Mechanical Properties of Mullite Investigated by Nanoindentation

Authors

  • Jovana Ružić Vinča" Institute of Nuclear Sciences - National Institute of thе Republic of Serbia, University of Belgrade: Belgrade, RS https://orcid.org/0000-0002-8076-0012
  • Jelena Maletaškić Department of Materials, “Vinča” Institute of Nuclear Sciences – National Institute of the Republic of Serbia, University of Belgrade, PO Box 522, 11001 Belgrade, Serbia https://orcid.org/0000-0002-3889-8499
  • Željko Radovanović Innovation Center of the Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, Belgrade, Serbia https://orcid.org/0000-0002-0602-3831
  • Svetlana Ilić Department of Materials, “Vinča” Institute of Nuclear Sciences – National Institute of the Republic of Serbia, University of Belgrade, PO Box 522, 11001 Belgrade, Serbia https://orcid.org/0000-0003-0459-1381

DOI:

https://doi.org/10.30544/MMD29

Abstract

The mechanical behavior of sintered mullite material was studied using nanoindentation tests. Mullite compact was obtained by cold pressing sol-gel synthesized mullite precursor powder and sintering at 1550 °C. Analysis of the microstructural parameters and phase composition was done by XRD (X-ray diffraction) and SEM-EDS (scanning electron microscopy with energy dispersive X-ray spectrometry). A Berkovich indenter was employed for nanoindentation measurements at various loads (1000-9000 µN). After each test, in situ SPM (scanning probe microscopy) imaging was performed. The XRD pattern of sintered mullite displayed peaks of mullite (93.3%) and corundum (6.7%). Results revealed average values of hardness and elastic modulus of sintered mullite as 15.55 GPa and 174.37 GPa, respectively. Moreover, nanoindentation results indicated that mullite follows the Hall-Petch hardening relation due to the presence of grains with a size range of 0.2-2 µm. Indentation in areas with smaller grains exhibits higher hardness values. Post-test SPM images disclosed the presence of pile-ups around the indents, which were formed under loads higher than 3000 µN.

Keywords:

mullite, mechanical properties, nanoindentation
Supporting Agencies
This work was funded by the Ministry of Education, Science and Technological Development of the Republic of Serbia, Contract No. 451-03-66/2024-03/200017, and 451-03-66/2024-03/200287.

References

Aksay, Ilhan A., Daniel M. Dabbs, and Mehmet Sarikaya. "Mullite for structural, electronic, and optical applications." Journal of the American Ceramic Society 74, no. 10 (1991): 2343-2358. https://doi.org/10.1111/j.1151-2916.1991.tb06768.x.

Biswal, Bijaylaxmi, D.K. Mishra, Satyaprakash Narayan Das, and Satyanarayan Bhuyan. "Structural, micro-structural, optical and dielectric behavior of mullite ceramics." Ceramics International 47, no. 22 (2021): 32252-32263. https://doi.org/10.1016/j.ceramint.2021.08.120.

Botero, C.A., E. Jimenez-Piqué, T. Kulkarni, G. Fargas, V.K. Sarin, and L. Llanes. "Cross-sectional nanoindentation and nanoscratch of compositionally graded mullite films." Surface and Coatings Technology 206, no. 7 (2011): 1927-1931. https://doi.org/10.1016/j.surfcoat.2011.07.032.

Botero, C.A., E. Jimenez-Piqué, J. Seuba, T. Kulkarni, V.K. Sarin, and L. Llanes. "Mechanical behavior of 3Al2O3·2SiO2 films under nanoindentation." Acta Materialia 60, no. 16 (2012): 5889-5899. https://doi.org/10.1016/j.actamat.2012.07.031.

Ebadzadeh, T. "Formation of mullite from precursor powders: Sintering, microstructure and mechanical properties." Materials Science and Engineering: A 355, no. 1-2 (2003): 56-61. https://doi.org/10.1016/S0921-5093(03)00049-2.

Ghahremani, D., T. Ebadzadeh, and A. Maghsodipour. "Spark plasma sintering of mullite: Relation between microstructure, properties and spark plasma sintering (SPS) parameters." Ceramics International 41, no. 5 (2015): 6409-6416. https://doi.org/10.1016/j.ceramint.2015.01.078.

Ilić, S., S. Zec, M. Miljković, D. Poleti, M. Pošarac-Marković, Dj. Janaćković, and B. Matović. "Sol–gel synthesis and characterization of iron doped mullite." Journal of Alloys and Compounds 612 (2014): 259-264. https://doi.org/10.1016/j.jallcom.2014.05.204.

Ilić, Svetlana, Valentin N. Ivanovski, Željko Radovanović, Adela Egelja, Maja Kokunešoski, Aleksandra Šaponjić, and Branko Matović. "Structural, microstructural and mechanical properties of sintered iron-doped mullite." Materials Science and Engineering: B 256 (2020): 114543. https://doi.org/10.1016/j.mseb.2020.114543.

Karimzadeh, A., S. S. R. Koloor, M. R. Ayatollahi, A. R. Bushroa, and M. Y. Yahya. "Assessment of nano-indentation method in mechanical characterization of heterogeneous nanocomposite materials using experimental and computational approaches." Scientific Reports 9, no. 1 (2019): 15763. https://doi.org/10.1038/s41598-019-51904-4.

Krenzel, Thomas F., Jürgen Schreuer, Derek Laubner, Michel Cichocki, and Hartmut Schneider. "Thermo-mechanical properties of mullite ceramics: New data." Journal of the American Ceramic Society 102, no. 1 (2019): 416-426. https://doi.org/10.1111/jace.15925.

Li, Yaqiang, Yue Li, and Rui Wang. "Quantitative evaluation of elastic modulus of concrete with nanoidentation and homogenization method." Construction and Building Materials 212 (2019): 295-303. https://doi.org/10.1016/j.conbuildmat.2019.04.002.

Liu, Dazhao, Kaixuan Gui, Jianzhou Long, Yu Zhao, Wenbo Han, and Gang Wang. "Low-temperature densification and mechanical properties of monolithic mullite ceramic." Ceramics International 46, no. 8 (2020): 12329-12334. https://doi.org/10.1016/j.ceramint.2020.01.282.

Luo, Zhiyu, Wengui Li, Kejin Wang, and Surendra P. Shah. "Research progress in advanced nanomechanical characterization of cement-based materials." Cement and Concrete Composites 94 (2018): 277-295. https://doi.org/10.1016/j.cemconcomp.2018.09.016.

Nath, Shekhar, A. Dey, A.K. Mukhopadhyay, and Bikramjit Basu. "Nanoindentation response of novel hydroxyapatite–mullite composites." Materials Science and Engineering: A 513-514 (2009): 197-201. https://doi.org/10.1016/j.msea.2009.02.052.

Oliver, W. C., and G. M. Pharr. "An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments." Journal of Materials Research 7, no. 6 (1992): 1564-1583. https://doi.org/10.1557/JMR.1992.1564.

PDXL Version 2.0.3.0 Integrated X-ray Powder Diffraction Software. Tokyo, Japan: Rigaku Corporation, 2011.

Rajaei, Hosein, Iman Mobasherpour, Mohammad Farvizi, and Mohammad Zakeri. "Effect of mullite synthesis methods on the spark plasma sintering behaviour and mechanical properties." Micro & Nano Letters 11, no. 8 (2016): 465-468. https://doi.org/10.1049/mnl.2016.0092.

Ren, Lin, Zhengyi Fu, Yucheng Wang, Fan Zhang, Jinyong Zhang, Weimin Wang, and Hao Wang. "Fabrication of transparent mullite ceramic by spark plasma sintering from powders synthesized via sol–gel process combined with pulse current heating." Materials & Design 83 (2015): 753-759. https://doi.org/10.1016/j.matdes.2015.06.046.

Ruzic, Jovana, Ikumu Watanabe, Kenta Goto, and Takahito Ohmura. "Nano-indentation measurement for heat resistant alloys at elevated temperatures in inert atmosphere." Materials Transactions 60, no. 8 (2019): 1411-1415. https://doi.org/10.2320/matertrans.MD201909.

Schneider, Hartmut, Reinhard X. Fischer, and Jürgen Schreuer. "Mullite: Crystal structure and related properties." Edited by D. J. Green. Journal of the American Ceramic Society 98, no. 10 (2015): 2948-2967. https://doi.org/10.1111/jace.13817

Downloads

Published

15-07-2024

Issue

Vol. 2 No. 2 (2024): Ceramic Materials for Advanced Application

Section

Ceramic Materials for Advanced Application

License

Copyright (c) 2024 Jovana Ružić, Jelena Maletaškić, Željko Radovanović, Svetlana Ilić

Creative Commons License

This work is licensed under a Creative Commons Attribution 4.0 International License.