Anisotropic Shrinkage and Microstructural Characterization of Additively Manufactured 94% Alumina
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Strong, Kevin Thomas↗
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Results for “Anisotropic shrinkage”
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Detailed modeling of hydrogen release and particle shrinkage during pyrolysis of inhomogeneous wood
Hydrogen release during pyrolysis of woody biomass is studied considering anisotropicity and inhomogeneity of wood structure. A new anisotropic shrinkage model is proposed based on the decomposition of main wood constituents, i.e., cellulose, hemicellulose, and lignin. The new shrinkage model can predict the temporal evolution of the wood structure, and the differences between axial and radial shrinkage during pyrolysis. The model agrees very well with several experimental data from the literature. Based on particle temperature during conversion, the pyrolysis is partitioned into four stages, and the hydrogen release and H 2 formation from each stage are investigated. Stage (IV) of pyrolysis, from 1000 to 1273 K, is found to be efficient for H 2 production owing to the production of considerable mass of H with a minimal amount of tar species. Furthermore, the char quality is found to be different at the end of stages (II), (III), and (IV), where around 67.7, 80.5, and 93.4% wt. of solid residue is made of carbon, respectively. The model is also used to explain how the heating rate affects the temperature distribution inside the particle and how it shifts the peak of hydrogen release. Finally, the pyrolysis of two inhomogeneous wood samples — a beech twig with bark and a beech dowel with growth rings — are investigated. The bark can affect the pyrolysis rate, products, and flow pattern inside the particle. The growth rings do not have a considerable effect on the pyrolysis rate and products, but they have a significant impact on the flow pattern. This has an important implication for char conversion studies where the internal surface area and porosity field distribution have a significant effect on the gasification and oxidation rates.
09 BIOMASS FUELS↗
Influence of Fiber Orientation on Deformation of Additive Manufactured Composites
Anisotropy caused by flow-induced fiber orientation of discontinuous fibers within the extrudate in the Extrusion Deposition Additive Manufacturing (EDAM) process gives rise to anisotropic shrinkage in printed parts and thereby, final part deformations. Three fiber orientation states, described by the second-order orientation tensor, were investigated to determine their influence upon final geometry. Two material systems were investigated including a short glass fiber-reinforced polyamide and a short carbon fiber-reinforced polyamide. A curvilinear geometry was modeled and printed virtually in the thermo-mechanical simulation, ADDITIVE3D©. The scale of the printed geometry was in the range of 300–400 mm and contained three semicircular geometry regions connected to linear regions, thereby inducing significant magnification of the spring-in deformation. The predicted deformation of the printed geometry for the three fiber orientation states and two material systems were compared. The deformation predicted for glass fiber-filled polyamide and carbon fiber-filled polyamide of the same fiber orientation states showed comparable deformations. In conclusion, the largest residual deformation was shown to correspond to the orientation tensor with the greatest degree of anisotropy.
36 MATERIALS SCIENCE↗
CO 2 Laser Sintering of Garnet-Type Solid-State Electrolytes
We report the processing of garnet-type solid-state electrolytes remains challenging as densification conventionally requires high sintering temperatures and long processing times, which can result in severe Li loss, the formation of secondary phases, and thus high porosity and low ionic conductivity. Here, we report an ultrafast sintering method based on CO 2 laser scanning with the assistance of a heating stage. We demonstrate the rapid densification of low-packing-density Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) films, which are difficult to densify by conventional furnace sintering methods. This unique approach has three fingerprint characteristics: (1) mitigation of Li loss through ultrafast sintering (dwelling time $\ll$1 s); (2) a unique anisotropic shrinkage behavior that greatly reduces film thickness; (3) wave-like surface topology from point scanning strategy that enables 3D interfacial contacts with electrode materials. Herein, highly dense (95.68%) and highly conductive (0.26 mS·cm –1 at 25 °C) LLZTO films are obtained through CO2 laser sintering. This work provides a unique, scalable, and widely applicable ultrarapid laser sintering technique to overcome the difficulties associated with classic methods for the integration of SSEs for practical all-solid-state Li-metal battery applications.
36 MATERIALS SCIENCE↗
Controlled current-rate AC flash sintering of uranium dioxide
Uranium dioxide (UO2) pellets with controlled microstructures were densified up to 93.4% of their theoretical density in less than 25 minutes at a furnace temperature of 873 K, utilizing controlled current-rate alternating current (AC) flash sintering (FS). Using this AC-FS method it was possible to control the sintering rate and thermal gradients, resulting in dense pellets with no appreciable hourglassing and good mechanical integrity. Moreover, the apparent sintering activation energy for FS and for conventionally sintered samples was estimated to be 108 kJ mol -1 and 380 kJ mol -1 , respectively using the master sintering curve method. The apparent activation energy for FS was remarkably close to those reported in the literature for spark plasma sintering of UO 2 . Furthermore, both these field assisted sintering methods utilize fast heating rates and electrical effects that are likely enhancing the grain boundary diffusion mechanism. Finally controlled current-rate AC-FS has been demonstrated as a technological advancement, capable of producing ceramic nuclear fuels in a fraction of the conventional processing time.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Additively Manufactured Carbon Fiber-Reinforced Siliconized Silicon Carbide Composites Using Carbon Fiber-Reinforced Poly-Ether-Ether-Ketone (PEEK) as a Precursor
Herein, we report a method to additively manufacture carbon fiber-reinforced siliconized silicon carbide composites. The process involves the pyrolysis of a 3D-printed carbon fiber-reinforced poly-ether-ether-ketone (PEEK) composite to produce a porous carbon fiber-reinforced carbon matrix composite preform, which is subsequently infiltrated with molten silicon to obtain a carbon fiber-reinforced siliconized silicon carbide composite. A key aspect of the method is limiting polymer melt flow during pyrolysis of PEEK, which is achieved by thermally annealing the 3D-printed carbon fiber-reinforced PEEK preform in air at a temperature below PEEK’s melting temperature. Rheological and differential scanning calorimetry (DSC) measurements demonstrate that the thermal annealing treatment altered the melting behavior of PEEK, while NMR and FTIR measurements provided a mechanistic explanation for the structural changes responsible for the behavior. It was also found that dimensional changes during pyrolysis were anisotropic with greater shrinkage in the stacking direction of the material.
Yoon, Bola [ORNL] (ORCID:0000000260875373)↗
Ettringite hysteresis under sorption from molecular simulations
Highlights: • Hybrid Grand Canonical Monte Carlo (GCMC) and Molecular Dynamics (MD) simulations are performed. • Anisotropic large strain coefficient of crystal shrinkage of ettringite is provided. • Entropy increases when ettringite converts into metaettringite. • Sorption-induced stress may lead to columns collapse upon drying. • H-bonds involving OH groups in columns play a role in hysteresis. The response of ettringite under sorption is critical for the utilization of this mineral as an energy storage material and to understand the concrete durability problems associated with ettringite formation. We report molecular simulations directly sampling the osmotic ensemble to understand the sorption processes and structural changes in ettringite-metaettringite transition. Desorption branch and sorption-induced volume changes from simulations agree with the experiments. The structural changes at low relative humidity are analyzed, revealing for the first time details of metaettringite structure. The reversibility under sorption observed experimentally is captured by simulation in the ettringite domain. The reversibility in the conversion of metaettringite into ettringite is not captured by the direct simulations in the osmotic ensemble due to the large volume changes associated with ettringite desorption. Finally, we discuss the role of hydrogen bonds on the hysteresis in ettringite.
36 MATERIALS SCIENCE↗
Silica Reusable Surface Insulation Improvement Research
Fiber characterization, fabrication processes, physical properties, and thermal responses are investigated to improve silica reusable surface insulation tiles. Criteria for fiber selection on the basis of chemical composition, shrinkage, and devitrification have been defined and a simple process for fabricating silica surface insulation materials has been developed that produces only 5% shrinkage and no devitrification of tiles at 1533 K in ten hours. Anisotropic tile with improved weak direction strength has been fabricated using conventional molding techniques.
Goldstein, H. E.↗
High Temperature Degradation Mechanisms in Polymer Matrix Composites
Polymer matrix composites are increasingly used in demanding structural applications in which they may be exposed to harsh environments. The durability of such materials is a major concern, potentially limiting both the integrity of the structures and their useful lifetimes. The goal of the current investigation is to develop a mechanism-based model of the chemical degradation which occurs, such that given the external chemical environment and temperatures throughout the laminate, laminate geometry, and ply and/or constituent material properties, we can calculate the concentration of diffusing substances and extent of chemical degradation as functions of time and position throughout the laminate. This objective is met through the development and use of analytical models, coupled to an analysis-driven experimental program which offers both quantitative and qualitative information on the degradation mechanism. Preliminary analyses using a coupled diffusion/reaction model are used to gain insight into the physics of the degradation mechanisms and to identify crucial material parameters. An experimental program is defined based on the results of the preliminary analysis which allows the determination of the necessary material coefficients. Thermogravimetric analyses are carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. Powdered samples are used to eliminate diffusion effects. Tests in both inert and oxidative environments allow the separation of thermal and oxidative contributions to specimen mass loss. The concentration dependency of the oxidative reactions is determined from the tests in pure oxygen. Short term isothermal tests at different temperatures are carried out on neat resin and unidirectional macroscopic specimens to identify diffusion effects. Mass loss, specimen shrinkage, the formation of degraded surface layers and surface cracking are recorded as functions of exposure time. Geometry effects in the neat resin, and anisotropic diffusion effects in the composites, are identified through the use of specimens with different aspect ratios. The data is used with the model to determine reaction coefficients and effective diffusion coefficients. The empirical and analytical correlations confirm the preliminary model results which suggest that mass loss at lower temperatures is dominated by oxidative reactions and that these reaction are limited by diffusion of oxygen from the surface. The mechanism-based model is able to successfully capture the basic physics of the degradation phenomena under a wide range of test conditions. The analysis-based test design is successful in separating out oxidative, thermal, and diffusion effects to allow the determination of material coefficients. This success confirms the basic picture of the process; however, a more complete understanding of some aspects of the physics are required before truly predictive capability can be achieved.
Cunningham, Ronan A.↗
High Temperature Degradation Mechanisms in Polymer Matrix Composites
Polymer matrix composites are increasingly used in demanding structural applications in which they may be exposed to harsh environments. The durability of such materials is a major concern, potentially limiting both the integrity of the structures and their useful lifetimes. The goal of the current investigation is to develop a mechanism-based model of the chemical degradation which occurs, such that given the external chemical environment and temperatures throughout the laminate, laminate geometry, and ply and/or constituent material properties, we can calculate the concentration of diffusing substances and extent of chemical degradation as functions of time and position throughout the laminate. This objective is met through the development and use of analytical models, coupled to an analysis-driven experimental program which offers both quantitative and qualitative information on the degradation mechanism. Preliminary analyses using coupled diffusion/reaction model are used to gain insight into the physics of the degradation mechanisms and to identify crucial material parameters. An experimental program is defined based on the results of the preliminary analysis which allows the determination of the necessary material coefficients. Thermogravimetric analyses are carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. Powdered samples are used to eliminate diffusion effects. Tests in both inert and oxidative environments allow the separation of thermal and oxidative contributions to specimen mass loss. The concentration dependency of the oxidative reactions is determined from the tests in pure oxygen. Short term isothermal tests at different temperatures are carried out on neat resin and unidirectional macroscopic specimens to identify diffusion effects. Mass loss, specimen shrinkage, the formation of degraded surface layers and surface cracking are recorded as functions of exposure time. Geometry effects in the neat resin, and anisotropic diffusion effects in the composites, are identified through the use of specimens with different aspect ratios. The data is used with the model to determine reaction coefficients and effective diffusion coefficients. The empirical and analytical correlations confirm the preliminary model results which suggest that mass loss at lower temperatures is dominated by oxidative reactions and that these reaction are limited by diffusion of oxygen from the surface. The mechanism-based model is able to successfully capture the basic physics of the degradation phenomena under a wide range of test conditions. The analysis-based test design is successful in separating out oxidative, thermal, and diffusion effects to allow the determination of material coefficients. This success confirms the basic picture of the process; however, a more complete understanding of some aspects of the physics are required before truly predictive capability can be achieved.
Cunningham, Ronan A.↗
Electrochemical-mechanical coupling failure mechanism of composite cathode in all-solid-state batteries
Composite cathode composed of active particles and solid electrolytes (SEs) can considerably enlarge the particle-SE contact areas and achieve high areal loadings in all-solid-state batteries (ASSBs). However, the challenging interfacial instability and particle damage problems remain unsolved. Herein, we establish a 3D electrochemical-mechanical coupled model to investigate the underlying failure mechanism by considering the governing electrochemical and physics processes. Micro-scale heterogeneous primary particles with random crystallographic orientation and size inside the LiNi 1/3 Co 1/3 Mn 1/3 O 2 (NCM111) secondary particle of the model result in the anisotropic Li diffusion and volume variation within the secondary particle, leading to significant nonuniformity of the Li concentration, and GPa-level stress distributions at primary particle boundaries, and finally causing the particle internal cracks. The particle volume shrinkage under the constraint of stiff Li 7 La 3 Zr 2 O 12 (LLZO) SE triggers the interface debonding (gap>50 nm) with increased interfacial impedance to degrade cell capacity. Higher C-rates result in larger residual stress (~100 MPa)/strain/debonding gap at dis-charging end, more likely to deteriorate the cell performance. Increasing the interfacial strength between the particle and SE can suppress the interface debonding but induces high stress (up to 10 GPa). In conclusion, results reveal the underlying mechanism of the electrochemical-mechanical coupling failure mechanism for composite cathode and provide promising guidance on the further improvement of a more robust composite cathode for ASSBs.
25 ENERGY STORAGE↗
X-ray verification of sol-gel resist shrinkage in substrate-conformal imprint lithography for a replicated blazed reflection grating
Surface-relief gratings fabricated through nanoimprint lithography (NIL) are prone to topographic distortion induced by resist shrinkage. Characterizing the impact of this effect on blazed diffraction efficiency is particularly important for applications in astrophysical spectroscopy at soft x-ray wavelengths ( λ ≈ 0.5 − 5 nm) that call for the mass-production of large-area grating replicas with sub-micron, sawtooth surface-relief profiles. A variant of NIL that lends itself well for this task is substrate-conformal imprint lithography (SCIL), which uses a flexible, composite stamp formed from a rigid master template to imprint nanoscale features in an inorganic resist that cures thermodynamically through a silica sol-gel process. While SCIL enables the production of several hundred imprints before stamp degradation and avoids many of the detriments associated with large-area imprinting in NIL, the sol-gel resist suffers shrinkage dependent on the post-imprint cure temperature. Through atomic force microscopy and diffraction-efficiency testing at beamline 6.3.2 of the Advanced Light Source, the impact of this effect on blaze response is constrained for a ∼160-nm-period grating replica cured at 90 ° C. Results demonstrate a ∼2 ° reduction in blaze angle relative to the master grating, which was fabricated by anisotropic wet etching in 〈311〉-oriented silicon to yield a facet angle close to 30 ° .
McCoy, Jake A. (ORCID:0000000216057517)↗
Fiber pushout test: A three-dimensional finite element computational simulation
A fiber pushthrough process was computationally simulated using three-dimensional finite element method. The interface material is replaced by an anisotropic material with greatly reduced shear modulus in order to simulate the fiber pushthrough process using a linear analysis. Such a procedure is easily implemented and is computationally very effective. It can be used to predict fiber pushthrough load for a composite system at any temperature. The average interface shear strength obtained from pushthrough load can easily be separated into its two components: one that comes from frictional stresses and the other that comes from chemical adhesion between fiber and the matrix and mechanical interlocking that develops due to shrinkage of the composite because of phase change during the processing. Step-by-step procedures are described to perform the computational simulation, to establish bounds on interfacial bond strength and to interpret interfacial bond quality.
Mital, Subodh K.↗
Fiber pushout test - A three-dimensional finite element computational simulation
A fiber pushthrough process was computationally simulated using three-dimensional finite element method. The interface material is replaced by an anisotropic material with greatly reduced shear modulus in order to simulate the fiber pushthrough process using a linear analysis. Such a procedure is easily implemented and is computational very effective. It can be used to predict fiber pushthrough load for a composite system at any temperature. The average interface shear strength obtained from pushthrough load can easily be separated into its two components: one that comes from frictioal stresses and the other that comes from chemical adhesion between fiber and the matrix and mechanical interlocking that develops due to shrinkage of the composite because of phase change during the processing. Step-by-step procedures are described to perform the computational simulation, to establish bounds on interfacial bond strength and to interpret interfacial bond quality.
Mital, Subodh K.↗
AGR-3/4 TRISO Fuel Compact Ceramography
The combined third and fourth irradiation in the Advanced Gas Reactor (AGR) program (AGR-3/4) contained tristructural isotropic (TRISO)-coated particle fuel and designed-to-fail (DTF) fuel particles. The DTF particles were only coated with highly anisotropic pyrocarbon (PyC) so they would purposely fail during the AGR-3/4 irradiation and provide a source of fission products for measurement. To observe the post-irradiation morphology of these DTF particles and the TRISO-coated particles, three AGR-3/4 compacts were mounted in epoxy, sectioned above their centerlines, and ground/polished. Three rounds of grinding/polishing and optical microscopy were performed so that the particles could be observed at multiple planes. Each compact contained approximately 1,872 TRISO particles and exactly 20 DTF particles. The three AGR-3/4 compacts examined covered a wide temperature range and featured both the hottest average irradiation temperature (1375°C) and the coldest/lowest burnup (872°C and 5.5% fissions per initial metal atom) of any compacts to undergo post-irradiation examination (PIE) in the AGR program to date. A total of 29 DTF particles were located and observed via microscopy across the three compacts. All the DTF particles observed via microscopy had completely failed PyC coatings. Some different DTF kernel and PyC morphologies were observed that have been attributed to the differences in irradiation temperature and/or burnup. At low and medium irradiation temperatures (roughly 850 to 1050°C), it appears irradiation-induced dimensional changes in the DTF PyC caused it to fracture and fold in on itself, and the kernel deformed to accommodate this PyC deformation. The extent of DTF kernel deformation to accommodate DTF PyC buckling tended to be greater for the medium-temperature fuel compared to the cold fuel. In the high-irradiation-temperature compact (1375°C), the DTF PyC layer appears to have completely reacted chemically with the kernel material. The only material surrounding the DTF particles in this hot compact resembles the compact matrix material. Observations of the TRISO-coated driver fuel particles and fuel compact graphitic matrix were also made. The TRISO particle kernels in the medium-temperature compact (1047°C), and many in the high-temperature compact (1375°C), showed morphologies consistent with what was seen in AGR-1 and AGR-2. In other TRISO particles from the high-temperature compact, a spatial gradient in the kernel appearance was evident. Here the cool side of the kernel (away from the center of the compact) had a much darker appearance (like that of the buffer and pyrocarbon). This is the first observation of this kind of kernel spatial gradient in AGR fuel. It is believed that the high irradiation temperature of that compact (an average of 1375°C) activates or accelerates an unidentified chemical reaction, and the temperature gradient within the fuel causes a sharp spatial gradient. The low-temperature/low-burnup compact also showed unique kernel morphologies where the TRISO-coated particles had clearly distinguishable oxide and carbide phases at the center of the kernel, an oxide rind surrounding this, and remnants of a carbide skin surrounding the oxide rind. These are features observed in the as-fabricated fuel that are no longer present in higher burnup fuel. Occasional gaps between the outer pyrolytic carbon (OPyC) and graphitic matrix material were observed in all compacts. Gaps were most often found in the small, matrix-filled spaces between adjacent particles. Finally, buffer morphologies in AGR-3/4 TRISO particles were like those observed in AGR-1 and AGR-2, and the buffer fracture frequencies in AGR-3/4 and AGR-2 TRISO particles were plotted versus fast neutron fluence and irradiation temperature. In AGR-3/4 the buffer fracture rate was highest (23%) for an irradiation temperature of 1047°C and a fast fluence of 5.18E25 n/m 2 . Increasing the irradiation temperature to 1375°C reduced the buffer fracture rate to 14%. Reducing the irradiation temperature to 872°C and the fast fluence by a factor of 3 reduced the buffer fracture rate to 7%. The temperature and fluence dependencies observed for AGR-3/4 buffer fracture were consistent with those observed in AGR-2. Lower fluences and/or higher temperatures significantly reduced the buffer fracture frequencies. Lower buffer fracture frequencies were also observed at lower temperatures as long as the fluence was also significantly reduced. This is believed to be due to lower fluence resulting in less irradiation-induced dimensional change (shrinkage) of the buffer, and a higher temperature promoting enhanced creep relaxation of stresses within the buffer, leading to less buffer fracture.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗