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At least 127 records · Page 7

Modeling Time-Dependent Surrogates of Additive-Manufactured Nuclear Fuels Processes

Additive manufacturing (AM) technology is being increasingly adopted in a wide variety of application areas for its ability to rapidly produce, prototype, and customize designs. Recently, a hybrid AM technique was successfully developed at Idaho National Laboratory (INL) to manufacture nuclear fuels [1]. Despite the advantages, this AM technique needs optimization due to defects from a highly complex melting and sintering process. The complex metallurgical phenomena during AM processes are strongly related to parameters such as applied laser power, traveling speed, and scan style, which could lead to differences in density, residual stress, crystallographic texture, and mechanical properties. In addition, stochastic variations in laser energy interaction and associated multiscale/multiphysics phenomena cause variations in microstructure evolution and mechanical properties. Currently, researchers at INL are focusing on developing a comprehensive modeling framework, leveraging INL’s simulation tools MOOSE/MARMOT/BISON/RAVEN [2-4] to describe all steps of this AM process across multiple length scales. Although this advanced framework plays a critical role in enabling enhancements to traditional trial and error approaches for design and optimization of nuclear fuel materials, it remains computationally intense, limiting its use in sensitivity and optimization analysis. In this case, an accurate and inexpensive surrogate becomes an effective tool for providing a tractable approximation of the underlying underline physics. Surrogate models generally not based on the physics of a system are purely mathematical models used to capture the relationships between specific system inputs and outputs. Popular approaches, including neural networks [5], response surfaces [6], and subspace-based reduced order models [7], have been applied to a wide range of disciplines, such as nuclear reactor design, aerospace design and automotive design. In this summary, we employ advanced time-dependent surrogate models such as high-dimensional model representation (HDMR) [8] and physics-informed deep neural network (PINNs) [9] to accelerate the design and optimization of AM process.

42 ENGINEERING↗

Status of Additive Manufacturing Capabilities for Processing Refractory Alloys Under the Mo-99 Program

The enriched 100 Mo target, denoted as aMo, that Northstar Medical Radioisotopes is developing to produce 99 Mo from an accelerator-based method is a disk-type geometry with a 0.5–0.715 mm thickness and a 29 mm outer diameter. A press and sinter method was adopted to fabricate these samples from aMo powder feedstock. Inherent porosity from the press and sinter method makes the disks more easily dissolvable during 99 Mo postprocessing. However, the disk-type geometry will be subject to thermal stresses due to temperature variations once the geometry is in line with the accelerated electron beam, causing warping and possible failure. Additive manufacturing (AM) processes such as laser powder bed fusion (LPBF) enable the manufacturing of custom, complex geometries that may otherwise be difficult to produce with more conventional methods (e.g., press and sinter approach). Therefore, the National Nuclear Security Administration’s Molybdenum-99 Program invested in developing an AM facility dedicated to processing and printing refractory powders. This report details the LPBF process, how irregular refractory powder can be prepared for LPBF, and the equipment that is available to support the program.

36 MATERIALS SCIENCE↗

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗

Development of Quality Control Methods for Robust and Reliable Sensor Design

The successful adoption of additive manufacturing for the rapid prototyping of printed sensors requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and sensor interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed sensor. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver prints on an aluminum alloy substrate. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work supports the establishment of process control steps that are necessary for verifying the reliability of printed devices prior to its deployment in critical experiments.

36 MATERIALS SCIENCE↗

Adhesion Testing of Direct-Write Printed Ink on Metallic Structural Components

The successful adoption of additive manufacturing for the rapid prototyping of direct-write printed electronics requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and printed film interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed device. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver printed films on aluminum alloy substrates. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work support the establishment of process control steps that are necessary for quickly verifying the reliability of printed devices prior to their deployment in critical experiments.

Adhesion test↗

A laser ultrasonics-based approach for rapid screening of high entropy alloys

This project demonstrates a laser ultrasonics-based characterization methodology for rapid metallic materials design and discovery via in situ determination of phases, microstructures and elastic properties with respect to temperature. Ultrasonic waves are strongly affected by material microstructure, and therefore serve as a facile means to probe elastic properties, phase content and their size distributions and volume fractions. In this study, a laser ultrasonic technique is used to systematically study the evolution of properties in a set of interrelated simple binary alloys and high entropy alloys (HEA). Phase transformations and microstructural changes inferred from the ultrasonic signals will be correlated with electron microscopy data and predictions using calculations of phase diagrams (CALPHAD). The non-contact and non-destructive ultrasonic testing approach developed in this study could overcome several limitations associated with current material characterization methods for materials discovery. It is expected that laser ultrasonics-based methodology developed in this work will be utilized to evaluate novel graded composition HEAs currently being developed at the Idaho National Laboratory (INL) using advanced manufacturing methods based on direct energy deposition and spark plasma sintering processes, and contribute to accelerate the discovery of HEAs.

36 MATERIALS SCIENCE↗

Understanding the effects of fabrication process on BaZr 0.9 Y 0.1 O 3– δ grain-boundary chemistry using atom probe tomography

Proton-conducting oxides, such as BaZr 0.9 Y 0.1 O 3–δ (BZY10), are receiving significant scientific attention for application in a variety of electrochemical applications. It has been shown that the synthesis route has a significant effect on the ionic behavior of these materials, especially the grain boundaries (GB). In this study, laser-pulsed atom probe tomography (APT) is used to characterize the GB chemistry of BZY10 samples prepared by four different methods: (1) spark plasma sintering (SPS), (2) conventional sintering followed by high-temperature annealing (HT), (3) conventional sintering with NiO used as a sintering aid (SSR-Ni), and (4) solid-state reactive sintering of oxide precursor powders with NiO as a reactive sintering aid (SSRS-Ni). Oxygen depletion (corresponding to oxygen vacancy accumulation) was observed at every GB in this study, consistent with the positive space-charge GB region commonly assigned to these materials. In contrast to the consistent trends associated with oxygen depletion, cation constituents showed varying segregation/depletion behaviors. The samples that used NiO revealed Ni preferentially segregating to the GB. The most common impurities in BZY10 are Al, Fe, Mg, Si, and Sr, all of which generally accumulate at GBs. In order to quantify these chemical trends, the APT method was optimized for this material supplemented with understanding from density functional theory (DFT). Finally, this APT study reveals the complexity of BZY10 GB chemistry and shows that even adjacent GBs in the same material can sometimes show surprisingly different GB chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

U 3 Si 2 and UO 2 composites densified by spark plasma sintering for accident-tolerant fuels

This work reports the synthesis and characterization of the U 3 Si 2 and UO 2 composites sintered by spark plasma sintering (SPS) with controlled microstructures for accident-tolerant fuel application. The U 3 Si 2 and UO 2 composites with different silicide and oxide ratios were synthesized by SPS at temperatures from 1000 to 1300 °C for 5 minutes. The microstructure and phase composition of the SPS densified composite fuels were characterized with scanning electron microscopy, X-ray diffraction (XRD), and energy dispersed spectroscopy (EDS). A systematic study of the thermal and mechanical properties was conducted using microhardness testing and laser flash apparatus, along with oxidation resistance measurements using thermogravimetric analysis (TGA). The results show that the synthesis of composite fuels can be achieved with a 90% theoretical density (TD) at 1000 °C and over 95% TD when sintered at 1300 °C. XRD and EDS results confirmed that the dominant phases in the composites are U 3 Si 2 and UO 2 . Improved physical density generally leads to improved hardness, fracture toughness, thermal diffusivity, and onset temperature during the oxidation process. U 3 Si 2 was found to play a dominant role in determining the mechanical and oxidation properties of the composite fuels, whereas UO 2 had a more important impact on controlling the thermal diffusivity of the composites. The composite with 50 wt% UO 2 sintered at 1300 °C displayed the onset oxidation temperature of 500 °C by dynamic oxidation testing using TGA at a ramp degree of 10 °C/min. The composite also achieved a high fracture toughness of ~3.5 MPa m ½ . Finally, these results highlight the potential of composite fuel forms densified by SPS with simultaneously enhanced fissile element density, fracture toughness, thermal transport properties, and oxidation resistance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

3D printed transparent ceramic YAG laser rods: Matching the core-clad refractive index

Yttrium Aluminum Garnet (YAG) solid state laser gain media rods with an active Neodymium-doped core and an optically-clear cladding region were additively manufactured via direct-ink-writing (DIW), followed by sintering and hot isostatic pressing to form fully dense optical ceramics. Lutetium and Gadolinium were chosen as optically-inert co-doping ions in the clad to match the increase in refractive index caused by the Neodymium in the core. Additionally, either 11.6% Lutetium or 3.8% Gadolinium can be used to match the index change from 2% neodymium; however, differences in diffusion distances across the core-clad interface lead to large fluctuations in index in that region. These index fluctuations can be minimized either by matching dopants with similar diffusion distances, or by implementing a gradual gradient in the doping profile, possible through DIW, rather than a sharp compositional interface attainable via more standard fabrication methods. This improvement in index homogeneity resulted in a 40% improvement in lasing performance compared with that of a core-clad rod fabricated with a sharp interface between the doped and undoped regions.

36 MATERIALS SCIENCE↗

Binderjet Additive Manufacturing for Complex Heat Exchanger Geometries

Concentrated Solar Power (CSP) systems play a role in the worlds development of renewable energy. Mirrors are used to concentrate sunlight that is converted into electricity or other forms of useful energy. CSP impact depends significantly on its overall economics. The U.S. Department of Energy’s (DOE’s) Solar Energy Technology Office (SETO) cost goals for 2030include $0.05/kWh levelized cost of electricity (LCOE) for a baseload plant [1]. The power cycle cost goal is $900/kWe [1]. The envisioned recompression supercritical carbondioxide (sCO2) power cycle includes four heat exchangers, which together are at least ¾ of the total power cycle cost. Meeting the cost target requires reducing the heat exchanger cost. The 260 bar and 588 °C heat exchanger requirements are challenging. Shell and tube heat exchangers can meet the requirements, but the size and cost are prohibitive. State-of-the-art diffusion bonded printed circuit heat exchanger designs are 3 m3 or larger and expensive to manufacture. Additive manufacturing enables novel heat exchanger geometries that can reduce heat exchanger size and mass [2]. Binderjet technology is an additive manufacturing modality. It selectively deposits binder material onto the powder bed to form a solid part one layer at a time. Once applied, the binder is cured, the remaining powder removed, and the part heat treated in steps to remove the binder, sinter the metal powder, and densify the part. The Binderjet printing process is more than 10x faster than the best-known metal additive modality, direct metal laser melting (DMLM), thus enabling 10x the part through-put rate [3]. The high throughput rate results in a low-cost manufacturing process capable of creating complex heat exchanger geometries. This paper introduces a complex heat exchanger geometry and methods of Binderjet processing to fabricate the geometry.

Barua, Ananda↗

Dissolution of Additively Manufactured Mo Disks and Structures for Accelerator Based Production of Mo-99

The press-and-sinter approach for production of Mo targets has been successfully tested and demonstrated. The main advantage of this process is that it uses readily available technology and tools that have been tuned for production of various metal and metal oxide targets. However, certain target design specifications, such as dimensional accuracy of the diameter and thickness of the disks, are required for proper fit into a target holder and therefore place strict tolerances on sintered Mo disks intended for accelerator production. Furthermore, having a target composed of multiple disks poses certain challenges for post-irradiation processing, where there is a potential for spillage of individual disks during the manipulation for dissolution inside a processing hot cell. Additive manufacturing (AM), also referred to as 3D printing, provides capabilities to design and build a single-piece Mo target that provides the opportunity for better geometry for optimized production of Mo-99, improved cooling capability, and safer post-irradiation handling. A drawback of AM Mo structures is roughness of finished surfaces, which could reduce the effectiveness of gas cooling systems. Process development for AM Mo structures using selective laser melting is described in work by Gibson and Lowden. For post-irradiation processing, it is important to look at the dissolution behavior of AM Mo structures in comparison to readily dissolved press-and-sinter Mo targets. The dissolution behavior of press-and-sinter targets has been well documented in our previous reports. In this report, we discuss results of dissolution experiments conducted with AM Mo disks and structures (provided by Oak Ridge National Laboratory [ORNL]) in 50% hydrogen peroxide (H 2 O 2 ).

36 MATERIALS SCIENCE↗

Microstructure evolution of gadolinium doped cerium oxide under large thermal gradients

In this report the effects of large thermal gradient annealing on the microstructure of 10 mol% gadolinium doped ceria (GDC) were investigated. GDC powder was prepared by solvent deficient method and sintered at 1650 °C for 10 h to achieve dense ceramics with ~8 μm grain size. The densified GDC samples were subsequently annealed using a 60 W infrared laser at over 2100 °C for 1 h under a thermal gradient equivalent to ~0.3–0.5 °C/μm. The post-annealed samples at 2150 °C for 1 h exhibit grains with average length and width of 37 and 28 μm, respectively. Electron backscattered diffraction (EBSD) analysis revealed that the post-annealed sample at 2150 °C consists of grains oriented close to five principal directions (<4 3 10>, <0 0 1> and <13 1 14> on [0 0 1], and <7 6 20> and <7 2 7> on [0 1 0]) within a tolerance angle of ±10°, whereas the grains of the pre-annealed sample are randomly oriented. Gadolinium diffuses 20–30 μm away from the irradiated surface, with the measured composition of regions deeper than 30 μm, Ce 0.86 Gd 0.14 O 1.93 , is close to that of the pre-annealed sample, Ce 0.87 Gd 0.13 O 1.94 . Enhancement of total conductivity of the post-annealed GDC (1.1 × 10 -3 S cm -1 at 500 °C, and 2.1 × 10 -2 S cm -1 at 700 °C) is observed when compared to the pre-annealed GDC (3.1 × 10 -5 S cm -1 at 500 °C, and 1.7 × 10 -3 S cm -1 at 700 °C), and points to the decrease in the grain boundary (GB) resistivity. This could be attributed to both the change in GB area and grain alignment.

36 MATERIALS SCIENCE↗

Orientation microscopy–assisted grain boundary analysis for protonic ceramic cell electrolytes

Abstract Grain boundaries in protonic ceramic cell (PCC) electrolytes hinder proton transport, reducing interfacial conductivity. In multicomponent PCC electrolytes, the inclusion of sintering aids further accentuates the complexity of grain boundaries. In this study, we synthesize nanocrystalline BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3− δ thin films via pulsed laser deposition and analyze their grain boundary character distributions using orientation data collected by precession electron diffraction technique. The results reveal an anisotropic distribution of grain boundary characters, with notably high populations of 180°‐tilt and twist grain boundaries. These findings provide critical insights into identifying the predominant grain boundaries in this PCC electrolyte material, assessing the vast five‐dimensional grain boundary space.

Patel, Sooraj [School of Aerospace and Mechanical ↗

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗

Versatile soil gas concentration and isotope monitoring: optimization and integration of novel soil gas probes with online trace gas detection

Abstract. Gas concentrations and isotopic signatures can unveil microbial metabolisms and their responses to environmental changes in soil. Currently, few methods measure in situ soil trace gases such as the products of nitrogen and carbon cycling or volatile organic compounds (VOCs) that constrain microbial biochemical processes like nitrification, methanogenesis, respiration, and microbial communication. Versatile trace gas sampling systems that integrate soil probes with sensitive trace gas analyzers could fill this gap with in situ soil gas measurements that resolve spatial (centimeters) and temporal (minutes) patterns. We developed a system that integrates new porous and hydrophobic sintered polytetrafluoroethylene (sPTFE) diffusive soil gas probes that non-disruptively collect soil gas samples with a transfer system to direct gas from multiple probes to one or more central gas analyzer(s) such as laser and mass spectrometers. Here, we demonstrate the feasibility and versatility of this automated multiprobe system for soil gas measurements of isotopic ratios of nitrous oxide (δ18O, δ15N, and the 15N site preference of N2O), methane, carbon dioxide (δ13C), and VOCs. First, we used an inert silica matrix to challenge probe measurements under controlled gas conditions. By changing and controlling system flow parameters, including the probe flow rate, we optimized recovery of representative soil gas samples while reducing sampling artifacts on subsurface concentrations. Second, we used this system to provide a real-time window into the impact of environmental manipulation of irrigation and soil redox conditions on in situ N2O and VOC concentrations. Moreover, to reveal the dynamics in the stable isotope ratios of N2O (i.e., 14N14N16O, 14N15N16O, 15N14N16O, and 14N14N18O), we developed a new high-precision laser spectrometer with a reduced sample volume demand. Our integrated system – a tunable infrared laser direct absorption spectrometry (TILDAS) in parallel with Vocus proton transfer reaction mass spectrometry (PTR-MS), in line with sPTFE soil gas probes – successfully quantified isotopic signatures for N2O, CO2, and VOCs in real time as responses to changes in the dry–wetting cycle and redox conditions. Broadening the collection of trace gases that can be monitored in the subsurface is critical for monitoring biogeochemical cycles, ecosystem health, and management practices at scales relevant to the soil system.

54 ENVIRONMENTAL SCIENCES↗

High temperature tensile properties of H13 tool steel fabricated via binder jet additive manufacturing

H13 is one of the most used steels for hot work tooling applications like die casting. Binder jet additive manufacturing (BJAM) offers a cost-effective solution to fabricate tools with performance enhancing features like internal cooling channels. While full densification of BJAM H13 has been demonstrated in the literature, the room and high temperature tensile properties of the material, and the effect of post-process treatments like hot isostatic pressing (HIP), and heat treatment (HT) are unknown. Here we use HIP+HT to obtain a combination of ultimate tensile strength (UTS) and elongation to failure that is superior to H13 fabricated via laser powder bed fusion and wire arc additive manufacturing. HIP+HT BJAM H13 has a superior UTS (1836 MPa) compared with conventionally processed (1671 MPa) H13 but has lower plastic elongation. We report that as-sintered samples have an extensive network of continuous grain boundary (GB) carbides that contribute to brittle fracture. HIP+HT results in partial dissolution of GB carbides and formation of a fine martensitic microstructure resulting in superior tensile strength and elongation compared with as-sintered H13. We use thermo-kinetic calculations to rationalize the effects of HIP+HT on microstructure and properties.

36 MATERIALS SCIENCE↗

Material jet printing of transparent ceramic Yb:YAG planar waveguides

A new, to the best of our knowledge, 3D additive manufacturing technique utilizing particle-loaded ink jet printing to fabricate transparent ceramic Yb:YAG planar waveguides for laser gain media was demonstrated. Rheological optimization of YAG particle-loaded inks resulted in successful droplet formation and printing resolution. Planar waveguides composed of a Yb:YAG guide encased in undoped YAG cladding were printed with guide thicknesses ranging between 25 and 350 µm and consolidated to high optical quality via solid-state sintering. Sufficiently low optical (1–3%/cm) and intermodal scatter allowed single-mode propagation with a core/clad index difference of &#x0394;<!-- Δ --> n &#x223C;<!-- ~ --> 5.0 &#x00D7;<!-- × --> 10 &#x2212;<!-- - --> 4 (corresponding to 3 at.% Yb). The waveguides were cladding-pumped longitudinally with a 940 nm diode array resulting in 23.6% slope efficiency in 2 ms pulsed operation.

36 MATERIALS SCIENCE↗

Additive manufacturing of amorphous metal soft magnetic composites

Soft magnet alloys are used as magnetic cores for electric motors, transformers, wind turbines and other power generation systems. Soft magnetic cores are expensive and time consuming to manufacture in the complex shapes required for next-generation devices using conventional press and sinter powder metallurgy. The objective of this effort is to additively manufacture high performance soft magnets, with reduced cost and reduced material waste and 10x lower energy (core) loss at the high operating frequencies of many electric machines. Laser powder bed fusion additive manufacturing is used as the fabrication method. Electrical steel and amorphous alloys atomized powders are used as a feedstock materials. Magnetic cores are printed in topology optimized structures such as the Hilbert curve because this has been shown to reduce energy losses by minimizing the eddy currents that circulate within the magnet at high frequencies. In our project, we succeed in printing FeSi 3.5wt% and FeSi 6.5wt% electrical steels, and iron-based soft magnetic amorphous alloys in the shape of Hilbert and Peano curve topology optimized structures. We found that the Peano curve has a higher cut-off frequency than the Hilbert curve, and that amorphous alloys have high cut-off frequencies and higher mechanical hardness than electrical steels. Processing conditions such as laser power, scan speed, and hatching pattern were optimized to achieve high density prints, and optimize magnetic performance. We find that the printing of amorphous alloy soft magnetic cores may be technoeconomically feasible for large scale applications such as transformers, for which supply chain issues and the labor costs of manual fabrication of magnetic cores is prohibitive in some cases.

36 MATERIALS SCIENCE↗