International Journal of Mineral Processing and Extractive Metallurgy

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Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview

Received: 05 March 2020    Accepted: 19 March 2020    Published: 31 March 2020
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Abstract

Solid-state reaction is one of some methods to synthesize LiFePO4 powder. However, the post-synthesis crystal structure was found to be imperfect, probably caused by the imperfection of the phospho-olivine structure. This study aimed to investigate the cause of its imperfection. A LiFePO4 powder synthesized via solid-state reaction path was used as a case study sample for this study. XRD characterization was done to investigate it. Orthorhombic crystal structure was found to be a perfect fit for this sample using precise lattice parameter analysis, as shown by the linear regression equation result. Further analysis was performed using Rietveld refinement method to pinpoint the actual coordinates of Li, Fe, P, and O atoms. The result shows that solid-state reaction can produce an order of orthorhombic crystal structure which constructed by ordered Li atoms arrangement. On the other hands, there is a disordered phospho-olivine structure due to the imperfection of the occupation of Fe, P, and O atoms. These disorders were found through analysis of anomalous peaks on the Rietveld refinement result when compared with PDF database. Loss of (200) plane was caused by imperfect occupation of O atoms, while imperfect occupation of Fe and P atoms leads to new (200) plane of FeP4 phase which has a monoclinic crystal structure.

DOI 10.11648/j.ijmpem.20200501.11
Published in International Journal of Mineral Processing and Extractive Metallurgy (Volume 5, Issue 1, March 2020)
Page(s) 1-6
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This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2024. Published by Science Publishing Group

Keywords

LiFePO4, Imperfection, Synthesis, Solid-state, Calcination, XRD

References
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Author Information
  • Research Centre for Metallurgy and Materials, Indonesian Institute of Sciences (LIPI), South Tangerang, Indonesia

  • Research Centre for Physics, Indonesian Institute of Sciences (LIPI), South Tangerang, Indonesia

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    Ibrahim Purawiardi, Christin Rina Ratri. (2020). Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview. International Journal of Mineral Processing and Extractive Metallurgy, 5(1), 1-6. https://doi.org/10.11648/j.ijmpem.20200501.11

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    Ibrahim Purawiardi; Christin Rina Ratri. Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview. Int. J. Miner. Process. Extr. Metall. 2020, 5(1), 1-6. doi: 10.11648/j.ijmpem.20200501.11

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    Ibrahim Purawiardi, Christin Rina Ratri. Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview. Int J Miner Process Extr Metall. 2020;5(1):1-6. doi: 10.11648/j.ijmpem.20200501.11

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  • @article{10.11648/j.ijmpem.20200501.11,
      author = {Ibrahim Purawiardi and Christin Rina Ratri},
      title = {Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview},
      journal = {International Journal of Mineral Processing and Extractive Metallurgy},
      volume = {5},
      number = {1},
      pages = {1-6},
      doi = {10.11648/j.ijmpem.20200501.11},
      url = {https://doi.org/10.11648/j.ijmpem.20200501.11},
      eprint = {https://download.sciencepg.com/pdf/10.11648.j.ijmpem.20200501.11},
      abstract = {Solid-state reaction is one of some methods to synthesize LiFePO4 powder. However, the post-synthesis crystal structure was found to be imperfect, probably caused by the imperfection of the phospho-olivine structure. This study aimed to investigate the cause of its imperfection. A LiFePO4 powder synthesized via solid-state reaction path was used as a case study sample for this study. XRD characterization was done to investigate it. Orthorhombic crystal structure was found to be a perfect fit for this sample using precise lattice parameter analysis, as shown by the linear regression equation result. Further analysis was performed using Rietveld refinement method to pinpoint the actual coordinates of Li, Fe, P, and O atoms. The result shows that solid-state reaction can produce an order of orthorhombic crystal structure which constructed by ordered Li atoms arrangement. On the other hands, there is a disordered phospho-olivine structure due to the imperfection of the occupation of Fe, P, and O atoms. These disorders were found through analysis of anomalous peaks on the Rietveld refinement result when compared with PDF database. Loss of (200) plane was caused by imperfect occupation of O atoms, while imperfect occupation of Fe and P atoms leads to new (200) plane of FeP4 phase which has a monoclinic crystal structure.},
     year = {2020}
    }
    

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  • TY  - JOUR
    T1  - Crystal Structure Imperfection of LiFePO4 Synthesized Through Solid-state Reaction: An XRD Overview
    AU  - Ibrahim Purawiardi
    AU  - Christin Rina Ratri
    Y1  - 2020/03/31
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    N1  - https://doi.org/10.11648/j.ijmpem.20200501.11
    DO  - 10.11648/j.ijmpem.20200501.11
    T2  - International Journal of Mineral Processing and Extractive Metallurgy
    JF  - International Journal of Mineral Processing and Extractive Metallurgy
    JO  - International Journal of Mineral Processing and Extractive Metallurgy
    SP  - 1
    EP  - 6
    PB  - Science Publishing Group
    SN  - 2575-1859
    UR  - https://doi.org/10.11648/j.ijmpem.20200501.11
    AB  - Solid-state reaction is one of some methods to synthesize LiFePO4 powder. However, the post-synthesis crystal structure was found to be imperfect, probably caused by the imperfection of the phospho-olivine structure. This study aimed to investigate the cause of its imperfection. A LiFePO4 powder synthesized via solid-state reaction path was used as a case study sample for this study. XRD characterization was done to investigate it. Orthorhombic crystal structure was found to be a perfect fit for this sample using precise lattice parameter analysis, as shown by the linear regression equation result. Further analysis was performed using Rietveld refinement method to pinpoint the actual coordinates of Li, Fe, P, and O atoms. The result shows that solid-state reaction can produce an order of orthorhombic crystal structure which constructed by ordered Li atoms arrangement. On the other hands, there is a disordered phospho-olivine structure due to the imperfection of the occupation of Fe, P, and O atoms. These disorders were found through analysis of anomalous peaks on the Rietveld refinement result when compared with PDF database. Loss of (200) plane was caused by imperfect occupation of O atoms, while imperfect occupation of Fe and P atoms leads to new (200) plane of FeP4 phase which has a monoclinic crystal structure.
    VL  - 5
    IS  - 1
    ER  - 

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