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Quantitative Characterization of the Microstructure-Property Relationships in Ni and MIEC Nanocatalyst-Infiltrated Ni/YSZ Anodes

The performance of solid oxide fuel cell (SOFC) anodes can be improved by infiltration of nanoscale electrocatalysts, which increases triple phase boundary (TPB) density, but only when the added TPBs are active. Quantitative characterization of the microstructure of infiltrated nanocatalysts remains a critical challenge in understanding their role in improved performance. This paper explores the relationship between electrochemical performance and microstructure for Ni/YSZ anodes infiltrated with Ni, gadolinium-doped-ceria (GDC), and Ni/GDC nanocatalysts using a combination of electrochemical impedance spectroscopy (EIS), distribution of relaxation times (DRT) analysis, scanning electron microscopy (SEM) microstructural characterization, and three-dimensional (3-D) anode reconstruction. Estimated polarization resistance improvements as a result of nickel nanoparticle infiltration are discussed.

Rix, Jillian↗

Survey of Modeling and Simulation Techniques for Advanced Manufacturing Technologies Volume I – Predicting Initial Microstructures

This report summarizes the current state of modeling and simulation methods for predicting the initial structure and properties of material in components assembled using advanced manufacturing technologies (AMTs). The report is the first volume in a two-volume series. This first volume focuses on predicting initial microstructures of AM material. The second volume discusses predicting material properties given the initial microstructure. The focus is on technologies of particular relevance to the design and manufacture of nuclear reactor components. The purpose of the report is to help develop the technical knowledge base to support regulatory decisions that will be needed to assess nuclear components manufactured with AMTs as these components are installed at nuclear power plants (NPPs). The report develops a list of AMTs of particular interest to the NRC and summarizes the key microstructural features and corresponding processing parameters relevant to each technology. Further sections describe available physically-based and data-driven prediction methods and survey widely available software tools. The report concludes with a summary of gaps that may be of particular interest to the NRC when evaluating modeling and simulation methods for AMTs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Effect of thermal aging on microstructure and crack growth response of Alloy 152 weld

Nickel-based Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate for 40-80 years. Likewise, advanced water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is a potential concern for the long-term performance of both existing and advanced nuclear power plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 152 weldments during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni2Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service). The microstructural characterization by means of synchrotron X-ray did not find evidence of LRO in any of the three heats aged to an equivalent of 60 years of service. Testing in a primary water environment of a heat of Alloy 152 aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloy. However, the SCC CGR response of the aged sample appears to show a deterioration in performance.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Quasi-static to Dynamic Response and Microstructure Development of Tantalum-Tungsten Alloys

Lawrence Livermore National Laboratory (LLNL) has a need to understand the quasi-static to dynamic mechanical response and microstructure evolution of tantalum-tungsten (Ta-W) alloys made by conventional wrought processing and additive manufacturing (AM). This two-year work scope will be performed at the Colorado School of Mines (Mines) and will include quasi-static (e.g., 10 -3 s -1 ) mechanical testing in tension and compression, along with high strain rate (Kolsky) pressure bar testing in tension and compression (e.g., 10 3 s -1 ), without and with temperature variations. Gas gun experiments at higher strain rates (e.g., over 10 3 s -1 ) will also be pursued. Complementary microstructure characterization will be performed on undeformed and deformed samples to fundamentally understand the role of processing on the microstructure characteristics and resulting deformation mechanisms that dictate the mechanical response of these alloys with variations in strain rate, temperature, and strain state. Alloys of interest will be Ta-based, containing up to 10 wt.% W. LLNL will supply initial wrought-processed material for sample machining. LLNL will also supply samples built by AM during the project for testing. Arc melting and casting may also be performed at Mines to produce small quantities of different alloys for machining and exploratory testing on an as-needed basis. This project will support multiple postdocs and graduate students at Mines, training them with the knowledge, skills, and abilities needed to study materials under extreme conditions of interest to the National Nuclear Security Agency.

36 MATERIALS SCIENCE↗

Damage Accumulations Predictions for Boiler Components Via Microstructurally Informed Material Models

The goal of the project was to model material behavior and degradation during cyclic plasticity— with and without hold time—for nickel-based superalloys used in USC (ultra-super-critical) and A-USC (advanced-ultra-super-critical) boiler components. The study provided physically informed models, capturing the microstructural changes taking place in the industrial components under cyclic loading and long duration stress (up to 300,000 hours) and high temperature exposure (1100°F/593°C to 1400°F/760°C). The major developments were: 1) Qualitative and quantitative understanding of microstructure evolution (gamma prime precipitates), deformation (dislocation density), and damage mechanisms of Haynes ® 282 alloy. 2) Qualitative understanding of microstructural features generating local strain variations. 3) A continuum damage mechanics model (CDM) for Haynes ® 282 alloy at 1100°F to 1400°F capturing cyclic behavior with and without hold time. 4) Structural analysis for creep and LCF life predictions of an USC thick-wall Grade 91 superheater steel header and understanding life sensitivity to wall thickness of an AUSC Haynes ® 282 header.

20 FOSSIL-FUELED POWER PLANTS↗

Effect of thermal aging on microstructure and stress corrosion cracking behavior of Alloy 152 weldment

Nickel-based Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate for 40-80 years. Likewise, water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is a potential concern for the long-term performance of both existing and advanced nuclear power plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 152 weldments during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni2Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged to an equivalent of 60 years of service. Testing in a primary water environment of two heats of Alloy 152 aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. However, the SCC CGR response of the aged samples appears to show a deterioration in performance, confirming our previous observation.

36 MATERIALS SCIENCE↗

BERT Non-Destructively Probes the Microstructure of Dissimilar Welds [Poster]

Energy-resolved neutron imaging (ERNI) utilizes contrast provided by diffraction. Microstructure with >100µm grains as in cast, annealed or welded materials is difficult to characterize by X-ray or electron-based methods $\Rightarrow$ Well-suited for neutron Bragg-edge radiography. BERT was applied to dissimilar welds of Inconel on steel produced by additive manufacturing. Viewing the sample at time-of-flight/energy/wavelength where a single grain orientation dominates the attenuation allows to map grain orientations. Similarly to electron-backscatter diffraction (EBSD) but on cm length scales and through-thickness. Combined with texture measurements on the HIPPO instrument, identifying major grain orientations, 2D and 3D grain orientation maps are feasible. Results can guide development of thermo-mechanical treatment avoiding or introducing such microstructures, characterize dissimilar welds, interpretation of acoustic signals for quality control, guide destructive examination with X-rays/electrons, or provide data for codes predicting such microstructures.

36 MATERIALS SCIENCE↗

Evaluation of In-Situ AM Process Monitoring Techniques and Potential for Detecting Process Anomalies and Undesirable Microstructures

The US Department of Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program is pursuing rapid qualification of new materials for fabrication of nuclear relevant components using advanced manufacturing techniques. Particular interest is placed on code-qualifying stainless steel (SS) 316H processed by laser powder bed fusion (LPBF) additive manufacturing. A paradigm that incorporates data from in-situ sensing during the printing, ex-situ characterization, and advanced artificial intelligence–based models was established under the Transformation Challenge Reactor (TCR) program to develop a pedigree for each fabricated component that could be tracked from the feedstock to the component’s release for application. Under the TCR program, the Peregrine software was developed as a tool for incorporating the vast amounts of in-situ and ex-situ characterization data collected; all data stored on a rapidly growing digital platform. The digital platform allows for users to link site-specific process anomalies to the macro- and microstructure. The platform will eventually be able to predict component performance, which will be crucial to qualifying materials and components in risk-averse industries such as those supporting and building nuclear reactors. Current in-situ process monitoring techniques that are already integrated with software like Peregrine are advantageous for identifying process anomalies including powder spatter, component edge swelling, recoating-build interactions, and so on. However, additional data are required to fully predict the resulting microstructures needed for identifying relationships to component performance. The rapid cooling rates observed in LPBF are some of the highest of any bulk manufacturing process, resulting in heterogenous microstructures and typically causing anisotropy in mechanical properties. Moreover, evolved residual thermal stresses are high, which can cause severe defects such as delamination or cracking. Therefore, other in-situ monitoring methods are warranted for exploration to measure and map the thermal history, and potentially the stress state, of each build. This report summarizes different in-situ monitoring strategies proposed for LPBF with a focus on the more developed sensor systems. Novel capabilities for measuring melt pool temperatures are also addressed to better inform modeling efforts.

36 MATERIALS SCIENCE↗

Effect of Thermal Aging on Microstructure and Stress Corrosion Cracking Behavior of an Alloy 152 1st Layer Butter Weldment

Nickel-based Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate for 40- 80 years. Likewise, water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is critical for the long-term performance of both existing and advanced nuclear power plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 152 weldments during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni2Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for different durations up to 75,000h (equivalent to 60 years of reactor service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged at 370°C and 450°C to an equivalent of 60 years of service. However, the first weld butter layer has high levels of deformation and is highly susceptible to SCC even in its non-aged condition. Nanohardness testing confirmed the extreme hardening with aging (ΔHV ≅ 100) at two locations within this weldment. In absence of LRO, hardening is suspected to be due to thermally-induced Cr carbide precipitation and coarsening. Testing in a primary water environment of the 1st layer of Alloy 152 weld butter aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. Similarly, the SCC CGR response of the aged weld butter does not appear to show a deterioration in performance, however, the difficult-to-test weldment geometry may affect the test results.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Modeling Oxygen Partial Pressure in Solid Oxide Electrolysis Cells: The Microstructure Effect

Oxygen partial pressure is an important thermodynamic state variable that affects both the performance and degradation of solid oxide electrolysis cells. In this work, a 3D model developed from Virkar’s 1D model has been applied to reconstructed and synthetic microstructures of Ni-YSZ-GDC-LSCF cell. The effect of the microstructures, including the thickness of the YSZ and GDC layer, and the compositions of the hydrogen and oxygen electrode, on the distribution of oxygen partial pressure has been investigated. The results show that the maximum oxygen partial pressure may occur on the interface between oxygen electrode and GDC layer or between GDC layer and YSZ layer depending on the rate of oxygen ion exchange between GDC and YSZ. A thicker GDC layer lowers the maximum oxygen partial pressure in the cell, while a thicker YSZ layer lowers the maximum oxygen partial pressure in the hydrogen electrode. In addition, the Ni:YSZ ratio and porosity also affects the maximum partial pressure. These findings provide insights on mitigating degradation in solid oxide electrolysis cell by tuning the microstructures.

Lei, Yinkai↗

Microstructural evaluation of the creep behavior in L-PBF Ni-based superalloys

This presentation at ICAM 2024 Conference focuses on the commonalities and differences in the creep rupture behavior and creep mechanisms for three distinct classes of laser powder-bed fusion (L-PBF) Ni-based superalloys (γ’-precipitate strengthened Haynes® 282®, γ’/γ”/δ-precipitate strengthened Alloy 718, and solid-solution strengthened Alloy 625) as compared to conventionally processed counterparts. A comparison of Larson-Miller parameter plots establishes that these alloys perform statistically within the bounds established for the wrought product, despite having dissimilar microstructural features and other artefacts associated with PBF-LB manufacturing and post-processing heat treatment. To understand the failure and the impact of composition, minor phases, and deformation defects on creep behavior, the fractography has been performed and microstructures have been evaluated in detail with SEM-EDS, EBSD, and HAADF-STEM. The underlying diffusional and dislocation creep mechanisms associated with this microstructural evaluation is discussed. This work is supported by NETL-FWP-1022408 Advanced Turbines.

Sudbrack, Chantal↗

Assessment of Microstructure Prediction Capabilities for Powder Bed Fusion Stainless Steel 316

The Advanced Materials and Manufacturing Technologies program aims to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy. However, the characteristic process-structure-property relationships of additive manufacturing (AM) materials pose challenges for the qualification and certification of AM nuclear components. In particular, component-scale variations in microstructure and properties can be driven by localized changes in melt pool dynamics due to how process parameters interact with different part geometries. Computational modeling tools can play a crucial role in predicting and controlling this variability. This report presents final results on process modeling tools designed to predict microstructure variability in additively manufactured stainless steel 316 parts. It details the software packages and physical modeling approaches employed to simulate an AM component within an automated process modeling workflow. Results are demonstrated through comparisons between predicted microstructures and experimental measurements across various representative processing conditions. The report concludes by discussing identified challenges and future opportunities for connecting the developed simulation workflow with mechanics simulations for prediction of part performance.

36 MATERIALS SCIENCE↗

Ultra-Fast Laser Fabrication of Alumina Micro-Sample Array and High-Throughput Characterization of Microstructure and Hardness

In the light of recent advances in material informatics, there is a great demand for high-throughput approaches of sample fabrication and property characterization. Currently, no high-throughput approach has been demonstrated for the fast sampling of the microstructure and the correlated properties. In this paper, we demonstrate the ultra-fast fabrication of an alumina sample array and the high-throughput hardness characterization of these sample units. The alumina sample array was fabricated using picosecond (PS) laser micromachining and CO2 laser sintering within a short time (i.e., less than a few minutes). After laser sintering, the hardness of these sample units was characterized using micro-indentation, and the microstructure was observed using scanning electron microscopy (SEM). In each sample unit, the microstructure was uniform for the entire top surface and within about 20 µm depth from the top surface. The relative density (RD) and corresponding micro-hardness of the sample units was found to continuously vary over a wide range from 89% RD with 600 kgf/mm2 hardness to 99% RD with 1609 kgf/mm2 hardness. For these laser-sintered samples, the correlation of hardness and relative density of the alumina matched well with the literature reports on sintered alumina obtained using conventional low-throughput furnace sintering experiments.

36 MATERIALS SCIENCE↗

Predicting Mechanical Properties from Microstructure Images in Fiber-Reinforced Polymers Using Convolutional Neural Networks

Evaluating the mechanical response of fiber-reinforced composites can be extremely time-consuming and expensive. Machine learning (ML) techniques offer a means for faster predictions via models trained on existing input–output pairs and have exhibited success in composite research. This paper explores a fully convolutional neural network modified from StressNet, which was originally used for linear elastic materials, and extended here for a non-linear finite element (FE) simulation to predict the stress field in 2D slices of segmented tomography images of a fiber-reinforced polymer specimen. The network was trained and evaluated on data generated from the FE simulations of the exact microstructure. The testing results show that the trained network accurately captures the characteristics of the stress distribution, especially on fibers, solely from the segmented microstructure images. The trained model can make predictions within seconds in a single forward pass on an ordinary laptop, given the input microstructure, compared to 92.5 h to run the full FE simulation on a high-performance computing cluster. These results show promise in using ML techniques to conduct fast structural analysis for fiber-reinforced composites and suggest a corollary that the trained model can be used to identify the location of potential damage sites in fiber-reinforced polymers.

Sun, Yixuan (ORCID:0000000311093380)↗

The Effect of Interlayer Delay on the Heat Accumulation, Microstructures, and Properties in Laser Hot Wire Directed Energy Deposition of Ti-6Al-4V Single-Wall

Laser hot wire directed energy deposition (LHW-DED) is a layer-by-layer additive manufacturing technique that permits the fabrication of large-scale Ti-6Al-4V (Ti64) components with a high deposition rate and has gained traction in the aerospace sector in recent years. However, one of the major challenges in LHW-DED Ti64 is heat accumulation, which affects the part quality, microstructure, and properties of as-built specimens. These issues require a comprehensive understanding of the layerwise heat-accumulation-driven process–structure–property relationship in as-deposited samples. In this study, a systematic investigation was performed by fabricating three Ti-6Al-4V single-wall specimens with distinct interlayer delays, i.e., 0, 120, and 300 s. The real-time acquisition of high-fidelity thermal data and high-resolution melt pool images were utilized to demonstrate a direct correlation between layerwise heat accumulation and melt pool dimensions. The results revealed that the maximum heat buildup temperature of the topmost layer decreased from 660 °C to 263 °C with an increase to a 300 s interlayer delay, allowing for better control of the melt pool dimensions, which then resulted in improved part accuracy. Furthermore, the investigation of the location-specific composition, microstructure, and mechanical properties demonstrated that heat buildup resulted in the coarsening of microstructures and, consequently, the reduction of micro-hardness with increasing height. Extending the delay by 120 s resulted in a 5% improvement in the mechanical properties, including an increase in the yield strength from 817 MPa to 859 MPa and the ultimate tensile strength from 914 MPa to 959 MPa. Cooling rates estimated at 900 °C using a one-dimensional thermal model based on a numerical method allowed us to establish the process–structure–property relationship for the wall specimens. The study provides deeper insight into the effect of heat buildup in LHW-DED and serves as a guide for tailoring the properties of as-deposited specimens by regulating interlayer delay.

36 MATERIALS SCIENCE↗

In Situ Prediction of Microstructure and Mechanical Properties in Laser-Remelted Al-Si Alloys: Towards Enhanced Additive Manufacturing

Laser surface remelting of aluminum alloys has emerged as a promising technique to enhance mechanical properties through refined microstructures. This process involves rapid cooling rates ranging from 10 3 to 10 8 °C/s, which increase solid solubility within aluminum alloys, shifting their eutectic composition to a larger value of silicon content. Consequently, the resulting microstructure combines a strengthened aluminum matrix with silicon fibers. This study focuses on the laser scanning of Al-Si aluminum alloy to reduce the size of aluminum matrix spacings and transform fibrous silicon particles from micrometer to nanometer dimensions. Analysis revealed that the eutectic structure contained 17.55% silicon by weight, surpassing the equilibrium eutectic composition of 12.6% silicon. Microstructure dimensions within the molten zones, termed ‘melt pools’, were extensively examined using Scanning Electron Microscopy (SEM) at intervals of approximately 20 μm from the surface. A notable increase in hardness, exceeding 50% compared to the base plate, was observed in the melt pool regions. Thus, it is exemplified that laser surface remelting introduces a novel strengthening mechanism in the alloy. Moreover, this study develops an in situ method for predicting melt pool properties and dimensions. A predictive model is proposed, correlating energy density and spectral signals emitted during laser remelting with mechanical properties and melt pool dimensions. This method significantly reduces characterization time from days to seconds, offering a streamlined approach for future studies in additive manufacturing.

36 MATERIALS SCIENCE↗

Microstructure of Neutron-Irradiated Al 3 Hf-Al Thermal Neutron Absorber Materials

A thermal neutron-absorbing metal matrix composite (MMC) comprised of Al 3 Hf particles in an aluminum matrix was developed to filter out thermal neutrons and create a fast flux environment for material testing in a mixed-spectrum nuclear reactor. Intermetallic Al 3 Hf particles capture thermal neutrons and are embedded in a highly conductive aluminum matrix that provides conductive cooling of the heat generated due to thermal neutron capture by the hafnium. These Al 3 Hf-Al MMCs were fabricated using powder metallurgy via hot pressing. The specimens were neutron-irradiated to between 1.12 and 5.38 dpa and temperatures ranging from 286 °C to 400 °C. The post-irradiation examination included microstructure characterization using transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy. This study reports the microstructural observations of four irradiated samples and one unirradiated control sample. All the samples showed the presence of oxide at the particle–matrix interface. The irradiated specimens revealed needle-like structures that extended from the surface of the Al 3 Hf particles into the Al matrix. An automated segmentation tool was implemented based on a YOLO11 computer vision-based approach to identify dislocation lines and loops in TEM images of the irradiated Al-Al 3 Hf MMCs. This work provides insight into the microstructural stability of Al 3 Hf-Al MMCs under irradiation, supporting their consideration as a novel neutron absorber that enables advanced spectral tailoring.

36 MATERIALS SCIENCE↗

The Influence of Microstructure on TCR for Inkjet-Printed Resistive Temperature Detectors Fabricated Using AgNO 3 /Ethylene-Glycol-Based Inks

This study investigated the influence of microstructure on the performance of Ag inkjet-printed, resistive temperature detectors (RTDs) fabricated using particle-free inks based on a silver nitrate (AgNO 3 ) precursor and ethylene glycol as the ink solvent. Specifically, the temperature coefficient of resistance (TCR) and sensitivity for sensors printed using inks that use monoethylene glycol (mono-EG), diethylene glycol (di-EG), and triethylene glycol (tri-EG) and subjected to a low-pressure argon (Ar) plasma after printing were investigated. Scanning electron microscopy (SEM) confirmed previous findings that microstructure is strongly influenced by the ink solvent, with mono-EG inks producing dense structures, while di- and tri-EG inks produce porous structures, with tri-EG inks yielding the most porous structures. RTD testing revealed that sensors printed using mono-EG ink exhibited the highest TCR (1.7 × 10 -3 /°C), followed by di-EG ink (8.2 × 10 -4 /°C) and tri-EG ink (7.2 × 10 -4 /°C). These findings indicate that porosity exhibits a strong negative influence on TCR. Sensitivity was not strongly influenced by microstructure but rather by the resistance of RTD. The highest sensitivity (0.84 Ω/°C) was observed for an RTD printed using mono-EG ink but not under plasma exposure conditions that yield the highest TCR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗