TITLE:
Microwave-Assisted Transition Metal Nanostructure Synthesis: Power-Law Signature Verification
AUTHORS:
Victor J. Law, Denis P. Dowling
KEYWORDS:
Microwave-Assisted Synthesis, Pd, Ag, Pt, Au, ZnO, Power-Law, Residual Error, Statistical Analysis, Parametric Cluster Analysis
JOURNAL NAME:
American Journal of Analytical Chemistry,
Vol.14 No.8,
August
30,
2023
ABSTRACT: A power-law (y = cxn) signature between process energy budget (kJ) and process energy density (kJ·ml-1) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml-1. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml-1. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml-1 at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.