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Specific weight changes of nickel-base superalloy B-1900 and B-1900 + 1% Si specimens were tested at 1273 K. B-1900 was losing weight at an increasing rate due to spalling of oxide scale while B-1900 + 1% Si was still gaining weight at low, nearly constant rate. Similar comparison in weight change was observed for specimens tested at 1373 K.
Aminopolymer-based adsorbents are a prominent class of materials being used for direct air capture of CO 2 at the industrial scale. However, improving their working lifetime, specifically by increasing their resilience to oxidative degradation, remains an ongoing challenge. Toward this end, functionalization of aminopolymers with non-amine functionalities such as hydroxyls has emerged in recent years as a promising strategy toward improving adsorbent lifetime. Although there is a growing body of work demonstrating the effectiveness of this approach and investigating the origin of this improved stability, studies to date have primarily focused on branched aminopolymer systems such as branched poly(ethylenimine). In this work, hydroxyl-functionalized linear poly(ethylenimine) is used to continue to probe the underlying protective mechanism of this strategy. A combination of thermogravimetric analysis, NMR relaxometry, differential scanning calorimetry, and computational simulations is used to better understand the relationship between the extent of chemical functionalization, physical properties, and adsorbent performance.
A polyimide is a polymer composed of alternating units of diamine and dianhydride, linked to each other via an imide bond. PMR polyimides, commonly used in the aerospace industry, are generally capped at each end by a norbornene endcap which serves a double function: (1) It limits the number of repeating units and, hence, the average molecular weight of the various polymer chains (oligomers), thereby improving processibility; (2) Upon further treatment (curing), the endcap crosslinks the various oligomer strands into a tough heat-resistant piece. Norbornenyl-end capped PMR polyimide resins' are widely used as polymer matrix composite materials for aircraft engine applications,2 since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a twestep approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, as shown for PMR-15.
A thermocouple is disclosed. The thermocouple is comprised of an electropositive leg formed of a noble metal-Al alloy and an electronegative leg electrically joined to form a thermocouple junction. The thermocouple provides for accurate and reproducible measurement of high temperatures (600 - 1300 C) in inert, oxidizing or reducing environments, gases, or vacuum. Furthermore, the thermocouple circumvents the need for expensive, strategic precious metals such as rhodium as a constituent component. Selective oxidation of rhodium is also thereby precluded.
Ground based testing of materials considered for polyimide (Kapton) solar array blanket protection and graphite-epoxy stroctural member protection was performed in an RF plasma asher. Protective coatings on Kapton from various commercial sources and from NASA Lewis Research Center were exposed to the air plasma; and mass loss per unit area was measured for each sample. All samples evaluated provided some protection to the underlying surface, but metal-oxide-fluoropolymer coatings provided the best protection by exhibiting very little degradation after 47 hr of asher exposure. Mica paint was evaluated as a protective coating for graphite-epoxy structural members. Mica appeared to be resistant to attack by atomic oxygen, but only offered limited protection as a paint. this is believed to be due to the paint vehicle ashing underneath the mica leaving unattached mica flakes lying on the surface. The protective coatings on Kapton evaluated so far are promising but further research on protection of graphite-epoxy support structures is needed.
Aluminum substituted for rhodium, which is scarce and expensive. Electromotive force increases with aluminum content in Pt/Al leg of Pt(Pt/Al) thermocouple. Wires baked longer in aluminizing bed produce larger voltages. Thermocouples containing platinum/aluminum legs used instead of thermocouples of type R in furnaces, heat engines, and chemical reactors. Expecially suited to high-velocity oxidizing environments. Constructed as thin-film sensors on turbine blades and vanes, where pre-oxidation provides insulating film needed between thermocouple legs. Because aluminum content slowly depleted by oxidation, long-term use recommended only where maximum temperature is 1,200 degrees C or less.
A Sialon of formula Si2.55Al0.6O0.72N3.52 was made from ball-milled alpha-Si3N4, AIN, and SiO2 by sintering the powder compacts at 1760 C for 4 hours in stagnant nitrogen. This Sialon had an average modulus of rupture ranging from 404 megapascals (58.6 ksi) at room temperature to 254 megapascals (36.8 ksi) at 1400 C. Oxidation tests at 1400 C in air showed it to have a parabolic oxidation rate constant less than or equal to 2.8x10 to the -10th power sq g/cm4 hr, which is smaller than that of any other Si3N4-base ceramic reported in the literature.
A number of leading-edge specimens of ATJ graphite and 0.5-percent titanium-molybdenum alloy were tested in a 6-inch subsonic low-pressure arc-powered tunnel and a 1,500-kw subsonic arc jet to determine the effectiveness of several refractory coatings in preventing the oxidation of these materials. The results indicate that the siliconized coating for the ATJ graphite and the W-2 and Durak MG coatings for the titanium-molybdenum alloy provide adequate protection at temperatures up to 3,000 F for the durations of the tests in these facilities, approximately 70 seconds in the arc tunnel and approximately 10 minutes in the arc jet. Weight losses (less than one-half of 1 percent) experienced by a few of the coated specimens indicate that tests of longer duration in these environments may prove deleterious and that the stability of these coatings may be depreciated under the low-pressure environmental conditions encountered during reentry.
Environmental barrier coatings (EBCs) are used to mitigate chemical reactions between SiC ceramic matrix composite (CMC) components and the H 2 O in combustion gas in turbine hot sections. CMCs are currently temperature-limited by the Si-bond coating, which melts at ~ 1414 °C. This work explores EBCs where the bond coating was removed to achieve higher operating temperatures. Various versions of enhanced roughness SiC were utilized to improve EBC adhesion to the substrates prior to 1 h furnace cycle testing in steam at 1250–1425 °C. The enhanced SiC roughness resulted in short coating lifetimes as the roughness was oxidized away with SiO 2 formation. Further, isothermal furnace exposures at 1400–1600 °C showed Yb 2 Si 2 O 7 /Yb 2 SiO 5 EBC microstructural changes, resulting in premature debonding from the substrates. Finally, this work provides baseline requirements for the development of both next-generation EBCs and bond coating strategies to overcome the current limitation of the Si-bond coating melting temperature.
For many decades the dramatic effect of trace amounts of reactive elements on alumina and chromia scale adhesion has been recognized and widely studied. Although various theories have been used to account for such behavior, the connection between scale adhesion and sulfur segregation was initially reported by Smeggil et al. This study found strong surface segregation of sulfur from very low levels in the bulk which could then be curtailed by the addition of reactive elements. It was assumed that the reactive elements, which are strong sulfide formers, acted by getting sulfur in the bulk thus precluding sulfur segregation and weakening of the oxide-metal bond. Subsequent studies confirmed that adhesion could be produced by reducing the sulfur impurity level, without reactive elements. The understanding of this phenomenon has been applied to modern single crystal superalloys, where the addition of Y, although very effective, is problematic. Also problematic is definition of the level of sulfur that is acceptable and below which no further adhesion benefit is reached. Published works have indicated a broad transition defined by various materials and oxidation tests. The present study describes the oxidation behavior of one superalloy (PWA 1480) as a function of various sulfur contents produced by hydrogen annealing for various temperatures, times, and sample thicknesses. The purpose is to define more precisely a criterion for adhesion based on total sulfur reservoir and segregation potential.
A composite thermal protection structure, for applications such as atmospheric re-entry vehicles, that can withstand temperatures as high as 3600.degree. F. The structure includes an exposed surface cap having a specially formulated coating, an insulator base adjacent to the cap with another specially formulated coating, and one or more pins that extend from the cap through the insulator base to tie the cap and base together, through ceramic bonding and mechanical attachment. The cap and insulator base have corresponding depressions and projections that mate and allow for differences in thermal expansion of the cap and base. A thin coating of a reaction cured glass formulation is optionally provided on the structure to allow reduce oxidization and/or to reduce catalytic efficiency.
Studies were conducted to determine the friction and wear properties of experimental carbon-graphites. Hemispherically tipped carbon-graphite rider specimens were tested in sliding contact with rotating Inconel X-750 disks in air. A surface speed of 1.33 m/sec, a load of 500 g, and a specimen temperature of 650 C were used. Results indicate: (1) hardness is not a major factor in determining friction and wear under the conditions of these studies. (2) Friction and wear as low as or lower than those observed for a good commercial seal material were attained with some of the experimental materials studied. (3) The inclusion of boron carbide (as an oxidation inhibitor) has a strong influence on wear rate. (4) Phosphate treatment reduces the friction coefficient when boron carbide is not present in the base material.
A comparative study was made of the surface recession (etching) of thin films of plasma polymerized tetrafluoro ethylene (PPTFE), polytetrafluoro ethylene (PTFE), and ion-beam sputter deposited polytetrafluoro ethylene (SPTFE) exposed to ground-state atomic oxygen downstream from a nonequilibrium radio-frequency O2 plasma. At 22 C, the etch rates for PTFE, SPTFE, and PPTFE were in the ratio of 8.7:1.8:1.0. A thin, conformal coating of PPTFE (etch rate of 0.3 nm/h at 22 C) was found to protect an underlying cast film of a reactive polymer, cis-1,4 polybutadiene, against ground-state atomic oxygen attack for the time required to fully etch away the PPTFE coating. From ESCA analysis, PTFE exhibited only minor surface oxidation (uptake of 0.5 atom percent O) upon etching, its F/C ratio decreasing slightly from 2.00 to 1.97; PPTFE exhibited considerable surface oxidation (uptake of 5.9 atom percent O) intermediate between those of PTFE and PPTFE, with a decrease in F/C ratio from 1.73 to 1.67. A plasma-polymerized fluorocarbon coating such as PPTFE might be useful for space applications to protect polymers that are vulnerable to oxidation or degradation by oxygen atoms.
Several substituted 1,2,3,6-tetrahydrophthalic anhydride end caps - including the 3-phenyl, 3-methoxy, 3-trimethylsilyloxy, and 3,6-diphenyl analogs - were synthesized via the Diels-Alder condensation of the corresponding butadienes and maleic anhydride. These anhydrides, as well as the commercially available 3-hydro and 4-methyl analogs, were each ground together with methylenedianiline in a 2:1 ratio and heated gradually from 204 C to 371 C, with the thermolysis followed by NMR. Generally speaking, a transformation via monoimide to bisimide was observed in the lower temperature range, followed by competition between crosslinking and aromatization. We believe that this competition produces a substantial percentage of aromatic product, with the concomitant lowering of the relative amount of crosslinking and is responsible for improving both thermal oxidative stability of tetrahydrophthalic end capped polyimides and their substantial frangibility. The thermolysis of the tetrahydrophthalimides under inert atmosphere dramatically lowers the amount of aromatization hence, the mechanism for aromatization is an oxidative one.
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Test conditions and results are reported for various coatings on a 1 percent zirconium columbium alloy at a temperature of 2000 deg F. Molybdenum silicide over molybdenum is most effective coating, tin-aluminum coating is adequately protective, chromium-molybdenum silicides are not protective.
Coated screens withstand temperature cycling in special transpiration-cooling systems and provide porous surface that is effective at temperatures well above those limiting superalloy screen efficiency. Thickness of coating depends on time, temperature and activator concentration. Coatings are uniform and resistant to thermal cycling.
The Co-18Cr-20Ni-4 Vol % ThO2 powders were prepared by a flash drying selective reduction process starting with an aqueous solution of metal salts and colloidal thoria. Powders were consolidated and extruded into rods with a minimum density of 99% of theoretical. Swaging and annealing studies were conducted to determine the conditions that would lead to a product with high stress-rupture strength. The best process yielded a stress-rupture life of 7.2 hours at 10 KSI (69 MN sq m and 2000 F (1094 C). The alloy recrystallized to a duplex (coarse-fine) structure and thus did not exhibit the desired strength of 3000 hours at 15 KSI (103.5MN/sq m and 2000 F (1094 C).