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All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Baseline Characterization Database Verification Report – IG-110 Billet 10X69

The purpose of this engineering calculations and analysis report (ECAR) is to present the data being collected in the Baseline Graphite Characterization program. This program is directly tasked with supporting Idaho National Laboratory’s (INL’s) research and development efforts in the Advanced Reactor Technologies (ART) program. This program populates a comprehensive database that will reflect the baseline properties of nuclear-grade graphite with regard to individual grade, billet, and position within individual billets. The physical- and mechanical-property information being collected will be transferred to the Nuclear Data Management and Analysis System (NDMAS), and that database will help populate the handbook of property data available to member nations of the Generation-IV International Forum. The transfer of these data from the applicable technical lead to the dissemination databases available to other end users requires a full review of test procedures and data-collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents that analysis for IG-110, Billet 10X69 and facilitates the release of the associated data to the NDMAS custodians.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

ECAR-3727 Baseline Characterization Database Verification Report - NBG-17 Billet 830-3

The purpose of this engineering calculations and analysis report is to present the data being collected in the Baseline Graphite Characterization Program, which is directly tasked with supporting the Idaho National Laboratory’s (INL’s) research and development efforts on the Advanced Reactor Technologies (ART) Program. This program is populating a comprehensive database that will reflect the baseline properties of nuclear-grade graphite with regard to individual grade, billet, and position within individual billets. The physical and mechanical property information being collected will be transferred to the Nuclear Data Management and Analysis System (NDMAS), and that database will help populate the handbook of property data available to member nations of the Generation IV International Forum. Transfer of these data from the applicable technical lead to the dissemination databases available to other end users requires a full review of the test procedures and data-collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents the analysis for NBG-17 Billet 830-3 and facilitates release of associated data to the NDMAS custodians.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2017

Baseline Characterization Database Verification Report – IG-110 Billet 08-9-052-7

The purpose of this Engineering Calculations and Analysis Report is to present the data being collected in the Baseline Graphite Characterization program, which is directly tasked with supporting the Idaho National Laboratory’s (INL’s) research and development efforts on the Advanced Reactor Technologies (ART) program. This program is populating a comprehensive database that will reflect the baseline properties of nuclear-grade graphite with regard to individual grade, billet, and position within individual billets. The physical and mechanical property information being collected will be transferred to the NGNP Nuclear Data Management and Analysis System (NDMAS), and from that database will help populate the handbook of property data available to member nations of the Generation IV International Forum (GIF). The transfer of this data from the applicable technical lead to the dissemination databases available to other end users requires a full review of the test procedures and data collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents that analysis for IG-110 billet 08-9-052-7 and facilitates the release of the associated data to the NDMAS custodians.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

ECAR-1930 BASELINE CHARACTERIZATION DATABASE VERIFICATION REPORT - NBG-18 BILLET 635-14

The purpose of this Engineering Calculations and Analysis Report is to present the data being collected in the Baseline Graphite Characterization program, which is directly tasked with supporting the Idaho National Laboratory’s (INL’s) research and development efforts on the Next Generation Nuclear Plant (NGNP)/Very High Temperature Reactor (VHTR). This program is populating a comprehensive database that will reflect the baseline properties of nuclear-grade graphite with regard to individual grade, billet, and position within individual billets. The physical and mechanical property information being collected will be transferred to the NGNP Data Management and Analysis System (NDMAS), and from that database will help populate handbook of property data available to member nations of the Generation IV International Forum (GIF). The transfer of this data from the applicable technical lead to the dissemination databases available to other end users requires a full review of the test procedures and data collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents that analysis for a single billet of nuclear grade graphite (NBG-18 billet 635-14) and facilitates the release of the associated data to the NDMAS custodians.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

NDMAS

Overview of Current ART-GCR Data: Fuel Fabrication, Irradiation Monitoring (Fuel & Graphite – near real-time for HDG-1), Post-Irradiation Examination (Fuel & Graphite), Graphite Characterization (Baseline and Irradiated), High Temperature Metals Mechanical Tests, Design, Methods, and Validation Data, Japan Atomic Energy Agency’s High Temperature Test Reactor (HTTR), Argonne National Laboratory’s Natural convection Shutdown heat removal Test Facility (NSTF), Oregon State University’s High Temperature Test Facility (HTTF), Generation IV International VHTR Materials Handbook, Additional related data, and Advanced Test Reactor operations (near real-time).

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Initial Comparison of Baseline Physical and Mechanical Properties for the VHTR Candidate Graphite Grades

High-purity graphite is the core structural material of choice in the Very High Temperature Reactor (VHTR) design, a graphite-moderated, helium-cooled configuration capable of producing thermal energy for power generation as well as process heat for industrial applications that require temperatures higher than the outlet temperatures of present nuclear reactors. The Baseline Graphite Characterization Program is establishing accurate as-manufactured mechanical and physical property distributions in nuclear-grade graphites by providing comprehensive data that captures the level of variation in measured values. In addition to providing a thorough comparison between these values in different graphite grades, the program is also carefully tracking individual specimen source, position, and orientation information in order to provide comparisons both in specific properties and in the associated variability between different lots, different billets, and different positions from within a single billet. This report is a preliminary comparison between each of the grades of graphite that are considered “candidate” grades from four major international graphite producers. These particular grades (NBG-18, NBG-17, PCEA, IG-110, and 2114) are the major focus of the evaluations presently underway on irradiated graphite properties through the series of Advanced Graphite Creep (AGC) experiments. NBG-18, a medium-grain pitch coke graphite from SGL from which billets are formed via vibration molding, was the favored structural material in the pebble-bed configuration. NBG-17 graphite from SGL is essentially NBG-18 with the grain size reduced by a factor of two. PCEA, petroleum coke graphite from GrafTech with a similar grain size to NBG-17, is formed via an extrusion process and was initially considered the favored grade for the prismatic layout. IG-110 and 2114, from Toyo Tanso and Mersen (formerly Carbone Lorraine), respectively, are fine-grain grades produced via an isomolding process. An analysis of the comparison between each of these grades will include not only the differences in fundamental and statistically-significant individual strength levels, but also the differences in the overall variability in properties within each of the grades that will ultimately provide the basis for predicting in-service performance. The comparative performance of the different types of nuclear-grade graphites will naturally continue to evolve as thousands more specimens are fully characterized with regard to strength, physical properties, and thermal performance from the numerous grades of graphite being evaluated.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Sectioning of NBG-17 Graphite Billet

The Advanced Reactor Technologies (ART) Baseline Graphite Characterization program at the Idaho National Laboratory (INL) is performing a comprehensive evaluation of inter-billet variations in as-produced nuclear-grade graphite. Before graphite test specimens are machined, the full-size billets must be pre-sectioned into sub-blocks that can be more easily handled and shipped. As manufactured, NBG-17 billets are rectangular in shape, nearly 6 feet in length, and may exceed 1,500 pounds in weight. Sectioning of these billets must be accomplished via a supplier that is capable of handling and cutting the billets into individual slabs and quartering these slabs into sub-blocks. Billets will be pre-labeled by the Purchaser prior to leaving controlled storage such that traceability of any individual sub-block is never lost during sectioning operations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Non-destructive structural characterization of graphite components using mechanical resonance and deep learning

As compared to conventional nuclear reactors, microreactors have the potential to significantly reduce construction timelines and capital costs, decreasing the barriers for advanced nuclear reactor technologies. However, the lower power output of these microreactors (typically < 20 MWe) creates challenging economics if operation and maintenance costs cannot be sufficiently reduced. The compact size of these designs presents an opportunity for comprehensive in-situ structural health monitoring to provide real-time feedback in order to reduce operational costs associated with maintenance and downtime. Many microreactor concepts use graphite for both in-core neutron moderation and as a structural material, which has typically required some form of periodic and laborious inspection. This report provides a description and assessment of recent work with graphite to couple acoustic-based experimental measurements and characterization with machine learning models to mature structural health monitoring capabilities and generate benefits for the nuclear microreactor industry. With resilient embedded sensors in development in other programs funded by the US Department of Energy’s Office of Nuclear Energy and elsewhere, the work described herein builds upon previously funded efforts to mature non-destructive testing technology that relates measured vibrational signatures to structural changes, using a combination of new experimental measurements and machine learning processing. Building on past successful demonstrations of predictive workflows to identify structural changes in a hexagonal stainless steel test article with excellent acoustic propagation, we first performed baseline characterization on graphite samples with canonical geometries to ensure compatibility and confidence in the applied techniques for a material with distinctly different mechanical properties. In contrast to efforts in previous years, we worked exclusively with unidirectional vibration data that is more comparable to those expected from the existing embedded sensor technologies which are suitable for deployment in a reactor setting. Established acoustic and modern machine-learning-based characterization approaches were applied to the resulting datasets from these simple geometries. Both approaches were found to be highly capable of detecting even small geometric irregularities amongst nominally identical samples. As such, we then moved to testing these approaches for detection of artificial local stress perturbations introduced into a more complex geometry: a hexagonal block with drilled holes. A main outcome of this work is that a generalizable ML workflow can be used to detect and predict the characteristics of small artificial anomalies in a graphite component with a relevant geometry. While this work was performed using surficial vibration data, we expect the approach to be flexible and viable for other monitoring scenarios, such as those with different arrangements or types of sensor arrays. As compared to previously funded efforts, an existing ML workflow based on neural networks was enhanced through the addition of recently developed Fourier neural operators. As applied to previously collected and new vibration datasets, prediction accuracies of anomaly characterizations were greatly improved with minimal added computational cost. As trained on small durations of vibration data (tens of seconds) collected over a realistic number of locations, the model was able to reliably determine the presence of a subtle stress anomaly and begin to provide location estimates. Such an approach is likely to be viable for more relevant reactor damage scenarios for graphite components, such as progressive crack growth or creep.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Summary of Graphite Data Stored within NDMAS

The Graphite Technology Development Project provides data to support the design of graphite core components within specific reactor service conditions of the next generation of high-temperature, gas-cooled nuclear reactors. Physical, mechanical, and thermal properties of nuclear grade graphite were characterized for specimens that were unirradiated, irradiated, and irradiated under various stress conditions. The material properties include diameter, length, mass, density, compressive strength, tensile strength, flexural strength, modulus, resistivity, thermal diffusivity, and thermal expansion coefficient. Baseline graphite specimens are unirradiated from different grades (2114, IG-110, NBG-17, NBG-18, and PCEA) and different types used in different characterization tests (compressive, flexural, tensile, one-inch cylinder, and quarter-inch cylinder). The Advanced Graphite Creep (AGC) irradiation specimens are from a much larger number of grades and cylinder types (creep, piggyback, and pencil). For baseline graphite, characterization data for 7,756 specimens extracted from thirteen graphite billets were captured to the NDMAS database. For AGC experiments, four irradiation campaigns have been completed: AGC-1, AGC-2, AGC-3, and AGC-4. The ongoing HDG-1 (High-Dose Graphite) experiment, which began irradiation with Cycle 168B on August 26, 2020, includes specimens previously irradiated in AGC-2 in addition to the specimens originally destined for AGC-5.. Besides the characterization data, the AGC data includes irradiation monitoring and physics data representing the irradiation conditions of AGC specimens. Currently, all data for AGC-1, AGC-2, and AGC-3 have been captured to the NDMAS database. Only AGC-4 pre-irradiation and irradiation monitoring data have been captured, and HDG-1 pre-irradiation data are in process of being captured for unirradiated specimens. To date, a total of 38,149 material property records have been captured into NDMAS database for baseline and AGC specimens. All characterization data are qualified for use according to their perspective data verification reports. For the AGC irradiation campaigns, a total of 41,502 qualified physics calculation records were added for AGC-1, AGC-2, and AGC-3. Finally, a total of 173,698,505 AGC irradiation monitoring data records (thermocouple temperature, gas flow rate, gas pressure, gas moisture, applied load, and specimen displacement) have been captured to NDMAS; the majority of those records (~94%) are qualified data records.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

PCEA Baseline Characterization: Billet XCP01S8 11 Compressive, Tensile, and Flexure Strengths

Grade PCEA graphite is one of several grades being considered for the core structures of the Next Generation Nuclear Plant (NGNP). An experimental program is underway to describe the statistical nature of the mechanical properties of PCEA graphite, information needed to support the design of graphite components and licensing of the NGNP. It will be necessary to characterize several billets from various lots or batches. The exact number of billets will depend on the observed variability in properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Coal to Carbon Fiber (C2CF) Continuous Processing for High Value Composites (Final Report)

Coal tar is a condensed and recovered by-product of the coking of metallurgical coal for steel production. The heaviest fraction of distilled coal tar is an isotropic pitch largely used as a binder in the manufacturing of carbonaceous electrodes for primary aluminum smelting and in electric arc furnaces. Coal tar pitch offers high carbon yield upon carbonization. In this project, a process to convert the domestically sourced isotropic coal tar pitch, containing very low particulates (QI = 0.32 wt.%), to form flow-domain mesophase pitch amenable for melt spinning into precursor (green) fibers for carbon fiber, was developed and optimized. The final reproducible processing developed is reviewed in this report, along with several characterizations of the mesophase pitch. A final definition of the characteristics of a ‘spinnable’ mesophase pitch is presented. With this mesophase pitch, reproducible and stable multifilament melt spinning was developed, producing green fiber tows with filament diameters of approximately 20 m. The multifilament melt spinning was the most challenging aspect of the project and required the most effort. The best practices learned from this project for melt spinning are reviewed in this report. Once spun, the green fibers were oxidatively stabilized, carbonized and graphitized under inert gas atmosphere to form the final carbon fibers. Given the relatively high softening point of the mesophase pitch, no issues of interfilament fusion were observed during batch oxidation, and subsequent batch carbonization and graphitization went smoothly in all cases. An ~ 80 wt.% conversion of the green fiber mass to final carbon fiber was achieved. After graphitization, the carbon fibers showed high tensile moduli (most were ~ 600 GPa, or 87 Msi) consistent with commercially-available high-performance pitch-based carbon fiber. However, tensile strength and strain to failure were comparatively low. Further work to reduce defects in and on the fiber surfaces would increase these properties. SEM imaging of the graphitic fiber textures is presented herein. Rudimentary composites were fabricated from the carbon fibers and characterized showing similar modulus to baseline composites fabricated with commercial carbon fiber. Finally, a basic economic analysis was done showing the potential to increase the value of the isotropic coal tar pitch by up to 13.6 to 136 times based on a carbon fiber value of $\$$5/lb to $\$$50/lb, respectively. Moreover, the site case study suggests that the coal tar from the single integrated steel mill could supply production of up to 16 kt/yr of carbon fiber. Finally, a technological gap analysis was done which shed light on remaining technical challenges. These challenges included: recovery and utilization of condensates from the mesophase pitch processing, further advancing and increasing stability of the multifilament melt spinning processing, optimization of the oxidation processing, defect reduction for increased carbon fiber strength, and the development of a weaving process towards carbon fiber fabrics. To maximize the coal value chain, the primary objectives of this project were to (a) develop and scale efficient processing technology for producing melt-spinnable mesophase pitch from isotropic coal tar pitch, (b) clarify and simplify tedious continuous fiber processing technologies (particularly multifilament melt spinning of mesophase pitch) towards the efficient production of high performance carbon fiber, and (c) demonstrate and characterize representative composite parts derived from the final carbon fiber. Immense progress was made on all 3 objectives and is detailed in this report.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2023

Microstructural characterization of nuclear graphite: from the microscale to the nanoscale

Multiple reactor designs use graphite as a moderator of the nuclear reactions and as structural support. During the lifetime of the reactor, multiple aging factors such as neutron irradiation, oxidation, and temperature along with others induce changes in the microstructure and crystal lattice of graphite components. The pore morphology and crystal structure of some phases in graphite can be used to trace the evolution of irradiation defects and mechanical properties of graphite. We present a combination of results from several microscopy techniques to investigate the differences between nuclear graphite grades and the effects of neutron irradiation and oxidation at multiple length scales. This multiscale approach is needed to understand the microstructural variations caused by the raw materials and manufacturing processes as well as how the different phases of graphite are affected by the reactor environment. The results provide insight into the oxidation- and radiation-induced changes of graphite and create a robust baseline of microstructure information that can be used for the selection of materials for the next generation of nuclear power stations. Moreover, the experiments conducted in this work provide an overview of the advantages and limitations of the most common techniques used to characterize nuclear graphite and how these techniques might be applied to study other carbon-based materials used in the nuclear industry.

Arregui Mena, Jose'↗
DOE OSTI2026

Quantitative measurement of pebble fuel anisotropy using generalized ellipsometry

The renewed development of high-temperature gas-cooled reactors has created a need to modernize pebble fuel quality control methods. One important specification in these methods is the coefficient of thermal expansion (CTE) anisotropy, which reflects graphite grain alignment and affects fuel performance. This study investigates the feasibility of using two-modulator generalized ellipsometry microscopy (2-MGEM) as a potential surrogate metric for CTE anisotropy. Graphite matrix compacts with controlled levels of anisotropy were fabricated by varying pre-pressures during forming and were subsequently characterized using both optical dilatometry and 2-MGEM. Measured responses were compared to an isotropic reference pebble produced using an industrial manufacturing process to provide a practical baseline. The resulting measurements revealed a strong quantitative correlation between the CTE anisotropy ratio and the corresponding diattenuation ratio. However, propagated measurement uncertainties in the optical method were found to limit definitive pass/fail discrimination, highlighting the need for improved precision before qualification as a quality control tool. Still, the results establish a quantitative relationship between optical and CTE anisotropy and support further development of 2-MGEM as a potential surrogate method for evaluating graphite matrix anisotropy in pebble fuel manufacturing.

Raftery, Alicia [ORNL] (ORCID:0000000259076427)↗
DOE OSTI2024

Production of Carbon Nanomaterials and Sorbents from Domestic U.S. Coal (Final Report)

The main goal of this project was to produce high-value carbon nanomaterials and carbon sorbents from domestic coal resources in a cost-effective manner. Four types of domestic coal samples were processed through a combination of deashing, devolatilization, oxidation, reduction, and activation treatments to produce graphene oxide (GO), reduced graphene oxide (RGO), and activated carbon (AC). The precursors and developed materials were extensively characterized by various methods to investigate the impact of the coal feedstock type on the yield and quality of each product. A commercial graphite-based GO sample was included in the experimental work as the baseline material for comparison with the coal-based materials developed in this work. The performed work also included a technoeconomic analysis and cost estimation for a plant processing 20 tons/day coal, a market evaluation for the graphene materials, and a technology gap analysis. A simple process by concentrated nitric acid oxidation is used to oxidize coal precursors for the production of GO. Fine oxidized coal particles that were separated from larger oxidized coal particles had significantly higher oxygen contents and were identified as coal-based GO samples. Coarse oxidized coal particles were used as precursors for production of AC. Based on the Raman spectroscopy results, coal-based GO samples exhibited G and D bands similar to those of graphite-based GO samples. X-ray photoelectron spectroscopy revealed that coal-based GO samples had surface oxygen contents of ~26-35% that were higher than the oxygen contents of graphite-based GO samples. Larger particles of oxidized coal samples were activated under different conditions to produce high surface area functionalized AC. Prepared materials had surface areas exceeding 1,500 m 2 /g and pore volumes more than 1 cm 3 /g with different pore size distributions. Reduced graphene oxide samples were prepared by thermal reduction of both coal-based and graphite-based GO samples at 170-2800 ºC. Coal-based and graphite-based RGO samples exhibited similar carbon contents, Raman spectra, and XRD profiles. Heat treatment above 1500 ºC shifted RGO to synthetic graphite. Among anthracite, bituminous, subbituminous, and lignite coals tested, anthracite was the best precursor to produce carbon nanomaterials exhibiting properties similar to those of graphite-based materials. Anthracite-based carbon nanomaterials also had the highest production yields. Technoeconomic analysis estimated the production cost of GO and RGO for anthracite-based samples at about 2,600 and 4,200 $/ton, respectively, which is about two orders of magnitude lower than the current estimated price of graphite-based materials. Several gaps to further develop the proposed technology were identified and discussed that include process and equipment optimization, process integration, need for additional bench- and pilot-scale experiments, and other items to reduce the scale up risk. Market analysis reports suggested a compound annual growth rate of 40% for graphene and related materials. Short-term applications include composites, inks, and coatings. However, energy storage applications appear to be the dominant potential long-term applications. Different applications of coal-based GO and RGO need to be explored and clear metrics and standards for each application need to be developed.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2017

Design and Demonstration of Three-Electrode Pouch Cells for Lithium-Ion Batteries

Simple three-electrode pouch cells which can be used in distinguishing the voltage and resistance in individual electrodes of lithium ion batteries have been designed. Baseline (1 mm-staggered alignment, cathode away from a reference electrode) and aligned electrodes to a reference electrode located outside of the anode and cathode were studied to see alignment effects on resistance analysis. Cells composed of A12 graphite anodes, LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC 532 or NCM 523) cathodes, lithium foil references, microporous tri-layer membranes, and electrolytes, were cycled with cathode cutoff voltages between 3.0 V and 4.3 V for formation cycles or 4.6 V for C-rate performance testing. By applying a hybrid pulse power characterization (HPPC) technique to the cells, resistances of the baseline cells contributed by the anode and cathode were found to be different from those of the aligned cells, although overall resistances were close to ones from aligned cells. As a result, resistances obtained via electrochemical impedance spectroscopy (EIS) and 2D simulation were also compared with those obtained from HPPC.

25 ENERGY STORAGE↗
DOE OSTI2018

Nuclear characterization of a general-purpose instrumentation and materials testing location in TREAT

The Transient Reactor Test facility (TREAT) was constructed in the late 1950s, provided thousands of transient irradiations before being placed in standby in 1994, and resumed operations in 2017 in order to reclaim its crucial role in nuclear-heated safety research. The latter half of TREAT’s historic operation was best known for integral-scale testing of fuel specimens under postulated reactor plant accident conditions, while TREAT’s earlier history included extensive simpler phenomena identification tests that elucidated fundamental behaviors and paved the way for these integral-scale tests. Advances in modern computational capabilities and a resurgence of interest in novel reactor technology have created an opportunity for emphasizing modernized science-based and separate effects test capabilities once again at TREAT. An innovative approach to this type of testing has been developed to leverage minor radioactivity built-in during brief TREAT irradiations in low activation hardware to facilitate handling for materials and instrumentation testing. This capability, termed the Minimal Activation Retrievable Capsule Holder (MARCH) irradiation vehicle system, will be used for inaugural fueled experiments in TREAT’s modern era as well as novel approaches to study materials undergoing neutron irradiation and instrumentation development and qualifications. This paper describes a comprehensive nuclear characterization, obtained via computational modeling, of the test position in the MARCH system. Though directly applicable to the MARCH system, the results also provide general quantification of the nuclear performance of the reactor and potential test materials, crucial for evaluating potential experiment design and response in TREAT. The neutron and photon flux environment was calculated via MCNP with ENDF/B-VII.1 nuclear data. Wire heating rate and DPA calculations were also performed and evaluated using historic TREAT test data. Furthermore, these calculations were performed to provide steady-state baseline reference values typical in both half- and full-slotted TREAT core configurations, enabling design scoping analysis prior to development of more specific design testing needs and transient testing experimentation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Demonstration of and future perspective on scaling ultrafast-laser-ablation microstructuring of Li-ion battery electrodes to roll-to-roll production and large-format cells

This work demonstrates integration of an ultrafast laser onto a roll-to-roll machine, the laser structuring of a double-sided, 700 m long roll of graphite battery anode and its subsequent manufacture into 27 Ah prismatic cells. The electrode was ablated with a novel hybrid-microstructure composed of both hexagonally arranged pores for enhanced rate performance and channels for fast electrolyte wetting. Subsequently, this anode and a non-ablated baseline anode are paired with an NMC111 cathode for cell building and electrochemical characterization. Compared to the baseline, laser ablated cells demonstrated a reduction in soaking time of at least 60%, an improvement in fast charge capability with >30% more capacity accepted during 6C charging, and an extension of cycle life of >40% during 0.5C cycling. Further, a perspective is provided on scaling ultrafast laser ablation of battery electrodes to industrial throughputs. Additionally, lessons learned from this pilot-scale demonstration are provided in regards to optical architecture, debris removal, and system control. A techno-economic analysis is used to demonstrate that laser ablation can be integrated into existing electrode manufacturing facilities with only ≈$\$$1.3 per kWh increase (≈2%) in manufacturing cost. Preemptive electrode design for laser ablation is discussed as a further method for enhancing performance. Finally, an analysis of available laser systems and beam-scanning architectures is used to determine design requirements to scale process throughput to a state-of-the-art speed of 50 m min −1 . This analysis demonstrates that laser ablating Li-ion battery electrodes has multiple benefits to manufacturing and battery performance, that the technology already exists to achieve high laser-ablation throughputs, and that integrating ultrafast laser ablation to electrode manufacturing will not create a cost or processing bottleneck.

25 ENERGY STORAGE↗
DOE OSTI2018

Research three-dimensional hierarchical graphite architectures for anodes for fast charging

With current lithium ion batteries optimized for performance under relatively low charge rate conditions, implementation of XFC has been hindered by drawbacks including Li plating, kinetic polarization, and heat dissipation. This project will utilize model-informed design of 3-D hierarchical electrodes to tune key XFC related variables like 1) bulk porosity/tortuosity 2) vertical pore diameter, spacing, and lattice 3) crystallographic orientation of graphite particles relative to exposed surfaces 4) interfacial chemistry of the graphite surfaces through "artificial sEr formation using ALD 5) current collector surface roughness (aspect ratio, roughness factor, etc.). A key aspect of implementing novel electrodes is characterizing them in relevant settings. For this project, ultimately led out of University of Michigan by Neil Dasgupta, that includes both coin cell and 2+ Ah pouch cell testing, as well as comparison testing against baselines. Sandia National Labs will be conducting detailed cell characterization on iterative versions/improvements of the model-based hierarchical electrodes, as well as COTS cells for baseline comparisons. Key metrics include performance under fast charge conditions, as well as the absence or degree of lithium plating. Sandia will use their unique high precision cycling and rapid EIS capabilities to accurately characterize performance and any lithium plating during 6C charging and beyond, coupling electrochemical observations with cell teardown. Sandia will also design custom fixturing to cool cells during rapid charge, to decouple any kinetic effects brought about by cell heating and allow comparisons between different cells and charge rates. Using these techniques, Sandia will assess HOH electrodes from the University of Michigan, as well as aiding in iterative model and electrode design.

25 ENERGY STORAGE↗