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SCIENCE CHINA Materials, Volume 64 , Issue 9 : 2348-2358(2021) https://doi.org/10.1007/s40843-021-1648-3

Development of micro-Laue technique at Shanghai Synchrotron Radiation Facility for materials sciences

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  • ReceivedJan 9, 2021
  • AcceptedFeb 17, 2021
  • PublishedMay 14, 2021

Abstract


Funded by

the National Key Research and Development Program of China(2016YFB0700404)

and the National Natural Science Foundation of China(91860109,U2032205,51671154,51927801)


Acknowledgment

This work was supported by the National Key Research and Development Program of China (2016YFB0700404), and the National Natural Science Foundation of China (91860109, U2032205, 51671154, and 51927801). Chen K appreciates the support from the International Joint Laboratory for Micro/Nano Manufacturing and Measurement Technologies and the Collaborative Innovation Center of High-End Manufacturing Equipment.


Interest statement

The authors declare that they have no conflict of interest.


Contributions statement

Tai R and Huang X proposed and supervised this work. Liu M, Dong X and Li ZL designed and built the micro-Laue beamline on BL09B. Jiang L, Yan S, Li L and Li ZJ prepared the superalloy specimens and conducted the 2D scans. Ren C, Kou J and Chen K developed the software packages, analyzed the data and interpreted the results. Chen K, Ren C, Li ZJ, Li ZL and Huang X wrote the paper. All authors contributed to the discussion.


Author information

Chenyu Ren is currently a PhD student at the Center for Advancing Materials Performance from the Nanoscale (CAMP-Nano), Xi’an Jiaotong University. Her research interests focus on the microstructure study of laser-processed Ni-based superalloys.


Li Jiang obtained his Master degree from Northwestern Polytechnical University in 2012 and PhD degree from the University of Chinese Academy of Sciences in 2017. He is now an associate professor at Shanghai Institute of Applied Physics, Chinese Academy of Sciences. His research interests focus on the design of superalloys for nuclear applications and the alloy corrosion behavior by fission products using advanced material characterization approaches such as synchrotron radiation-based techniques.


Jiawei Kou obtained his Bachelor degree in 2018 and then continued his graduate study at the CAMP-Nano, Xi’an Jiaotong University. He is dedicated to the development of high-speed in-depth Laue diffraction data mining algorithms and software packages. He applies these new approaches to the study of the microstructures of advanced alloys.


Kai Chen obtained his Bachelor and PhD degrees from Peking University and the University of California Los Angeles in 2005 and 2009, respectively. After two postdoctoral stints at the University of California Berkeley and Lawrence Berkeley National Laboratory, he has been a professor at Xi’an Jiaotong University since 2011. He is interested in pushing the software and hardware developments for synchrotron micro-Laue diffraction and applying this advanced characterization method to the study of advanced engineering materials.


Zhongliang Li obtained his PhD degree from the National Synchrotron Radiation Laboratory, University of Science and Technology of China in 2011. He is currently an associate professor in the optical group of Shanghai Synchrotron Radiation Facility. His research interests focus on the X-ray measurement methodology of beamline instruments and optical elements, synchrotron radiation-based science and technology, and the microstructural evolution of alloys under corrosive conditions of fission products.


Zhijun Li obtained his PhD degree from Harbin Institute of Technology in 2007. He holds the professorship at Shanghai Institute of Applied Physics, Chinese Academy of Sciences. His research interests focus on the design and characterization of alloys for nuclear energy applications using advanced synchrotron radiation-based techniques.


Renzhong Tai obtained his PhD degree from the Graduate University for Advanced Studies, Japan in 1999. After postdoctoral research on coherent X-ray applications at Japan Atomic Energy Research Institute, he holds the professorship at Shanghai Institute of Applied Physics, Chinese Academy of Sciences. He is currently the executive deputy director of Shanghai Synchrotron Radiation Facility. His research interests focus on synchrotron radiation science and techniques, X-ray microscopy, X-ray detector technology, X-ray interference lithography, photon correlation spectroscopy, and beamline development.


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  • Figure 1

    Schematic layout of the micro-Laue diffraction setup on BL09B in SSRF.

  • Figure 2

    Focused X-ray beam spot shape and size. (a) The X-ray beam spot is symmetric on the scintillator; (b, c) the FWHMs in the horizontal and vertical directions measured to be ~43.5 and 50.5 µm, respectively.

  • Figure 3

    Laue diffraction pattern visualization and indexation using the software package PPCIA. A typical Laue pattern is (a) loaded into the software, (b) binarized, and indexed, with the Miller indices of the Laue reflections marked.

  • Figure 4

    Laue peak profile analysis using the software package LDat. The 157 reflection on the pattern shown in Fig. 3 is (a) enlarged, (b) converted to the 2θ-χ space, and (c, d) projected to 2θ- and χ-axes, respectively.

  • Figure 5

    The microstructure distribution of the scanned base metal. (a) Inverse pole figure shows the scanned area contains only one crystal grain. (b) The filtered intensity, (c) KAM, and (d) misorientation of each scanning pixel with respect to the bottom left point show inhomogeneous orientation. (e, f) Non-uniform FWHM of the 135 reflection demonstrates heterogeneous defect distribution.

  • Figure 6

    Diagonal strain tensor components of the scanned area in the base metal.

  • Figure 7

    The microstructure distribution of the scanned weld joint area. (a) Inverse pole figure and (b) the filtered intensity show the columnar grain structure; (c) KAM and (d) intragranular misorientation distribution suggest higher orientation gradient than in the base metal.

  • Figure 8

    Diagonal strain tensor components of the scanned area in the fusion zone.

  • Figure 9

    Comparisons of the Laue diffraction peak profiles and strains in both scans. (a, b) The Laue reflections taken on the base metal are sharper than those on the fusion zone; (c, d) the von Mises strains in the base metal are lower and more narrowly distributed than those in the fusion zone.

  • Table 1   A summary of the micro-Laue beamline specifications all over the world

    Micro-Laue beamline

    Energy range (keV)

    Beam size (μm2)

    Uniqueness

    34-ID-E@APS

    7–30

    0.3 × 0.3

    3D diffraction

    12.3.2@ALS

    5–22

    ~1 × 1

    Versatile data analysis software

    21A@TPS

    5–30

    0.1 × 0.1

    Ultra-high sub-100 nm resolution

    microXAS@SLS

    3–23

    ~1 × 1

    Ultra-fast 20 kHz data collection

    B16@DLS

    5–25

    ~50 × 50

     

    BM32@ESRF

    5–25

    ~0.5 × 0.5

     

    VESPERS@CLS

    6–30

    ~4 × 4

     

    Currently on 09B, finally on 03B@SSRF

    4–30

    40 × 50 on 09B (Jun. 2020); 1 × 1.5 on 03B (designed)

    High-speed data analysis for simultaneous microstructure visualization

  • Table 2   Chemical compositions of the GH3535 plate and ERNiMo-2 welding wire in wt%

    Ni

    Cr

    Mo

    Fe

    Si

    C

    Al

    Mn

    S

    P

    ERNiMo-2 filler alloy

    Bal.

    6.89

    16.4

    3.62

    0.43

    0.053

    0.06

    0.58

    <0.001

    0.002

    GH3535 base metal

    Bal.

    6.96

    16.3

    3.88

    0.33

    0.061

    0.08

    0.52

    0.001

    0.003

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