetics with an activation energy of 165.9 +/- 9.5 kJ/mol. In contrast, the oxidation kinetics for the Cu-17%Cr- 5%Al alloy exhibited a parabolic oxidation kinetics during the initial stages followed by a quartic relationship in the later stages of oxidation. Alternatively, the oxidation behavior of Cu-17%CR- 5%Al could be better represented by a logarithmic relationship. The parabolic rate constants and activation energy data for the two alloys are compared with literature data to gain insights on the nature of the oxidation mechanisms dominant in these alloys.

Raj. Sai V.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17%Cr and Cu-17%Cr-5%Al: Oxidation Kinetics - Part 1

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. These observations reveal that Cu- 17%Cr-5%Al oxidizes at significantly slower rates than Cu-17%Cr. The rate constants for the alloys were determined from generalized analyses of the data without an a priori assumption of the nature of the oxidation kinetics. Detailed analyses of the isothermal thermogravimetric weight change data revealed that Cu-17%Cr exhibited parabolic oxidation kinetics with an activation energy of 165.9 9.5 kJ mol-1. In contrast, the oxidation kinetics for the Cu-17%Cr- 5%Al alloy exhibited a parabolic oxidation kinetics during the initial stages followed by a quartic relationship in the later stages of oxidation. Alternatively, the oxidation behavior of Cu-17%CR- 5%Al could be better represented by a logarithmic relationship. The parabolic rate constants and activation energy data for the two alloys are compared with literature data to gain insights on the nature of the oxidation mechanisms dominant in these alloys.

Raj. Sai V.↗
NASA NTRS1995

High-temperature oxidation behavior of reaction-formed silicon carbide ceramics

The oxidation behavior of reaction-formed silicon carbide (RFSC) ceramics was investigated in the temperature range of 1100 to 1400 C. The oxidation weight change was recorded by TGA; the oxidized materials were examined by light and electron microscopy, and the oxidation product by x-ray diffraction analysis (XRD). The materials exhibited initial weight loss, followed by passive weight gain (with enhanced parabolic rates, k(sub p)), and ending with a negative (logarithmic) deviation from the parabolic law. The weight loss arose from the oxidation of residual carbon, and the enhanced k(sub p) values from internal oxidation and the oxidation of residual silicon, while the logarithmic kinetics is thought to have resulted from crystallization of the oxide. The presence of a small amount of MoSi, in the RFSC material caused a further increase in the oxidation rate. The only solid oxidation product for all temperatures studied was silica.

Ogbuji, Linus U. J. T.↗