Substantially enhanced homogeneous plastic flow in hierarchically nanodomained amorphous alloys

Wu, Ge; Liu, Sida; Wang, Qing; Rao, **g; **a, Wenzhen; Yan, Yong-Qiang; Eckert, Jürgen; Liu, Chang; Ma, En; Shan, Zhi-Wei

doi:10.1038/s41467-023-39296-6

Substantially enhanced homogeneous plastic flow in hierarchically nanodomained amorphous alloys

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Published: 20 June 2023

Volume 14, article number 3670, (2023)
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Substantially enhanced homogeneous plastic flow in hierarchically nanodomained amorphous alloys

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Ge Wu ORCID: orcid.org/0000-0002-4543-5011¹,
Sida Liu²,
Qing Wang³,
**g Rao⁴,
Wenzhen **a⁵,
Yong-Qiang Yan¹,
Jürgen Eckert^6,7,
Chang Liu ORCID: orcid.org/0000-0001-6755-6327⁸,
En Ma ORCID: orcid.org/0000-0002-7468-4340⁸ &
…
Zhi-Wei Shan¹

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Abstract

To alleviate the mechanical instability of major shear bands in metallic glasses at room temperature, topologically heterogeneous structures were introduced to encourage the multiplication of mild shear bands. Different from the former attention on topological structures, here we present a compositional design approach to build nanoscale chemical heterogeneity to enhance homogeneous plastic flow upon both compression and tension. The idea is realized in a Ti-Zr-Nb-Si-XX/Mg-Zn-Ca-YY hierarchically nanodomained amorphous alloy, where XX and YY denote other elements. The alloy shows ~2% elastic strain and undergoes highly homogeneous plastic flow of ~40% strain (with strain hardening) in compression, surpassing those of mono- and hetero-structured metallic glasses. Furthermore, dynamic atomic intermixing occurs between the nanodomains during plastic flow, preventing possible interface failure. Our design of chemically distinct nanodomains and the dynamic atomic intermixing at the interface opens up an avenue for the development of amorphous materials with ultrahigh strength and large plasticity.

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Introduction

Homogeneous plastic flow, different from shear banding, is a ductile deformation mode of metallic glasses (MGs) when the sample size is reduced to sub-100 nm^1,2. Computational simulations have shown their advantages in predicting nanostructures of MGs with homogeneous plastic flow. Evolutionary algorithms³ are able to search for MG candidates with excellent glass forming ability (GFA), and thus optimize the existing MGs. Machine learning based modelings^4,5,6 can predict structure heterogeneities for different MG systems and correlate their structures with mechanical properties. Multiscale modelings by molecular dynamics simulations^7,8 demonstrate that heterogeneous MGs (nanoglasses or nanolaminated composites) have enhanced homogeneous deformation. In experiments, however, it is difficult to achieve very large heterogeneity as that in simulations and the mechanical strain rates are much lower (~10⁻³s⁻¹ vs. ~10⁷s⁻¹). Adding crystalline phase into the amorphous matrix^{9,Full size image}

Here, we realize this idea by using magnetron sputtering to alternately deposit 3.4-nm-thick Ti-Zr-Nb-Si-XX and 2.9-nm-thick Mg-Zn-Ca-YY nanodomains using Ti₆₀Zr₁₀Nb₁₅Si₁₅ (at.%) and Mg₆₀Zn₃₅Ca₅ (at.%) targets, respectively. The received material shows a high yield strength of 1.6 GPa and plastic deformation of over 60% strain (including ~40% homogeneous plastic flow). During plastic flow, dynamic atomic intermixing occurs between the amorphous nanodomains, originating from atomic rearrangements via profuse shear transformation events. This behavior prevents possible interface failure and thus leads to mechanical stabilization of the whole material.

Results

Enthalpy-guided alloy design

It is worthwhile noting that severe interdiffusion (>50 at.%) occurs in sputtered nanolaminates when the nanolayer thickness is reduced to ~3 nm²². The thermodynamic driving force is large negative mixing enthalpy of the constituent elements²⁰ in the adjoining nanolayers. To reduce this effect, here we used Mg and Ti with positive mixing enthalpy, as the principal constituent elements of the nanodomains. It is reported that hierarchical herringbone-like microstructure is efficient to provide crack buffering effect in a crystalline high-entropy alloy²³. Here we introduced structure/composition hierarchy into amorphous materials, exploiting the different growth modes of the nanodomains. We noted that the as-deposited Mg-Zn-Ca alloy has a nano-dual-phase amorphous structure, where Ca-enriched amorphous filaments with a diameter of ~5 nm are aligned in a Mg-enriched amorphous matrix from the growth direction (Supplementary Fig. 1). We thus used Mg-Zn-Ca amorphous nanolayer as a precursor to realize skeleton-like hierarchical nanostructure (Fig. 1b) of the whole material, distinct from multilayer structure of conventional films fabricated also by alternate deposition²⁴. Both the two domains are amorphous, as indicated by the halo ring feature (inset, Fig. 1c) in selected-area electron diffraction (SAED). Figure 1d, e shows that the Ti-Zr-Nb-Si-XX and Mg-Zn-Ca-YY domains are bright and dark regions in aberration-corrected high-angle-annular dark-field (HAADF) scanning transmission electron microscopy (STEM) image (Fig. 1c), respectively. The compositions of the alternately sputter-deposited amorphous domains are Ti₅₅Zr₅Nb₆Si₁₅Mg₆Zn₁₀Ca₃ (at.%) and Mg₃₇Zn₃₅Ca₃Ti₁₅Zr₂Nb₂Si₆ (at.%). The side-view TEM image of the material shows a wavy structure, which is vertically separated by Mg, Zn and Ca-enriched regions with a thickness of ~5 nm and a wavelength of ~65 nm. Correspondingly, the plan-view TEM image (Fig. 1b) shows ~65-nm-diameter amorphous granular regions surrounded by ~5-nm-thick amorphous intergranular layers. The wavy structure shown in the side-view images (Fig. 1b, c) results from the columnar growth of nanolaminates²⁵. As a comparison, the sputtered Ti-Zr-Nb-Si reference amorphous alloy shows a homogeneous composition without the wavy structure (Supplementary Fig. 2).

Mechanical properties

We carried out micro-compression tests on micro-pillars fabricated from the materials to investigate their mechanical responses at room temperature. The compression experiments were conducted on Mg-Zn-Ca amorphous alloy, Ti-Zr-Nb-Si amorphous alloy and the hierarchically nanodomained amorphous alloy pillar samples with a diameter of 1 µm and height of 2 µm to avoid sample size effect^2,26. The Mg-Zn-Ca and Ti-Zr-Nb-Si reference amorphous alloys have yield strength of 1.0 GPa and 2.2 GPa, respectively, and identical elastic strain of ~2% (Fig. 2a). Their stress-strain curves reveal large serrations after yielding, which are related to the generation and propagation of shear bands. The mechanical responses and deformed pillar morphologies (Fig. 2b, c) of the reference amorphous alloys show a brittle deformation mode, consistent with other micro-compression reports for MGs^27,28,29. In contrast, the hierarchically nanodomained amorphous alloy reveals a yield strength of 1.6 GPa and plastic deformation of over 60% strain (including ~40% homogeneous deformation) (Fig. 2a). The pillar compression tests under identical conditions were repeated for at least three times to ensure statistical significance (Supplementary Fig. 3). Figure 2e shows improved mechanical property of the hierarchically nanodomained amorphous alloy compared with that of other amorphous alloys with similar sample dimensions^27,28,29,30. The yield strength is normalized by Young’s modulus (σ_y/E). The normalized yield strength of all samples lies in the regime typical for MGs (σ_y = E/50)¹⁴. However, the plastic flow of the hierarchically nanodomained amorphous alloy is substantially more homogeneous, which is usually seen in the supercooled liquid but with low normalized yield strength. The deformed pillar after >60% strain shows a relatively homogeneous deformation feature with only a few small shear bands (Fig. 2d). We checked the morphology of the deformed pillar with ~30% strain, and it shows no shear bands (inset, Fig. 2a). Therefore, the stress deviation (apart from the green dashed line on Fig. 2a) and small serrations on the stress-strain curve after 40% strain correspond to multiple shear banding events.

**Fig. 2: Improved mechanical property of the hierarchically nanodomained amorphous alloy compared with that of reference mono- and hetero-MGs.**

The apparent stress increase after pop-in events for the reference amorphous alloys results from a sudden increase of pillar diameter by shear banding but does not represent strain hardening. However, the stress-strain curve of the hierarchically nanodomained amorphous alloy reveals a continuous deviation from the linear elastic region as the stress increases from 1.6 to 2.0 GPa (Fig. 2a), suggesting a strain hardening response. We further did compression experiments on nanopillars extracted from pre-deformed and un-deformed samples (Supplementary Fig. 4). The yield strength of the pre-deformed material is 1.8 GPa, 0.2 GPa higher than that of the un-deformed material, due to a change in chemical composition and structure (atomic intermixing between the two nanodomains).

It is reported that MGs can be rejuvenated to an elevated energy state by confined deformation³¹, which facilitates the homogeneous plastic flow of ~1% strain (with strain hardening) in compression. It is known that the elevated energy³¹ of MGs corresponds to ultra-fast cooling at ~10⁶K/s, three to four orders of magnitude higher than the possible cooling rate for a conventional cast rod, but that effective cooling rate is lower than what we used in magnetron sputtering deposition (~10¹⁰K/s)³². Therefore, it is supposed that the deposited hierarchically nanodomained amorphous alloy has an elevated energy. However, the as-deposited Mg-Zn-Ca and Ti-Zr-Nb-Si reference amorphous alloys show shear banding-dominated plastic deformation, which therefore indicates that the large homogeneous plastic flow and the observed strain hardening of the hierarchically nanodomained amorphous alloy are not due to energy elevation.

Deformation mechanism

We performed micro-indentation and pillar compression on the hierarchically nanodomained amorphous alloy and then conducted aberration-corrected STEM on the deformed materials to investigate the deformation mechanism. The period thickness of the Ti-Zr-Nb-Si-XX /Mg-Zn-Ca-YY domains decreases from 6.3 to 5.5 nm (13% strain), as the strain increases. The deformed region with >70% strain shows low contrast between the amorphous domains in HAADF-STEM imaging (Fig. 3c), indicating the reduced compositional difference. The maze-like pattern in the BF-STEM image confirms the amorphous structure (Fig. 3d). Near-atomic resolution EDS map**s were performed on these regions with different strains. One-dimensional (1D) compositional profiles probed from the regions with strains from 0% to >70% show that the amplitude of the elemental concentration difference decreases as the strain increases (Fig. 3e–g). This indicates that dynamic atomic intermixing between the adjacent amorphous domains occurs during homogeneous plastic flow. It has been reported that the deformed MGs usually show elemental re-distribution inside shear bands, where specific element enriched and depleted regions both exist^33,34. However, the hierarchically nanodomained amorphous alloy here shows a composition homogenization of the amorphous domains. The atomic intermixing is usually observed in highly deformed crystalline alloys^35,36, known as an externally driven mechanical alloying effect. It was found that dislocations drag highly concentrated atoms from one phase to another^35,36, inducing composition homogenization of the alloy during plastic deformation. Different from that in crystalline alloys, plasticity carriers in MGs are shear transformation (ST) zones^37,38 instead of dislocations. The homogeneous plastic flow of MGs is based on the activation of profuse ST events³⁹, which induce appreciable rearrangement of atoms between the adjacent amorphous nanodomains. This kinetic process facilitates homogenization of the nanodomains, rather than phase separation toward equilibrium reported inside some shear bands³⁴.

**Fig. 3: Dynamic atomic intermixing of the hierarchically nanodomained amorphous alloy during plastic deformation.**

We use a schematic diagram to illustrate the advantages of the chemically distinct nanodomains and deformation-induced dynamic atomic intermixing mechanism (Fig. 4). The Young’s modulus of the Mg-Zn-Ca-YY domain is expected to be smaller than that of the Ti-Zr-Nb-Si-XX domain, considering that the Young’s modulus of the Mg-Zn-Ca and Ti-Zr-Nb-Si reference amorphous alloys is 45 GPa and 110 GPa, respectively, obtained from nanoindentation. Therefore, the profuse ST events occur earlier in the Mg-Zn-Ca-YY domain, and as the flow stress increases, these events occur in the Ti-Zr-Nb-Si-XX domain afterward. The non-homogeneous deformation⁴⁰ of the two amorphous domains induces tiny serrated stress flow (from ~5 to ~40% strain, Fig. 2a) during homogeneous plastic flow. In this process, the dynamic atomic intermixing reduces compositional difference (Fig. 3) and in turn reduces Young’s modulus mismatch between the two amorphous domains¹⁴. This decreases stress concentrations between the amorphous domains, preventing any potential interface failure. Furthermore, extrusion of softer phases during pillar compression, often observed in crystalline (softer)-amorphous (harder) nanolaminates⁴¹, does not occur in the current material. This facilitates co-deformation of the amorphous domains with reduced plastic strain difference after the atomic intermixing. The dynamic atomic intermixing thus enhances the mechanical stability of the hierarchically nanodomained amorphous alloy during homogeneous plastic flow. The atomic intermixing between the amorphous domains becomes severe after the material undergoes large strains (Fig. 3c). Eventually, the composition or Young’s modulus of the two amorphous domains would be homogenized to become similar (Fig. 3c, g).

**Fig. 4: Illustration of the dynamic atomic intermixing mechanism.**

Tensile behavior

We further conducted in-situ tension experiments in an aberration-corrected TEM to reveal the tensile behavior of the hierarchically nanodomained amorphous alloy at room temperature (Fig. 5). The thickness of TEM lamella is ~50 nm before tension. The TEM lamella contains more than seven of the Ti-Zr-Nb-Si-XX/Mg-Zn-Ca-YY structural units in the thickness direction of the specimen and should reflect an average mechanical response of the whole material in tension. The material undergoes a large strain of 7.8% before the onset of cracking (Fig. 5c), indicating a stable flow behavior. A similar ductilization phenomenon by dual-amorphous phase has been achieved in a Co-Fe-Ta-B-O oxide glass⁴², which shows an enhanced tensile plasticity of 2.7%. Furthermore, during cracking, the current hierarchically nanodomained amorphous alloy shows nano-bridging behavior for cracks and subsequent plastic flow of the bridging regions (Fig. 5d–h), in contrast to shear band induced cracking behavior of conventional MGs (Fig. 5j–l). Previous successful ductilization approaches for MGs have demonstrated that heterogeneous amorphous structures^43,44,45, embedded crystalline phases^{9,Mechanical characterization}

Micro-compression and tension were performed using a Hysitron TI950 nanoindenter and a PI95 PicoIndenter with a diamond punch and a W gripper, respectively under displacement-control mode and at a strain rate of ~2 × 10⁻³s⁻¹. The Hysitron TI950 nanoindenter is an ex-situ instrument in air, and thus the electron beam-induced composition and structure changes can be ruled out during compression. Micro-pillar and dog-bone-shaped samples were fabricated using FIB, with 30 kV/7 pA as the final milling condition. The aspect ratio (height/diameter) of the pillar was 2, and the taper angle of each pillar was less than 1.5°. The engineering stress σ was calculated using F/A₀, where F is the measured force and A₀ is the original cross-sectional area at the top of pillar samples or the cross-sectional area of dog-bone-shaped samples. The engineering strain ε was calculated using L/L₀, where L is the measured displacement and L₀ is the original length of the samples.

In-situ TEM tension

The in-situ TEM tension experiments at room temperature were conducted by using a Gatan model 654 single-tilt straining holder with the normal e-beam density in an image aberration-corrected FEI Titan (Themis 80-300).

Data availability

All data generated or analyzed during this study are included in the article and its Supplementary Information files, and are available from the corresponding authors upon request.

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Acknowledgements

G.W. acknowledges support from the National Natural Science Foundation of China (52271114). G.W. and C.L. acknowledge supports from National Natural Science Fund for Excellent Young Scientists Fund Program (Overseas). We thank D. Raabe, D. Ponge and J. Best at Max-Planck-Institut für Eisenforschung and J. Lu at the City University of Hong Kong for helpful discussions. We thank P.-C. Zhang, P. Zhang, Q.-Q. Fu and D.-L. Zhang at **’an Jiaotong University for technical support.

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Authors and Affiliations

Center for Advancing Materials Performance from the Nanoscale (CAMP-Nano) and Hysitron Applied Research Center in China (HARCC), State Key Laboratory for Mechanical Behavior of Materials, **’an Jiaotong University, 710049, **’an, China
Ge Wu, Yong-Qiang Yan & Zhi-Wei Shan
Institute for Advanced Technology, Shandong University, 250061, **an, China
Sida Liu
Laboratory for Microstructures, Institute of Materials, Shanghai University, 200072, Shanghai, China
Qing Wang
Max-Planck-Institut für Eisenforschung, Max-Planck-Straße 1, Düsseldorf, 40237, Germany
**g Rao
School of Metallurgical Engineering, Anhui University of Technology, 243000, Maanshan, China
Wenzhen **a
Erich Schmid Institute of Materials Science, Austrian Academy of Sciences, Jahnstraße 12, Leoben, A-8700, Austria
Jürgen Eckert
Department of Materials Science, Chair of Materials Physics, Montanuniversität Leoben, Jahnstraße 12, Leoben, A-8700, Austria
Jürgen Eckert
Center for Alloy Innovation and Design (CAID), State Key Laboratory for Mechanical Behavior of Materials, **’an Jiaotong University, 710049, **’an, China
Chang Liu & En Ma

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Ge Wu
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Contributions

C.L. designed the alloys and guided the project with Z.W.S.; C.L. and G.W. conducted FIB and TEM experiments; G.W. and C.L. conducted APT characterization and data analysis; C.L., G.W., S.L., J.R., W.X. and Y.Q.Y. conducted micro-compressions and micro-indentations; G.W. and C.L. conducted (S)TEM characterization and in-situ tension experiments; C.L., Q.W., J.E., E.M. and Z.W.S. contributed to the interpretations of the observations; G.W., C.L. and E.M. wrote the paper; all authors contributed to the discussion of the results.

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Wu, G., Liu, S., Wang, Q. et al. Substantially enhanced homogeneous plastic flow in hierarchically nanodomained amorphous alloys. Nat Commun 14, 3670 (2023). https://doi.org/10.1038/s41467-023-39296-6

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Received: 30 January 2023
Accepted: 05 June 2023
Published: 20 June 2023
DOI: https://doi.org/10.1038/s41467-023-39296-6
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