article · Journal of Sol-Gel Science and Technology
Controlling crystallite size and phase purity in the sol-gel production of alumina ceramic nanoparticles is complicated because manufacturing variables are usually investigated individually. A multi-response statistical framework combining the Taguchi method with Grey Relational Analysis was applied to examine precursor choice, calcination temperature, and calcination duration simultaneously. Testing evaluated aluminium nitrate, aluminium sulphate, and aluminium chloride across temperatures between 800 and 1200 degrees Celsius and durations of 3 to 6 hours. Structural analysis revealed various alumina phases with crystallite sizes between 5.2 and 26.5 nanometres, while mass loss ranged from 4.90 to 6.53 per cent. Calcination temperature proved to be the most influential factor. The optimal combination of aluminium sulphate, a 1200-degree temperature, and a four-hour duration yielded predominantly alpha-alumina with an ultra-fine crystallite size of 5.3 nanometres, matching theoretical predictions and establishing a reproducible synthesis method.
Alumina nanoparticles are widely used, but making them consistently with very small crystallite sizes and high phase stability has remained difficult. By demonstrating how precursor chemistry and heating conditions interact, this statistical approach removes trial-and-error guesswork. It ensures manufacturers can reliably produce nanoscale alpha-alumina with controlled dimensions and superior thermal stability.
The abstract points to applications in catalysis, ceramic reinforcement, and protective coatings. Industrial material formulators and coating manufacturers could adopt the validated parameters to produce uniform alpha-alumina nanoparticles. Because the findings derive from laboratory-scale sol-gel synthesis and a small orthogonal test matrix, the technology is at an early experimental stage and requires pilot-scale testing before commercial deployment.
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Controlling crystallite size and phase purity remains a persistent challenge in the sol–gel synthesis of alumina (Al₂O₃) nanoparticles, as prior studies have largely examined process parameters in isolation rather than through integrated multi-response optimization. This study aimed to identify the combination of precursor material, calcination temperature, and calcination time that minimizes both crystallite size and thermogravimetric mass loss in sol–gel-derived alumina synthesis. Nine samples were prepared using aluminum nitrate, aluminum sulfate, and aluminum chloride precursors via the Taguchi L9(3³) orthogonal array. Calcination was performed at 800–1200 °C for 3–6 h. Samples were characterized by X-ray diffraction (XRD) and thermogravimetric analysis (TGA). Grey Relational Analysis (GRA), along with the Taguchi signal-to-noise ratio, was used to simultaneously optimize both responses. XRD identified different alumina phases (α, θ, δ, and γ) with crystallite sizes ranging from 5.2 to 26.5 nm, while TGA mass loss ranged from 4.90% to 6.53%. ANOVA of the S/N ratios ranked calcination temperature as the dominant factor. The optimal combination of aluminum sulfate, 1200 °C, and 4 h was validated by a confirmation experiment that reproduced predominantly α-Al₂O₃ with a crystallite size of 5.3 nm against a predicted 5.2 nm. This work establishes an integrated Taguchi–GRA framework that jointly optimizes crystallite size and thermal stability for sol–gel alumina synthesis and provides a reproducible, statistically grounded route for producing nanocrystalline α-alumina for catalytic, ceramic-reinforcement, and protective-coating applications. Graphical Abstract
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DOI: 10.1007/s10971-026-07236-7
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