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NASA NTRS1989

Sodium sulfate - Deposition and dissolution of silica

The hot-corrosion process for SiO2-protected materials involves deposition of Na2SO4 and dissolution of the protective SiO2 scale. Dew points for Na2SO4 deposition are calculated as a function of pressure, sodium content, and sulfur content. Expected dissolution regimes for SiO2 are calculated as a function of Na2SO4 basicity. Controlled-condition burner-rig tests on quartz verify some of these predicted dissolution regimes. The basicity of Na2SO4 is not always a simple function of P(SO3). Electrochemical measurements of an (Na2O) show that carbon creates basic conditions in Na2SO4, which explains the extensive corrosion of SiO2-protected materials containing carbon, such as SiC.

Jacobson, Nathan S.↗

NASA NTRS1975

Sodium sulfate: Vaporization thermodynamics and role in corrosive flames

Gaseous species over liquid Na2SO4 were identified by the technique of molecular beam mass spectrometry. The heat and entropy of vaporization of the Na2SO4 molecule were measured directly. Comparisons of the experimental entropy with values calculated using various molecular parameters were used to estimate the molecular structure and vibrational frequencies. The thermodynamic properties of gaseous and condensed phase Na2SO4, along with additional pertinent species, were used in a computer program to calculate equilibrium flame compositions and temperatures for representative turbine engine and burner rig flames. Compositions were calculated at various fuel-to-oxidant ratios with additions of sulfur to the fuel and the components of sea salt to the intake air. Temperatures for condensation of Na2SO4 were obtained as a function of sulfur and sea salt concentrations.

Kohl, F. J.↗

NASA NTRS1979

The role of NaCl in flame chemistry, in the deposition process, and in its reactions with protective oxides as related to hot corrosion

Sodium chloride is believed to be the primary source of turbine engine contamination that contributes to hot corrosion. The behavior of NaCl-containing aerosols ingested with turbine intake air is very complex; some of the NaCl may vaporize during combustion while some may remain as particulates. The NaCl can lead to Na2SO4 formation by several possible routes or it can contribute to corrosion directly. Hydrogen or oxygen atom reaction with NaCl(c) was shown to result in the release of Na(g). Gaseous NaCl in flames can be partially converted to gaseous Na2SO4 by homogeneous reactions. The remaining gaseous NaCl and other Na-containing molecules can act as sodium carriers for condensate deposition of Na2SO4 on cool surfaces. A frozen boundary layer theory was developed to predict the rates of deposition. The condensed phase NaCl can be converted directly to condensed Na2SO4 by reaction with sulfur oxides and O2. Reaction of gaseous NaCl with Cr2O3 results in the vapor phase transport of chromium by the formation of complex Cr-containing gaseous molecules. Similar gaseous complexes are formed with molybdenum. The presence of gaseous NaCl was shown to affect the oxidation kinetics of Ni-Cr alloys. It also causes changes in the surface morphology of Al2O3 scales formed on Al-containing alloys.

Kohl, F. J.↗

NASA NTRS1981

Investigation into the role of NaCl deposited on oxide and metal substrates in the initiation of hot corrosion

Morphological aspects of the conversion to Na2SO4 of NaCl deposits over the temperature range 500-700 C, in air with added SO2 and H2O. Progress of the reaction was observed by withdrawing samples at various times and examining them under the scanning electron microscope using EDAX to assess the extent of chloride to sulfate conversion. These initial results show that the conversion to Na2SO4 proceeds directly on the sodium chloride surface as well as on the surrounding substrate due to evaporation of NaCl from the solid particle. The mechanism of this reaction could involve reaction in the vapor to produce Na2SO4 which then deposits, alternatively Na2SO4 could form directly on the substrate surface due to direct reaction there between the vapors NaCl, SO2 and O2.

Birks, N.↗

NASA NTRS1986

Corrosion of metals and alloys in sulfate melts at 750 C

The corrosion of Ni, Co, Ni-10Cr, Co-21Cr, and IN738 was studied at 750 C in the presence of molten sulfate mixtures (Na2SO4-Li2SO4 and Na2SO4-CoSO4) and in an atmosphere consisting of O2 + 0.12 percent SO2-SO3. The corrosion was observed to be similar for both Na2SO4-Li2SO4 and Na2SO4-CoSO4 melts. The corrosion of Ni and Co took place by the formation of a mixed oxide plus sulfide scale, very similar to the corrosion in SO2 or SO3 alone. The initial stage for the corrosion of Ni-10Cr involved the formation of a thick NiO + Ni3S2 duplex scale, and Cr sulfide was formed during the later stages. A pitting type of morphology was observed for both Co-21Cr and IN738. The pit was Cr sulfide at the beginning, and subsequently the sulfides oxidized to Cr2O3. A base-metal oxide layer was present above the pit, and this was observed to be formed very early in the corrosion process. A mechanism is proposed to explain this. In general, the formation of sulfides appears to be the primary mode of degradation in mixed sulfide melts.

Misra, A. K.↗

NASA NTRS1986

Reactions occurring during the sulfation of sodium chloride deposited on alumina substrates

The reaction between solid NaCl and air containing 1 pct SO2 has been studied between 500 and 700 C. The reaction product, Na2SO4, forms not only on the surface of the NaCl but also on surrounding areas of the substrate due to the volatility of the NaCl at these temperatures. At the higher temperatures, the vapor pressure of NaCl is so high that the majority of the reaction product is distributed on the substrate. Above 625 C, the reaction product is a liquid solution of NaCl and Na2SO4 that exists only so long as NaCl is supplied from the original crystal source. Eventually, the liquid solidifies by constitutional solidification as the NaCl is converted to Na2SO4. While it exists, the liquid NaCl-Na2SO4 solution is shown to be highly corrosive to Al2O3 and, on a scale of Al2O3 growing on alloy HOS 875, particularly attacks the grain boundaries of the scale at preferred sites where chromium and iron oxides and sulfides rapidly develop. This is proposed as one mechanism by which NaCl deposition contributes to the initiation of low temperature hot corrosion.

Wu, C. S.↗

NASA NTRS1977

Gaseous sodium sulfate formation in flames and flowing gas environments

Formation of Na2SO4(g) in flames and hot flowing gas systems was studied by high pressure, free-jet expansion, modulated molecular beam mass spectrometric sampling. Fuel-lean CH4-O2 flames doped with SO2, H2O and NaCl yielded the gaseous Na2SO4 molecule in residence times of less than one millisecond. Intermediate species NaSO2(g) and NaSO3(g) were also observed and measured. Composition profiles were obtained for all reaction products. Nonflame flowing gas experiments showed that Na2SO4 and NaSO3 gaseous molecules were formed at 1140 C in mixtures of O2, H2O(g), SO2 and NaCl(g). Experimental results are compared with calculated equilibrium thermodynamic predictions.

Stearns, C. A.↗

NASA NTRS1977

Gaseous sodium sulfate formation in flames and flowing gas environments

Formation of Na2SO4(g) in flames and hot flowing gas systems was studied by high pressure, free-jet expansion, modulated molecular beam mass spectrometric sampling. Fuel-lean CH4-O2 flames doped with SO2, H2O and NaCl yielded the gaseous Na2SO4 molecule in residence times of less than one millisecond. Intermediate species NaSO2(g) and NaSO3(g) were also observed and measured. Composition profiles were obtained for all reaction products. Non-flame flowing gas experiments showed that Na2SO4 and NaSO3 gaseous molecules were formed at 1140 C in mixtures of O2, H2O(g), SO2 and and NaCl(g). Experimental results are compared with calculated equilibrium thermodynamic predictions.

Stearns, C. A.↗

NASA NTRS1980

Hot corrosion of Co-Cr, Co-Cr-Al, and Ni-Cr alloys in the temperature range of 700-750 deg C

The effect of SO3 pressure in the gas phase on the Na2SO4 induced hot corrosion of Co-Cr, Ni-Cr, and Co-Cr-Al alloys was studied in the temperature range 700 to 750 C. The degradation of the Co-Cr and Ni-Cr alloys was found to be associated with the formation of liquid mixed sulfates (CoSO4-Na2SO4 or NiSO4-Na2SO4) which provided a selective dissolution of the Co or Ni and a subsequent sulfidation oxidation mode of attack which prevented the maintenance of a protective Cr2O3 film. A clear mechanism was not developed for the degradation of Co-Cr-Al alloys. A pitting corrosion morphology was induced by a number of different mechanisms.

Chiang, K. T.↗

NASA NTRS1983

Reactions of NaCl with Gaseous SO3, SO2, and O2

Hot corrosion of gas turbine engine components involves deposits of Na2SO4 which are produced by reactions between NaCl and oxides of sulfur. For the present investigation, NaCl single crystals were exposed at 100 to 850 C to gaseous mixtures of SO3, SO2, and O2. The products formed during this exposure depend, primarily, on the temperatures. The four product films were: NaCl-SO3; Na2S2O7; Na2SO4; and NaCl-Na2SO4. The kinetics of the reactions were measured.

Fielder, W. L.↗

NASA NTRS1983

Low temperature hot corrosion

The reaction of Co-Cr, Ni-Cr, Co-Cr-Al, and Ni-Cr-Al alloys with Na2SO4 in the presence of SO3 at temperatures between 700 and 750 C leads to the formation of liquid CoSO4-Na2SO4 or NiSO4-Na2SO4 deposits on the alloy surface. The formation of Cr2O3 and/or Al2O3 below this deposit results in a locally low P(O2) and a higher P(S2) and P(SO2). It is noted that these conditions can prevent protective oxide formation either by sulfide formation in the alloy, which localizes the Cr and/or Al in discrete particles, or by acid fluxing involving a reaction between Al2O3 or Cr2O3 and SO2 to form a salt-soluble species and subsequent reprecipitation as porous oxides in regions of higher P(O2). These processes may occur simultaneously, although a given alloy generally exhibits features of predominantly one type. Here, the Ni-Cr and Ni-Cr-Al alloys, and to some extent the Co-Cr alloys, exhibit features indicative of the sulfidation mechanism, whereas the morphology for the Co-Cr-Al alloy is more consistent with a predominant acid fluxing mechanism.

Chiang, K. T.↗

NASA NTRS1985

Oxidation and hot corrosion of hot-pressed Si3N4 at 1000 deg C

The oxidation and hot corrosion of a commercial, hot-pressed Si3N4 were investigated at 1000 C under an atmosphere of flowing O2. For the hot corrosion studies, thin films of Na2SO4 were airbrushed on the Si3N4 surface. The hot corrosion attack was monitored by the following techniques: continuous weight measurements, SO2 evolution, film morphology, and chemical analyses. Even though the hot corrosion weight changes after 25 hr were relatively small, the formation of SiO2 from oxidation of Si3N4 was an order of magnitude greater in the presence of molten Na2SO4. The formation of a protective SiO2 phase at the Si3N4 surface is minimized by the fluxing action of the molten Na2SO4 thereby allowing the oxidation of the Si3N4 to proceed more rapidly. A simple process is proposed to account for the hot corrosion process.

Fielder, W. L.↗

NASA NTRS1984

Reactions of NaCl with gaseous SO3, SO2, and O2

Fielder, W. L.↗

DOE OSTI2023

Water-coupled monovalent and divalent ion transport in polyviologen networks

Redox-active polymers (RAPs) are of interest as environmentally friendly and earth-abundant energy storage materials. Polyviologens are promising RAPs, but they tend to dissolve during operation. Further, the two-electron redox reaction for polyviologens in various electrolytes is not always reversible, highlighting the need for a deeper understanding of the redox mechanism. Here, the energy storage mechanism for a cross-linked viologen (PTPM) is demonstrated using electrochemical quartz crystal microbalance with dissipation monitoring (EQCM-D), comparing NaCl and Na2SO4 aqueous electrolytes. E-QCMD reveals that the ion-electron transport mechanism is strongly dependent on the valency of the anion. More sudden and dramatic changes in the electrode's mass were observed for the divalent sulfate ion as compared to the smooth mass transitions associated with the monovalent chloride ion. Meanwhile, there was marked hysteresis in the mass transfer profile for NaCl, but little hysteresis for Na2SO4. Our results demonstrate that electrolyte design, and specifically ion valency, will have a large impact on the nature of mass transport in polymer-based electrodes. This work enables electrolyte selection for the next generation polymer batteries with improved performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1977

Hot corrosion of S-57, 1 cobalt-base alloy

A cobalt base alloy, S-57, was hot corrosion tested in Mach 0.3 burner rig combustion gases at maximum alloy temperatures of 900 and 1000 C. Various salt concentrations were injected into the burner: 0.5, 2, 5, and 10 ppm synthetic sea salt and 4 ppm sodium sulfate (Na2SO4). S-57 underwent accelerated corrosion only under the most severe test conditions, for example, 4 ppm Na2SO4 at 900 C. The process of the accelerated corrosion was primarily sulfidation.

Santoro, G. J.↗

NASA NTRS1979

X-ray photoelectron spectroscopy study of nickel and nickel-base alloy surface alterations in simulated hot corrosion conditions with emphasis on eventual application to turbine blade corrosion

Research on the high temperature oxidation and Na2SO4 induced hot corrosion of some nickel base superalloys was accomplished by using ESCA to determine the surface composition of the oxidized or corroded samples. Oxidation was carried out at 900 or 1000 C in slowly flowing O2 for samples of B-1900, NASA-TRW VIA, 713C, and IN-738. Oxidation times ranged from 0.5 to 100 hr. Hot corrosion of B-1900 was induced applying a coating of Na2SO4 to peroxidized samples, the heating to 900 C in slowly flowing O2. For oxidized samples, the predominant type of scale formed by each superalloy was determined, and a marked surface enrichment of Ti was found in each case. For corroded samples, the transfer of significant amounts of material from the oxide layer to the surface of the salt layer was observed to occur long before the onset of accelerating weight-gain. Changes in surface composition were observed to coincide with the beginning of accelerating corrosion, the most striking of which was a tenfold decrease in the sulfur to sodium ration and an increase in the Cr(VI) ratio.

Mateescu, G. D.↗

NASA NTRS1980

ESCA study of oxidation and hot corrosion of nickel-base superalloys

A study of the high-temperature oxidation and Na2SO4-induced hot corrosion of nickel-base superalloys has been accomplished by using ESCA to determine the surface composition of the oxidized or corroded samples. Oxidation was carried out at 900 or 1000 C in slowly flowing O2 for samples of B-1900, NASA-TRW VIA, 713C, and IN-738. Hot corrosion of B-1900 was induced by applying a coating of Na2SO4 to preoxidized samples, then heating to 900 C in slowly flowing O2. For oxidized samples, the predominant type of scale formed by each superalloy showed a marked surface enrichment of Ti. For corroded samples, the transfer of significant amounts of material from the oxide layer to the surface of the salt layer was observed before the onset of rapidly accelerating weight gain. Marked changes in surface composition coincided with the beginning of accelerating corrosion, the most striking of which were a tenfold decrease in the sulfur to sodium ratio and an increase in the Cr(VI) to Cr(III) ratio.

Smith, S. R.↗

NASA NTRS1982

Mechanism of hot corrosion of IN-738

The Na2SO4 - induced hot corrosion of IN-738 in the temperature range 900 C to 1000 C is characterized by an initiation stage during which the corrosion rate is slow followed by a propagation stage during which the corrosion rate is markedly accelerated. In the second stage, corrosion is accelerated due essentially to a sulfidation/oxidation mechanism; in the third stage, the rate becomes catastrophic due to acid fluxing induced by an accumulation of refractory metal oxides (particularly MoO3) in the Na2SO4. The sequential stages in the corrosion process are described and a mechanism proposed. The influence of alloy microstructure on the corrosion mechanism is also discussed.

Meier, G. H.↗