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Synthesis of ultra-fine and controllable size distribution nanocrystalline MgAl2O4 powders and ascertainment of aluminum loss by introducing inert atmosphere pre-calcination during combustion

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Abstract

Nanocrystalline magnesium aluminate spinel (MgAl2O4) powders were synthesized in this study by employing a modified nitrate–citrate combustion route, in which the heat treatment was continuously performed by two separate processes. One process was in nitrogen during the carbonization of the precursors, and the other was subsequently in air. This can greatly decrease the heat release during the combustion process. X-ray diffraction and high-resolution transmission electron microscopy, differential scanning calorimetry, thermogravimetry, infrared spectroscopy, and inductively coupled plasma atomic emission spectrometer were utilized to reveal the reaction process and characterize the physical properties of precursors and powders. To achieve well-crystallized spinel powders with smallest possible and controllable crystallite sizes, the effect of carbonization in nitrogen on the calcined spinel powders was investigated in detail. The introduction of the inert atmosphere at the pre-calcination stage, with appropriate temperature and holding time, allowed ultra-fine, well-crystallized and size-controllable MgAl2O4 powders with average crystallite sizes of 5–25 nm to be obtained. Despite the benefit from the pre-calcination in nitrogen, it was found that the stoichiometry of precursors can be compromised due to the loss of aluminum during the heat treatment in N2 as the temperature was too high (>900 °C) with sufficient holding time. The mechanism of the carbothermal reduction was investigated in this study.

Graphical Abstract

By introducing inert atmosphere pre-calcination combustion, ultra-fine well-crystallized and crystalline size-controllable MgAl2O4 spinel powders were thus obtained.

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Acknowledgments

This work was supported by the National Natural Science Foundation of the People’s Republic of China under Grant Nos. 11145006 and 91326103, the ITER Program (No. 2014GB125002), the Major Science and Technology Programs of China, the Foundation of Key Laboratory of Neutron Physics, CAEP, the National High Technology Research and Development Program (863), the Science and Technology Innovation Team of Sichuan Province under Grant No. 15CXTD0025, and the Foundation of Science and Technology Bureau of Shantou, Guangdong Province.

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Authors and Affiliations

  1. College of Physical Science and Technology, Sichuan University, Chengdu, 610064, Sichuan, People’s Republic of China

    Lei Hu, Xiumin Xie, Jianqi Qi, Qiwu Shi, Yida Zhou, Maureen Willis, Nian Wei & Tiecheng Lu

  2. Key Laboratory of Radiation Physics and Technology of Ministry of Education, Sichuan University, Chengdu, 610064, Sichuan, People’s Republic of China

    Xiumin Xie, Jianqi Qi & Nian Wei

  3. Key Laboratory of High Energy Density Physics of Ministry of Education, Sichuan University, Chengdu, 610064, Sichuan, People’s Republic of China

    Maureen Willis & Tiecheng Lu

  4. School of Physical Electronics, University of Electronic Science and Technology of China, Chengdu, 610054, Sichuan, People’s Republic of China

    Wei Liu

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  1. Lei Hu
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Correspondence to Jianqi Qi or Tiecheng Lu.

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Hu, L., Xie, X., Qi, J. et al. Synthesis of ultra-fine and controllable size distribution nanocrystalline MgAl2O4 powders and ascertainment of aluminum loss by introducing inert atmosphere pre-calcination during combustion. J Sol-Gel Sci Technol 75, 336–344 (2015). https://doi.org/10.1007/s10971-015-3704-6

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  • DOI: https://doi.org/10.1007/s10971-015-3704-6

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