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Composite Technology for Exploration (CTE) Project: Infusing Bonded Joint Technology into Space Launch System Block 1b Flight Structures
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Microcracking of Materials for Space
The effect of thermal-cycling-induced microcracking in fiber-reinforced polymer matrix composites is studied. Specific attention is focused on microcrack density as a function of the number of thermal cycles, and the effect of microcracking on the dimensional stability of composite materials. Changes in laminate coefficient of thermal expansion (CTE) and laminate stiffness are of primary concern. Included in the study are materials containing four different Thornel fiber types: a PAN-based T50 fiber and three pitch-based fibers, P55, P75, and P120. The fiber stiffnesses range from 55 Msi to 120 Msi. The fiber CTE's range from -0.50 x 1O(exp -6)/degrees F to -0.80 x 10(exp -6)/degrees F. Also included are three matrix types: Fiberite's 934 epoxy, Amoco's ERL1962 toughened epoxy, and YLA's RS3 cyanate ester. The lamination sequences of the materials considered include a cross-ply configuration, [0/90](sub 2s), and two quasi-isotropic configurations, [0/+45/-45/90](sub s), and [0/+45/90/-45](sub s). The layer thickness of the materials range from a nominal 0.001 in. to 0.005 in. In addition to the variety of materials considered, three different thermal cycling temperature ranges are considered. These temperature ranges are +/-250 degrees F, +/-l5O degrees F, and +/-50 degrees F. The combination of these material and geometric parameters and temperature ranges, combined with thermal cycling to thousands of cycles, makes this one of the most comprehensive studies of thermal-cycling-induced microcracking to date. Experimental comparisons are presented by examining the effect of layer thickness, fiber type, matrix type, and thermal cycling temperature range on microcracking and its influence on the laminates. Results regarding layer thickness effects indicate that thin-layer laminates microcrack more severely than identical laminates with thick layers. For some specimens in this study, the number of microcracks in thin-layer specimens exceeds that in thick-layer specimens by more than a factor of two. Despite the higher number of microcracks in the thin-layer specimens, small changes in CTE after thousands of cycles indicate that the thin-layer specimens are relatively unaffected by the presence of these cracks compared to the thick-layer specimens. Results regarding fiber type indicate that the number of microcracks and the change in CTE after thousands of cycles in the specimens containing PAN-based fibers are less than in the specimens containing comparable stiffness pitch-based fibers. Results for specimens containing the different pitch-based fibers indicate that after thousands of cycles, the number of microcracks in the specimens does not depend on the modulus or CTE of the fiber. The change in laminate CTE does, however, depend highly on the stiffness and CTE of the fiber. Fibers with higher stiffness and more negative CTE exhibit the lowest change in laminate CTE as a result of thermal cycling. The overall CTE of these specimens is, however, more negative as a result of the more negative CTE of the fiber. Results regarding matrix type based on the +/-250 degree F temperature range indicate that the RS3 cyanate ester resin system exhibits the greatest resistance to microcracking and the least change in CTE, particularly for cycles numbering 3000 and less. Extrapolations to higher numbers of cycles indicate, however, that the margin of increased performance is expected to decrease with additional thermal cycling. Results regarding thermal cycling temperature range depend on the matrix type considered and the layer thickness of the specimens. For the ERL1962 resin system, microcrack saturation is expected to occur in all specimens, regardless of the temperature range to which the specimens are exposed. By contrast, the RS3 resin system demonstrates a threshold effect such that cycled to less severe temperature ranges, microcracking does not occur. For the RS3 specimens with 0.005 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between +/-150 degree F or +/- 50 degree F. For the RS3 specimens with 0.002 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between +/-50 degree F. Results regarding laminate stiffness indicate negligible change in laminate stiffness due to thermal cycling for the materials and geometries considered in this investigation. The study includes X-ray examination of the specimens, showing that cracks observed at the edge of the specimens penetrate the entire width of the specimen. Glass transition temperatures of the specimens are measured, showing that resin chemistry is not altered as a result of thermal cycling. Results are also presented based on a one-dimensional shear lag analysis developed in the literature. The analysis requires material property information that is difficult to obtain experimentally. Using limited data from the present investigation, material properties associated with the analysis are modified to obtain reasonable agreement with measured microcrack densities. Based on these derived material properties, the analysis generally overpredicts the change in laminate CTE. Predicted changes in laminate stiffness show reasonable correlation with experimentally measured values.
Composite Laminate With Coefficient of Thermal Expansion Matching D263 Glass
The International X-ray Observatory project seeks to make an X-ray telescope assembly with 14,000 flexible glass segments. The glass used is commercially available SCHOTT D263 glass. Thermal expansion causes the mirror to distort out of alignment. A housing material is needed that has a matching coefficient of thermal expansion (CTE) so that when temperatures change in the X-ray mirror assembly, the glass and housing pieces expand equally, thus reducing or eliminating distortion. Desirable characteristics of this material include a high stiffness/weight ratio, and low density. Some metal alloys show promise in matching the CTE of D263 glass, but their density is high compared to aluminum, and their stiffness/weight ratio is not favorable. A laminate made from carbon fiber reinforced plastic (CFRP) should provide more favorable characteristics, but there has not been any made with the CTE matching D263 Glass. It is common to create CFRP laminates of various CTEs by stacking layers of prepreg material at various angles. However, the CTE of D263 glass is 6.3 ppm/ C at 20 C, which is quite high, and actually unachievable solely with carbon fiber and resin. A composite laminate has been developed that has a coefficient of thermal expansion identical to that of SCHOTT D263 glass. The laminate is made of a combination of T300 carbon fiber, Eglass, and RS3C resin. The laminate has 50% uni-T300 plies and 50% uni-E-glass plies, with each fiber-layer type laid up in a quasi-isotropic laminate for a total of 16 plies. The fiber volume (percent of fiber compared to the resin) controls the CTE to a great extent. Tests have confirmed that a fiber volume around 48% gives a CTE of 6.3 ppm/ C. This is a fairly simple composite laminate, following well established industry procedures. The unique feature of this laminate is a somewhat unusual combination of carbon fiber with E-glass (fiberglass). The advantage is that the resulting CTE comes out to 6.3 ppm/ C at 20 C, which matches D263 glass. The trick with this laminate is to establish the proper fiber volume to get the desired CTE. Laminates were made with several different fiber volumes and coupons were tested to establish the relationship between fiber volume and CTE. Testing proved that fiber volume should be about 48%.
Sensitivity of the coefficients of thermal expansion of selected graphite reinforced composite laminates to lamina thermoelastic properties
An analytical study of the sensitivity of the laminate coefficient of thermal expansion, CTE, to changes in lamina elastic properties has been made. High modulus graphite/epoxy (P75/934, P100/934, P120/934), graphite/aluminum (P100/Al), and graphite/glass (HMS/Gl) composite materials were considered in quasi-isotropic, low thermal stress, and 'near-zero' thermal expansion laminate configurations. The effects of a positive or negative 10 percent change in lamina properties on laminate CTE is strongly dependent upon both the composite material and the laminate configuration. A 10 percent change in all of the lamina properties had very little effect on the laminate CTE of the HMS/Gl composite laminates investigated. The sensitivity and direction of change in the laminate CTE of Gr/934 depended very strongly on the fiber properties. A 10 percent change in the lamina transverse CTE resulted in changes as large as 0.216 ppm/C in the laminate CTE of a quasi-isotropic Gr/934 laminate. No significant difference was observed in the sensitivity of the laminate CTE of the P100/934 and P120/934 composite materials due to changes in lamina properties. Large changes in laminate CTE can result from measured temperature and radiation effects on lamina properties.
Increasing the Thermal Stability of Aluminum Titanate for Solid Oxide Fuel Cell Anodes
Solid-oxide fuel cells (SOFCs) show great potential as a power source for future space exploration missions. Because SOFCs operate at temperatures significantly higher than other types of fuel cells, they can reach overall efficiencies of up to 60% and are able to utilize fossil fuels. The SOFC team at GRC is leading NASA's effort to develop a solid oxide fuel cell with a power density high enough to be used for aeronautics and space applications, which is approximately ten times higher than ground transport targets. layers must be able to operate as a single unit at temperatures upwards of 900'C for at least 40,000 hours with less than ten percent degradation. One key challenge to meeting this goal arises from the thermal expansion mismatch between different layers. The amount a material expands upon heating is expressed by its coefficient of thermal expansion (CTE). If the CTEs of adjacent layers are substantially different, thermal stresses will arise during the cell's fabrication and operation. These stresses, accompanied by thermal cycling, can fracture and destroy the cell. While this is not an issue at the electrolyte-cathode interface, it is a major concern at the electrolyte-anode interface, especially in high power anode-supported systems. electrolyte are nearly identical. Conventionally, this has been accomplished by varying the composition of the anode to match the CTE of the yittria-stabilized zirconia (YSZ) electrolyte (approx.10.8x10(exp -6/degC). A Ni/YSZ composite is typically used as a base material for the anode due to its excellent electrochemical properties, but its CTE is about 13.4x10(exp -6/degC). One potential way to lower the CTE of this anode is to add a small percentage of polycrystalline Al2TiO5, with a CTE of 0.68x10(exp -6/degC, to the Ni/YSZ base. However, Al2TiO5 is thermally unstable and loses its effectiveness as it decomposes to Al2O3 and TiO2 between 750 C and 1280 C. be used as additives to increase the thermal stability of Al2TiO5 in SOFC operating conditions without adversely affecting the electrochemical properties of the SOFC anode. Three candidate materials were chosen through an extensive literature review: MgO, Fe2O3, and ZrTiO4. Although all three have been shown to prevent Al2TiO5 decomposition under various conditions, their effectiveness in the temperature range and atmosphere of the SOFC has not yet been evaluated. Several batches of Al2TiO5 with varying amounts of additives were prepared, exposed to reducing and oxidizing atmospheres at elevated temperatures, and the resulting decomposition of Al2TiO5 was measured. The most promising additives were further evaluated with the goal of ultimately preparing low CTE anodes that are chemically compatible to current systems. Adding minor constituents to stabilize Al2TiO5 could ultimately preserve its low CTE for the life of the fuel cell and improve the cell's long-term performance without a drop in anode conductivity. Further, these low CTE filler additions could allow the use of new sulfur tolerant anode materials, improving the viability of SOFCs for future aeronautics and space applications. Every SOFC consists of a cathode and an anode separated by an electrolyte, These three One way to avoid this problem is to design the cell such that the CTEs of the anode and The objective of this summer research project was to evaluate several materials that could
Space structures concepts and materials
An extension is preseted of the evaluation of graphite/aluminum metal matrix composites (MMC) for space structures application. A tubular DWG graphite/aluminum truss assembly was fabricated having the structural integrity and thermal stability needed for space application. DWG is a proprietary thin ply continuous graphite reinforced aluminum composite. The truss end fittings were constructed using the discontinuous ceramic particulate reinforced MMC DWAl 20 (trademark). Thermal stability was incorporated in the truss by utilizing high stiffness, negative coefficient of thermal expansion (CTE) P100 graphite fibers in a 6061 aluminum matrix, crossplied to provide minimized CTE in the assembled truss. Tube CTE was designed to be slightly negative to offset the effects of the end fitting and sleeve, CTE values of which are approx. 1/2 that of aluminum. In the design of the truss configuration, the CTE contribution of each component was evaluated to establish the component dimension and layup configuration required to provide a net zero CTE in the subassemblies which would then translate to a zero CTE for the entire truss bay produced.
Electrode Elastic Modulus as the Dominant Factor in the Capping Effect in Ferroelectric Hafnium Zirconium Oxide Thin Films
The discovery of ferroelectricity in hafnia based thin films has catalyzed significant research focused on understanding the ferroelectric property origins and means to increase stability of the ferroelectric phase. Prior studies have revealed that biaxial tensile stress via an electrode “capping effect” is a suspected ferroelectric phase stabilization mechanism. This effect is commonly reported to stem from a coefficient of thermal expansion (CTE) incongruency between the hafnia and top electrode. Despite reported correlations between ferroelectric phase fraction and electrode CTE, the thick silicon substrate dominates the mechanics and CTE-related stresses, negating any dominant contribution from an electrode CTE mismatch toward the capping effect. In this work, these discrepancies are reconciled, and the origin of these differences deriving from electrode elastic modulus, not CTE, is demonstrated. Pt/M/TaN/Hf 0.5 Zr 0.5 O 2 /TaN/Si devices, where M is platinum, TaN, iridium, tungsten, and ruthenium, were fabricated. Sin 2 (ψ)-based X-ray diffraction measurements of biaxial stress in the HZO layer reveal a strong correlation between biaxial stress, remanent polarization, and electrode elastic modulus. Conversely, a low correlation exists between the electrode CTE, HZO biaxial stress, and remanent polarization. A higher elastic modulus enhances the resistance to electrode elastic deformation, which intensifies the capping effect during crystallization, and culminates in the tandem restriction of out-of-plane hafnia volume expansion and preferential orientation of the polar c-axis normal to the plane. These behaviors concomitantly increase the ferroelectric phase stability and polarization magnitude. This work provides electrode material selection guidelines toward the development of high-performing ferroelectric hafnia into microelectronic devices, such as nonvolatile memories.
Effects of changes in composite lamina properties on laminate coefficient of thermal expansion
An analytical study of the effects of changes in composite lamina properties on the laminate coefficient of thermal expansion, CTE, has been made. Low modulus graphite/epoxy (T300/934) and high modulus graphite/epoxy (P75/934, P100/934, P120/934), graphite/aluminum (P100/Al), and graphite/glass (HMS/Gl) composite materials were considered in quasi-isotropic and near-zero CTE laminate configurations. The effects of changes in lamina properties on the laminate CTE strongly depend upon the type of composite material as well as the laminate configuration. A 10 percent change in the lamina transverse CTE resulted in changes as large as 0.22 ppm/C in the laminate CTE of a quasi-isotropic Gr/934 laminates. No significant differences were observed in the sensitivities of the laminate CTEs of the P100/934 and P120/934 composite materials due to identical changes in lamina properties. Large changes in laminate CTE can also result from measured temperature and radiation effects on lamina properties.
CALPHAD-based Bayesian optimization to accelerate alloy discovery for high-temperature applications
Two crucial properties influencing the performance of high-temperature alloys are coefficient of thermal expansion (CTE) and phase constitution. It is desirable to have alloys with low CTE, which reduces CTE mismatch with the surface oxide and the likelihood of oxide spallation. Reducing the amount of brittle intermetallic phases such as Sigma (σ) enhances alloy ductility and processability. Here, we propose a multi-objective Bayesian Optimization (BO) model to simultaneously minimize CTE (at an operational temperature of 1150 °C) and T σ (temperature when the Sigma phase completely dissolves in the metal matrix), properties which are obtained from high-throughput CALculation of PHAse Diagrams (CALPHAD). The model successfully identifies several alloys with CTE ≤ 2 × 10 –5 /K and T σ ≤ 500 °C by exploring just 7% of the nickel–chromium–cobalt–aluminum–iron (Ni–Cr–Co–Al–Fe) composition space. Such multi-objective alloy design frameworks can be used to inform additive manufacturing experiments and accelerate alloy discovery for high-temperature energy applications.
Special report, cross calibration of JHU test equipment with GSFC vacuum optical bench
Tests were conducted to confirm the validity of the absolute calibrations which have been performed with the Apollo 17 ultraviolet spectrometer (UVS) in the calibration test equipment (CTE) which were constructed for that purpose. To accomplish this the prototype UV spectrometer SN/01 was retrofitted to be substantially identical to the qualification unit and to the two flight units. It was renamed the cross calibration unit (CCU). The instrument was first calibrated in the JHU calibration test equipment (CTE), then installed in the vacuum optical bench (VOB) at Goddard Space Flight Center and calibrated. The following day a second CTE calibration was conducted which provided substantially the same calibration values as were obtained on the first CTE calibration, and showed remarkably close agreement with the VOB calibration values at two of the wavelengths which were studied. The VOB results at the third wavelength (1216 A) indicate the CTE calibration at 1216 A is 15% too low. This apparent discrepancy is discussed and presents a very important result of the cross calibration effort.
The effect of bromination of carbon fibers on the coefficient of thermal expansion of graphite fiber-epoxy composites
To examine the effect of bromination of carbon fibers on the coefficient of thermal expansion (CTE) of carbon fiber epoxy composites, several pristine and brominated carbon fiber-epoxy composite samples were subjected to thermomechanical analysis. The CTE's of these samples were measured in the uniaxial and transverse directions. The CTE was dominated by the fibers in the uniaxial direction, while it was dominated by the matrix in the transverse directions. Bromination had no effect on the CTE of any of the composites. In addition, the CTE of fiber tow was measured in the absence of a polymer matrix, using an extension probe. The results from this technique were inconclusive.
Thermal Cycling of Thin and Thick Ply Composites
An experimental study was conducted to determine the effects of ply thickness in composite laminates on thermally induced cracking and changes in the coefficient of thermal expansion (CTE). After a few thermal cycles, laminates with thick-plies cracked, resulting in large changes in CTE. CTE's of the thin-ply laminates were unaffected by microcracking during the first 500 thermal cycles, whereas, the CTE's of the thick-ply laminates changed significantly. After about 1500 cycles, microdamage had also reduced the CTE of the thin-ply laminates to a value of about half of their initial value.
Thermal Protection Supplement for Reducing Interface Thermal Mismatch
A thermal protection system that reduces a mismatch of thermal expansion coefficients CTE between a first material layer (CTE1) and a second material layer (CTE2) at a first layer-second layer interface. A portion of aluminum borosilicate (abs) or another suitable additive (add), whose CTE value, CTE(add), satisfies (CTE(add)-CTE1)(CTE(add)-CTE2)<0, is distributed with variable additive density,.rho.(z;add), in the first material layer and/or in the second material layer, with.rho.(z;add) near the materials interface being relatively high (alternatively, relatively low) and.rho.(z;add) in a region spaced apart from the interface being relatively low (alternatively, relatively high).
Modeling the Extremely Lightweight Zerodur Mirror (ELZM) Thermal Soak Test
Exoplanet science requires extreme wavefront stability (10 pm change/10 minutes), so every source of wavefront error (WFE) must be characterized in detail. This work illustrates the testing and characterization process that will be used to determine how much surface figure error (SFE) is produced by mirror substrate materials' CTE distributions. Schott's extremely lightweight Zerodur mirror (ELZM) was polished to a sphere, mounted, and tested at Marshall Space Flight Center (MSFC) in the X-Ray and Cryogenic Test Facility (XRCF). The test transitioned the mirror's temperature from an isothermal state at 292K to isothermal states at 275K, 250K and 230K to isolate the effects of the mirror's CTE distribution. The SFE was measured interferometrically at each temperature state and finite element analysis (FEA) has been completed to assess the predictability of the change in the mirror's surface due to a change in the mirror's temperature. The coefficient of thermal expansion (CTE) distribution in the ELZM is unknown, so the analysis has been correlated to the test data. The correlation process requires finding the sensitivity of SFE to a given CTE distribution in the mirror. A novel hand calculation is proposed to use these sensitivities to estimate thermally induced SFE. The correlation process was successful and is documented in this paper. The CTE map that produces the measured SFE is in line with the measured data of typical boules of Schott's Zerodur glass.
Quantitative measurement of pebble fuel anisotropy using generalized ellipsometry
The renewed development of high-temperature gas-cooled reactors has created a need to modernize pebble fuel quality control methods. One important specification in these methods is the coefficient of thermal expansion (CTE) anisotropy, which reflects graphite grain alignment and affects fuel performance. This study investigates the feasibility of using two-modulator generalized ellipsometry microscopy (2-MGEM) as a potential surrogate metric for CTE anisotropy. Graphite matrix compacts with controlled levels of anisotropy were fabricated by varying pre-pressures during forming and were subsequently characterized using both optical dilatometry and 2-MGEM. Measured responses were compared to an isotropic reference pebble produced using an industrial manufacturing process to provide a practical baseline. The resulting measurements revealed a strong quantitative correlation between the CTE anisotropy ratio and the corresponding diattenuation ratio. However, propagated measurement uncertainties in the optical method were found to limit definitive pass/fail discrimination, highlighting the need for improved precision before qualification as a quality control tool. Still, the results establish a quantitative relationship between optical and CTE anisotropy and support further development of 2-MGEM as a potential surrogate method for evaluating graphite matrix anisotropy in pebble fuel manufacturing.
Space environmental effects: Construction and utilization of a system to measure low thermal strain in one meter graphite epoxy tubes
A system for measuring the expansion of low coefficient of thermal expansion (CTE) materials was constructed around a H.P. 5526-A laser measuring system. The vacuum CTE measurements in the -150 F to +120 F range were made over a 6 month period on a graphite epoxy tube yielding CTE values of 2.5 to one fifty-millionth/F above ambient and 2 + or - one ten-millionth F below ambient temperature. To assure that the below ambient, approximately 10 microns high open loop nature of the delta L/L vs. T curves was not apparatus related, similar size quartz tubes (A and B) were checked and found to have only a 2 micron (negligable for quartz) open loop component. These two quartz tubes, A and B, had ambient CTE values 20% and 45% respectively higher than the average handbook value. The overnight microcreep diminished an order of magnitude during the first several cycles after the system had been reopened.
Thermally stable deployable structure
A deployable structure which meets stringent thermal and strength requirements in a space environment was developed. A mast with a very low coefficient of thermal expansion (CTE) was required to limit the movement from thermal distortion over the temperature range of -200 C to 80 C to .064 cm (.025 in). In addition, a high bending strength over the temperature range and weight less than 18.1 kg (40 lbs) was needed. To meet all of the requirements, a composite, near-zero CTE structure was developed. The measured average CTE over the temperature range for the mast was .70 x .000001/C (.38 x .000001/F). The design also has the advantage of being adjustable to attain other specific CTE if desired.