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.
References
[1]
Gedye, R.N., Smith, F. and Westaway, K.C. (1988) The Rapid Synthesis of Organic Compounds in Microwave Ovens. Canadian Journal Chemistry, 66, 17-26. https://doi.org/10.1139/v88-003
[2]
Gedye, R.N., Rank, W. and Westaway, K.C. (1991) The Rapid Synthesis of Organic Compounds in Microwave Ovens. II. Canadian Journal Chemistry, 69, 706-711. https://doi.org/10.1139/v91-106
[3]
Rinaldi, L., Carnaroglio, D., Rotolo, L. and Cravotto, G. (2015) A Microwave-Based Chemical Factory in the Lab: From Milligram to Multigram Preparations. Journal of Chemistry, 2015, Article ID: 879531. https://doi.org/10.1155/2015/879531
[4]
Grewal, A.S., Kumar, K., Redhu, S. and Bhardwaj, S. (2013) Microwave Assisted Synthesis: A Green Synthesis Chemistry Approach. International Research Journal of Pharmaceutical and Applied Sciences, 3, 278-285.
[5]
Priecel, P. and Lopez-Sanchez, J.A. (2018) Advantages and Limitations of Microwave Reactors: From Chemical Synthesis to the Catalytic Valorization of Biobased Chemicals. ACS Sustainable Chemistry and Engineering, 7, 3-21. https://doi.org/10.1021/acssuschemeng.8b03286
[6]
Law, V.J. and Dowling, D.P. (2022) Microwave-Assisted Inactivation of Fomite-Microorganism Systems: Energy Phase-Space Projection. American Journal Analytical Chemistry, 13, 255-276. https://doi.org/10.4236/ajac.2022.137018
[7]
Law, V.J. and Dowling, D.P. (2023) Revisiting “Non-Thermal” Batch Microwave oven Inactivation of Microorganisms. American Journal of Analytical Chemistry, 14, 28-54. https://doi.org/10.4236/ajac.2023.141003
[8]
Law, V.J. and Dowling, D.P. (2023) Microwave-Assisted Au and Ag Nanoparticle Synthesis: An Energy Phase-Space Projection Analysis. American Journal Analytical Chemistry, 14, 149-174. https://doi.org/10.4236/ajac.2023.144009
[9]
Hanel, R., Corominas-Murtra, B., Liu, B. and Thurner, S. (2017) Fitting Power-Laws in Empirical Data with Estimators That Work for All Exponents. PLOS ONE, 12, e0170920. https://doi.org/10.1371/journal.pone.0170920
[10]
Huxley, J.S. and Teissier, G. (1936) Terminology of Relative Growth. Nature, 137, 780-781. https://doi.org/10.1038/137780b0
[11]
Calder III, W.A. (1981) Scaling of Physiological Processes in Homeothermic Animals. Annual Review of Physiology, 43, 301-322. https://doi.org/10.1146/annurev.ph.43.030181.001505
[12]
Stumpf, M.P.H. and Porter, M.A. (2012) Critical Truths about Power Laws. Science, 355, 665-666. https://doi.org/10.1126/science.1216142
[13]
Dong, H., Li, M., Liu, R., Wu, C. and Wu, J. (2017) Allometric Scaling in Scientific Fields. Scientometrics, 112, 583-594. https://doi.org/10.1007/s11192-017-2333-y
[14]
Blosi, M., Al-bonetti, S., Gatti, F., Dondi, M., Migliori, A., Ortolani, L., Morandi, V. and Baldi, G. (2010) Au, Ag and Au-Ag Nanoparticles: Microwave-Assisted Synthesis in Water and Applications in Ceramic and Catalysis. Nanotech, 1, 352-355.
[15]
Rai, P., Majhi, S.M., Yu, Y.T. and Lee, J.H. (2015) Synthesis of Plasmonic Ag@SnO2 Core-Shell Nanoreactors for Xylene Detection. RSC Advances, 5, 17653-17659. https://doi.org/10.1039/C4RA13971B
[16]
Alfano, B., Polichetti, T., Mauriello, M., Miglietta, M.L., Ricciardella, F., Massera, E. and Francia, G.D. (2016) Modulating the Sensing Properties of Graphene through an Eco-Friendly Metal-Decoration Process. Sensors and Actuators B: Chemical, 222, 1032-1042. https://doi.org/10.1016/j.snb.2015.09.008
[17]
Miglietta, M.L., Alfano, B., Polichetti, T., Massera, E., Schiattarella, C. and Di Francia, G. (2018) Effective Tuning of Silver Decorated Graphene Sensing Properties by Adjusting the Ag NPs Coverage Density. In: Andò, B., Baldini, F., Di Natale, C., Marrazza, G. and Siciliano, P., Eds., CNS 2016: Sensors, Springer, Cham, 82-89.
[18]
Marinoiu, A., Andrei, R., Vagner, I., Niculescu, V., Bucra, F., Constantinescu, M. and Carcadea, E. (2020) One Step Synthesis of Au Nanoparticles Supported on Graphene Oxide Using an Eco-Friendly Microwave-Assisted Process. Materials Science, 26, 249-254. https://doi.org/10.5755/j01.ms.26.3.21857
[19]
Gonçalves, R.A., Toled, R.P., Joshi, N. and Berengue, O.M. (2021) Green Synthesis and Applications of ZnO and-TiO2 Nanostructures. Molecules, 26, Article 2236. https://doi.org/10.3390/molecules26082236
[20]
Pal, J., Deb, M.K., Deshmukh, D.K. and Sen, B.K. (2014) Microwave-Assisted Synthesis of Platinum Nanoparticles and Their Catalytic Degradation of Methyl Violet in Aqueous Solution. Applied Nanoscience, 4, 61-65. https://doi.org/10.1007/s13204-012-0170-0
[21]
Pal, J., Deb, M.K. and Deshmukh, D.K. (2014) Microwave-Assisted Synthesis of Silver Nanoparticles Using Benzo-18-Crown-6 as Reducing and Stabilizing Agent. Applied Nanoscience, 4, 507-510. https://doi.org/10.1007/s13204-013-0229-6
[22]
Harpeness, R. and Gedanken, A. (2004) Microwave Synthesis of Core-Shell Gold/ Palladium Bimetallic Nanoparticles. Langmuir, 20, 3431-3434. https://doi.org/10.1021/la035978z
[23]
Abdelsayed, V., Aljarash, A. and El-Shall, M.S. (2009) Microwave Synthesis of Bimetallic Nanoalloys and Co Oxidation on Ceria-Supported Nanoalloys. Chemistry of Materials, 21, 2825-2834. https://doi.org/10.1021/cm9004486
[24]
Siamaki, A.R., Khder, A.E.R.S., Abdelsayed, V., El-Shall, M.S. and Gupton, B.F. (2011) Microwave-Assisted Synthesis of Palladium Nanoparticles Supported on Graphene: A Highly Active and Recyclable Catalyst for Carbon-Carbon Cross-Coupling Reactions. Journal of Catalysis, 279, 1-11. https://doi.org/10.1016/j.jcat.2010.12.003
[25]
Rai, P., Kim, S.G. and Yu, Y.T. (2012) Microwave Assisted Synthesis of Flower-Like ZnO and Effect of Annealing Atmosphere on Its Photoluminescence Property. Journal of Mater Science: Mater Electron, 23, 344-348. https://doi.org/10.1007/s10854-011-0384-z
[26]
Prakash, T., Jayaprakash, R., Neri, G. and Kumar, S. (2013) Synthesis of ZnO Nanostructures by Microwave Irradiation Using Albumen as a Template. Journal of Nanoparticles, 2013, Article ID: 274894. https://doi.org/10.1155/2013/274894
[27]
Zhang, J. and Bai, X. (2017) Microwave-Assisted Synthesis of Pd Nanoparticles and Catalysis Application for Suzuki Coupling Reactions. The Open Materials Science Journal, 11, 1-8. https://doi.org/10.2174/1874088X01711010001
[28]
Gomez-Bolivar, J., Mikheenko, I.P., Macaskie, L.E. and Merroun, M.L. (2019) Characterization of Palladium Nanoparticles Produced by Healthy and Microwave Injured Cells of Desulfovibrio desulfuricans and Escherichia coli. Nanomaterials, 9, Article 857. https://doi.org/10.3390/nano9060857
[29]
Nishida, Y., Wada, Y., Chaudhari, C., Sato, K. and Nagaoka, K. (2019) Preparation of Noble-Metal Nanoparticles by Microwave-Assisted Chemical Reduction and Evaluation as Catalysts for Nitrile Hydrogenation under Ambient Conditions. Journal of the Japan Petroleum Institute, 62, 220-227. https://doi.org/10.1627/jpi.62.220
[30]
Yalcin, M. (2020) Microwave-Assisted Synthesis of ZnO Nanoflakes: Structural, Optical and Dielectric Characterization. Materials Research Express, 7, Article ID: 055019. https://doi.org/10.1088/2053-1591/ab940f
[31]
Jaimes-Paez, C.D., Vences-Alvarez, E., Salinas-Torres, D., Morallón, E., Rangel-Mendez, J.R. and Cazorla-Amorós, D. (2023) Microwave-Assisted Synthesis of Carbon-Supported Pt Nanoparticles for Their Use as Electrocatalysts in the Oxygen Reduction Reaction and Hydrogen Evolution Reaction. Electrochimica Acta, 464, Article ID: 142871. https://doi.org/10.1016/j.electacta.2023.142871
[32]
Andriani, P. and McKelvey, B. (2009) From Gaussian to Paretian Thinking: Causes and Implications of Power Laws in Organizations. Perspective Organization Science, 20, 1053-1071. https://doi.org/10.1287/orsc.1090.0481
[33]
Law, V.J., Tewordt, M., Ingram, S.G. and Jones, G.A.C. (1991) Alkane Based Plasma Etching of GaAs. Journal of Vacuum Science & Technology B, 9, 1449-1455. https://doi.org/10.1116/1.585449
[34]
Law, V.J., Ingram, S.G., Tewordt, M. and. Jones, G.A.C. (1991) Reactive Ion Etching of GaAs Using CH4: In He, Ne and Ar. Semiconductor Science and Technology, 6, 411-413. https://doi.org/10.1088/0268-1242/6/5/019
[35]
Kurilovich, D., et al. (2018) Power-Law Scaling of Plasma Pressure on LaserablAted Tin Microdroplets. Physics of Plasmas, 25, Article ID: 012709. https://doi.org/10.1063/1.5010899
[36]
Tynan, J., Law, V.J., Twomey, B., Hynes, A.M., Daniels, S., Byrne, G. and Dowling, D.P. (2009) Evaluation of Real-Time Non-Invasive Performance Analysis Tools for the Monitoring of Atmospheric Pressure Plasma. Measurement Science and Technology, 20, Article ID: 115703. https://doi.org/10.1088/0957-0233/20/11/115703
[37]
Law, V.J., Tynan, J., Byrne, G., Dowling, D.P. and Daniels, S. (2010) The Application of Multivariate Analysis Tools for Non-Invasive Performance Analysis of Atmospheric Pressure Plasma. In: Skiadas, C.H. and Dimotikalis, I., Eds., Chaotic Systems: Theory and Applications, World Scientific Publishing, Singapore, 147-154. https://doi.org/10.1142/9789814299725_0019
[38]
Chen, J., Wang, J., Zhang, X. and Jin, Y. (2008) Microwave-Assisted Green Synthesis of Silver Nanoparticles by Carboxymethyl Cellulose Sodium and Silver Nitrate. Materials Chemistry and Physics, 108, 421-424. https://doi.org/10.1016/j.matchemphys.2007.10.019
[39]
Elazab, H.A., Moussa, S., Gupton, B.F. and El-Shall, M.S. (2014) Microwave-Assisted Synthesis of Pd Nanoparticles Supported on Fe3O4, Co3O4, and Ni(OH)2 Nanoplates and Catalysis Application for CO Oxidation. Journal of Nanoparticle Research, 16, Article No. 2477. https://doi.org/10.1007/s11051-014-2477-0
[40]
Elazab, H.A., Sadek, M.A. and El-Idreesy, T.T. (2018) Microwave-Assisted Synthesis of Palladium Nanoparticles Supported on Copper Oxide in Aqueous Medium as an Efficient Catalyst for Suzuki Cross-Coupling Reaction. Adsorption Science & Technology, 36, 1362-1365. https://doi.org/10.1177/0263617418771777
[41]
Rademacher, L., Yen Beglau, T.H., Heinen, T., Barthel, J. and Janiak, C. (2020) Microwave-Assisted Synthesis of Iridium Oxide and Palladium Nanoparticles Supported on a Nitrogen-Rich Covalent Triazine Framework as Superior Electrocatalysts for the Hydrogen Evolution and Oxygen Reduction Reaction. Frontiers of Chemistry, 10, Article 94526. https://doi.org/10.3389/fchem.2022.945261
[42]
Bayazit, M.K., Yue, J., Cao, E., Gavriilidis, A. and Tang, J. (2016) Controllable Synthesis of Gold Nanoparticles in Aqueous Solution by Microwave Assisted Flow Chemistry. ACS Sustainable Chemistry & Engineering, 4, 6435-6442. https://doi.org/10.1021/acssuschemeng.6b01149
[43]
Li, D. and Komarneni, S. (2006) Synthesis of Pt Nanoparticles and Nanorods by Microwave-Assisted Solvothermal Technique. Zeitschrift fuer Naturforschung B, 61, 1566-1572. https://doi.org/10.1515/znb-2006-1214
[44]
Kundu, P., Nethravathi, C., Deshpande, P.A., Rajamathi, M., Madras, G. and Ravishankar, N. (2011) Ultrafast Microwave-Assisted Route to Surfactant-Free Ultrafine Pt Nanoparticles on Graphene: Synergistic Co-Reduction Mechanism and High Catalytic Activity. Chemistry of Materials, 23, 2772-2778. https://doi.org/10.1021/cm200329a
[45]
Wojnicki, M., Luty Błocho, M., Kwolek, P., Gajewska, M., Socha, R.P., Pędzich, Z., Csapó, E. and Hessel, V. (2021) The Influence of Dielectric Permittivity of Water on the Shape of PtNPs Synthesized in High Pressure High Temperature Microwave Reactor. Scientific Reports, 11, Article No. 4851. https://doi.org/10.1038/s41598-021-84388-2
[46]
Cao, J. and Wang, J. (2004) Microwave-Assisted Synthesis of Flower-Like ZnO Nanosheet Aggregates in a Room-Temperature Ionic Liquid. Chemistry Letters, 33, 1332-1333. https://doi.org/10.1246/cl.2004.1332
[47]
Li, H., Liu, E., Chan, F.Y.E., Lu, Z. and Chen, R. (2011) Fabrication of Ordered Flower-Like ZnO Nanostructures by a Microwave and Ultrasonic Combined Technique and Their Enhanced Photocatalytic Activity. Materials Letters, 65, 3440-3443. https://doi.org/10.1016/j.matlet.2011.07.049
[48]
Cao, Y., Liu, B., Huang, R., Xia, Z. and Ge, S. (2011) Flash Synthesis of Flower-Like ZnO Nanostructures by Microwave-Induced Combustion Process. Materials Letters, 65, 160-163. https://doi.org/10.1016/j.matlet.2010.09.072
[49]
Li, X., Wang, C., Zhou, X., Liu, J., Sun, P. and Lu, G. (2014) Gas Sensing Properties of Flower-Like ZnO Prepared by a Microwave-Assisted Technique. Royal Society of Chemistry Advances, 4, 47319-47324. https://doi.org/10.1039/C4RA07425D
[50]
Hasanpoor, M., Aliofkhazraei, M. and Delavari, H. (2015) Microwave-Assisted Synthesis of Zinc Oxide Nanoparticles. Procedia Materials Science, 11, 320-325. https://doi.org/10.1016/j.mspro.2015.11.101
[51]
Krishnapriya, R., Praneetha, S. and Murugan, A.V. (2016) Investigation of the Effect of Reaction Parameters on the Microwave-Assisted Hydrothermal Synthesis of Hierarchical Jasmine-Flower-Like ZnO Nanostructures for Dye-Sensitized Solar Cells. New Journal of Chemistry, 40, 5080-5089. https://doi.org/10.1039/C6NJ00457A
[52]
Wojnarowicz, J., Chudoba, T., Gierlotka, S., Sobczak, K. and Lojkowski, W. (2018) Size Control of Cobalt-Doped ZnO Nanoparticles Obtained in Microwave Solvothermal Synthesis. Crystals, 8, Article 179. https://doi.org/10.3390/cryst8040179
[53]
Wojnarowicz, J. (2023) Private Communication Regarding Operating Pressure of ERTEC Microwave Applicator.
[54]
Liu, H., Liu, H., Yang, J., Zhai, H., Liu, X. and Jia, H. (2019) Microwave-Assisted One-Pot Synthesis of Ag Decorated Flower-Like ZnO Composites Photocatalysts for Dye Degradation and NO Removal. Ceramics International, 45, 20133-20140. https://doi.org/10.1016/j.ceramint.2019.06.279
[55]
Aljaafari, A., Ahmed, F., Awada, C. and Shaalan, N.M. (2020) Flower-Like ZnO Nanorods Synthesized by Microwave-Assisted One-Pot Method for Detecting Reducing Gases: Structural Properties and Sensing Reversibility. Frontiers in Chemistry, 8, Article 456. https://doi.org/10.3389/fchem.2020.00456
[56]
Cai, Y. and Hung, J. (2023) Preparation and Photocatalysis Characteristics of Flower-Like ZnO by Microwave Method. Journal of Physics: Conference Series, 2437, Article ID: 012039. https://doi.org/10.1088/1742-6596/2437/1/012039
[57]
Hennig, C. (2003) Clusters, Outliers, and Regression: Fixed Point Clusters. Journal of Multivariate Analysis, 86, 183-212. https://doi.org/10.1016/S0047-259X(02)00020-9
[58]
Loureiro, A., Torgo, L. and Soares, C. (2004) Outlier Detection Using Clustering Methods: A Data Cleaning Application. Proceedings of KDNet Symposium on Knowledge-Based Systems for the Public Sector, Bonn, June 2004.
[59]
Lara, J.A., Lizcano, D., Rampérez, V. and Soriano, J. (2020) A Method for Outlier Detection Based on Cluster Analysis and Visual Expert Criteria. Expert Systems, 37, e12473. https://doi.org/10.1111/exsy.12473
