R&D for Safety Codes and Standards: Materials and Components Compatibility.
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The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å –1 , together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, the validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.
The Lawrence Livermore National Laboratory – Center for Accelerator Mass Spectrometry compact 1 MV biomedical accelerator mass spectrometer was repurposed and optimized for the semi-automated radiocarbon measurement of natural abundance environmental samples. Here we present results from 15 months of routine system operation and evaluate the system performance based on 30 sample wheels measured with consistent operating conditions over 7 months from August 2019 to March 2020. Additionally, the average measurement precision was 2.7 ± 0.7‰. System accuracy was assessed with measurements of 14 C-free materials, standard materials with 14 C-content spanning 0.5 to 1.5 F 14 C, and by comparison to split samples measured with the 10 MV AMS system. Overall, this system can routinely measure samples as small as 300 µgC and less than 33000 years without the need for size-specific correction protocols.
Carbon/phenolic composites are used extensively as ablative insulating materials in the nozzle region of solid rocket motors. The current solid rocket motor (RSRM) on the space shuttle is fabricated from woven rayon cloth which is carbonized and then impregnated with the phenolic resin. These plies are layed up in the desired configuration and cured to form the finished part. During firing, the surface of the carbon/phenolic insulation is exposed to 5000 F gases from the rocket exhaust. The resin pyrolizes and the material chars to a depth which progresses with time. The rate of charring and erosion are generally predictable, and the insulation depth is designed to allow adequate safety margins over the firing time of the motor. However, anomalies in the properties and response of the carbon/phenolic materials can lead to severe material damage which may decrease safety margins to unacceptable levels. Three macro damage modes which were observed in fired nozzles are: ply lift, 'wedge out', and pocketing erosion. Ply lift occurs in materials with plies oriented nearly parallel to the surface. The damage occurs in a region below the charred material where material temperatures are relatively low - about 500 F. Wedge out occurs at the intersection of nozzle components whose plies are oriented at about 45 deg. The corner of the block of material breaks off along a ply interface. Pocketing erosion occurs in material with plies oriented normal to the surface. Thermal expansion is restrained in two directions resulting in large tensile strains and material failure normal to the surface. When a large section of material is removed as a result of damage, the insulation thickness is reduced which may lead to failure of the nozzle due to excessive heating of critical components. If these damage events cannot be prevented with certainty, the designer must increase the thickness of the insulator thus adding to both weight and cost. One of the difficulties in developing a full understanding of these macro damage mechanisms is that the loading environment and the material response to that environment are extremely complex. These types of damage are usually only observed in actual motor firings. Therefore, it is difficult and expensive to evaluate the reliability of new materials. Standard material tests which measure mechanical and thermal properties of test specimens can only provide a partial picture of how the material will respond in the service environment. The development of the ANALOG test procedure which can combine high heating rates and mechanical loads on a specimen will improve the understanding of the interactive effects of the various loads on the system. But a mechanistic model of material response which can account for the heterogeneity of the material, the progression of various micromechanical damage mechanisms, and the interaction of mechanical and thermal stresses on the material is required to accurately correlate material tests with response to service environments. A model based on fundamental damage mechanisms which is calibrated and verified under a variety of loading conditions will provide a general tool for predicting the response of rocket nozzles. The development of a micromechanical simulation technique was initiated and demonstrated to be effective for studying across-ply tensile failure of carbon/phenolic composites.
Standard wool fabric is investigated as a potential reference material. A screening test method for relative toxicity exposes four albino male rats enclosed in a 4.2 liter hemispherical chamber to pyrolysis effluents produced by pyrolyzing a 1.00 g sample under a variety of test conditions (200-800 C with a 40 C/min heating rate). It is found that for fabrics containing 86-100% wool, animal response remains virtually unchanged, although a 100% wool fabric is preferred as it eliminates local composition differences as a source of variation.
The importance of data curation has been recognized in multiple areas of research; however, the discussion of this important issue is only beginning to emerge in materials science. In this Perspective, we highlight the benefits of using the standardized data curation protocols in materials science and discuss current gaps in accurate and reproducible data reporting using case studies drawn from high-impact materials science papers and well-known databases such as the Crystallography Open Database (COD) and the Cambridge Structural Database (CSD). We argue that both experimental and computational materials scientists need to embrace a culture of rigorous data curation as part of modern research data management. We propose a sample data curation pipeline for materials chemistry and illustrate its use by creating two new materials chemistry databases. Here, we hope that this perspective will serve to catalyze further discussion and promote the continuous development of rigorous data curation practices within the materials science research community. We posit that adherence to best practices of data curation will promote and enhance the reliability, reproducibility, and integrity of materials research and enable the development of reliable AI and machine learning models that critically depend on the use of quality data.
To standardize materials and component characterization for next generation hydrogen production and energy generation solid oxide cell (SOC) technologies, test protocols are being established to facilitate comparison across the numerous laboratories and research institutions where SOC development for application in solid oxide fuel cells (SOFCs) and solid oxide electrolyzes cells (SOEC) is conducted. This paper proposes guiding protocols for fundamental electrical properties characterization of SOC materials, including temperature- and oxygen partial pressure (pO 2 )-dependent conductivity measurements, and use of the electromotive force for determining the transference numbers, or contributions of each charge carrier (i.e., ions and electrons), to the total conductivity. The protocol for Archimedes density measurements is also provided as an integral technique to both of these methods.
Standard heat treatments for metals of a particular composition are typically designed with the assumption of a conventional starting microstructure, such as that produced by casting or wrought processing. When applied to metals fabricated by Laser Powder Bed Fusion (LPBF) metal additive manufacturing (AM), these heat treatments can produce inconsistent performance due to the unique as-built microstructures. This study investigates how modifications to standard heat treatments for 17-4 PH steel influence the microstructure and mechanical properties of LPBF-fabricated material. Specimens were produced and subjected to varying solutionizing and homogenizing treatments followed by standard aging treatments. Microstructures were characterized using optical microscopy, Electron Backscatter Diffraction (EBSD), and X-ray diffraction (XRD), and mechanical properties were evaluated through uniaxial tensile testing. Based on these results, recommendations are provided for achieving improved wrought-like performance in LPBF 17-4 PH steel.