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At least 19 records

Comparison of Autoclave and Out-of-Autoclave Composites

The National Aeronautics and Space Administration (NASA) Exploration Systems Mission Directorate initiated an Advanced Composite Technology Project through the Exploration Technology Development Program in order to support the polymer composite needs for future heavy lift launch architectures. As an example, the large composite dry structural applications on Ares V inspired the evaluation of autoclave and out-of-autoclave (OOA) composite materials. A NASA and industry team selected the most appropriate materials based on component requirements for a heavy lift launch vehicle. Autoclaved and OOA composites were fabricated and results will highlight differences in processing conditions, laminate quality, as well as initial room temperature thermal and mechanical performance. Results from this study compare solid laminates that were both fiber-placed and hand-laid. Due to the large size of heavy-lift launch vehicle composite structures, there is significant potential that the uncured composite material or prepreg will experience significant out-life during component fabrication. Therefore, prepreg out-life was a critical factor examined in this comparison. In order to rigorously test material suppliers recommended out-life, the NASA/Industry team extended the out-time of the uncured composite prepreg to values that were approximately 50% beyond the manufacturers out-time limits. Early results indicate that the OOA prepreg composite materials suffered in both composite quality and mechanical property performance from their extended out-time. However, the OOA materials performed similarly to the autoclaved composites when processed within a few days of exposure to ambient "shop" floor handling. Follow on studies evaluating autoclave and OOA aluminum honeycomb core sandwich composites are planned.

Sutter, James K.↗

Buckling Testing and Analysis of Honeycomb Sandwich Panel Arc Segments of a Full-Scale Fairing Barrel Part 1: 8-Ply In-Autoclave Facesheets: 8-Ply In-Autoclave Facesheets - Part 1

Four honeycomb sandwich panels, representing 1/16th arc segments of a 10-m diameter barrel section of the heavy lift launch vehicle, were manufactured under the NASA Composites for Exploration program and the NASA Space Launch Systems program. Two configurations were chosen for the panels: 6-ply facesheets with 1.125 in. honeycomb core and 8-ply facesheets with 1.000 in. honeycomb core. Additionally, two separate carbon fiber/epoxy material systems were chosen for the facesheets: inautoclave IM7/977-3 and out-of-autoclave T40-800b/5320-1. Smaller 3.00- by 5.00-ft panels were cut from the 1/16th barrel sections. These panels were tested under compressive loading at the NASA Langley Research Center. Furthermore, linear eigenvalue and geometrically nonlinear finite element analysis was performed to predict the compressive response of the 3.00- by 5.00-ft panels. This manuscript summarizes the experimental and analytical modeling efforts pertaining to the panel composed of 8-ply, IM7/977-3 facesheets (referred to Panel A). To improve the robustness of the geometrically nonlinear finite element model, measured surface imperfections were included in the geometry of the model. Both the linear and nonlinear models yield good qualitative and quantitative predictions. Additionally, it was predicted correctly that the panel would fail in buckling prior to failing in strength. Furthermore, several imperfection studies were performed to investigate the influence of geometric imperfections, fiber misalignments, and three-dimensional (3 D) effects on the compressive response of the panel.

Myers, David E.↗

Development of Additively Manufactured Complex Tools for Autoclave Cure Composites

IACMI Project 4.9, Tooling for Composites with Washout Features Produced by Additive Manufacturing, assembled a team including the industry lead, Ability Composites, NREL and Colorado State University (CSU). Ability Composites had originally expressed interest in alternate methods of producing tooling for composite parts. In follow-up discussions, it became clear that one of the bigger tooling challenges revolved around small production volume composite parts that were tooled on washout material due to the complex geometry. To build an understanding of the potential, both from a technology and a cost perspective, for replacing conventional washout tooling with 3D printed thermoplastic tooling, a number of commercially available dissolvable FDM printing materials were evaluated, leading to tooling representative of commercial articles of interest to Ability Composites. Ultimately, Ability Composites was able to directly compare autoclave processed prepreg composite parts produced on conventional washout tooling to composite parts molded on 3D printed dissolvable tooling produced at CSU. Small, laboratory test specimens were developed to investigate the structural performance of the candidate materials under autoclave processing conditions, which were nominally 121 °C (250 °F) and 345 kPa (50 psi). In addition, several internal structural configurations (infills) were evaluated under autoclave conditions using model materials. The results of these tests indicated that two materials, Stratasys ST 130 and Infinite Materials Solutions Aquasys 180 (AQ 180), were the best candidates, given the specified autoclave processing conditions. ST-130 was slightly more robust than AQ-180; however, the AQ-180 was carried forward as it was dissolvable in water, not requiring the basic solution needed to dissolve ST-130. Based on the preliminary material and 3D printed structures evaluations, larger tools with a truncated square pyramid geometry were created to produce prepreg composite test articles for 3D printed dissolvable tool evaluation under standard autoclave fabrication conditions. Two tools were manufactured using ST-130 and one tool using traditional ceramic washout tooling media. The tools were evaluated for geometric fidelity and surface roughness changes before and after carbon fiber/epoxy prepreg composites were manufactured on the tooling. The autoclave processing did not impact the geometry significantly and was completed at 121 °C and 345 kPa, indicating satisfactory tool performance. The results from surface roughness testing of both the resulting composite and the associated tooling indicated that an adequate surface resulted without the need for a surface sealing step, as was required for the conventional washout tooling. Based on results of the truncated pyramid tests as a basis, ST-130, AQ-120 and AQ-180 materials were carried forward to the tool geometry of interest to Ability Composites. These hollow rectangular bent ducts, which were complex in nature and not extractable after cure, were used to understand the impacts of tool material and thickness. One ST-130 tool was produced as a partially solid part, with an enclosed 40% dense infill region to reduce weight and material use. This was the same approach evaluated in the truncated pyramid portion of the study. This tool was to be envelope vacuum bagged and directly compared to a monolithic tool of conventional washout material. The traditional monolithic ceramic tool was manufactured by Ability composites using CNC-based subtractive methods. An additional five dissolvable polymer tools, manufactured from ST-130, AQ-120, and AQ-180, using a hollow design were 3D printed and used to produce carbon fiber/epoxy composite evaluation articles. These hollow dissolvable tools were expected to be less influenced by the autoclave conditions as the wall was solid and vacuum bagging was inside and outside the tool. This alternative geometry was also evaluated as an option in techno-economic modeling. Print times were reduced from in excess of 3 days to under 30 hours, while surface quality and and tool integrity were substantially improved in the transition from the partially solid tool to the hollow tooling concept. Ability Composites produced autoclave-cured prepreg ducts on each of these tools. The autoclave conditions utilized were more severe than those of the initial trials, reaching temperatures of 160 °C and a pressure of 414 kPa. Under these conditions, the partially solid 3D printed tool with skin and 40% dense infill crushed significantly; however, the thicker ST-130 hollow tool showed good promise, deforming only slightly. The thinner hollow tool walls were unsuccessful as were the other materials. Overall, the hollow tool manufacturing process saved significant amounts of time and material in manufacturing as compared to the solid ducts and produced composite surface quality improvements compared to the traditional washout tooling. The TEM was developed to allow direct comparisons between conventional washout tool manufacturing processes and those developed at CSU. It also allowed for two separate 3D printed tool geometries to be analyzed and compared. In this case, the square bent duct tool geometry was determined to be representative of common washout tools. This geometry was compared with a scaled-up version of it to assess differences in the two manufacturing processes based on tool size. The model was developed to make use of user input in the form of geometry details, process steps, manufacturing parameters, bulk material costs, capital equipment costs, and general costs to calculate overall labor, material, capital equipment, and energy costs per manufactured tool for the conventional and additive manufacturing processes for the two representative geometries. It was also able to estimate step-by-step process times for the manufacturing process and geometries. Based on significant input from Ability Composites and CSU from their knowledge gained from hands-on manufacturing of the 3D printed bent duct tool geometry, costs and process times were calculated for the two manufacturing processes. Results showed that the additive manufacturing techniques developed at CSU can substantially reduce the costs of tool manufacturing by reducing labor times and material usage. This is because additive manufacturing is a relatively hands-off process and allows for the tool design to be optimized to reduce material usage. The disadvantage, however, is that process times for additive manufacturing are significantly longer. The three-dimensional (3D) printing process is slow if tight tolerances are required, but the analysis did show that print times could be reduced with the hollow tool geometry. Also, further advances in additive manufacturing could expedite the process. Costs and process times for the tool washout process were calculated separately. They showed that costs are relatively insignificant when compared to the overall tool manufacturing processes, but with increases in tool size, costs for the conventional manufacturing approach are larger than for additive manufacturing. Again, the washout process for conventional tools is very hands-on, whereas for additively manufactured tools the print medium is dissolved in an automated detergent bath at the sacrifice of process time. The analysis showed that optimizing the additively manufactured tools may also reduce washout times. Overall, Project 4.9 demonstrated that commercially available dissolvable 3D printing materials exist that can be used to produce dissolvable tooling capable of surviving prepreg composites fabrication under autoclave conditions of 121 °C (250 °F) and 345 kPa (50 psi). An alternative hollow dissolvable tool design was developed which was structurally superior to the initial concept and was cost and time effective versus conventional washout tooling. The 3D printed sacrificial tool required no added surface sealing steps prior to composite part layup and cure, offering a significant advantage over the porous conventional washout tooling.

36 MATERIALS SCIENCE↗

Autoclave treatment of the classical scrapie agent US No. 13-7 and experimental inoculation to susceptible VRQ/ARQ sheep via the oral route results in decreased transmission efficiency

Scrapie, a prion disease of sheep, is highly resistant to conventional deactivation. Numerous methods to deactivate scrapie have been tested in laboratory animal models, and adequate autoclave treatment can reduce or remove the infectivity of some classical scrapie strains depending on the heating parameters used. In this study, we autoclaved brain homogenate from a sheep with US scrapie strain 13–7 for 30 minutes at 121°C. Genetically susceptible VRQ/ARQ sheep were orally inoculated with 3 grams of the autoclaved brain homogenate. For comparison, a second group of sheep was inoculated with a non-autoclaved brain homogenate. Rectal biopsies were used to assess antemortem scrapie disease progression throughout the study. Five out of ten (5/10) sheep that received autoclaved inoculum ultimately developed scrapie after an experimental endpoint of 72 months. These sheep had a mean incubation period of 26.99 months. Two out of five (2/5) positive sheep had detectable PrP Sc in antemortem rectal biopsies, and two (2/5) other sheep had PrP Sc in postmortem rectal tissue. A single sheep (1/5) was positive for scrapie in the CNS, small intestine, and retropharyngeal lymph node but had negative rectal tissue. All of the sheep (10/10) that received non-autoclaved inoculum developed scrapie with a mean incubation period of 20.2 months and had positive rectal biopsies at the earliest timepoint (14.7 months post-inoculation). These results demonstrate that sheep are orally susceptible to US derived classical scrapie strain 13–7 after autoclave treatment at 121°C for 30 minutes. Differences in incubation periods and time interval to first positive rectal biopsies indicate a partial reduction in infectivity titers for the autoclaved inoculum group.

59 BASIC BIOLOGICAL SCIENCES↗

Elevated Temperature, Notched Compression Performance of Out of Autoclave Processed Composites

Curved honeycomb sandwich panels composed of carbon fiber reinforced toughened-epoxy polymer facesheets are being evaluated for potential use as payload fairing components on the NASA heavy-lift space launch system (HL-SLS). These proposed composite sandwich panels provide the most efficient aerospace launch structures, and offer mass and thermal advantages when compared with existing metallic payload fairing structures. NASA and industry are investigating recently developed carbon fiber epoxy prepreg systems which can be fabricated using out-of autoclave (OOA) processes. Specifically, OOA processes using vacuum pressure in an oven and thereby significantly reducing the cost associated with manufacturing large (up to 10 m diameter) composite structures when compared with autoclave. One of these OOA composite material systems, CYCOM(R) 5320-1, was selected for manufacture of a 1/16th scale barrel portion of the payload fairing; such that, the system could be compared with the well-characterized prepreg system, CYCOM(R) 977-3, typically processed in an autoclave. Notched compression coupons for each material were obtained from the minimum-gauge flat laminate [60/-60/0]S witness panels produced in this manufacturing study. The coupons were also conditioned to an effective moisture equilibrium point and tested according to ASTM D6484M-09 at temperatures ranging from 25 C up to 177 C. The results of this elevated temperature mechanical characterization study demonstrate that, for thin coupons, the OHC strength of the OOA laminate was equivalent to the flight certified autoclave processed composite laminates; the limitations on the elevated temperature range are hot-wet conditions up to 163 C and are only within the margins of testing error. At 25 C, both the wet and dry OOA material coupons demonstrated greater OHC failure strengths than the autoclave processed material laminates. These results indicate a substantial improvement in OOA material development and processing since previous studies have consistently reported OOA material strengths on par or below those of autoclave processed composite laminates.

Grimsley, Brian W.↗

An Artificial-Intelligence and Machine-Learning-Based Methodology to Conduct Seemingly Strain-Controlled Fatigue Test in a Pressurized-Water-Reactor-Test-Loop-Autoclave, While Not Controlling the Strain

In general, low cycle fatigue analysis of pressurized water reactor (PWR) components, requires strain-controlled fatigue test data such as using strain versus life (ε–N) curves. Conducting strain-controlled fatigue tests under in-air conditions is not an issue. However, controlling strain in a PWR-test-loop-autoclave is a challenge, since an extensometer cannot be placed in a narrow autoclave (typically used in a high-temperature-pressure PWR-test-loop). This is due to lack of space inside an autoclave that houses the test specimen. In addition, installing a contact-type extensometer in the path of a high-pressure flow can be a challenge. These difficulties of using an extensometer inside an autoclave led us to use an outside-autoclave displacement sensor which measures the displacement of pull-rod-specimen assembly. However, in our study (based on in-air fatigue test data), we found that a pull-rod-controlled based fatigue test can lead to substantial cyclic hardening/softening resulting in substantially different cyclic strain amplitudes and their rates compared to the desired cyclic strain amplitudes and its rates. In this paper, we propose an Artificial-Intelligence and Machine-Learning based technique such as using k-means clustering technique to improve the pull-rod-control based fatigue test method, such that the gage-area strain amplitude and rates can reasonably be achieved. In support of this, we present the fatigue test results for both 316 SS base and 81/182 dissimilar-metal-weld specimens.

42 ENGINEERING↗

THERMAL ANALYSIS AND DESIGN OF SELF-HEATING MOLDS USING LARGE-SCALE ADDITIVE MANUFACTURING FOR OUT-OF-AUTOCLAVE APPLICATIONS

Autoclave processing is a commonly used state-of-the-art fiber-reinforced composite manufacturing technology, albeit high capital cost, long cycle times and high energy consumption. Alternatively, out-of-autoclave processing reduces the initial and operating costs while producing composite structures with similar quality as that of autoclave parts. Additive Manufacturing (AM) the scaled-up molds for out-of-autoclave process using carbon fiber (CF) reinforced composite offers design flexibility, enhanced mechanical, and thermal properties in addition to reduction in weight and cost. However, heating of these molds using an oven is still expensive and necessitates an energy-efficient heating process. In this study, resistive heating through heating elements embedded within fiber reinforced composite molds is used as an efficient heating mechanism. The goal is to design wire embeddings and determine the optimal heat flux density to achieve a target uniform temperature of 1000C across the mold surface. To this end, numerical analyses were performed to evaluate the temperature distribution across the composite mold surface for a given wire placement and mold configuration. Constant thermal properties of the 20 wt.% short CF reinforced acrylonitrile butadiene styrene (ABS) were used in the thermal analysis. Time taken to reach the steady state temperature was also estimated. Design guidelines for wire embeddings were included to enable efficient manufacturing of fiber-reinforced composites through out-of-autoclave molds.

Pokkalla, Deepak↗

The 700 F properties of autoclave cured PMR-2 composites

Studies were conducted to develop autoclave processing parameters for graphite reinforced PMR-2 resin composite materials intended for use in applications at temperatures up to 371 degrees (700 F). The effect of resin composition on autoclaveability was investigated. The effect of various graphite fibers and resin composition on 343 C (650 F) and 371 C (700 F) thermo-oxidative stability and mechanical properties was also investigated. The results of the processing studies show that PMR-2 resin composites can be easily fabricated under autoclave conditions. Autoclaved laminates exposed to 1 atm of air at 343 C (650 F) and 371 C (700 F) exhibited less than 5 percent weight loss after 750 hr exposure to 650 F air and 8 percent weight loss during exposure to 700 F air for 500 hr. After 500 hr exposure, autoclaved laminates exhibited greater than 90 percent retention of initial 650 and 700 F flexural and interlaminar shear strengths. The effect of resin formulated molecular weight and postcure conditions on laminate glass transition temperature is also discussed.

Vannucci, Raymond D.↗

700 F properties of autoclave cured PMR-II composites

Studies were conducted to develop autoclave processing parameters for graphite reinforced PMR-2 resin composite materials intended for use in applications at temperatures up to 371 degrees (700 F). The effect of resin composition on autoclaveability was investigated. The effect of various graphite fibers and resin composition on 343 C (650 F) and 371 C (700 F) thermo-oxidative stability and mechanical properties was also investigated. The results of the processing studies show that PMR-2 resin composites can be easily fabricated under autoclave conditions. Autoclaved laminates exposed to 1 atm of air at 343 C (650 F) and 371 C (700 F) exhibited less than 5 percent weight loss after 750 hr exposure to 650 F air and 8 percent weight loss during exposure to 700 F air for 500 hr. After 500 hr exposure, autoclaved laminates exhibited greater than 90 percent retention of initial 650 and 700 F flexural and interlaminar shear strengths. The effect of resin formulated molecular weight and postcure conditions on laminate glass transition temperature is also discussed.

Cifani, Diane↗

ASRM test report: Autoclave cure process development

ASRM insulated segments will be autoclave cured following insulation pre-form installation and strip wind operations. Following competitive bidding, Aerojet ASRM Division (AAD) Purchase Order 100142 was awarded to American Fuel Cell and Coated Fabrics Company, Inc. (Amfuel), Magnolia, AR, for subcontracted insulation autoclave cure process development. Autoclave cure process development test requirements were included in Task 3 of TM05514, Manufacturing Process Development Specification for Integrated Insulation Characterization and Stripwind Process Development. The test objective was to establish autoclave cure process parameters for ASRM insulated segments. Six tasks were completed to: (1) evaluate cure parameters that control acceptable vulcanization of ASRM Kevlar-filled EPDM insulation material; (2) identify first and second order impact parameters on the autoclave cure process; and (3) evaluate insulation material flow-out characteristics to support pre-form configuration design.

Nachbar, D. L.↗

Face-Sheet Quality Analysis and Thermo-Physical Property Characterization of OOA and Autoclave Panels

Increased application of polymer matrix composite (PMC) materials in large vehicle structures requires consideration of non-autoclave manufacturing technology. The NASA Composites for Exploration project, and its predecessor, Lightweight Spacecraft Structures and Materials project, were tasked with the development of materials and manufacturing processes for structures that will perform in a heavy-lift-launch vehicle environment. Both autoclave and out of autoclave processable materials were considered. Large PMC structures envisioned for such a vehicle included the payload shroud and the interstage connector. In this study, composite sandwich panels representing 1/16th segments of the barrel section of the Ares V rocket fairing were prepared as 1.8 m x 2.4 m sections of the 10 m diameter arc segment. IM7/977-3 was used as the face-sheet prepreg of the autoclave processed panels and T40-800B/5320-1 for the out of autoclave panels. The core was 49.7 kilograms per square meters (3.1 pounds per cubic feet (pcf)) aluminum honeycomb. Face-sheets were fabricated by automated tape laying 153 mm wide unidirectional tape. This work details analysis of the manufactured panels where face-sheet quality was characterized by optical microscopy, cured ply thickness measurements, acid digestion, and thermal analysis.

Miller, Sandi G.↗

Face-Sheet Quality Analysis and Thermo-Physical Property Characterization of OOA and Autoclave Panels

Increased application of polymer matrix composite (PMC) materials in large vehicle structures requires consideration of non-autoclave manufacturing technology. The NASA Composites for Exploration project, and its predecessor, Lightweight Spacecraft Structures and Materials project, were tasked with the development of materials and manufacturing processes for structures that will perform in a heavy-lift-launch vehicle environment. Both autoclave and out of autoclave processable materials were considered. Large PMC structures envisioned for such a vehicle included the payload shroud and the interstage connector. In this study, composite sandwich panels representing 1/16th segments of the barrel section of the Ares V rocket fairing were prepared as 1.8 m x 2.4 m sections of the 10 m diameter arc segment. IM7/977-3 was used as the face-sheet prepreg of the autoclave processed panels and T40-800B/5320-1 for the out of autoclave panels. The core was 49.7 kg/sq m (3.1 lb/cu ft (pcf)) aluminum honeycomb. Face-sheets were fabricated by automated tape laying 153 mm wide unidirectional tape. This work details analysis of the manufactured panels where face-sheet quality was characterized by optical microscopy, cured ply thickness measurements, acid digestion, and thermal analysis.

Miller, Sandi G.↗

Optimization of the autoclave preparation process for improving resistant starch content in rice grains

Abstract The autoclave preparation process to increase the content of resistant starch (RS) in rice grains was optimized, and the results showed that the optimal preparation process was obtained with a water content of 41.63%, a pH of 5.95, an autoclave time of 60.96 min, and a refrigeration time of 17.11 hr. Under these conditions, the theoretical value of RS content in rice grains reached 17.57%. After autoclaving, the estimated glycemic index (EGI) in rice grains was reduced from 78.35 to 66.08 measured after cooking, suggesting that autoclaving was capable of increasing the RS content in rice grains and reducing its EGI value. These results may help spark new concepts and methods for the development of specialized foods for specific populations, such as people with diabetes.

Zheng, Yunzhan↗

Effect of autoclave heat treatments on the mechanical properties of the prealloyed powder cobalt-base alloy HS-31

The cobalt-base alloy HS-31 was atomized into powder and then consolidated by extrusion or by hot isostatic pressing (HIP) in an autoclave over a range of temperatures spanning the solidus, approximately 2340 F. Extrusions were subsequently autoclaved at the same conditions. Extrusions autoclaved at 2420 F had a life of 300 hours at 1200 F and 30 hours at 1800 F at stresses that result in a 10-hour life with cast HS-31. Superior stress rupture lives of autoclaved material are probably related to the solidification structure at the grain boundaries as well as to the increased grain size.

Freche, J. C.↗

Out-of-Autoclave Cure Composites

As the size of aerospace composite parts exceeds that of even the largest autoclaves, the development of new out-of-autoclave processes and materials is necessary to ensure quality and performance. Many out-of-autoclave prepreg systems can produce high-quality composites initially; however, due to long layup times, the resin advancement commonly causes high void content and variations in fiber volume. Applied Poleramic, Inc. (API), developed an aerospace-grade benzoxazine matrix composite prepreg material that offers more than a year out-time at ambient conditions and provides exceptionally low void content when out-of-autoclave cured. When compared with aerospace epoxy prepreg systems, API's innovation offers significant improvements in terms of out-time at ambient temperature and the corresponding tack retention. The carbon fiber composites developed with the optimized matrix technology have significantly better mechanical performance in terms of hot-wet retention and compression when compared with aerospace epoxy matrices. These composites also offer an excellent overall balance of properties. This matrix system imparts very low cure shrinkage, low coefficient of thermal expansion, and low density when compared with most aerospace epoxy prepreg materials.

Hayes, Brian S.↗

Re-establishment of Sandia National Labs super-critical carbon dioxide testing autoclave capability for exposure of metal alloys and polymers (Level 4 Milestone Report)

The sCO 2 system located in 916/160A, Sandia National Laboratories, CA, was constructed in 2014, for testing of materials in the presence of supercritical carbon dioxide (sCO 2 ) at high pressures (up to 3500 psi) and temperatures (up to 650°C). The basic design of the system consists of a thermally insulated IN625 autoclave, a high-pressure supercritical CO 2 compressor, autoclave heaters, temperature controllers, gas manifold, and temperature and pressure diagnostics. This system was modified in 2016 (sCO 2 compressor was removed) to enable corrosion studies with metal alloys in gaseous CO 2 at lower pressure (up to 300 psi) at 500°C. The capability was not used much afterwards until 2020, when preliminary tests using this capability (again without the supercritical CO 2 compressor) involved the exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours in gaseous CO 2 . Using this capability, we finished experiments with low pressure (450 psi/ 3 MPa), high temperature (650°C) exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours. The data from these experiments will be compared to that gathered from experiments performed in 2020 using the tube furnace and presented in a future report. It is to be noted that the tube furnace experiments ran 500-1500 hours, unlike the 168 hours of exposure in the recent experiment. This can help validate the use of the sCO 2 autoclave for both CO 2 and sCO 2 experiments.

36 MATERIALS SCIENCE↗