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DOE OSTI2021

Observation of Stepwise Ultrafast Crystallization Kinetics of Donor–Acceptor Conjugated Polymers and Correlation with Field Effect Mobility

The semicrystalline microstructures of donor-acceptor conjugated polymers strongly impact their optoelectronic properties. The control of the microstructure relies on the understandings of the crystallization processes in these polymers, from packing structures to crystallization kinetics. How fast these conjugated polymer chains crystallize and how their chemical structures and pre-existing microstructure history influence their crystallization have so far remained unclear, due to the fast crystallization rate caused by chain rigid structures and strong interactions. Here, ultrafast scanning calorimetry (FSC) is employed to reveal the crystallization behaviors of high perform- ance diketopyrrolopyrrole (DPP)-based conjugated polymers with scanning rates up to 500 000 K/s. Through elaborately designed nonisothermal and isothermal crystallization studies, we probed the fast crystallization kinetics and extracted the two-step crystallization process of these polymers quantitatively. We found that both the rigidity of the chain backbones and the preinduced crystalline microstructures can influence the crystallization rate over an order of magnitude at the same degree of undercooling. We further demonstrated the manipulated crystallization kinetics in the DPP-based polymer films with different amounts of preinduced crystallites and correlate it to the polymers’ charge transport mobility.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Development of Multilayered Coatings for Nerva-Type Graphite Fuel Elements- An Overview

“Mid-passage corrosion” (MPC) was observed in NbC and ZrC-coated graphite (Gr)-based nuclear fuels during the NERVA/Rover programs. A new multilayered coating concept was proposed to solve this problem. The concept envisions designing a compliant multilayered coatings architecture to accommodate the thermal expansion mismatch strains between the ZrC outer coating and the Gr/(U,Zr)C fuel matrix. Additionally, the coating architecture uses diffusion barriers to minimize carbon diffusion from the substrate, and hydrogen diffusion from the flowing gas stream, into the multilayer coating. The present paper provides a brief overview of the development of multilayered coatings deposited on Gr disks, as well as within the inner channels of a19-hole hexagonal rod 152.4 mm long, by chemical vapor deposition (CVD) in proof-of concept studies. The cross-sectional microstructural observations are discussed. These trials have established that it is possible to deposit multilayered coatings by CVD in 19-hole hexagonal rods similar to the NERVA fuel rod design although the quality of the coatings and the uniformity of their thicknesses require further improvement.

Multilayer coatings, graphite, nuclear thermal pro↗

DOE OSTI2017

Characterization of Flame Cut Heavy Steel: Modeling of Temperature History and Residual Stress Formation

Heavy steel plates are used in demanding applications that require both high strength and hardness. An important step in the production of such components is cutting the plates with a cost-effective thermal cutting method such as flame cutting. Flame cutting is performed with a controlled flame and oxygen jet, which burns the steel and forms a cutting edge. However, the thermal cutting of heavy steel plates causes several problems. A heat-affected zone (HAZ) is generated at the cut edge due to the steep temperature gradient. Consequently, volume changes, hardness variations, and microstructural changes occur in the HAZ. In addition, residual stresses are formed at the cut edge during the process. In the worst case, unsuitable flame cutting practices generate cracks at the cut edge. The flame cutting of thick steel plate was modeled using the commercial finite element software ABAQUS. The results of modeling were verified by X-ray diffraction-based residual stress measurements and microstructural analysis. The model provides several outcomes, such as obtaining more information related to the formation of residual stresses and the temperature history during the flame cutting process. In addition, an extensive series of flame cut samples was designed with the assistance of the model.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Nano-scale mechanical behavior of uranium silicide compounds

Uranium silicide compounds exhibit a range of attractive material properties for nuclear fuel applications, but little is known regarding their mechanical behavior. The structure of nuclear fuels at high burnup can prove to be especially difficult given the significant changes in both chemistry and microstructure caused by fission products. Nano-indentation appears to be a valuable addition to post irradiation examination. The present focus is assessment of the room temperature modulus and hardness of U{sub 3}Si{sub 2}, U{sub 3}Si{sub 5} and USi materials. Each of the compositions under investigation was synthesized via arc melting of the pure metals in an Ar atmosphere using a titanium getter to remove O{sub 2} contamination. The resulting pellets following milling and sintering of the arc melted material were between 96 and 98% of density. Coupling different techniques (SEM and Chemical Analysis), microstructural investigations of the samples has been performed. Preliminary nano-mechanical response of U-Si fuel materials has been demonstrated, on a Hysitron Tribo-indenter which will impact the ability to design advanced fuel materials for enhanced high temperature performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Manufacturing Dissolvable Alloy Components using ShAPE: A Study on Solid Phase Processing of Mg-W Composites and WJ11 Alloys

Dissolvable alloys and composites are an emerging class of materials that demonstrate tailored sorptivity in corrosive environments. This work explored the viability of solid phase processing (SPP) techniques, namely the shear assisted processing and extrusion (ShAPETM) method, to manufacture dissolvable magnesium composites and alloys components such as rods and tubes. The study also determined the effects of material composition and manufacturing process conditions on material microstructures developed during SPP and the resulting performance of the components. Explicit properties of interest included ultimate tensile strength, ultimate compressive strength, and yield strength. The application fields of interest for dissolvable alloys were identified as oil-and-gas operations and biomedical implants. Accordingly, PNNL collaborated with industrial and academia partners, Fortek Industries, Houston and University of Pittsburgh, during the course of this project for material and ShAPE process development. PNNL determined the viability of the using ShAPE to process the custom-designed materials provided by the project partners. This was done by identifying process parameters such as tool rotation rate, tool plunge rate, and process cooling optimal for manufacturing components with consolidated microstructures. Subsequently, PNNL also performed microstructural characterization on unprocessed and processed samples and mechanical property testing. One of the major findings from this work is that ShAPE was able to manufacture dissolvable magnesium composite and alloy rods and tubes with consolidated homogeneous microstructures and minimal macroscale defects on component surfaces. It was observed that samples processed via ShAPE demonstrated an average grain size < 2 - 5 µm, which was markedly lower than that of the precursors with 8 – 13 µm grains. Results showed that the ShAPE synthesized dissolvable magnesium composite and alloy strength was on par with or better than those components that were manufactured using traditional manufacturing processes such as forging and extrusion. It is noteworthy that the ShAPE samples were made with considerably lower number of process steps.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Fabrication and Design Aspects of High-Temperature Compact Diffusion Bonded Heat Exchangers

The Very High Temperature Reactor (VHTR) using gas-cooled reactor technology is anticipated to be the reactor type for the Next Generation Nuclear Plant (NGNP). In this reactor concept with an indirect power cycle system, a high-temperature and high integrity Intermediate Heat Exchanger (IHX) with high effectiveness is required to efficiently transfer the core thermal output to a secondary fluid for electricity generation, hydrogen production, and/or industrial process heat applications. At present, there is no proven IHX concept for VHTRs. The current Technology Readiness Level (TRL) status issued by NGNP to all components associated with the IHX for reduced nominal reactor outlet temperatures of 750–800 degrees C is 3 on a 1–10 scale, with 10 indicating omplete technological maturity. Among the various potential IHX concepts available, diffusion bonded heat exchangers (henceforth called printed circuit heat exchangers, or PCHEs) appear promising for NGNP applications. The design and fabrication of this key component of NGNP with Alloy 617, a candidate high-temperature structural material for NGNP applications, are the primary focus of this paper. In the current study, diffusion bonding of Alloy 617 has been demonstrated, although the optimum diffusion bonding process parameters to engineer a quasi interface-free joint are yet to be determined. The PCHE fabrication related processes, i.e., photochemical etching and diffusion bonding are discussed for Alloy 617 plates. In addition, the authors’ experiences with these non-conventional machining and joining techniques are discussed. Two PCHEs are fabricated using Alloy 617 plates and are being experimentally investigated for their thermal-hydraulic performance in a High-Temperature Helium Facility (HTHF). The HTHF is primarily of Alloy 800H construction and is designed to facilitate experiments at temperatures and pressures up to 800 degrees C and 3 MPa, respectively. Furthermore, some preliminary microstructural and mechanical property characterization studies of representative diffusion bonded Alloy 617 specimens are presented. The characterization studies are restricted and less severe from an NGNP perspective but provide sufficient confidence to ensure safe operation of the heat exchangers in the HTHF. The test results are used to determine the design operating conditions for the PCHEs fabricated.

99 GENERAL AND MISCELLANEOUS↗

NASA NTRS2001

Flight Computer Processing Avionics for Space Station Microgravity Experiments: A Risk Assessment of Commercial Off-the-Shelf Utilization

NASA/Marshall Space Flight Center (MSFC) is continually looking for ways to reduce the costs and schedule and minimize the technical risks during the development of microgravity programs. One of the more prominent ways to minimize the cost and schedule is to use off-the-shelf hardware (OTS). However, the use of OTS often increases the risk. This paper addresses relevant factors considered during the selection and utilization of commercial off-the-shelf (COTS) flight computer processing equipment for the control of space station microgravity experiments. The paper will also discuss how to minimize the technical risks when using COTS processing hardware. Two microgravity experiments for which the COTS processing equipment is being evaluated for are the Equiaxed Dendritic Solidification Experiment (EDSE) and the Self-diffusion in Liquid Elements (SDLE) experiment. Since MSFC is the lead center for Microgravity research, EDSE and SDLE processor selection will be closely watched by other experiments that are being designed to meet payload carrier requirements. This includes the payload carriers planned for the International Space Station (ISS). The purpose of EDSE is to continue to investigate microstructural evolution of, and thermal interactions between multiple dendrites growing under diffusion controlled conditions. The purpose of SDLE is to determine accurate self-diffusivity data as a function of temperature for liquid elements selected as representative of class-like structures. In 1999 MSFC initiated a Center Director's Discretionary Fund (CDDF) effort to investigate and determine the optimal commercial data bus architecture that could lead to faster, better, and lower cost data acquisition systems for the control of microgravity experiments. As part of this effort various commercial data acquisition systems were acquired and evaluated. This included equipment with various form factors, (3U, 6U, others) and equipment that utilized various bus structures, (VME, PC104, STD bus). This evaluation of hardware was performed in conjunction with a trade study that considered over twenty (20) different factors relevant to the selection of an optimum design approach. These factors included; safety, sizing and timing, radiation hardness and single event upset, power consumption, heat dissipation, size and volume, expected service life, maintainability, heritage, operating systems, requirements for software reuse, availability of compatible interface boards, relative cost, schedule, reliability, EMI/EMC factors, "hot swap" capability, standards for conduction cooling, I/O capabilities, unique carrier requirements and operating system considerations. The approach to evaluate Safety as part of this study included a review of the Preliminary Hazard Analysis (PHA) for each of the experiment designs and a determination of how each hazard could be addressed and eliminated when different processors were selected. This included evaluating various design approaches and trade-offs between fault tolerant designs and fail-safe designs in accordance with NSTS 1700.7B. This will include the results of radiation testing where available. Various operating systems, such as VxWorks, Linux, QNX, and Embedded NT are evaluated and the advantages and disadvantages of their utilization are also addressed. Design implementation strategies for the various operating systems are considered and discussed. This paper presents the results and recommendations from this trade study. Preliminary conclusions from this study are that safety concerns from lack or radiation testing on COTS equipment can be addressed by additional testing and design considerations, the PC104 bus provided adequate I/O for the SDLE and EDSE microgravity experiments, and PC104 bus components offered significant advantages over VME and cPCI for weight and space reductions.

Estes, Howard↗

NASA NTRS2011

Evaluation of Aluminum Alloy 2050-T84 Microstructure and Mechanical Properties at Ambient and Cryogenic Temperatures

Aluminum alloy 2050 is being considered for the fabrication of cryogenic propellant tanks to reduce the mass of future heavy-lift launch vehicles. The alloy is available in section thicknesses greater than that of the incumbent aluminum alloy, 2195, which will enable designs with greater structural efficiency. While ambient temperature design allowable properties are available for alloy 2050, cryogenic properties are not available. To determine its suitability for use in cryogenic propellant tanks, tensile, compression and fracture tests were conducted on 4 inch thick 2050-T84 plate at ambient temperature and at -320degF. Various metallurgical analyses were also performed in order to provide an understanding of the compositional homogeneity and microstructure of 2050.

Hafley, Robert A.↗

DOE OSTI2022

Multi-Modal Characterization of Nuclear Fuels and Materials at the Idaho National Laboratory Materials & Fuels Complex

The Idaho National Laboratory (INL) leads cutting-edge research pertaining to the advancement of nuclear reactor technologies, including nuclear fuels and materials. The INL Irradiated Materials Characterization Laboratory (IMCL), Electron Microscopy Laboratory (EML), and future Sample Preparation Laboratory (SPL) are available to the nuclear research community to assess the behavior of nuclear fuels and materials, efficiently and comprehensively characterizing from the engineering to atomistic scale. The IMCL is a unique, 12,000-square-foot facility located at the INL Materials and Fuels Complex designed for analysis of irradiated materials. The facility operates advanced characterization instruments that are sensitive to vibration, temperature, and electromagnetic interference in modular radiological shielding and confinement systems, granting researchers the ability to assess the microstructural, chemical, mechanical and thermophysical properties of nuclear materials, especially irradiated fuels. The EML is dedicated to advanced characterization of materials with optical and electron microscopy tools, including scanning electron microscopy/focused-ion beam (SEM/FIB) and transmission electron microscopy (TEM). Upon construction, the SPL will be a 3 story, 49,000 sq. ft facility, that is the most modern reactor structural materials testing and analysis facility in the world, designed to investigate reactor structural materials in support of life-extension programs and development of advanced reactor concepts, including mechanical testing and advanced characterization capabilities. This presentation will showcase some of the main capabilities available at both IMCL, EML, and SPL, specifically illustrating how these characterization techniques are incorporated into multi-modal characterization work scopes to elucidate the degradation of nuclear structural materials and irradiated fuels.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Modeling the thermodynamics of the FeTi hydrogenation under para-equilibrium: An ab-initio and experimental study

We report FeTi-based hydrides have recently re-attracted attention as stationary hydrogen storage materials due to favorable reversibility, good sorption kinetics and relatively low costs compared to alternative intermetallic hydrides. Employing the OpenCalphad software, the thermodynamics of the (FeTi) 1-x H x (0 ≤ x ≤ 1) system were assessed as a key basis for modeling hydrogenation of FeTi-based alloys. New thermodynamic data were acquired from our experimental pressure-composition-isotherm (PCI) curves, as well as first-principles calculations utilizing density functional theory (DFT). The thermodynamic phase models were carefully selected based on critical analysis of literature information and ab-initio investigations. Key thermodynamic properties such as dissociation pressure, formation enthalpies and phase diagrams were calculated in good agreement to our performed experiments and literature-reported data. This work provides an initial perspective, which can be extended to account for higher-order thermodynamic assessments and subsequently enables the design of novel FeTi-based hydrides. In addition, the assessed thermodynamic data can serve as key inputs for kinetic models and hydride microstructure simulations.

08 HYDROGEN↗

DOE OSTI2021

Evolution of thermo-mechanical properties of concrete with calcium aluminate cement and special aggregates for energy storage

Highlights: • CAC Concrete with stable aggregates is suitable for high temperatures with cycles. • Concrete suffered performance changes after the first thermal cycle (dehydration). • Subsequent thermal cycles showed stabilization and slight performance decreases. With the ever-expanding presence of solar energy, the design of cost-efficient heat energy storage systems is becoming increasingly relevant. Concrete is a potential solid material for these systems but raises questions of its response at high temperatures in operating conditions. This work studies concrete designed with calcium aluminate cement and three types of aggregates that are stable at high temperatures. The designed concrete mixes were exposed to thermal cycles (290–550 °C), and their thermal fatigue response was evaluated with mechanical, cracking, thermal, and microstructural analyses at room temperature after heat cycles. The obtained results show that the main changes are mostly produced after the first thermal cycle and are stabilized during successive thermal cycles, with only a slight decrease in the thermo-mechanical properties. The results showed stabilization of cracking, crack widths between 10 and 80 μm, reduction of compressive strength, around 50–65%, and reduction of the thermal conductivity by 30%.

36 MATERIALS SCIENCE↗

DOE OSTI2011

New Poly(dimethylsiloxane)/Poly(perfluorooctylethyl acrylate) Block Copolymers: Structure and Order Across Multiple Length Scales in Thin Films

Three sets of a new class of low surface tension block copolymers were synthesized consisting of a poly(dimethylsiloxane) (PDMS) block and a poly(perfluorooctylethyl acrylate) (AF8) block. The polymers were prepared using a bromo-terminated PDMS macroinitiator, to which was attached an AF8 block grown using atom transfer radical polymerization (ATRP) in such a designed way that the molecular weight and composition of the two polymer blocks were regularly varied. The interplay of both the phase separated microstructure and the mesomorphic character of the fluorinated domains with their effect on surface structure was evaluated using a suite of analytical tools. Surfaces of spin-coated and thermally annealed films were assessed using a combination of X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure (NEXAFS) studies. Both atomic force microscopy (AFM) measurements and grazing incidence small angle X-ray scattering (GISAXS) studies were carried out to evaluate the microstructure of the thin films. Even in block copolymers in which the PDMS block was the majority component, a significant presence of the lower surface energy AF8 block was detected at the film surface. Moreover, the perfluorooctyl helices of the AF8 repeat units were highly oriented at the surface in an ordered, tilted smectic structure, which was compared with those of the bulk powder samples using wide-angle X-ray powder diffraction (WAXD) studies.

36 MATERIALS SCIENCE↗

DOE OSTI2014

How much improvement in thermoelectric performance can come from reducing thermal conductivity?

Large improvements in the performance of thermoelectric materials have come from designing materials with reduced thermal conductivity. Yet as the thermal conductivity of some materials now approaches their amorphous limit, it is unclear if microstructure engineering can further improve thermoelectric performance in these cases. In this contribution, we use large data sets to examine 300 compositions in 11 families of thermoelectric materials and present a type of plot that quickly reveals the maximum possible zT that can be achieved by reducing the thermal conductivity. This plot allows researchers to quickly distinguish materials where the thermal conductivity has been optimized from those where improvement can be made. Moreover, through these large data sets we examine structure-property relationships to identify methods that decrease thermal conductivity and improve thermoelectric performance. We validate, with the data, that increasing (i) the volume of a unit cell and/or (ii) the number of atoms in the unit cell decreases the thermal conductivity of many classes of materials, without changing the electrical resistivity.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Computational studies of physical properties of Nb-Si based alloys

The overall goal is to provide physical properties data supplementing experiments for thermodynamic modeling and other simulations such as phase filed simulation for microstructure and continuum simulations for mechanical properties. These predictive computational modeling and simulations may yield insights that can be used to guide materials design, processing, and manufacture. Ultimately, they may lead to usable Nb-Si based alloy which could play an important role in current plight towards greener energy. The main objectives of the proposed projects are: (1) developing a first principles method based supercell approach for calculating thermodynamic and mechanic properties of ordered crystals and disordered lattices including solid solution; (2) application of the supercell approach to Nb-Si base alloy to compute physical properties data that can be used for thermodynamic modeling and other simulations to guide the optimal design of Nb-Si based alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2012

AGC-1 PIE Experimental Plan

Here we report the Post-Irradiation Examination planned for the AGC-1 creep samples. The key data obtained for each grade of graphite included in the AGC-1capsule are dimension, volume, mass and density changes, creep strain, electrical resistivity, Elastic constants (E, G, υ) from sonic velocity, dynamic modulus (from fundamental frequency of vibration), coefficient of thermal expansion, microstructural characterization, and fracture strength. The effect of creep strain on the above properties will be determined. These data are critical to the design of the Next Generation Nuclear Plant. Moreover, the data supports ongoing work in the area of model development, e.g., irradiation effects models such as dimensional change. The data will be used to help underpin the existing American Society of Mechanical Engineers (ASME) design code for graphite core components.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Evaluation of printability methodologies and feasibility to down select LBPF steel and other materials for nuclear applications

In this work, new research is underway to produce alloys beyond well-known alloys with modified compositions that are better suited to be produced with additive manufacturing. These alloys can only possess improved radiation tolerance but also improved high temperature strength, creep resistance while also using elements that reduce the amount of activation after irradiation. This work package supports the vision and goals of the Advanced Materials and Manufacturing Technology (AMMT) program relevant to accelerate the development and deployment of advanced manufacturing processes. This work focuses on evaluating the methodology for designing alloys best suited for AM processes based on “printability”, literature research to evaluate and down select steel alloy systems. In this work, microstructural characterization and testing activities have been performed on certain steel alloys to support the efforts from collaborating laboratories during the evaluation and printing of the test articles. The final recommendation will be performed by all four participating laboratories.

316L↗

NASA NTRS1973

Generation of long time creep data on refractory alloys at elevated temperatures

Four separate studies of various aspects of the vacuum creep behavior of two tantalum alloys (T-111 and ASTAR 811C) and of pure CVD tungsten are reported. The first part of the program involved a study of the influence of high temperature pre-exposure to vacuum or to liquid lithium on the subsequent creep behavior T-111 alloy. Results of this study revealed significant effects of pre-exposure on the 1% creep life of T-111, with life reductions of about 3 orders of magnitude being observed in extreme cases. The second part of this study involved an investigation of the creep behavior of T-111 under conditions of continuously increasing stress and decreasing temperature which simulated the conditions anticipated in radioisotope capsule service. Results of this study showed that such test conditions produced a creep curve having a very unusual shape, and led to the identification of a new creep design parameter for this type of service. The third area of investigation was a study of the influence of heat treatment on the microstructure and creep behavior of ASTAR 811C. The fourth part of the program was directed toward a preliminary characterization of the 1% creep life of CVD tungsten as obtained from two different sources.

Sheffler, K. D.↗

NASA NTRS2003

A Comparison between Growth Morphology of "Eutectic" Cells/Dendrites and Single-Phase Cells/Dendrites

Directionally solidified (DS) intermetallic and ceramic-based eutectic alloys with an in-situ composite microstructure containing finely distributed, long aspect ratio, fiber, or plate reinforcements are being seriously examined for several advanced aero-propulsion applications. In designing these alloys, additional solutes need to be added to the base eutectic composition in order to improve heir high-temperature strength, and provide for adequate toughness and resistance to environmental degradation. Solute addition, however, promotes instability at the planar liquid-solid interface resulting in the formation of two-phase eutectic "colonies." Because morphology of eutectic colonies is very similar to the single-phase cells and dendrites, the stability analysis of Mullins and Sekerka has been extended to describe their formation. Onset of their formation shows a good agreement with this approach; however, unlike the single-phase cells and dendrites, there is limited examination of their growth speed dependence of spacing, morphology, and spatial distribution. The purpose of this study is to compare the growth speed dependence of the morphology, spacing, and spatial distribution of eutectic cells and dendrites with that for the single-phase cells and dendrites.

Tewari, S. N.↗