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The objective was to characterize several lots of materials used for carbon/carbon and carbon/phenol product manufacture. Volume one is organized into testing categories based on raw material of product form. Each category contains a discussion of the sampling plan, comments and observations on each test method utilized, and a summary of the results obtained each category.
Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR, The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected real-time, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in the selection of other appropriate analytical procedures for further material characterization.
Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR. The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected realtime, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in the selection of other appropriate analytical procedures for further material characterization.
Oak Ridge National Laboratory (ORNL) is leveraging decades of experience in neutron characterization of advanced materials together with resources such as the Spallation Neutron Source (SNS) and the High Flux Isotope Reactor (HFIR) shown in Fig. 1 to solve challenging problems in additive manufacturing (AM). Additive manufacturing, or three-dimensional (3-D) printing, is a rapidly maturing technology wherein components are built by selectively adding feedstock material at locations specified by a computer model. The majority of these technologies use thermally driven phase change mechanisms to convert the feedstock into functioning material. As the molten material cools and solidifies, the component is subjected to significant thermal gradients, generating significant internal stresses throughout the part (Fig. 2). As layers are added, inherent residual stresses cause warping and distortions that lead to geometrical differences between the final part and the original computer generated design. This effect also limits geometries that can be fabricated using AM, such as thin-walled, high-aspect- ratio, and overhanging structures. Distortion may be minimized by intelligent toolpath planning or strategic placement of support structures, but these approaches are not well understood and often "Edisonian" in nature. Residual stresses can also impact component performance during operation. For example, in a thermally cycled environment such as a high-pressure turbine engine, residual stresses can cause components to distort unpredictably. Different thermal treatments on as-fabricated AM components have been used to minimize residual stress, but components still retain a nonhomogeneous stress state and/or demonstrate a relaxation-derived geometric distortion. Industry, federal laboratory, and university collaboration is needed to address these challenges and enable the U.S. to compete in the global market. Work is currently being conducted on AM technologies at the ORNL Manufacturing Demonstration Facility (MDF) sponsored by the DOE's Advanced Manufacturing Office. The MDF is focusing on R&D of both metal and polymer AM pertaining to in-situ process monitoring and closed-loop controls; implementation of advanced materials in AM technologies; and demonstration, characterization, and optimization of next-generation technologies. ORNL is working directly with industry partners to leverage world-leading facilities in fields such as high performance computing, advanced materials characterization, and neutron sciences to solve fundamental challenges in advanced manufacturing. Specifically, MDF is leveraging two of the world's most advanced neutron facilities, the HFIR and SNS, to characterize additive manufactured components.
U-Zr metallic fuel is a promising fuel candidate for Gen Ⅳ fast spectrum reactors. Previous experimental irradiation campaigns showed that the sodium thermal bonded U-10Zr fuel design can achieve a burnup of 10% fissions per initial heavy metal atom (FIMA). Advanced metallic fuel designs are pushing the burnup limit to 20% or even 30% FIMA. To achieve the higher burnup and eliminate the pyrophoric sodium, a prototypical annular fuel has been designed, fabricated, clad with HT-9 in the Materials and Fuels Complex, and irradiated in the Advanced Test Reactors of Idaho National Laboratory (INL) to a peak burnup of 3.3% FIMA. During irradiation, the mechanical contact between fuel and cladding acts as a thermal bond. The irradiation lasted for 132 days in the reactor. Recently, the archived fresh and irradiated fuel samples were characterized using advanced characterization capabilities in the Irradiated Materials Characterization Laboratory (IMCL) of INL. This article summarizes the results of advanced characterization and computer vision-based materials informatics to reveal the irradiation effects on U-Zr metallic fuel. Future work will focus on further implementation of advanced characterization and statistical data mining to improve the fidelity of fuel performance modeling and support U-Zr metallic fuel qualification for fast spectrum reactors.
Leaky Lamb Wave (LLW) propagation in composite materials has been studied extensively since it was first observed in 1982. The wave is induced using a pitch-catch arrangement and the plate wave modes are detected by identifying minima in the reflected spectra to obtain the dispersion data.
The values of phase velocities of ultrasonic waves in transversely isotropic media are presented in terms of the fiber volume fraction of a unidirectional fiberglass epoxy composite with constant matrix properties and the ratio between extensional moduli in the longitudinal and transverse directions of the composite when the properties of the fibers are changed, at a constant fiber volume fraction. The model of a homogeneous transversely isotropic medium is adopted to describe the relations between elastic properties and velocities. The displacements due to an oscillatory point source in an infinite medium are used as one measure of comparison of the behavior of the unidirectional composite according to the variations of the parameters, as described above. Values of phase velocities, elastic moduli, Poisson's ratios and displacements due to a point source can be read from the parameterized plots for a known fiber volume fraction or a known ratio between extensional moduli of the composite. Alternatively fiber volume fraction and the ratio between extensional moduli can be inferred from the plots when the values of the phase velocities are known; for example from experimental measurements. Therefore, such parameterized curves may be useful in nondestructive mechanical property and material degradation characterizations.
Developments in fracture mechanics and elastic wave theory enhance the understanding of many physical phenomena in a mathematical context. Available literature in the material, and fracture characterization by NDT, and the related mathematical methods in mechanics that provide fundamental underlying principles for its interpretation and evaluation are reviewed. Information on the energy release mechanism of defects and the interaction of microstructures within the material is basic in the formulation of the mechanics problems that supply guidance for nondestructive evaluation (NDE).
The 1971 and 1973 Goldstone radar data on the Memnonia Fossae region of Mars is used as a test case for the characterization of surface materials. In addition to the discovery of greater relief in the radar-derived topographic measurements of this area than had been inferred from Mariner 9 estimates, and although a tendency for the radar measurements to break down over very rugged terrain has been observed, good correlation is found between radar topography and surface features. Photogeological mapping has identified six surface units which have distinctive radar properties that correlate well with surface features observed in the Viking Orbiter's 10 m/pixel resolution images
The composite materials proposed for use in the Advanced Communications Technology Satellite (ACTS) Program contains a new, high modulus graphite fiber as the reinforcement. A study was conducted to measure certain mechanical properties of the new fiber-reinforced material as well as of a composite-faced aluminum honeycomb sandwich structure. Properties were measured at -157, 22, and 121 C. Complete characterization of this material was not intended. Longitudinal tensile, picture-frame shear, short-beam shear, and flexural tests were performed on specimens of the composite face-sheet materials. Unidirectional, cross-plied, and quasi-isotropic fiber composite ply layup designs were fabricated and tested. These designs had been studied by using NASA's Integrated Composite Analyzer (ICAN) computer program. Flexural tests were conducted on (+/- 60/0 deg) sub s composite-faced sandwich structure material. Resistance strain gages were used to measure strains in the tensile, picture-frame, and sandwich flexural tests. The sandwich flexural strength was limited by the core strength at -157 and 22 C. The adhesive bond strength was the limiting factor at 121 C. Adhesive mechanical properties are reflected in sandwich structure flexural properties when the span-to-depth ratio is great enough to allow a significant shear effect on the load-deflection behavior of the sandwich beam. Most measured properties agreed satisfactorily with the properties predicted by ICAN.
The composite materials proposed for use in the Advanced Communications Technology Satellite (ACTS) program contains a new, high modulus graphite fiber as the reinforcement. A study was conducted to measure certain mechanical properties of the new fiber-reinforced material as well as of a composite-faced aluminum honeycomb sandwich structure. Properties were measured at -157, 22, and 121 C. Complete characterization of this material was not intended. Longitudinal tensile, picture-frame shear, short-beam shear, and flexural tests were performed on specimens of the composite face-sheet materials. Unidirectional, cross-plied, and quasi-isotropic fiber composite ply layup designs were fabricated and tested. These designs had been studied by using NASA's Integrated Composite Analyzer (ICAN) computer program. Flexural tests were conducted on (+/- 60/0 deg) sub s composite-faced sandwich structure material. Resistance strain gages were used to measure strains in the tensile, picture-frame, and sandwich flexural tests. The sandwich flexural strength was limited by the core strength at 157 and 22 c. The adhesive bond strength was the limiting factor at 121 C. Adhesive mechanical properties are reflected in sandwich structure flexural properties when the span-to-depth ratio is great enough to allow a significant shear effect on the load-deflection behavior of the sandwich beam. Most measured properties agreed satisfactorily with the properties predicted by ICAN.
A significant portion of Layered Pressure Vessels (LPVs) manufactured for NASA in the 1950s and ’60s are of non-code construction. These vessels were constructed to the standards of individual manufacturers rather than an industry or consensus standard and often contain legacy or proprietary materials, which have poor or no characterization. Obtaining correct material properties is the first step in assuring vessel safety and predicting life and critical failure modes before they happen. This report details the efforts of the LPV Project related to material properties and characterization. The goal in testing materials from deconstructed vessels was to provide material characterization utilizing modern test methods that would give a strong probabilistic base as an option for future analysis. ASTM E1820, Standard Test Method for Measurement of Fracture Toughness was used for fracture toughness; ASTM E1921, Standard Test Method for Determination of Reference Temperature, T0, for Ferritic Steels in the Transition Range for transition temperature; and ASTM E647, Standard Test Method for Measurement of Fatigue Crack Growth Rates for fatigue crack growth. Particular focus was placed on determination of transition temperature through evaluation of the T0 reference temperature in accordance with ASTM E1921. Transition temperature testing allows for a probabilistic analysis of vessel materials that may be operating at temperatures below the transition from ductile tearing to brittle cleavage failure. This test method was not available at the time of construction and has proved invaluable to the characterization of older ferritic steels. The values reported are specific to the largest body of materials found in the current NASA fleet, but do not claim to be all inclusive. As demonstrated in this report, some materials contain extreme lot-to-lot variability. In some cases, this can be comfortably bounded by worst case probabilistic methods, however it is always recommended that vessel specific data be collected in as much depth as possible to ensure correct assumptions and avoid unduly restricting vessel usage.
In this review paper different methods and techniques for representing fiber orientation in advanced polymer matrix composites are presented. A description of the effect of fiber orientation on processing, fabrication and mechanical properties of a composite material is presented. The paper discusses the mathematical modeling and modeling techniques for fiber structure representation in polymeric composites, with an emphasis on fiber orientation in a composite part. The paper is divided into two sections; namely—destructive techniques and non-destructive techniques. The capabilities and limitations of each technique with respect to fiber orientation detection and measurements are discussed.
Full-field, quantitative visualization techniques, such as digital image correlation (DIC), have unlocked vast opportunities for experimental mechanics. However, DIC has traditionally been a surface measurement technique, and has not been extended to perform measurements on the interior of specimens for dynamic, full-scale laboratory experiments. This limitation restricts the scope of physics which can be investigated through DIC measurements, especially in the context of heterogeneous materials. The focus of this study is to develop a method for performing internal DIC measurements in dynamic experiments. The aim is to demonstrate its feasibility and accuracy across a range of stresses (up to 650 MPa), strain rates (10 3 - 10 6 s -1 ), and high-strain rate loading conditions (e.g., ramped and shock wave loading). Internal DIC is developed based on the concept of applying a speckle pattern at an inner-plane of a transparent specimen. The high-speed imaging configuration is coupled to the traditional dynamic experimental setups, and is focused on the internal speckle pattern. During the experiment, while the sample deforms dynamically, in-plane, two-dimensional deformations are measured via correlation of the internal speckle pattern. In this study, the viability and accuracy of the internal DIC technique is demonstrated for split-Hopkinson (Kolsky) pressure bar (SHPB) and plate impact experiments. The internal DIC experimental technique is successfully demonstrated in both the SHPB and plate impact experiments. In the SHPB setting, the accuracy of the technique is excellent throughout the deformation regime, with measurement noise of approximately 0.2% strain. In the case of plate impact experiments, the technique performs well, with error and measurement noise of 1% strain. The internal DIC technique has been developed and demonstrated to work well for full-scale dynamic high-strain rate and shock laboratory experiments, and the accuracy is quantified. Here, the technique can aid in investigating the physics and mechanics of the dynamic behavior of materials, including local deformation fields around dynamically loaded material heterogeneities.
This study reports the first use of in-situ synchrotron X-ray diffraction (SXRD) to study the effects of ultrasonic melt processing (USMP) on phase and grain size evolution during solidification in a commercial Al–Si–Mg casting alloy. USMP is a technique that, when applied to aluminum as it solidifies, can be used to refine the local microstructure of large-scale castings. Analysis of the in-situ SXRD data to estimate the average grain size of primary α-Al grains during USMP demonstrates that USMP slows the growth rate of α-Al grains and reduces grain size by 36 pct. Furthermore, there is also evidence that USMP causes the primary α-Al grains to move relative to the X-ray beam; such motion increases the probability of primary α-Al grains colliding and fragmenting. This movement becomes constrained at the onset of the Al–Si binary eutectic, suggesting that USMP ceases to effectively refine the microstructure once the Al–Si binary eutectic begins to form. Complementary laboratory-scale X-ray diffraction (XRD) data were used to correlate the lattice parameters of the α-Al and Si (D-A4) phases with temperature to estimate cooling rate during solidification. Thus, this study can guide the design of novel castings with spatially distributed fine-grained regions produced using local ultrasonic processing.
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Increasing the grain size is a potential strategy to reduce grain-boundary recombination and improve performance of thin-film solar cells. Here, CdTe thin films with a range of grain sized were produced by varying the CdC1 2 post-deposition treatment temperature. We use high-resolution cathodoluminescence (CL) microscopy to study recombination and shallow defect levels in detail. Intensities from room temperature CL maps were compared across samples. We find that the CL intensity initially increases with grain size, as expected, but then plateaus as the grain size is increased further. The plateau is correlated with a decrease in the characteristic length-related to the carrier diffusion length-determined from CL intensity profiles near grain boundaries. In addition, low-temperature CL measurements demonstrate the evolution of the defect levels with CdC1 2 temperature.
The relative intensities of XPS core levels, scaled by their photoionization cross sections, are regularly used to determine sample atomic composition. Cross sections, however, give the intensity to all possible final states for the core ionizations, not just to the main peak. This includes all intrinsic satellite structure (shake states and, for open shell systems, the different ionic multiplets). In practice, for solids, this is usually experimentally impossible to determine accurately because such a satellite structure sits on the inelastically scattered electron background and cannot be easily separated. Therefore, usually, only the intensity of the main peak is used. This limits the ultimate possible accuracy of XPS composition determination. The purpose of the present paper is to examine the contributions that a theoretical analysis of losses of intensity can make to improve quantitation. For an MgO single crystal, we show that the correct stoichiometry of 1:1 can be recovered using the theoretical analysis of the experimental MgO peak ratio intensities. For materials with a sufficient bandgap for the XPS main peaks to be separated from the scattered background, the intensity of main peaks can often be accurately determined. Thus, if one uses theory to calculate that fraction of the total intensity lost from a main peak into all its satellite structure, the intensity of just main peaks could then be used to more accurately determine relative atom % composition. This work tests this approach using a single crystal MgO (50% Mg, 50% O) standard. Ab initio electronic structure theory of representative MgO clusters is used to determine Hartree–Fock wave functions for the ground state and final ionized states corresponding to the main Mg 2p and O1s XPS peaks of the oxide. The sudden approximation, SA, is used to determine the fractional losses from these main peaks to shake satellites, which is found to be greater for O1s than Mg2p. This results in predicted “apparent composition” for stoichiometric MgO of 55.2% Mg, 44.8% O instead of the true 50% Mg, 50% O. Equivalent theory for CaO results in a predicted apparent Ca value of 53.4%. Experimentally, using Mg2s or 2p intensity ratio to O1s, we find values between 52.2% and 56.0% Mg using two crystals and four different instrument electron pass energies. The average value of the measurements is 54.5% Mg when corrected for the presence of an adventitious carbon overlayer and slight surface hydroxide. Though this agreement with theory may be somewhat fortuitous, given the potential experimental errors, which are fully discussed, it is similar to that in our earlier study on LiF. We also present preliminary experimental data on Mg(OH) 2 and MgSO 4 , which show a similar trend of apparently higher than 50% Mg, but we have no theory values. We are not yet able to experimentally test for validation of the difference between apparent composition for MgO (55.2% Mg) and CaO (53.4% Ca), owing to significant carbonate formation at the surface of the single crystal CaO. Here, an important conclusion is that the theoretical determination of shake losses, obtained with ab initio wavefunctions and the SA, is likely to be a useful way to calibrate the accuracy and reliability of compositions obtained from XPS intensities and merits further study.