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High-pressure strengthening in ultrafine-grained metals

Nature volume 579, pages 67–72 (2020)Cite this article

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Abstract

The Hall–Petch relationship, according to which the strength of a metal increases as the grain size decreases, has been reported to break down at a critical grain size of around 10 to 15 nanometres1,2. As the grain size decreases beyond this point, the dominant mechanism of deformation switches from a dislocation-mediated process to grain boundary sliding, leading to material softening. In one previous approach, stabilization of grain boundaries through relaxation and molybdenum segregation was used to prevent this softening effect in nickel–molybdenum alloys with grain sizes below 10 nanometres3. Here we track in situ the yield stress and deformation texturing of pure nickel samples of various average grain sizes using a diamond anvil cell coupled with radial X-ray diffraction. Our high-pressure experiments reveal continuous strengthening in samples with grain sizes from 200 nanometres down to 3 nanometres, with the strengthening enhanced (rather than reduced) at grain sizes smaller than 20 nanometres. We achieve a yield strength of approximately 4.2 gigapascals in our 3-nanometre-grain-size samples, ten times stronger than that of a commercial nickel material. A maximum flow stress of 10.2 gigapascals is obtained in nickel of grain size 3 nanometres for the pressure range studied here. We see similar patterns of compression strengthening in gold and palladium samples down to the smallest grain sizes. Simulations and transmission electron microscopy reveal that the high strength observed in nickel of grain size 3 nanometres is caused by the superposition of strengthening mechanisms: both partial and full dislocation hardening plus suppression of grain boundary plasticity. These insights contribute to the ongoing search for ultrastrong metals via materials engineering.

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Fig. 1: Size strengthening of nanograined nickel.
Fig. 2: Inverse pole figures for the texture evolution of nickel with various grain sizes.
Fig. 3: Computational simulation results and the modified Hall–Petch relationship.
Fig. 4: TEM examinations of nickel samples quenched from 40 GPa of three grain sizes.

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Data availability

The data that support the findings of this study are available from the corresponding authors upon reasonable request.

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Acknowledgements

We thank K. Lu, D. J. Jensen, N. Hansen, S.-I. Karato, G. Fan, J. Liu and F. Zhao for pre-review and discussions. X. Z. thanks F. Lin for EVPSC tutoring. We acknowledge support from the National Natural Science Foundation of China (NSFC) under grant numbers 11621062, 11772294, U1530402 and 11811530001. X.Z. acknowledges the Advanced Light Source Doctoral Fellowship in Residence Program and Collaborative Postdoctoral Fellowship Program. L.Z. acknowledges support from the Fundamental Research Funds for the Central Universities of China (2018XZZX001–05). L.M. acknowledges support from CDAC and NSF (EAR-1654687). Z.F., T.H. and X.H. acknowledge support from the National Key Research and Development Program of China (2016YFB0700400). This research used the resources of the Advanced Light Source, which is a DOE Office of Science User Facility under contract number DE-AC02-05CH11231 and the Shanghai Synchrotron Radiation Facility. This research was partially supported by COMPRES, the Consortium for Materials Properties Research in Earth Sciences under NSF Cooperative Agreement EAR 1606856.

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Author notes

  1. These authors contributed equally: Xiaoling Zhou, Zongqiang Feng, Linli Zhu, Jianing Xu

Authors and Affiliations

  1. Center for High Pressure Science and Technology Advanced Research, Pudong, Shanghai, China

    Xiaoling Zhou, Jianing Xu, Hongliang Dong, Hongwei Sheng, Yanju Wang, Hengzhong Zhang & Bin Chen

  2. Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA, USA

    Xiaoling Zhou, Jinyuan Yan, Nobumichi Tamura & Martin Kunz

  3. Department of Geology and Geophysics, University of Utah, Salt Lake City, UT, USA

    Xiaoling Zhou & Lowell Miyagi

  4. International Joint Laboratory for Light Alloys (MOE), College of Materials Science and Engineering, Chongqing University, Chongqing, China

    Zongqiang Feng & Xiaoxu Huang

  5. Center for X-Mechanics, Zhejiang University, Hangzhou, China

    Linli Zhu

  6. Key Laboratory of Soft Machines and Smart Devices of Zhejiang Province, School of Aeronautics and Astronautics, Zhejiang University, Hangzhou, China

    Linli Zhu

  7. Department of Physics, Fudan University, Shanghai, China

    Jianing Xu

  8. State Key Lab of Superhard Materials, College of Physics, Jilin University, Changchun, China

    Quan Li & Yanming Ma

  9. International Center for Computational Method and Software, College of Physics, Jilin University, Changchun, China

    Quan Li & Yanming Ma

  10. International Center for Future Science, Jilin University, Changchun, China

    Quan Li & Yanming Ma

  11. Department of Chemistry, University of California, Berkeley, CA, USA

    Katie Lutker

  12. Shenyang National Laboratory for Materials Science, Chongqing University, Chongqing, China

    Tianlin Huang

  13. Unaffiliated, Fremont, CA, USA

    Darcy A. Hughes

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  1. Xiaoling Zhou
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Contributions

B.C. conceived the project. X.H. directed the TEM examinations. J.X., H.D., H.Z. and K.L. performed the nanocrystal synthesis. X.Z., B.C., L.M., J.Y., N.T. and M.K. performed the high-pressure XRD experiments. Z.F., Y.W., D.A.H., T.H. and X.H. performed the TEM experiments and analysis. L.Z., H.S., Q.L. and Y.M. performed the computational and molecular dynamics simulations. X.Z. and L.M. performed the EVPSC modelling. X.Z. and B.C. wrote the manuscript. All authors discussed the results and commented on the manuscript.

Corresponding authors

Correspondence to Xiaoxu Huang or Bin Chen.

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Extended data figures and tables

Extended Data Fig. 1 The experimental setup of radial DAC XRD.

Kapton is a polyimide film. hkl represents the lattice planes; δ is the azimuthal angle; and θ represents the diffraction angle.

Extended Data Fig. 2 Grain size distribution of nickel samples.

a–d, Grain size distributions in 3-nm, 8-nm, 12-nm and 20-nm nickel; e–h, Grain size distribution of 40-nm, 70-nm, 100-nm and 200-nm nickel. The particle sizes of the nickel samples were re-checked with XRD characterization.

Extended Data Fig. 3

Raw powder samples. a–d, TEM images of raw powder samples of 3 nm (a), 8 nm (b), 12 nm (c) and 20 nm (d) nickel powder before compression. e–h, Scanning electron microscopy characterization of 40 nm (e), 70 nm (f), 100 nm (g) and 200 nm (h) nickel powder before compression.

Extended Data Fig. 4 Plot of differential stress versus hydrostatic lattice strain in the nickel of various grain sizes.

The circles, squares and triangles represent (220), (200) and (111) lattice planes, respectively. Strong strength anisotropy is exhibited for different lattice planes, especially at smaller grain sizes. The lattice strain is calculated from the relative change in the unit cell parameter at a given applied stress to the unit cell parameter under ambient pressure (see Supplementary Information). The error bars for differential stress is calculated based on the error of deviatoric strain Q(hkl) and equations (6) to (9). Note that for some of the data points the error bars (see Supplementary Information for definition) are smaller than the sizes of symbols.

Extended Data Fig. 5 EVPSC modelling results of nickel.

a, Comparison between simulated Q(hkl) curves versus pressure and measured Q(hkl) values (solid symbols) obtained from experiments. b, Simulated texture of nickel at the highest strain (pressure). c, Simulated differential stress of nickel versus plastic strain during zero pressure compression. d, Extrapolated yield strength of nickel at ambient conditions without GB sliding. The size-strengthening trend is consistent with that shown in Fig. 1b, although the strength of 40-nm-grain-size nickel obtained with EVPSC is slightly lower.

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Zhou, X., Feng, Z., Zhu, L. et al. High-pressure strengthening in ultrafine-grained metals. Nature 579, 67–72 (2020). https://doi.org/10.1038/s41586-020-2036-z

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