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DOE OSTI2023

Mechanical properties of an Al 10 Nb 20 Ta 15 Ti 30 V 5 Zr 20 A2/B2 refractory superalloy and its constituent phases

Refractory superalloys (RSAs) are a new class of high-temperature structural materials consisting of a nanometer-sized mixture of two coherent A2 (disordered BCC) and B2 (ordered) phases. While these RSAs typically exhibit superior mechanical properties at elevated temperatures, they suffer from limited plasticity at lower temperatures, often attributed to the continuous ordered B2 matrix in these two-phase alloys. To knowledgably control the microstructure and mechanical properties of these alloys, the properties of the constitutive phases in RSAs should be known. Currently this information is absent. Here, in the present work, the microstructure and mechanical properties (at 20–1200 °C) of a candidate Al 0.5 NbTa 0.8 Ti 1.5 V 0.2 Zr RSA and two single-phase alloys, which compositions correspond to the compositions of the A2 and B2 phases in the selected RSA, are reported. Interestingly, and quite unexpectedly, the intrinsic mechanical behavior of the constituent A2 and B2 phases, deciphered for the first time in the present study, revealed that they are softer and substantially more ductile than the parent two-phase RSA. Furthermore, the ordered B2 phase exhibits a deformation twinning mechanism leading to twinning induced plasticity (TWIP) coupled with a low APB energy and activity of 1/2<111> dislocations. These mechanisms are thought to be responsible for the high plasticity of the ordered B2 phase. The results presented here question the current assumption that the ordered B2 phase in these RSAs has limited plasticity and strongly indicate that the nature of the B2/A2 interface boundaries and coherency strengthening play an important role in controlling the mechanical properties of the two-phase RSA.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microstructure and mechanical behavior of a TiC nanoprecipitate strengthened V Alloy

The V-4Cr-4Ti (V44) alloys have been proposed as the prime candidate structural material for self-cooled liquid Li blanket and other designs for fusion energy applications. However, the applications of the V44 alloy are limited to a narrow operation temperature window, due to reduction in creep strength at or above 700 °C and susceptibility to irradiation hardening and embrittlement when irradiated below 400 °C. Here, in this work, we explore the feasibility of designing a novel V alloy to form a high number density of TiC nanoprecipitates, in order to simultaneously improve creep strength and provide defect sinks to mitigate irradiation hardening. Computational thermodynamics was used to design a new alloy (V44C) to achieve our goal of high TiC nanoprecipitates density within the alloy V44 matrix. To ensure scalability, the new alloy was made through arc-melting and ingot-casting followed by hot forging, cold rolling and heat treatments of homogenization and precipitation aging. The microstructure was characterized by SEM, TEM, XRD and APT, confirming the existence of nanoprecipitates predicted in the thermodynamic calculations. In addition to microstructural evaluation tensile properties at room temperature and 700 °C, and Charpy impact energy at room temperature were measured. The microstructure and mechanical properties were then compared with those from a historic reference V44 alloy. The tensile strength improvement in V44C was rationalized based on particle and solid solution strengthening mechanism. The fracture behavior was discussed based on the fractography results and necking deformation behavior.

Alloys development↗

NASA NTRS1987

Materials analysis by ultrasonics: Metals, ceramics, composites

Research results in analytical ultrasonics for characterizing structural materials from metals and ceramics to composites are presented. General topics covered by the conference included: status and advances in analytical ultrasonics for characterizing material microstructures and mechanical properties; status and prospects for ultrasonic measurements of microdamage, degradation, and underlying morphological factors; status and problems in precision measurements of frequency-dependent velocity and attenuation for materials analysis; procedures and requirements for automated, digital signal acquisition, processing, analysis, and interpretation; incentives for analytical ultrasonics in materials research and materials processing, testing, and inspection; and examples of progress in ultrasonics for interrelating microstructure, mechanical properties, and dynamic response.

Vary, Alex↗

DOE OSTI2023

Advanced characterization-informed machine learning framework and quantitative insight to irradiated annular U-10Zr metallic fuels

Abstract U-10Zr Metal fuel is a promising nuclear fuel candidate for next-generation sodium-cooled fast spectrum reactors. Since the Experimental Breeder Reactor-II in the late 1960s, researchers accumulated a considerable amount of experience and knowledge on fuel performance at the engineering scale. However, a mechanistic understanding of fuel microstructure evolution and property degradation during in-reactor irradiation is still missing due to a lack of appropriate tools for rapid fuel microstructure assessment and property prediction based on post irradiation examination. This paper proposed a machine learning enabled workflow, coupled with domain knowledge and large dataset collected from advanced post-irradiation examination microscopies, to provide rapid and quantified assessments of the microstructure in two reactor irradiated prototypical annular metal fuels. Specifically, this paper revealed the distribution of Zr-bearing secondary phases and constitutional redistribution across different radial locations. Additionally, the ratios of seven different microstructures at various locations along the temperature gradient were quantified. Moreover, the distributions of fission gas pores on two types of U-10Zr annular fuels were quantitatively compared.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Application of NSUF Capabilities Towards Understanding the Emulation of High Dose Neutron Irradiations with Ion Beams

Development of new materials for current nuclear power plants (NPPs) or materials for new NPPs requires extensive research, development, and deployment programs. Central to these efforts, particularly for core internals, are studies on the microstructural and mechanical changes due to neutron irradiation. These radiation effects studies are typically completed using materials test reactors followed by expensive and time-consuming post-irradiation examinations (PIE). This sluggish approach has severely limited the nuclear materials field to develop new materials or verify materials for new reactor design use. It is also very difficult to achieve the high levels of damage proposed for future reactors. A logical approach to accelerating the field is the application of ion beams to simulate neutron damage, especially for high dose applications. Ion beams have been used for decades to study radiation effects but not to emulate high dose reactor irradiations. In this regard, new (or renewed) methods for ion beam irradiations, new developments in materials characterization, and greater understanding on the governing mechanisms controlling observed radiation effects have led to a need for further studies to refine the technique. A primary challenge is the ability to determine the ion irradiation conditions that produce microstructures and mechanical properties relevant to in-core neutron irradiation conditions. A large, multi-disciplinary, multi-laboratory program deemed the High Fidelity Ion Beam Simulation of High Dose Neutron Irradiation has been formed to assess and overcome the challenges associated with emulating high dose neutron irradiations using ion beams. Central to this program is the use of dual-beam ion irradiations and corresponding neutron irradiations within the BOR-60 fast reactor. These irradiations have produced hundreds of specimens for microstructural and mechanical characterization. A significant issue regarding the samples is the radioactivity of the neutron irradiated specimens as well as the need to characterize both irradiation types using the same equipment to maintain consistency and repeatability. The use of the Nuclear Science User Facilities (NSUF) has been central towards overcoming the mentioned issues and thereby enabling robust PIE in both the ion and neutron irradiated specimens of interest. In particular, the electron microscopes housed within the Low Activation Materials Development and Analysis (LAMDA) facility at Oak Ridge National Laboratory (ORNL) - an NSUF partner facility - has been instrumental in gathering high quality data for analysis. This paper will briefly highlight the PIE efforts using the NSUF capabilities within LAMDA.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Accelerated Ion Irradiation for Emulation of In-reactor Radiation Damage

Reactor core materials in both fast reactors and LWRs granted life extension must withstand irradiation to high doses at high temperature. Ferritic-martensitic (F-M) alloys are attractive candidates for structural components and fuel cladding in fast and thermal reactors, and high chromium and high nickel-containing austenitic steels are potential replacement alloys for LWR core materials. To reach high doses, self-ion irradiation is conducted with simultaneous He injection into both F-M and austenitic alloys, accompanied by reactor irradiations conducted in the BOR-60 fast reactor to assess the capability of ion irradiation to emulate the evolution of microstructure and mechanical properties in reactor. Computational models for defect cluster evolution are being developed and benchmarked against experimental data to ultimately provide predictive capability for the response of both microstructure (loops, voids, precipitates, etc.), and mechanical properties (hardening, ductility, slip behavior) to irradiation. A research program is aimed at understanding how to emulate neutron irradiation using ion irradiation. Results to date have been focused on microstructure and properties of ion irradiated alloys T91, 800H and Fe21Ce32Ni. Data from single ion irradiations are thus far in good agreement with that expected based on previous ion and neutron irradiation data. Dual ion irradiations and neutron irradiated samples are being evaluated and these will be the focus of future work. (authors)

36 MATERIALS SCIENCE↗

DOE OSTI2016

Comparison of Ion and Neutron Irradiations to 3 dpa at 500 deg. C in Ferritic-Martensitic Alloys

The growing global demand for energy will increasingly call upon advanced nuclear fission reactors to supply safe and reliable electricity. The structural and fuel cladding components of these reactors will be subject to extreme conditions of irradiation damage up to several hundred displacements per atom (dpa) at temperatures as high as 700 deg. C. Ferritic-martensitic (F-M) steels are leading candidates for these challenging conditions due to their strength and dimensional stability under irradiation. In order to accelerate the process for evaluating F-M alloys, charged particles are increasingly being used to emulate neutron irradiations. Charged particle irradiations allow the possibility of conducting irradiation experiments within a shorter time period (i.e. at a rate up to 4 orders of magnitude faster) and with minimal radioactivation of the material, enabling lower cost and faster turnaround of post irradiation examination and analysis. However, the irradiation dose rate, damage cascade morphologies, and irradiation damage depth profiles all differ widely between protons, heavier ions, and neutrons. Currently, there is limited understanding of the significance of these physical differences and how they manifest in the irradiated microstructure and mechanical properties of F-M steels. The objective of this study is to evaluate charged particles as a surrogate for neutron irradiations in F-M alloys by assessing common irradiation conditions using Fe{sup ++} ions, protons, and neutrons. Keeping the temperature and dose consistent enables isolation of the effects of each irradiating particle and their respective dose rates and cascade morphologies. Specimens of HCM12A and HT9 were irradiated separately with protons, self-ions, and neutrons to a common dose of 3 dpa at 500 deg. C. The microstructure of each specimen was characterized with TEM and LEAP and compared to evaluate proton and self-ion irradiation as a surrogate for neutron irradiation at these conditions. - Proton, self-ion, and neutron irradiations produced consistent sizes and number densities of grains, carbides, dislocation lines, and dislocation loops. Voids were absent in all conditions. The charged particle irradiations have successfully reproduced the neutron irradiation results for these microstructural features without a temperature shift. - Nano-cluster evolution of Si-Mn-Ni-P and Cu-rich clusters was markedly different for each irradiating particle type. Some cluster morphology trends could be explained by differences in cascade volume for differing irradiating species. But dose rate likely also influences cluster evolution. - Cr-rich nanoclusters nucleated only in the neutron-irradiated HCM12A and HT9. This is likely due to thermal aging at 500 deg. C over a longer experimental time, as compared to the proton and self-ion irradiations. (authors)

36 MATERIALS SCIENCE↗

DOE OSTI2018

Automated coupling of NanoIndentation and Quantitative Energy-Dispersive Spectroscopy (NI-QEDS): A comprehensive method to disclose the micro-chemo-mechanical properties of cement pastes

Engineering cement-based composites requires a comprehensive understanding of the microstructure features governing macroscopic properties. This work aims to foster the latest chemo-mechanical technique to disclose the micro-mechanical properties of intimately intermixed phases. Considering a typical Portland cement paste as a study case, we compared the so-far developed nanoindentation analysis methods with a new automatic method coupling Nano-Indentation and Quantitative Energy-Dispersive Spectroscopy (NI-QEDS). Besides evincing advantages and disadvantages of previous methods, the NI-QEDS analyses enabled distinguishing chemical phases having strongly overlapping mechanical properties. Results suggested the presence at the sub-micrometre scale of extra calcium, aluminum and sulfur into (or in the vicinity of) outer C–S–H. The quantitative chemistry allowed identifying the rare occurrence of nanoindentation volumes located on ''pure'' phases (e.g., inner C–S–H). Finally, NI-QEDS provided new knowledge on cement pastes' micro-chemo-visco-mechanical properties and showed to be a powerful tool for investigating even more heterogeneous systems.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Hybrid Al Casting + AM Components for Automotive Applications

Although casting Aluminum (Al) alloys is widely used for automotive application, the conventional casting process is showing limitations for modern vehicle production. A hybrid manufacturing method that is capable of fabricating automotive structures with tailored functionality and tuned attributes at a high production rate is proposed in this project, utilizing the merits of conventional casting methods and additive manufacturing (AM) methods. Ford is interested in supplementing conventional casting processes (e.g., shape casting, high pressure die casting) with local modifications to geometry and microstructure using additive manufacturing techniques. Two additive manufacturing methods, wire-arc and laser hot-wire directed energy deposition AM process, were evaluated by deposition of 4043 filler wire onto high-pressure die cast and permanent mold cast Al-Si alloys. The feasibility of this hybrid manufacturing method was determined through trial deposition and evaluation of defects, microstructure, and mechanical properties. Laser hot-wire deposition was found to be beneficial for this application with low porosity, a refined microstructure, and mechanical properties similar to those reported in the literature for 4043. The mechanical properties of the interface between the A356 casting and deposited 4043 were found to be controlled by the weaker deposit material.

36 MATERIALS SCIENCE↗

NASA NTRS2017

Pulsed-Laser Irradiation Space Weathering Of A Carbonaceous Chondrite

Grains on the surfaces of airless bodies experience irradiation from solar energetic particles and melting, vaporization and recondensation processes associated with micrometeorite impacts. Collectively, these processes are known as space weathering and they affect the spectral properties, composition, and microstructure of material on the surfaces of airless bodies, e.g. Recent efforts have focused on space weathering of carbonaceous materials which will be critical for interpreting results from the OSIRIS-REx and Hayabusa2 missions targeting primitive, organic-rich asteroids. In addition to returned sample analyses, space weathering processes are quantified through laboratory experiments. For example, the short-duration thermal pulse from hypervelocity micrometeorite impacts have been simulated using pulsed-laser irradiation of target material e.g. Recent work however, has shown that pulsed-laser irradiation has variable effects on the spectral properties and microstructure of carbonaceous chondrite samples. Here we investigate the spectral characteristics of pulsed-laser irradiated CM2 carbonaceous chondrite, Murchison, including the vaporized component. We also report the chemical and structural characteristics of specific mineral phases within the meteorite as a result of pulsed-laser irradiation.

Thompson, M. S.↗

NASA NTRS2000

Assessment of Low Cycle Fatigue Behavior of Powder Metallurgy Alloy U720

The fatigue lives of modem powder metallurgy disk alloys are influenced by variabilities in alloy microstructure and mechanical properties. These properties can vary as functions of variables the different steps of materials/component processing: powder atomization, consolidation, extrusion, forging, heat treating, and machining. It is important to understand the relationship between the statistical variations in life and these variables, as well as the change in life distribution due to changes in fatigue loading conditions. The objective of this study was to investigate these relationships in a nickel-base disk superalloy, U720, produced using powder metallurgy processing. Multiple strain-controlled fatigue tests were performed at 538 C (1000 F) at limited sets of test conditions. Analyses were performed to: (1) assess variations of microstructure, mechanical properties, and LCF failure initiation sites as functions of disk processing and loading conditions; and (2) compare mean and minimum fatigue life predictions using different approaches for modeling the data from assorted test conditions. Significant variations in life were observed as functions of the disk processing variables evaluated. However, the lives of all specimens could still be combined and modeled together. The failure initiation sites for tests performed at a strain ratio R(sub epsilon) = epsilon(sub min)/epsilon(sub max) of 0 were different from those in tests at a strain ratio of -1. An approach could still be applied to account for the differences in mean and maximum stresses and strains. This allowed the data in tests of various conditions to be combined for more robust statistical estimates of mean and minimum lives.

Gabb, Tomothy P.↗

DOE OSTI2016

Microstructure and partitioning behavior characteristics in low carbon steels treated by hot-rolling direct quenching and dynamical partitioning processes

In this work, a new process and composition design are proposed for “quenching and partitioning” or Q&P treatment. Three low carbon steels were treated by hot-rolling direct quenching and dynamical partitioning processes (DQ&P). The effects of proeutectoid ferrite and carbon concentration on microstructure evolution and mechanical properties were investigated. The present work obtained DQ&P prototype steels with good mechanical properties and established a new notion on compositions for Q&P processing. Microstructures were characterized by means of electro probe microanalyzer (EPMA), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray diffraction (XRD), especially the morphology and size of retained austenite. Mechanical properties were measured by uniaxial tensile tests. The results indicated that introducing proeutectoid ferrite can increase the volume fraction of retained austenite and thus improve mechanical properties. TEM observation showed that retained austenite included the film-like inter-lath austenite and blocky austenite located in martensite/ferrite interfaces or surrounded by ferrites. It was interesting that when the carbon concentration is as low as ~ 0.078%, the film-like inter-lath untransformed austenite cannot be stabilized to room temperature and almost all of them transformed into twin martensite. The blocky retained austenite strengthened the interfaces and transformed into twin martensite during the tensile deformation process. The PSEs of specimens all exceeded 20 GPa.%. - Highlights: •This study focused on a new process: Q&P process applying dynamical partitioning. •Ferrite can increase the volume fraction of retained austenite. •The film-like austenite and the blocky austenite were observed. •The low carbon steels treated by new process reached PSEs higher than 20 GPa.%.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Characterization of the fatigue threshold behavior of UHMWPE

Ultra-high-molecular-weight-polyethylene (UHMWPE) has been the material of choice for bearings in total joint replacements (TJRs) for decades as a result of its excellent wear resistance, chemical inertness, energetic toughness, low friction, and biocompatibility. Utilization of this polymer in orthopedic devices requires oxidation, wear, and fatigue resistance. Balancing these important properties by tailoring processing techniques and modulating microstructural features has been an ongoing endeavor in the field. Research into the clinical applications of UHMWPE has primarily focused on the challenges of wear and oxidation while studies into the realm of fatigue have been more limited. Literature gaps exist in fully understanding the fatigue crack initiation near notches or propagation of small existing flaws in UHMWPE used in TJRs. In particular, the characterization of the fatigue thresholds and near-threshold fatigue behavior of orthopedic grade UHMWPE has yet to be thoroughly explored. In this work, we characterized the fatigue crack arrest threshold of clinically-relevant UHMWPE formulations. Correlations between the fatigue thresholds and bulk mechanical properties as well as microstructural properties were examined across these medical resins. The important role played by crosslinking in influencing the fatigue performance of UHMWPE is highlighted in this study. In addition, it is established that J-integral fracture toughness is the best predictor of fatigue thresholds and could possibly be used as a stand-in metric for fatigue performance if thresholds cannot be directly ascertained. Finally, this study corroborates that the true constitutive parameters best describe the mechanical behavior of UHMWPE.

Cross-linking↗

DOE OSTI2020

Influence of non-magnetic Cu on enhancing the low temperature magnetic properties and Curie temperature of FeCoNiCrCu(x) high entropy alloys

The microstructure and magnetic properties of three face-centered cubic (FCC) FeCoNiCrCu(x) high entropy alloys (HEAs) (x=0, 0.5, 1) are investigated. Interestingly, addition of the nonmagnetic element Cu to FeCoNiCr HEA is found to enhance exchange interactions and low temperature saturation magnetization. The paramagnetic to ferromagnetic Curie transition temperature increases from 85 K for FeCoNiCr to 118 K for FeCoNiCrCu. This is counterintuitive since Cu is nonmagnetic; however, atom probe tomography revealed Cu rich clusters containing 5 at% Ni and 1 at% each of Fe, Co, Cr, within FCC matrix, these clusters altered the matrix composition and consequently its magnetic properties.

Chaudhary, Varun↗

DOE OSTI2026

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

DOE OSTI2022

ExaAM: Metal additive manufacturing simulation at the fidelity of the microstructure

Additive manufacturing (AM), or 3D printing, of metals is transforming the fabrication of components, in part by dramatically expanding the design space, allowing optimization of shape and topology. However, although the physical processes involved in AM are similar to those of welding, a field with decades of experimental, modeling, simulation, and characterization experience, qualification of AM parts remains a challenge. The availability of exascale computational systems, particularly when combined with data-driven approaches such as machine learning, enables topology and shape optimization as well as accelerated qualification by providing process-aware, locally accurate microstructure and mechanical property models. We describe the physics components comprising the Exascale Additive Manufacturing simulation environment and report progress using highly resolved melt pool simulations to inform part-scale finite element thermomechanics simulations, drive microstructure evolution, and determine constitutive mechanical property relationships based on those microstructures using polycrystal plasticity. We report on implementation of these components for exascale computing architectures, as well as the multi-stage simulation workflow that provides a unique high-fidelity model of process–structure–property relationships for AM parts. In addition, we discuss verification and validation through collaboration with efforts such as AM-Bench, a set of benchmark test problems under development by a team led by the National Institute of Standards and Technology.

3D printing↗

DOE OSTI2018

Cetyltrimethylammonium Bromide (CTAB) Surfactant-Assisted Synthesis of BiFeO{sub 3} Nanoparticles by Sol-Gel Auto-Combustion Method

In this research, BiFeO{sub 3} nanoparticles were synthesized by sol-gel auto-combustion method with and without the addition of cetyltrimethylammonium bromide (CTAB) surfactant. The effect of different amounts of CTAB addition (0, 1.5, 3, and 6 wt.%) on phase constituents, microstructure, and magnetic properties of the synthesized samples were evaluated using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), and vibration sample magnetometer (VSM). Also, BiFeO{sub 3} nanoparticles were used for the degradation of methylene blue (MB) as a typical dye pollutant under UV irradiation. XRD results showed the formation of BiFeO{sub 3} mainly with some minute impurity phases such as Bi{sub 2}O{sub 3} and γ-Fe{sub 2}O{sub 3}. Proper amounts of CTAB addition (1.5 wt.%) considerably eliminates Bi{sub 2}O{sub 3} and γ-Fe{sub 2}O{sub 3} residuals in the combustion product. FESEM micrographs show particle size reduction and also more uniform particle size distribution when using 0.75 wt.% of CTAB addition. In the presence of the BiFeO{sub 3}, the UV irradiation for 120 min resulted in 26% degradation of MB, in a sample with 0.75 wt.% CTAB. The synthesized nanoparticles of BiFeO{sub 3} in the sample with 0.75 wt.% CTAB after calcination at 650 {sup ∘}C showed a weak ferromagnetism behavior with saturation magnetization of 0.54 emu/g. {sub i}H{sub C} values of the samples are in the range of 200 to 238 Oe, depending on the crystallite size and phase constituents of the samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Heat-treated glassy carbon under pressure exhibiting superior hardness, strength and elasticity

Glassy carbon (GC) is a type of non-graphitizing disordered carbon material at ambient pressure and high temperatures, which has been widely used due to its excellent mechanical properties. Here we report the changes in the microstructure and mechanical properties of GC treated at high pressures (up to 5 GPa) and high temperatures. The formation of intermediate sp 2 –sp 3 phases is identified at moderate treatment temperatures before the complete graphitization of GC, by analyzing synchrotron X-ray diffraction, Raman spectra, and transmission electron microscopy images. The intermediate metastable carbon materials exhibit superior mechanical properties with hardness reaching up to 10 GPa and compressive strength reaching as high as 2.5 GPa, nearly doubling those of raw GC, and improving elasticity and thermal stability. The synthesis pressure used in this study can be achieved in the industry on a commercial scale, enabling the scalable synthesis of this type of strong, hard, and elastic carbon materials.

36 MATERIALS SCIENCE↗