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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

In-Situ and Ex-Situ Studies on the Morphology Changes of Polymer Pipeline Materials for Use in Hydrogen Gas Environments

The US natural gas infrastructure is a national asset that could be used to deliver hydrogen and hydrogen blends of natural gas as a pathway to reduce carbon emissions. The distribution system comprises nearly 50% plastic pipe composed of medium- and high-density polyethylene materials (MDPE and HDPE). While these materials perform adequately for natural gas, research on their hydrogen compatibility is essential to understand if any immediate and long-term risks are associated with hydrogen addition. The Blended Gas CRADA, a HyBlend project, has established a comprehensive test method for evaluating MDPE and HDPE of various plastic resin compositions of pipeline material in pure hydrogen and 20% hydrogen/80% methane blends. Both in-situ and ex-situ measurements were performed to capture hydrogen-induced changes in the polyethylene material's crystalline, amorphous and their interphase regions. We investigated MDPE and HDPE pipeline materials made from different polymer resin systems to evaluate the effects of hydrogen gas. The materials were characterized by their density, diffusion coefficient, free volume ratio, and degree of crystallinity. Various advanced characterization methods, including in situ NMR, ex situ XRD, ex situ DSC, and ex situ TDA, were used to analyze the effects of changes in crystalline, amorphous, and interphase regions due to gas exposure. Time-dependent post-decompression quasi-static tensile tests were conducted to explore the effects of gas exposure time on the mechanical behavior of the pipe materials. This work will highlight the time sensitivities during and after gas exposure. The correlation between gas-induced polyethylene morphology changes and the associated material performance will be addressed for the intended applications. These studies will show that polyethylene resin composition and material exposure are important factors when considering whether hydrogen gas affects pipeline materials positively or negatively.

Simmons, Kevin L.↗
NASA NTRS1994

Sapphire reinforced alumina matrix composites

Unidirectionally reinforced A1203 matrix composites have been fabricated by hot pressing. Approximately 30 volume % of either coated or uncoated sapphire fiber was used as reinforcement. Unstabilized ZrO2 was applied as the fiber coating. Composite mechanical behavior was analyzed both after fabrication and after additional heat treatment. The results of composite tensile tests were correlated with fiber-matrix interfacial shear strengths determined from fiber push-out tests. Substantially higher strength and greater fiber pull-out were observed for the coated fiber composites for all processing conditions studied. The coated fiber composites retained up to 95% and 87% of their as-fabricated strength when heat treated at 14000C for 8 or 24 hours, respectively. Electron microscopy analysis of the fracture surfaces revealed extensive fiber pull-out both before and after heat treatment.

Jaskowiak, Martha H.↗
NASA NTRS2017

Strain Monitoring of Flexible Structures

One of the biggest challenges facing NASA's deep space exploration goals is structural mass. A long duration transit vehicle on a journey to Mars, for example, requires a large internal volume for cargo, supplies and crew support. As with all space structures, a large pressure vessel is not enough. The vehicle also requires thermal, micro-meteoroid, and radiation protection, a navigation and control system, a propulsion system, and a power system, etc. As vehicles get larger, their associated systems also get larger and more complex. These vehicles require larger lift capacities and force the mission to become extremely costly. In order to build large volume habitable vehicles, with only minimal increases in launch volume and mass, NASA is developing lightweight structures. Lightweight structures are made from non-metallic materials including graphite composites and high strength fabrics and could provide similar or better structural capability than metals, but with significant launch volume and mass savings. Fabric structures specifically, have been worked by NASA off and on since its inception, but most notably in the 1990's with the TransHAB program. These TransHAB developed structures use a layered material approach to form a pressure vessel with integrated thermal and micro-meteoroid and orbital debris (MMOD) protection. The flexible fabrics allow the vessel to be packed in a small volume during launch and expand into a much larger volume once in orbit. NASA and Bigelow Aerospace recently installed the first human-rated inflatable module on the International Space Station (ISS), known as the Bigelow Expandable Activity Module (BEAM) in May of 2016. The module provides a similar internal volume to that of an Orbital ATK Cygnus cargo vehicle, but with a 77% launch volume savings. As lightweight structures are developed, testing methods are vital to understanding their behavior and validating analytical models. Common techniques can be applied to fabric materials, such as tensile testing, fatigue testing, and shear testing, but common measurement techniques cannot be used on fabric. Measuring strain in a material and during a test is a critical parameter for an engineer to monitor the structure during the test and correlate to an analytical model. The ability to measure strain in fabric structures is a challenge for NASA. Foil strain gauges, for example, are commonplace on metallic structures testing, but are extremely difficult to interface with a fabric substrate. New strain measuring techniques need to be developed for use with fabric structures. This paper investigates options for measuring strain in fabric structures for both ground testing and in-space structural health monitoring. It evaluates current commercially available options and outlines development work underway to build custom measurement solutions for NASA's fabric structures.

Litteken, Douglas A.↗
DOE OSTI2023

A Summary of the Microstructural Characterization Results for the A709 Commercial Heats

To improve high temperature strength for advanced nuclear reactors, it is necessary to qualify additional structural materials for introduction into the American Society of Mechanical Engineers (AMSE) Boiler and Pressure Vessel Code (BPVC). Specifically, Alloy 709 was identified as a material for Sodium-cooled Fast Reactors to enhance time-dependent mechanical properties compared to 316H stainless steel, a code qualified high temperature alloy. Idaho National Laboratory (INL) and Oak Ridge National Laboratory (ORNL) performed initial microstructure and mechanical property testing on a third, commercial heat of Alloy 709 stainless steel. The Alloy 709 plate was produced by Allegheny Technology Inc. (ATI) and in the solution annealed condition. The chemical composition was within the limits for an American Society of Testing and Materials (ASTM) A213 specification for seamless tube for material UNS S31025. Grain size was measured as an average ASTM size of 6.5, which was larger than the ASTM 7 required according to ASTM A213 for seamless tube. The chemical composition was within the limits for an ASTM A213, and the room temperature tensile tests and hardness data met ASTM A213 specifications. Creep-fatigue results showed similar behavior to previous heats of Alloy 709.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Prediction of softening kinetics and recrystallization texture in non-isothermally annealed bulged tubes using CPFEM and CA models

A hierarchically coupled cellular automata (CA) model, crystal plasticity finite element method (CPFEM), and thermal finite element (FE) model is developed to predict the softening kinetics of the bulged steel tube during non-isothermal annealing. Through the developed model, the kinetics of softening mechanisms including static recovery (SRV) and static recrystallization (SRX), as well as the recrystallization texture are predicted. Later, the Johnson-Mehl-Avrami-Kohnogorov (JMAK) model based on the predicted SRX data is developed to interpret the recrystallization behavior of the material. To perform this study, diverse experimental tests including tube hydroforming (THF), annealing, uniaxial tensile test, hardness test, as well as microstructure observations through optical microscopy and Electron Backscatter Diffraction (EBSD) tests on steel tube are performed. The obtained experimental data are utilized to calibrate and verify the implemented CPFEM model for simulation of THF process, thermal FE model for prediction of the local temperature over annealing time, and CA algorithm for modeling of the softening kinetics and texture evolution throughout the annealing process. The study shows that the predicted deformation characteristics, softening kinetics, recrystallization texture and temperature profile during non-isothermal annealing are in good agreement with experimental data. During the annealing process, a total of four stages for the kinetics of softening mechanisms is observed: No softening; SRV only; SRV dominant; and SRX dominant. During the progress of SRX, the behavior of recrystallization is abruptly changed, confirming that two different mechanisms are controlling the kinetics of transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Structural and Mechanical Analysis of Individual Mineralized Collagen Fibrils Using In Situ Transmission Electron Microscopy

Bone serves as an example of nature’s architectured material with its characteristic blend of strength and toughness, all at a lightweight design. Given the hierarchical nature of these materials, it is essential to understand the governing mechanisms and organization of their constituents across length scales for bioinspired structural design. Despite recent advances in transmission electron microscopy (TEM) that have allowed us to witness the hierarchical arrangement of bone at micro-down to the nanoscale, we are still missing the details about the structural organization and mechanical properties of the main building blocks of bone─mineralized collagen fibrils (MCFs). Here, we present a method to extract individual MCFs from nature’s model material, mineralized turkey leg tendon, using a dropcasting procedure. By isolating the MCFs onto TEM supporting grids, we visualized the arrangement of organic and mineral phases within individual MCFs at the nanoscale. Using a four-dimensional scanning transmission electron microscopy (4D-STEM) approach, the orientation of individual mineral crystals within the MCFs was examined. Furthermore, we conducted in situ tensile experiments, revealing exceptional tensile strains of at least 8%, demonstrating the intricate relationship between structural organization and the mechanical behavior of MCFs. These insights into the ultrastructure of mineralized tissue building blocks, as well as the proposed sample-extraction method compatible with in situ mechanical testing, provide a strong basis for research into nature-inspired material design.

4D-STEM↗
DOE OSTI2021

In Situ TEM Tensile Testing of Bicrystals with Tailored Misorientation Angles

Grain boundaries have complex structural features that influence strength, ductility and fracture in metals and alloys. Grain boundary misorientation angle has been identified as a key parameter that controls their mechanical behavior, but the effect of misorientation angle has been challenging to isolate in polycrystalline materials. Here, we describe the use of bicrystal Au thin films made using a rapid melt growth process to study deformation at a single grain boundary. Tensile testing is performed on bicrystals with different misorientation angles using in situ TEM, as well as on a single crystalline sample. Plastic deformation is initiated through dislocation nucleation from free surfaces. Grain boundary sliding is not observed, and failure occurs away from the grain boundary through plastic collapse in all cases. The failure behavior in these nanoscale bicrystals does not appear to depend on the misorientation angle or grain boundary energy but instead has a more complex dependence on sample surface structure and dislocation activity.

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 NTRS2002

Three-Dimensional Stress Fields and Slip Systems for Single Crystal Superalloy Notched Specimens

Single crystal superalloys have become increasingly popular for turbine blade and vane applications due to their high strength, and creep and fatigue resistance at elevated temperatures. The crystallographic orientation of a single crystal material greatly affects its material properties, including elastic modulus, shear modulus, and ductility. These directional properties, along with the type of loading and temperature, dictate an anisotropic response in the yield strength, creep resistance, creep rupture ductility, fatigue resistance, etc. A significant amount of research has been conducted to determine the material properties in the <001> orientation, yet the material properties deviating from the <001> orientation have not been assessed for all cases. Based on the desired application and design criteria, a crystal orientation is selected to yield the maximum properties. Currently, single crystal manufacturing is able to control the primary crystallographic orientation within 15 of the target orientation, which is an acceptable deviation to meet both performance and cost guidelines; the secondary orientation is rarely specified. A common experiment is the standard load-controlled tensile test, in which specimens with different orientations can be loaded to observe the material response. The deformation behavior of single-crystal materials under tension and compression is known to be a function of not only material orientation, but also of varying microdeformation (i.e. dislocation) mechanisms. The underlying dislocation motion causes deformation via slip, and affects the activation of specific slip systems based on load and orientation. The slip can be analyzed by observing the visible traces left on the surface of the specimen from the slip activity within the single crystal material. The goal of this thesis was to predict the slip systems activated in three-dimensional stress fields of a notched tensile specimen, as a function of crystal orientation, using finite element analysis without addressing microstructural deformation mechanisms that govern their activation. Out of three orientations tested, the specimen with a [110] load orientation and a [001] growth direction had the lowest maximum resolved shear stress; this specimen orientation appears to be the best design candidate for a tensile application.

Magnan, Shannon M.↗
DOE OSTI2023

Influence of the Ozone Dose Time during Atomic Layer Deposition on the Ferroelectric and Pyroelectric Properties of 45 nm-Thick ZrO 2 Films

Over a decade ago, ferroelectricity was discovered in doped HfO 2 thin films. The HfO 2 -based thin films have attracted much attention due to their remarkable scalability and CMOS compatibility. Other than the HfO 2 -based thin films, the undoped ZrO 2 thin films are understudied despite their commonly reported antiferroelectric behavior. However, being of the same fluorite structure as HfO 2 -based thin films, the undoped ZrO 2 also displayed considerable ferroelectricity as demonstrated in recent studies. Here, 45 nm-thick polycrystalline undoped ZrO 2 films are synthesized using atomic layer deposition with different ozone dose times. The ZrO 2 films are crystallized after atomic layer deposition at 350 °C without anneals. In general, the longer ozone dose time causes a lower in-plane tensile stress and oxygen vacancy content, which help facilitate an irreversible non-polar tetragonal to polar orthorhombic phase transition with electric-field cycling. However, the lower in-plane tensile stress and oxygen vacancy content also stabilize the monoclinic phase so that a long ozone dose time (>17.5 s) reduces the ferroelectric behavior. After wake-up cycles, the ZrO 2 thin film with an ozone dose time of 17.5 s exhibits a remanent polarization of 6 μC·cm –2 and a pyroelectric coefficient of -35 μC·K –1 ·m –2 . Moreover, the wake-up behavior is consistent between the ferroelectric and pyroelectric response. As essential factors in optimizing the growth of fluorite-structure thin films for ferroelectric applications, the in-plane tensile stress and oxygen vacancy content significantly influence the ferroelectric and pyroelectric properties. Additionally, the low thermal budget for processing ferroelectric ZrO 2 thin films is valuable for semiconductor back-end-of-line processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Mechanical behavior analysis using small-size graphite disc compression testing with digital image correlation methods

The ASTM International Standard Test Method for Tensile Stress-Strain of Carbon and Graphite (ASTM C749) requires dog-bone shaped specimens. Unfortunately, specimen sizes required in ASTM C749 are much too large for irradiation within a test reactor and are incompatible with irradiation capsule volumes, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed as an alternative that provides a means for testing tensile properties using smaller specimens when geometric constraints are present. However, the important stress–strain relation throughout the test loading history that could be recorded using ASTM C749 is lost by using ASTM D8289 because of the difficulties involved with using traditional strain gauges or extensometers on such a small specimen. In this work, a digital image correlation (DIC) method, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 splitting tensile test on eight small samples of graphite grade Mersen 2114 to track their deformation during compressive loading. Initial results showed that the DIC technique can measure the surface displacement/strain on these small (Ø6 × 3 mm) graphite specimens with high accuracy and good repeatability, indicating that the DIC technique, combined with the small-disc splitting tensile test in ASTM D8289, can capture the strain evolution in the test. In conclusion, further comparison of measured strains with analytical and numerical simulation results provides additional understanding of the mechanical behaviour of this nuclear graphite material in complex stress states.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Engine materials characterization and damage monitoring by using x ray technologies

X ray attenuation measurement systems that are capable of characterizing density variations in monolithic ceramics and damage due to processing and/or mechanical testing in ceramic and intermetallic matrix composites are developed and applied. Noninvasive monitoring of damage accumulation and failure sequences in ceramic matrix composites is used during room-temperature tensile testing. This work resulted in the development of a point-scan digital radiography system and an in situ x ray material testing system. The former is used to characterize silicon carbide and silicon nitride specimens, and the latter is used to image the failure behavior of silicon-carbide-fiber-reinforced, reaction-bonded silicon nitride matrix composites. State-of-the-art x ray computed tomography is investigated to determine its capabilities and limitations in characterizing density variations of subscale engine components (e.g., a silicon carbide rotor, a silicon nitride blade, and a silicon-carbide-fiber-reinforced beta titanium matrix rod, rotor, and ring). Microfocus radiography, conventional radiography, scanning acoustic microscopy, and metallography are used to substantiate the x ray computed tomography findings. Point-scan digital radiography is a viable technique for characterizing density variations in monolithic ceramic specimens. But it is very limited and time consuming in characterizing ceramic matrix composites. Precise x ray attenuation measurements, reflecting minute density variations, are achieved by photon counting and by using microcollimators at the source and the detector. X ray computed tomography is found to be a unique x ray attenuation measurement technique capable of providing cross-sectional spatial density information in monolithic ceramics and metal matrix composites. X ray computed tomography is proven to accelerate generic composite component development. Radiographic evaluation before, during, and after loading shows the effect of preexisting volume flaws on the fracture behavior of composites. Results from one-, three-, five-, and eight-ply ceramic composite specimens show that x ray film radiography can monitor damage accumulation during tensile loading. Matrix cracking, fiber-matrix debonding, fiber bridging, and fiber pullout are imaged throughout the tensile loading of the specimens. In situ film radiography is found to be a practical technique for estimating interfacial shear strength between the silicon carbide fibers and the reaction-bonded silicon nitride matrix. It is concluded that pretest, in situ, and post-test x ray imaging can provide greater understanding of ceramic matrix composite mechanical behavior.

Baaklini, George Y.↗
NASA NTRS2019

Mechanical Tensile Testing of Hiperco 50A at Cryogenic Temperature

Hiperco 50A is a highly desired material for use in cryogenic applications, specifically for adiabatic demagnetization refrigerators (ADRs) due to its magnetic field shielding capabilities. Although the alloy has good strength, there is a concern with the material's brittle behavior which is believed to worsen at low temperature based on previous tests. The testing described here investigates the mechanical properties of Hiperco 50A at cryogenic temperature through mechanical tensile testing to failure and evaluation of the failed coupons. The methods and techniques used to determine the elongation, yield strength, ultimate tensile strength, and break strength of the material as well as the results will be presented here.

material properties↗
NASA NTRS1992

Relative sliding durability of candidate high temperature fiber seal materials

The relative sliding durability behavior of six candidate ceramic fibers for high temperature sliding seal applications is reviewed and compared. Pin on disk tests were used to evaluate potential seal materials by sliding a tow or bundle of the candidate ceramic fiber against a superalloy test disk. Tests were conducted in air under a 2.65 N load, at a sliding velocity of 0.025 m/sec and at temperatures from 25 to 900 C. Friction was measured during the tests and fiber wear, indicated by the extent of fibers broken in the tow or bundle, was measured at the end of each test. For most of the fibers, friction and wear increase with test temperature. The relative fiber durability ranking correlates with tensile strength, indicating that tensile data, which is more readily available than sliding durability data, may be useful in predicting fiber wear behavior under various conditions. A dimensional analysis of the wear data shows that the fiber durability is related to a dimensionless durability ratio which represents the ratio of the fiber strength to the fiber stresses imposed by sliding. The analysis is applicable to fibers with similar diameters and elastic moduli. Based upon the results of the research program, three fiber candidates are recommended for further study as potential seal materials. They are a silicon based complex carbide-oxide fiber, an alumina-boria-silica and an aluminosilicate fiber.

Dellacorte, Christopher↗
NASA NTRS2003

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.↗
DOE OSTI2022

Origin, parameters, and underlying deformation mechanisms of propagating deformation bands in irradiated 316L stainless steel

Lüders-type propagating deformation bands were observed in specimens of irradiated 316L stainless steel samples removed from Spallation Neutron Source target vessels after service. Mechanical testing with digital image correlation (DIC) and in-situ tensile testing with scanning electron microscopy electron backscatter diffraction showed that the observed Lüders-type behavior was not related to the known transformation-induced plasticity or twinning-induced plasticity behavior. Instead, the phenomenon occurs at small local strain values before a significant amount of martensite or deformation twins appear in the microstructure. Microstructural analysis and in-situ mechanical test results suggest Lüders-type band formation and propagation were related to the appearance and evolution of defect-free channels—analogous to slip bands. A modified Swift equation with a Ludwigson-like component was offered to rationalize the phenomenon and model the strain-softening processes at small strain values. Finally, the results indicate complex microstructural processes and deformation mechanisms were active at small strain values and underline the benefits of advanced mechanical test approaches such as DIC.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Micromechanical properties of spherical and facetted He bubble loaded copper

Exploring new irradiation resistant materials requires understanding their mechanical responses to irradiation. Resistance to helium bubble formation and understanding bubble effects on the mechanical response of candidate materials are crucial factors to qualify materials as irradiation resistant. Here, in this paper, we explore the effect of spherical and facetted helium bubbles on the mechanical response of copper via in-situ micromechanical tensile testing at room temperature. Bubble formation and shape effects on strength and ductility, and their behavior on grain boundaries are discussed and compared to literature. Loading Cu with helium bubbles is shown here to increase strength but decrease ductility.

42 ENGINEERING↗
DOE OSTI2025

Enabling room-temperature ferromagnetism in few-layered MoS 2 films via strain engineering

Strain engineering presents a promising pathway for modulating the physical properties of two-dimensional (2D) transition metal dichalcogenides materials. Here, in this study, we investigate the strain-induced magnetic behavior of diamagnetic MoS 2 films prepared by the DC magnetron sputtering technique. By applying +1% tensile strain to few-layered MoS 2 films (∼3.5 nm), we observe the emergence of room-temperature ferromagnetism with a magnetization saturation of about ∼130 emu/cm 3 , in stark contrast to bulk films (∼40 nm), which remain diamagnetic under similar conditions. Raman spectroscopy reveals a pronounced reduction in the intensity and the splitting of the E′ mode in 1% strained few-layered films, indicating a possible bond elongation and symmetry breaking under tensile stress. Additionally, x-ray absorption spectroscopy at the Mo M 3 edge further confirms a strain-induced electronic structure modification in few-layered films, with no corresponding shift observed in bulk counterparts. Moreover, the strain-induced magnetic and structural changes are largely reversible upon strain release. We attribute the origin of ferromagnetism in few-layered films to the combined influence of tensile strain and defect-assisted bond weakening, which facilitates crystal field transitions within the Mo 4d orbitals. These findings demonstrate that strain engineering can effectively induce and modulate magnetism in 2D materials, providing opportunities for developing strain-controlled spintronic applications.

36 MATERIALS SCIENCE↗