Optimizing stress impedance and medium-range ordered structure in Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy through tailored annealing treatment
0 Abstract
Amorphous alloys are emerging as a highly promising category of materials for mechanical sensing, attributed to their favorable stress impedance performance. However, the practical achievement of the stress impedance ratio still falls considerably short of its theoretical potential, and the atomic-scale mechanisms underlying this phenomenon remain largely unexplored. Here, we report that the stress impedance ratio of Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy can be significantly enhanced by a tailored annealing treatment around the glass transition temperature (Tg), giving rise to the highest stress impedance ratio reaching up to 124%. Utilizing the high-energy synchrotron X-ray total scattering technique, the strong correlation between the stress impedance performance and the medium-range ordered structure of amorphous alloys is elucidated. Our findings revealed that an increase in edge-sharing atomic connection mode plays a pivotal role in enhancing the stress impedance performance. Furthermore, a composite film combining the amorphous alloy with silicone rubber was fabricated under the same annealing treatment, demonstrating a significantly improved sensitivity compared to the ribbon (706.10 vs.
Keywords
INTRODUCTION
Amorphous alloys have attracted considerable interest due to their unique physical and chemical properties compared to their crystalline counterparts. The inherent atomic disorder in these alloys eliminates magnetic domain structures, leading to an overall magnetic isotropy. This unique characteristic endows the majority of amorphous alloys to exhibit soft magnetic properties characterized by low coercivity, high permeability, and a high saturation magnetic flux density[1-6]. Furthermore, the soft magnetic features allow these amorphous alloys to exhibit a greater tendency for magnetic domain deflection under external forces. This, in turn, facilitates a more pronounced change in magnetic permeability, leading to high-sensitivity magnetoelastic coupling effects and a high stress impedance ratio. Therefore, the soft-magnetic amorphous alloys are becoming increasingly important in advanced sensor applications[7,8], surface coatings[9], and 3D printed components[10]. The stress impedance effect, referring to a significant impedance change under varying stress levels[11,12], establishes a link between applied stress and magnetostriction, emphasizing critical interplays of both mechanical and magnetic properties. Despite extensive engineering, the unexplored atomic-scale mechanism hinders the full potential and widespread adoption of stress impedance-based sensors.
So far, substantial efforts towards improving stress impedance properties have been made via various methods[13-18], wherein introducing nanocrystals to enhance structural anisotropy is an effective approach[19]. For example, a recent research work involved small bcc nanoclusters into the amorphous matrix, significantly enhancing the stress impedance and lowering local magnetic anisotropy. Another inspiring approach is to anneal the amorphous alloys at sub-Tg temperatures, where the Tg refers to glass transition temperatures. It has been found that annealing Fe-Dy-B-Nb amorphous at a temperature just below Tg, known as TAEP annealing, increases stress impedance by about 30% compared to the as-cast state[20,21]. For this reason, Tong et al. revealed that annealing near Tg leads to improved magnetization and reduced coercivity, triggering evolution of short- and medium-range structures[22]. Here, short-range ordering (SRO) refers to atomic ordering within a range of 0-5 Å, while medium-range ordering (MRO) corresponds to a larger ordering range of 5-20 Å. However, at present, there remains a gap regarding the correlation between the short- to medium-range ordered structure in amorphous alloys and the stress impedance effect.
In this work, we improve the stress impedance ratio of Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy through a precisely tailored annealing treatment around Tg. Using high-energy synchrotron X-ray techniques, we establish a strong correlation between stress impedance and the medium-range ordered structure of the amorphous alloy. It has been revealed that the edge-sharing atomic connection mode plays a crucial role. Furthermore, a composite film combining the amorphous alloy with silicone rubber was made using the same annealing treatment, which exhibits a much better sensitivity. This research provides insights into atomic-scale mechanisms and suggests a promising annealing strategy for advanced sensing applications.
EXPERIMENTAL SECTION
Sample preparation
Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 ingots were first prepared through vacuum induction melting using high-purity elements (> 99.95%). These ingots were then cast into dense, chemically homogeneous metal ingots through arc melting. Subsequently, the metal ingots were made into amorphous ribbons using a single roller melt spinning method. The thickness of the amorphous ribbons ranged from 10 to 0.02 μm, with a width between 1 and 1.4 mm. Before preparing the amorphous ribbons, the oxide layer on the surface of the metal ingots was removed using a grinding machine to ensure uniform nucleation.
The achieved Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous ribbons were positioned within a round-bottom flask. This assembly was then evacuated using a vacuum sealing machine (model MRVS-1002) to achieve vacuum conditions. After sealing, the encapsulated materials were placed inside a muffle furnace (model
Characterization
The crystal structures of the ribbons and powders were analyzed using X-ray diffraction (XRD, Bruker D8 Advance) with Cu Kα target (λ = 0.154 nm) operated at 40 kV. The morphology and composition were characterized using a scanning electron microscope (IT500HR SEM) equipped with X-ray energy dispersive spectroscopy (EDS). Differential scanning calorimetry (DSC) experiments were carried out using a Netzsch Pegasus DSC equipment under a high-purity Ar atmosphere, with a heating rate of 20 K min-1. The mass of the test sample was about 30 mg.
Pair distribution function analysis
The synchrotron X-ray total scattering measurements were performed at the BL13SSW beamline of the Beijing Synchrotron Radiation Source (BSRF) (λ = 0.2061) using the transmission mode. The Qmax and Qmin values of S(Q) are 16.9 and 0.02 Å-1, respectively. The background signal of the Kapton tape was subtracted from the raw data before the Fourier transform. The raw data were analyzed using the PDFgetX2 software to obtain the structure factor S(Q) (Q = 4πsinθ/λ, where θ is the scattering angle, and λ is the X-ray wavelength). The pair distribution function (PDF) G(r) was calculated via Fourier transform:
where r is the distance of atom pairs, and Qmax is the maximum value of Q after Fourier transform. The peaks of G(r) were fitted according to the exponential decay function f(r) = A × exp(-r/ξ), where ξ describes the decay rate of the order. The G(r) was converted to the atomic PDF g(r) using:
where ρ0 is the average number density. The g(r) was converted to structural entropy Seq using
The first peak of G(r) was transformed into T(r) through the equation T(r) = 4πrρ0 + G(r), where the T(r) is believed to accord better with the Gaussian function than g(r) and is more frequently employed to describe the SRO in amorphous alloys. The first T(r) peak can be decomposed into the sum of the weighted Gaussian functions:
ω = 2cicjbibj/b2 (i ≠ j) or cibi/b2 (i = j)
where i and j are the ith and jth atomic species, ωij is the weight of the i-j pair, ci (cj ) is the atom fraction, bi
Stress impedance performance testing
To measure the change in impedance (Z) in response to tensile stress (σ) of the amorphous ribbons at a frequency of 1 MHz, an impedance analyzer (LCR Meter IM3536, HIOKI) and a microcomputer-controlled electronic universal testing machine (UTM4304GD, SUNS) were employed. The entire testing process was carried out at room temperature. The stress-impedance ratio (SI) is defined as:
where Z(σ) is the impedance measured under tensile stress σ, and Z(0) is the impedance measured without applying tensile stress σ.
Magnetic testing
A comprehensive physical property measurement system model, QYNACOOL-9 (QUANTUM DESIGN, Inc., USA), was used to measure the hysteresis loops of the amorphous alloys. A portion of the amorphous alloy ribbon with a size of about 2 mm × 3 mm was intercepted, weighed and attached to a sample rod and placed in a sample chamber, with helium gas as a protective gas. The Vibrating Sample Magnetometer (VSM) option was activated to select the appropriate program for the test. The hysteresis loop was measured with a constant temperature setting of 300 K and an applied magnetic field of 0-10,000 Oe.
The magnetostrictive property test system used in this work consists of an MTI-2000 fiber optic displacement measuring instrument (resolution up to 0.1 μm), a signal generator (Agilent 33500B,
RESULTS AND DISCUSSION
Figure 1A provides the DSC curve of the Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 ribbon. During the annealing process, the amorphous alloy gradually crystallizes, with the Tg at 833 K and the onset temperature of crystallization (Tx) at 893 K. The inset displays the XRD pattern of the amorphous ribbon, revealing a broad hump indicating the amorphous nature of the as-cast Fe-Cr-Mo-Si-B-C. Figure 1B shows the S(Q)s of the as-prepared and annealed samples at different temperatures. For the as-prepared sample, the S(Q) data shows a smooth feature without sharp crystallization peaks, further demonstrating the fully amorphous nature. Even after annealing at 828 K, the amorphous ribbon remains amorphous. The sharp crystallization peaks appear when annealing at 858 and 893 K, above Tg, consistent with the DSC results.
Figure 1. (A) DSC curve of Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy measured at a heating rate of 20 K·min-1. The inset is the XRD pattern of the Fe-Cr-Mo-Si-B-C. (B) S(Q) curves of Fe-Cr-Mo-Si-B-C annealed at different temperatures.
The above annealing treatment can eliminate the internal residual stress and tailor the atomic-scale structure of the amorphous alloy, which influences the magnetic domain structure and thereby enhances stress impedance performance[24-27] (discussed later). Figure 2A shows the stress impedance of Fe-Cr-Mo-Si-B-C ribbons annealed at variable temperatures. The stress impedance ratio increases with the annealing temperature increasing from 575 to 823 K, reaching up to about 124%. As the temperature further increases, the material experiences a decline in stress impedance ratio due to crystallization. Meanwhile, as shown in Figure 2B, the magnetization of the Fe-Cr-Mo-Si-B-C ribbon presents a similar temperature-dependent trend with the stress impedance ratio, exhibiting an initial increase followed by a subsequent decline with increasing temperature. The sample annealed at 823 K exhibits optimal soft magnetic performance. This demonstrates a close correlation between the stress impedance performance and soft magnetic properties of amorphous alloys, which could be derived from their atomic structures. As shown in Figure 2C, we explored the effect of annealing time on the stress impedance properties and the best stress impedance properties were measured for the amorphous strip annealed at 15 min. Figure 2D presents the magnetostriction for the ribbons annealed at varying temperatures. When lower magnetic fields (< 250 Oe) are applied, the magnetostrictions of the as-prepared and the 573K-treated samples are relatively strong, corresponding to higher stress impedance ratios under low stress for these two samples (see Figure 2A). However, at 300 Oe, the 823K-treated sample displays the strongest magnetostriction, consistent with the best stress impedance ratio at high stress.
Figure 2. (A) Stress impedance performance and (B) soft magnetic properties of the as-prepared sample and those annealed at 573, 823, and 858 K, respectively. (C) Stress impedance performance of samples with different holding times at 823 K. (D) Magnetostriction of the as-prepared ribbon and those annealed at 573, 823, 858 and 893 K, respectively.
To probe the atomic structure of the Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 ribbons, high-energy synchrotron X-ray total scattering measurements were conducted. Figure 3A displays the PDF analysis of the total scattering data. The analysis of the decay trend of the PDF peak intensities was performed using the exponential decay function[28,29], as described in the Experimental Section. The simulated ξ values increase from 2.87 for the 573 K-treated sample to 3.34 for the 823 K-treated sample. This indicates that annealing the sample around Tg would enhance the degree of atomic ordering. For samples annealed at higher temperatures, the second PDF peak, corresponding to the MRO of the amorphous alloys, shows clear splits, which fingerprints a more ordered atomic structure in crystallized samples. In order to correlate atomic ordering in amorphous alloys with soft magnetic and stress impedance properties, the concept of structural entropy has been introduced (see Experimental Section). The structural entropy can be employed to systematically describe the SRO and MRO structures interconnected by the SRO units. As presented in Figure 3B, the structural entropy phenomenon we obtained is consistent with phenomena in the previous literature[23]. The consistent variation of structural entropy and stress impedance with temperature further proves the strong correlation between atomic ordering and stress impedance performance in amorphous alloys.
Figure 3. (A) Pair distribution function G(r) patterns analyzed by exponential decay function. (B) Relationship between structural entropy and stress impedance ratio at different temperatures.
When converting G(r) into atomic PDF g(r), the second g(r) peak at 3.5-5.5 Å corresponds to the MRO atomic clusters connected by SRO units, including point-shared (1-atom connection), edge-shared (2-atom connection), face-shared (3-atom connection), and embedded (4-atom connection) modes. Given the isotropic nature of amorphous alloys, a Gaussian function was used for fitting the second peak[30], as shown in Figure 4A-C. Cluster connectivity analysis reveals significant differences in atomic stacking after annealing treatments. Annealing treatment at Tg (i.e., 823 K) increases the proportion of edge-sharing modes and decreases the proportion of face-connecting modes, indicating the formation of uniform Fe-M (M refers to Si, B, P) atomic clusters. According to the solute-solute avoidance phenomenon[31,32], since the combination of Fe-M is more stable than M-M or Fe-Fe, there is a greater negative heat of mixing of Fe and M elements when annealing is performed at 823 K, which results in the formation of increasing homogeneous clusters of Fe-M atoms. In the medium-range order, the uniform Fe-M atomic clusters and the configuration stability of the residual matrix promote ferromagnetic exchange interactions[33]. These uniform Fe-M clusters weaken the heterogeneity of coupling energy, facilitating coherent movement and rotation of domain walls during the magnetoelastic coupling process, resulting in excellent response to applied stress[34,35]. Further annealing at higher temperatures reduces nanoscale heterogeneity, decreasing stress impedance performance. The PDF analysis reveals that the 823 K-annelaed sample exhibits the highest stress impedance ratio, confirming that the edge-sharing mode in MRO is beneficial for enhancing the stress impedance performance of amorphous alloys. When the temperature reaches 893 K, the proportion of edge-shared modes further increases, but the ribbon becomes fragile due to crystallization at this temperature, giving rise to a severe drop in the stress impedance ratio.
Figure 4. (A) Fitting results of different cluster connectivity modes in the second shell of as-prepared, (B) 823 K-annealed
Figure 4D and E shows the fitting results of the first-shell peak for the as-prepared and 823 K-annealed samples, respectively. The amorphous ribbons annealed near Tg show a significant decrease in (Fe, Cr)-(Fe, Cr) and an increase in (Fe, Cr, Mo)-Mo in the first shell coordination. So, the annealing treatment also changes SRO, promoting magneto-electric conversion in amorphous alloys. The structural coordination in the short- and medium-range orders synergistically promotes the magnetic softening and stress impedance performance of the Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy. Further annealing at 893 K increases (Fe, Cr)-(Fe, Cr) and decreases (Fe, Cr, Mo)-Mo compared to 823 K [Figure 4F], accompanied with crystallization and fragility of the ribbon.
To validate the practical applicability of the high stress impedance performance of Fe-Mo-Cr-B-Si-C amorphous alloy, a composite film was fabricated by mechanically blending amorphous powders of the same composition with silicone rubber. Figure 5A presents the change of stress impedance ratio with the content of as-cast amorphous powders in the composition film. As the powder content increases, the stress impedance ratio initially decreases and then rises, reaching its maximum value at a powder content of
Figure 5. (A) Stress impedance performance of the composite films containing 20, 40, 60 and 80 wt% amorphous powders. (B) Stress impedance performance and (C) hysteresis loops of the composite films containing 80 wt% amorphous powders annealing at different temperatures.
CONCLUSIONS
To summarize, our study demonstrates that the stress impedance performance of Fe-Cr-Mo-Si-B-C amorphous alloys could be enhanced by annealing treatment at the temperature around Tg. By high-energy synchrotron X-ray total scattering, we reveal a strong correlation between stress impedance performance and the medium-range ordered structure of amorphous alloys, specifically emphasizing the crucial role of increased edge-sharing atomic connection modes. Moreover, the successful fabrication of a composite film combining the amorphous alloy with silicone rubber under the same annealing treatment enables a remarkable improvement in sensitivity compared to traditional ribbons. This work proposes a general annealing strategy for preparing amorphous alloys with high stress impedance performance, which may promote the potential applications of amorphous alloys in advanced sensing technologies.
DECLARATIONS
Acknowledgment
Zhu H and Lan S acknowledge the support of the Beijing Synchrotron Radiation Facility.
Authors’ contributions
Design: Lan S, Zhu H
Experiments and data collection: Gu Y, Zhao Y, Fan L, Zhang S
Data analysis: Gu Y, Zhao Y, Zhu H
Data analysis, manuscript writing: Ge J
Manuscript writing: Gu Y, Zhu H, Zhao Y
Manuscript revision and supervising: Lan S, Zhu H
All authors have read and agreed to the published version of the manuscript.
Availability of data and materials
The data that support the findings of this study are available from the corresponding author upon reasonable request.
Financial support and sponsorship
This study was financially supported by the National Key R&D Program of China (No. 2021YFB3802800), the National Natural Science Foundation of China (No. 52222104, No. 12261160364, and No. 22275089), and the Natural Science Foundation of Jiangsu Province (No. BK20200019). This research used the resources of high energy synchrotron radiation light source, Beijing Synchrotron Radiation Facility operated for Institute of High Energy Physics, Chinese Academy of Sciences.
Conflicts of interest
Lan S is an Editorial Board Member of the journal Microstructures. The other authors declare that there are no conflicts of interest.
Ethical approval and consent to participate
Not applicable.
Consent for publication
Not applicable.
Copyright
© The Author(s) 2024.
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Cite This Article
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Gu, Y.; Zhao Y.; Ge J.; Fan L.; Zhang S.; Zhu H.; Lan S. Optimizing stress impedance and medium-range ordered structure in Fe46.6Mo8.6Cr24.5B9.5C10Si0.6 amorphous alloy through tailored annealing treatment. Microstructures. 2024, 4, 2024060. http://dx.doi.org/10.20517/microstructures.2024.05
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