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Research Article | Open Access

Laboratory-based X-ray diffractometer with fast time resolution for operando battery studies

Zhenzhong Li1,2, Chao Wang1, Fanqiang Meng3, Zhou Zhou4, Lei Li2, Chunzhen Yang1(), Dongbai Sun5()
School of Materials, Sun Yat-Sen University, Shenzhen 518107, China
Institute of Advanced Science Facilities, Shenzhen 518107, China
Sino-French Institute of Nuclear Engineering and Technology, Sun Yat-Sen University, Zhuhai 519082, China
School of Physics, Sun Yat-Sen University, Guangzhou 510275, China
School of Materials Science and Engineering, Sun Yat-Sen University, Guangzhou 510275, China
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Abstract

Operando X-ray diffraction (XRD) is an important characterization tool for real-time monitoring of structural changes in materials under different reaction conditions. In this study, we developed a laboratory-based diffractometer that could capture a full XRD spectrum within 10 s. The instrument has several advanced features. First, it uses a Ga–In alloy metal-jet X-ray source, thereby achieving high X-ray flux with a brightness of up to 3.0 × 1010 photons/(s·mm2·mrad2). Second, it employs an ellipsoidal mirror with a multilayer coating to produce quasi-parallel monochromatic light characterized by a divergence of 0.6 mrad and an energy resolution of 5.9 × 10−3. Third, it is equipped with a high-efficiency, high-signal-to-noise-ratio Pilatus 3R 1M detector for collecting diffraction signals. These features make the developed instrument applicable in studying rapid phase transitions in lithium-ion batteries, especially under extremely fast charge–discharge conditions. The data quality was comparable to that of synchrotron radiation XRD.

Keywords

X-ray diffractometermetal-jet X-ray sourceextreme fast-charging batterystructure evolutiondevice assembly

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Energy Materials and Devices
Volume 3 Issue 1,
March 2025
Article number: 9370057
DOI: 10.26599/EMD.2025.9370057
Cite this article:
Li Z, Wang C, Meng F, et al. Laboratory-based X-ray diffractometer with fast time resolution for operando battery studies. Energy Materials and Devices, 2025, 3(1): 9370057. https://doi.org/10.26599/EMD.2025.9370057
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Main technical parameters of Pilatus 3R 1M[9]

Technical specification
Sensor materialSi
Pixel size (W × H)172 µm × 172 µm
Energy range5–36 keV
Pixel array format (W × H)981 pixels × 1043 pixels
Image bit depth32 bit
Maximum count rate1 × 107 photons/s per pixel
Maximum frame rate5 Hz

Parameter comparison

ParametersEnergy (keV)Energy bandwidth (eV)Photon flux (photons/s)
IASF-XRD9.2555 (Ga Kα1 + Kα2)7 × 108
KIT-XRD[27]17.45150 (Mo Kα1 + Kα2)1 × 108
TAU-XRD[28]8.0540 (Cu Kα1 + Kα2)5 × 107
SSRF (BL16B1)4–202 eV@10 keV (Si (111))3 × 1011@10 keV