Aluminum oxide (oxide Al?O?), or alumina, is one of the most critical and widely used ceramic oxides in high-temperature mechanical applications. This is due to its reliable mechanical properties, thermal stability, and chemical resistance. Alumina has various polymorphs and transition sequences from the metastable polytypes of ?, ?, ?, and ? to the stable ?-phase can lead to a defining step in application performance. Recent developments (2020-2025) in alumina powder synthesis, thermal characterization and bonding have been organized in this review with emphasis on the use of Thermogravimetric Analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR). The first technique addressed an understanding of powder thermal processing incorporating dehydration, decomposition, phase stability with TGA. The second technique addressed an understanding of Al–O bonding vibrations in the forms of structural and hydroxyl group vibrational modes with FTIR to develop a dimensional understanding of bonding transformations during calcination. These analyses have been integrated to provide an understanding of how different powder synthesis routes (sol–gel, hydrothermal, combustion and additive manufacturing) affect thermal transport, microstructural evolution and the associated mechanical behaviour of alumina powders. Other factors influencing densification and reliability of the ceramic including dopants, sintering atmosphere and conditions are summarized.The review discusses the challenges of spectral overlaps, ephemeral identification, and scaling to commercial production, and connects them to future opportunities in multi-technique in situ analysis, computational modeling, and sustainable processing approaches to optimize alumina powders for next-generation aerospace, energy, and refractory applications.
Introduction
Aluminum oxide (Al?O?), or alumina, is a crucial ceramic material known for its chemical inertness, corrosion resistance, and high melting point, making it ideal for high-temperature mechanical applications such as aerospace, automotive, electronics, and energy sectors. Alumina exists in multiple polymorphic forms (γ, δ, θ, κ, and α), with the α phase being thermodynamically stable at high temperatures. Understanding and controlling the phase transformations and chemical bonding are key to optimizing its thermomechanical performance.
Characterization Techniques:
Thermogravimetric Analysis (TGA) tracks weight changes during heating, revealing thermal stability, dehydration, decomposition, and phase transitions.
Fourier Transform Infrared Spectroscopy (FTIR) monitors changes in chemical bonding, such as Al–O lattice vibrations and surface hydroxyl groups, during thermal treatment.
Combined TGA-FTIR offers detailed insights into the structure-property relationships, beneficial for advanced ceramic development.
Synthesis and Microstructure:
Alumina powders’ microstructure and phase purity are influenced by synthesis methods, including wet-chemical (sol-gel, hydrothermal) and dry industrial processes.
Polymorphic transformations from metastable forms to α-alumina around 1100–1300 °C affect densification and mechanical properties.
Doping with elements like Fe?O? or TiO? can stabilize phases and alter transformation kinetics.
Mechanical Properties:
Alumina nanocomposites demonstrate high flexural strength (up to 500 MPa), hardness (>20 GPa), and fracture toughness (3–5 MPa·m^1/2).
These materials also show superior wear and fatigue resistance.
Research Gaps:
Lack of standardized protocols for coupled TGA-FTIR experiments, causing inconsistent results.
Limited quantitative analysis of volatile species and intermediates during phase transitions, especially in composites.
Insufficient atomic-scale understanding of dopant effects on phase stability and transformation kinetics.
Low industrial adoption of integrated multi-technique approaches due to cost and complexity.
Need for computational integration, including machine learning, to predict and optimize alumina powder synthesis and properties.
Addressing these gaps will enhance the design and application of alumina ceramics for demanding high-temperature environments.
Conclusion
The purpose of this review is to detail the thermal stability and bonding evolution of aluminum oxide (Al?O?) powders, with a particular focus on TGA (thermogravimetric analysis) and FTIR (Fourier transform infrared spectroscopic) characterization. The polymorphism of alumina and therefore the transition from metastable to stable alumina is very important when considering the suitability of alumina in high-temperature mechanical applications. By reviewing over fifty published studies, this review suggests the synthesis route, calcination conditions, and addition of dopants are important to the thermal transport, densification, and mechanical reliability of alumina. TGA provides useful quantification of dehydration, degradation, and thermal phenomena, while FTIR can be used to gain additional information via the understanding of Al–O lattice vibrations and bond transitions. Collectively, both characterization techniques provide a powerful approach to exploring structure–property relationships that are relevant for industrial applications.
References
[1] F. Yang, Y. Jiang, R. Jiang, H. Liu, Y. Zhang, and X. Sun, “Microstructure, mechanical properties and thermal stability of Al2O3/Al2O3 ceramic matrix composites obtained from submicron-sized powers,” Ceram Int, vol. 50, no. 6, pp. 9710–9720, Mar. 2024, doi: 10.1016/J.CERAMINT.2023.12.289.
[2] D. H. A. Besisa, E. M. M. Ewais, and H. H. Mohamed, “Thermal performance and mechanical durability of Al2O3/CuO ceramics as solar receiver materials for solar thermal applications,” Ceram Int, vol. 48, no. 16, pp. 23609–23617, Aug. 2022, doi: 10.1016/J.CERAMINT.2022.05.009.
[3] B. M. Shi et al., “(B4C+Al2O3)/Al composites with excellent high temperature strength and thermal stability prepared by sintering in air atmosphere,” Ceram Int, vol. 50, no. 19, pp. 36166–36173, Oct. 2024, doi: 10.1016/J.CERAMINT.2024.07.001.
[4] S. Ibrahim, A. M. Fayad, A. A. El-Kheshen, Y. M. Hamdy, M. M. Ibrahim, and M. A. Marzouk, “Characterization and optimization of amorphous alumina-doped silica thin layer material of low emissivity coating technology for energy-saving applications,” Energy Build, vol. 341, p. 115836, Aug. 2025, doi: 10.1016/J.ENBUILD.2025.115836.
[5] M. Mashkovtsevet al., “Spectroscopic Study of Five-Coordinated Thermal Treated Alumina Formation: FTIR and NMR Applying,” Int J Mol Sci, vol. 24, no. 6, p. 5151, Mar. 2023, doi: 10.3390/IJMS24065151/S1.
[6] H. Wang, H. Zheng, M. Hu, Z. Ma, and H. Liu, “Synergistic effect of Al2O3-decorated reduced graphene oxide on microstructure and mechanical properties of 6061 aluminium alloy,” Sci Rep, vol. 14, no. 1, pp. 1–14, Dec. 2024, doi: 10.1038/S4159802467004X;SUBJMETA=1023,1026,166,301,639,988;KWRD=MECHANICAL+ENGINEERING,METALS+AND+ALLOYS,STRUCTURAL+MATERIALS.
[7] H. Attil, A. AKSAS, M. Sebais, and O. Halimi, “Synthesis and Characterization of Alumina Powders Obtained at Various Temperatures Via Sol-Gel Method,” Metallurgical and Materials Engineering, vol. 30, no. 3, pp. 67–79, Nov. 2024, doi: 10.63278/1071.
[8] M. Balamurugan, “CHARACTERIZATION OF ALUMINA (Nano and Bulk Particles) Master of Science in Chemistry”, Accessed: Sep. 06, 2025. [Online]. Available: www.sathyabama.ac.in
[9] Y. N. Zan et al., “Enhancing High-Temperature Strength and Thermal Stability of Al2O3/Al Composites by High-Temperature Pre-treatment of Ultrafine Al Powders,” ???????, vol. 33, no. 7, pp. 913–921, Jul. 2020, doi: 10.1007/S40195-020-01038-8.
[10] S. Said, S. Mikhail, and M. Riad, “Recent processes for the production of alumina nano-particles,” Mater Sci Energy Technol, vol. 3, pp. 344–363, Jan. 2020, doi: 10.1016/J.MSET.2020.02.001.
[11] Y. S. Tay, E. J. R. Phua, Z. Chen, and C. L. Gan, “Simultaneous Enhancement of Polymerization Kinetics and Properties of Phthalonitrile Using Alumina Fillers,” ACS Omega, vol. 7, no. 37, pp. 32996–33003, Sep. 2022, doi: 10.1021/ACSOMEGA.2C02667/ASSET/IMAGES/LARGE/AO2C02667_0007.JPEG.
[12] V. S. D. C, “Study on Mechanical, Wear and Thermal Properties of AL2O3/Graphite Reinforced AA2024 Aluminum Alloy Based Metal Matrix Composites,” Int J Res Appl Sci Eng Technol, vol. 10, no. 12, pp. 1390–1403, Dec. 2022, doi: 10.22214/IJRASET.2022.48218.
[13] F. van S. Eric N. Coker, Sandia National Laboratories, and N. M. Albuquerque, “https://www.osti.gov/servlets/purl/1140853.” Accessed: Sep. 10, 2025. [Online]. Available: https://www.osti.gov/servlets/purl/1140853#page=1.00&gsr=0
[14] A. Bachmaier and R. Pippan, “Effect of oxide particles on the stabilization and final microstructure in aluminium,” Materials Science & Engineering, vol. 528, no. 25–26, p. 7589, 2011, doi: 10.1016/J.MSEA.2011.06.071.
[15] M. E. Mahmoud, M. A. Khalifa, R. M. El-Sharkawy, and M. R. Youssef, “Effects of Al2O3 and BaO nano-additives on mechanical characteristics of high-density polyethylene,” Mater Chem Phys, vol. 262, p. 124251, Apr. 2021, doi: 10.1016/J.MATCHEMPHYS.2021.124251.
[16] H. K. A. El-Hamid, A. A. Gaber, R. E. A. Ngida, H. E. H. Sadek, R. M. Khattab, and H. S. Mandour, “Study of microstructure and corrosion behavior of nano-Al2O3 coating layers on TiO2 substrate via polymeric method and microwave combustion,” Sci Rep, vol. 14, no. 1, p. 18417, Dec. 2024, doi: 10.1038/S41598-024-68566-6.
[17] G. Kadirgamaet al., “Characterization and machine learning analysis of hybrid alumina-copper oxide nanoparticles in therminol 55 for medium temperature heat transfer fluid,” Sci Rep, vol. 15, no. 1, pp. 1–24, Dec. 2025, doi: 10.1038/S41598-025-92461-3;SUBJMETA=166,301,639;KWRD=ENGINEERING,MATERIALS+SCIENCE.
[18] G. Gullifa, L. Barone, E. Papa, S. Materazzi, and R. Risoluti, “On-Line Thermally Induced Evolved Gas Analysis: An Update-Part 2: EGA-FTIR,” Molecules, vol. 27, no. 24, Dec. 2022, doi: 10.3390/MOLECULES27248926.
[19] S. P. Goutam, S. K. Avinashi, M. Yadav, D. Roy, and R. Shastri, “Green Synthesis and Characterization of Aluminium Oxide Nanoparticles Using Leaf Extract of Rosa,” Adv Sci Eng Med, vol. 10, no. 7, pp. 719–722, Oct. 2018, doi: 10.1166/ASEM.2018.2236.
[20] S. Sachin et al., “Synthesis of Aluminum Oxide (Al2O3) Nanoparticles Decorated With Polymeric Carbon (Al2O3/AC) Nanocomposites for High Specific Capacitance Value,” Polym Adv Technol, vol. 35, no. 10, p. e6604, Oct. 2024, doi: 10.1002/PAT.6604.
[21] Y. Sun et al., “Recent Advancements in Alumina-Based High-Temperature Insulating Materials: Properties, Applications, and Future Perspectives,” High-Temperature Materials 2025, Vol. 2, Page 10001, vol. 2, no. 1, p. 10001, Jan. 2025, doi: 10.70322/HTM.2025.10001.
[22] A. H. K. Shargh et al., “Enhanced mechanical and optical properties of alumina ceramics via simultaneous magnesium, lanthanum, and zirconium oxide addition in spark plasma sintering,” Sci Rep, vol. 15, no. 1, pp. 1–15, Dec. 2025, doi: 10.1038/S41598-025-06197-1;SUBJMETA.
[23] C. Qian, K. Hu, Z. Shen, Q. Wang, P. Li, and Z. Lu, “Effect of sintering aids on mechanical properties and microstructure of alumina ceramic via stereolithography,” Ceram Int, vol. 49, no. 11, pp. 17506–17523, Jun. 2023,doi: 10.1016/J.CERAMINT.2023.02.118.
[24] C. Rahmawati, S. Aprilia, T. Saidi, T. B. Aulia, and A. E. Hadi, “The Effects of Nanosilica on Mechanical Properties and Fracture Toughness of Geopolymer Cement,” Polymers (Basel), vol. 13, no. 13, p. 2178, Jul. 2021, doi: 10.3390/POLYM13132178.
[25] M. N. Nduni, A. M. Osano, and B. Chaka, “Synthesis and characterization of aluminium oxide nanoparticles from waste aluminium foil and potential application in aluminium-ion cell,” Clean Eng Technol, vol. 3, Jul. 2021, doi: 10.1016/J.CLET.2021.100108.
[26] J. Zygmuntowiczet al., “The Structural and Mechanical Properties of Al2O3–Ni Composites Obtained by Magnetic Field-Assisted Centrifugal Slip Casting,” Materials, vol. 17, no. 16, p. 3902, Aug. 2024, doi: 10.3390/MA17163902.
[27] M. L. Rahman, M. S. Islam, M. F. Ahmed, B. Biswas, N. Sharmin, and A. J. M. T. Neger, “Extraction and characterization of highly pure alumina (?, ?, and ?) polymorphs from waste beverage cans: A viable waste management approach,” Arabian Journal of Chemistry, vol. 16, no. 2, p. 104518, Feb. 2023, doi: 10.1016/J.ARABJC.2022.104518.
[28] J. Zygmuntowicz, P. Wieci?ska, M. Wachowski, M. Kurek, and W. Kaszuwara, “Thermogravimetric analysis coupled with mass spectrometry of ceramic–metal ternary composites Al2O3-Cu-Mo,” Measurement, vol. 217, p. 113049, Aug. 2023, doi: 10.1016/J.MEASUREMENT.2023.113049.
[29] Y. Bian, T. Gao, Y. Zhao, G. Liu, and X. Liu, “Synthesis of an Al-Based Composite Reinforced by Multi-Phase ZrB2, Al3BC and Al2O3 with Good Mechanical and Thermal Properties at Elevated Temperature,” Materials, vol. 13, no. 18, p. 4048, Sep. 2020, doi: 10.3390/MA13184048.
[30] Y. Sun et al., “Recent Advancements in Alumina-Based High-Temperature Insulating Materials: Properties, Applications, and Future Perspectives,” sciepublish.com, Accessed: Jun. 17, 2025. [Online]. Available: https://www.sciepublish.com/article/pii/394