Browsing by Author "Kang, Huixiao"

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    Characterization of dynamic morphological changes of tin anode electrode during (de)lithiation processes using in operando synchrotron transmission X-ray microscopy
    (Elsevier, 2019) Li, Tianyi; Zhou, Xinwei; Cui, Yi; Lim, Cheolwoong; Kang, Huixiao; Yan, Bo; Wang, Jiajun; Wang, Jun; Fu, Yongzhu; Zhu, Likun; Mechanical and Energy Engineering, School of Engineering and Technology
    The morphological evolution of tin particles with different sizes during the first lithiation and delithiation processes has been visualized by an in operando synchrotron transmission X-ray microscope (TXM). The in operando lithium ion battery cell was operated at constant current condition during TXM imaging. Two-dimensional projection images with 40 nm resolution showing morphological evolution were obtained and analyzed. The analysis of relative area change shows that the morphology of tin particles with different sizes changed simultaneously. This phenomenon is mainly due to a negative feedback mechanism among tin particles in the battery electrode at a constant current operating condition. For irregular-shaped tin particles, the contour analysis shows that the regions with higher curvature started volume expansion first, and then the entire particle expanded almost homogeneously. This study provides insights for understanding the dynamic morphological change and the particle-particle interactions in high capacity lithium ion battery electrodes.
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    Geometric and Electrochemical Characteristics of LiNi1/3Mn1/3Co1/3O2 Electrode with Different Calendering Conditions
    (Elsevier, 2017-04) Kang, Huixiao; Lim, Cheolwoong; Li, Tianyi; Fu, Yongzhu; Yan, Bo; Houston, Nicole; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun; Department of Mechanical Engineering, School of Engineering and Technology
    The impact of calendering process on the geometric characteristics and electrochemical performance of LiNi1/3Mn1/3Co1/3O2 (NMC) electrode was investigated in this study. The geometric properties of NMC electrodes with different calendering conditions, such as porosity, pore size distribution, particle size distribution, specific surface area and tortuosity were calculated from the computed tomography data of the electrodes. A synchrotron transmission X-ray microscopy tomography system at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain the tomography data. The geometric and electrochemical analysis show that calendering can increase the electrochemically active area, which improves rate capability. However, more calendering will result in crushing of NMC particles, which can reduce the electrode capacity at relatively high C rates. This study shows that the optimum electrochemical performance of NMC electrode at 94:3:3 weight ratio of NMC:binder:carbon black can be achieved by calendering to 3.0 g/cm3 NMC density.
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    Geometric and electrochemical characteristics of lithium ion batteries
    (2017-05) Kang, Huixiao; Zhu, Likun
    The geometric and electrochemical characteristics of different lithium ion batteries (LIBs) are investigated in this study. The core work is to study the impact of the calendering process on NMC cathode electrodes performance. X-ray CT image processing by Python, MATLAB, ImageJ and Avizo is utilized in this study. NMC electrodes with different calendering conditions were fabricated to calculate electrochemical properties of the cells. Charge/discharge of the electrodes under 0.1C, 0.2C, 0.4C, 1C, 2C, 4C and 0.1C (retention test) rates were cycled for three times respectively between 4.2 V and 3.0 V. Electrochemical impedance spectroscopy testing was used to further explain the effects of NMC density on rate capability. Geometric properties of NMC electrodes with different calendering conditions were calculated from the computed tomography data of the electrodes. A synchrotron transmission X-ray microscopy tomography system at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain the tomography data. X-ray CT image processing before the data analysis was introduced. Python based Tomopy and ASTRA toolbox were used to filter the original HDF5 data and reconstruction. ImageJ was used to help remove noise, adjust contrast and cropping. Iso2mesh and image processing tool box were used in MATLAB to generate meshed 3D structure of CT data. Geometric properties of NMC electrodes including porosity, pore size distribution, particle size distribution, specific surface area and tortuosity were calculated from the computed tomography data of the electrodes. The geometric and electrochemical analysis show that calendering can increase the electrochemically active area, which lead to improving of the rate capability. However, more calendering will result in crushing of NMC particles, which can reduce the electrode capacity at relatively high C rates. This study shows that the optimum electrochemical performance of NMC electrode at 94:3:3 weight ratio of NMC:binder:carbon black can be achieved by calendering to 3.0 g/cm3 NMC density. LTAP solid electrolyte and NMC cathode material mix electrode-electrolyte X-ray CT data was studied in last chapter. By using 8 kev X-ray energy, we could distinguish NMC active material, LTAP solid electrolyte and the others three phase. On the basis of NMC electrode image processing method, dilation and multiply threshold method is applied to get three-phase 3D geometry. A comparing of connection area between NMC and LTAP of 700psi and 1300psi electrode was analyzed. Geometric properties like tortuosity, di_usion length and e_ective di_usivity were generated from the CT data.
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    Geometric and Electrochemical Characteristics of NMC Electrodes with Different Calendering Conditions
    (Office of the Vice Chancellor for Research, 2016-04-08) Kang, Huixiao; Lim, Cheolwoong; Fu, Yongzhu; Zhu, Likun
    The energy and power capabilities of Li ion batteries (LIBs) have been considered critical factors to determine the commercial values of the LIB powered applications. Many efforts have been done to improve the energy density and rate capability of LIBs. In addition to intrinsic material properties of anode and cathode active materials, the structure of electrode at micro and nano scales also plays a critical role in determining the energy density and rate capability of a LIB [1-3]. Calendering is a process in battery manufacturing to lower the porosity of the electrode and increase electrical contact. Increased calendering can increase the packing density of active materials in LIB electrodes, thereby increasing the volumetric energy density. The specific energy density is also increased by calendering via decreasing the percentage of inactive materials, such as current collector and separator. However, higher fraction of active materials in LIB electrodes can change electrodes’ structural properties significantly, such as porosity, specific surface area, pore size distribution and tortuosity [4]. To this end, there are few reports on the geometric characteristics and their impact on the electrochemical performance of LIB electrodes with different calendering conditions due to the inhomogeneity, complexity, and three-dimensional (3D) nature of the electrode’s microstructure [5-6]. Recently, porous electrode microstructures have been reconstructed by advanced tomography techniques such as X-ray nano-computed tomography (nano-CT) and focused ion beam scanning electron microscope (FIB-SEM)[7-8]. The reconstructed microstructures have been employed to investigate the geometric characteristics and spatial inhomogeneity of porous electrodes. In this study, we investigated real 3D Li[Ni1/3Mn1/3Co1/3]O2 (NMC) electrode microstructures under different calendering conditions and the effect of calendering on the performance of LIBs[4]. To investigate geometric characteristics of porous microstructures, cathode electrodes were fabricated from a 94:3:3 (weight %) mixture of NMC, PVDF, and super-P carbon black. To change the calendering condition, initial thickness of the electrodes was set 50μm, 80um, 90um, 100um. Then all electrodes were pressed down to 50 μm by using a rolling press machine. A synchrotron X-ray nano-CT at the Advanced Photon Source of Argonne National Lab was employed to obtain morphological data of the electrodes, with voxel size of 58.2 × 58.2 × 58.2 nm3. The morphology data sets were quantitatively analyzed to characterize their geometric properties. The geometric analysis showed that high packing density can result in smaller pore size and more uniform pore size distribution. The specific surface area and tortuosity of different electrodes will be reported. The charge/discharge experiments were also conducted for these electrodes. The geometric properties and cell testing results will be analyzed and reported.
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    Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries
    (IUCR, 2017) Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun; Mechanical Engineering, School of Engineering and Technology
    The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment for in situ monitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon–binder matrix by the accumulated X-ray dose is the key factor of radiation damage. For in situ TXM tomography, intermittent X-ray exposure during image capturing can be used to avoid the morphology change caused by radiation damage on the carbon–binder matrix.
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    In Situ and Operando Investigation of the Dynamic Morphological and Phase Changes of Selenium-doped Germanium Electrode during (De)Lithiation Processes
    (RSC, 2020-01) Li, Tianyi; Lim, Cheolwoong; Cui, Yi; Zhou, Xinwei; Kang, Huixiao; Yan, Bo; Meyerson, Melissa L.; Weeks, Jason A.; Liu, Qi; Guo, Fangmin; Kou, Ronghui; Liu, Yuzi; De Andrade, Vincent; De Carlo, Francesco; Ren, Yang; Sun, Cheng-Jun; Mullins, C. Buddie; Chen, Lei; Fu, Yongzhu; Zhu, Likun; Mechanical and Energy Engineering, School of Engineering and Technology
    To understand the effect of selenium doping on the good cycling performance and rate capability of a Ge0.9Se0.1 electrode, the dynamic morphological and phase changes of the Ge0.9Se0.1 electrode were investigated by synchrotron-based operando transmission X-ray microscopy (TXM) imaging, X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The TXM results show that the Ge0.9Se0.1 particle retains its original shape after a large volume change induced by (de)lithiation and undergoes a more sudden morphological and optical density change than pure Ge. The difference between Ge0.9Se0.1 and Ge is attributed to a super-ionically conductive Li–Se–Ge network formed inside Ge0.9Se0.1 particles, which contributes to fast Li-ion pathways into the particle and nano-structuring of Ge as well as buffering the volume change of Ge. The XRD and XAS results confirm the formation of a Li–Se–Ge network and reveal that the Li–Se–Ge phase forms during the early stages of lithiation and is an inactive phase. The Li–Se–Ge network also can suppress the formation of the crystalline Li15Ge4 phase. These in situ and operando results reveal the effect of the in situ formed, super-ionically conductive, and inactive network on the cycling performance of Li-ion batteries and shed light on the design of high capacity electrode materials.
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    Three-Dimensional Reconstruction and Analysis of All-Solid Li-Ion Battery Electrode Using Synchrotron Transmission X-ray Microscopy Tomography
    (ACS, 2018-05) Li, Tianyi; Kang, Huixiao; Zhou, Xinwei; Lim, Cheolwoong; Yan, Bo; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun; Mechanical Engineering, School of Engineering and Technology
    A synchrotron transmission X-ray microscopy tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source was employed to obtain three-dimensional morphological data of all-solid Li-ion battery electrodes. The three-phase electrode was fabricated from a 47:47:6 (wt %) mixture of Li(Ni1/3Mn1/3Co1/3)O2 as active material, Li1.3Ti1.7Al0.3(PO4)3 as Li-ion conductor, and Super-P carbon as electron conductor. The geometric analysis show that particle-based all-solid Li-ion battery has serious contact interface problem which significantly impact the Li-ion transport and intercalation reaction in the electrode, leading to low capacity, poor rate capability and cycle life.