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Optimization of a carbon dioxide - assisted nanoparticle deposition process using sequential experimental design with adaptive design space / Michael J. Casciato in Industrial & engineering chemistry research, Vol. 51 N° 11 (Mars 2012) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 51 N° 11 (Mars 2012) . - pp. 4363–4370 Titre : Optimization of a carbon dioxide - assisted nanoparticle deposition process using sequential experimental design with adaptive design space Type de document : texte imprimé Auteurs : Michael J. Casciato, Auteur ; Sungil Kim, Auteur ; J. C. Lu, Auteur Année de publication : 2012 Article en page(s) : pp. 4363–4370 Note générale : Chimie industrielle Langues : Anglais (eng) Mots-clés : Optimization  Carbon  Dioxide Résumé : A sequential design of experiments methodology with an adaptive design space is proposed and implemented to optimize a nanofabrication technique that possesses significant uncertainty in terms of design region and model structure along with an engineering tolerance requirement. This method is termed Layers of Experiment (LoE) with Adaptive Combined Design (ACD) and is developed specifically for advanced technology processes where there is little or no foreknowledge of the design region and/or model structure from either mechanistic understanding or empirical studies. This technique was applied to optimize an elevated pressure, elevated temperature carbon dioxide (epet-CO2) nanoparticle deposition process where silver nanoparticles were deposited directly from an organometallic precursor in the fluid phase onto a silicon wafer surface. A target mean nanoparticle size of 40 nm was chosen, with surface enhanced Raman spectroscopy (SERS) as the motivating application. Using the LoE/ACD method, it was possible to find the process optimum for the epet-CO2 process and build a reliable model using only 12 experiments conducted in two sequential layers. With temperature as the design variable, the first layer of experiments was conducted in the region [60 °C, 150 °C], while the second layer was conducted in the region [98 °C, 128 °C], indicating that the LoE/ACD algorithm reduced the size of the design region by 60 °C while building a reliable model for statistical inference. In the first layer, a purely space-filling design was used since the model structure was unknown; in the second layer, the ACD approach yielded a design weighted between space-filling and D-optimal, favoring the D-optimal design. The optimized temperature for fabricating 40 nm diameter silver nanoparticles in this system was 117 °C. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie2028574#cor1 [article] Optimization of a carbon dioxide - assisted nanoparticle deposition process using sequential experimental design with adaptive design space [texte imprimé] / Michael J. Casciato, Auteur ; Sungil Kim, Auteur ; J. C. Lu, Auteur . - 2012 . - pp. 4363–4370. Chimie industrielle Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 51 N° 11 (Mars 2012) . - pp. 4363–4370 Mots-clés : Optimization  Carbon  Dioxide Résumé : A sequential design of experiments methodology with an adaptive design space is proposed and implemented to optimize a nanofabrication technique that possesses significant uncertainty in terms of design region and model structure along with an engineering tolerance requirement. This method is termed Layers of Experiment (LoE) with Adaptive Combined Design (ACD) and is developed specifically for advanced technology processes where there is little or no foreknowledge of the design region and/or model structure from either mechanistic understanding or empirical studies. This technique was applied to optimize an elevated pressure, elevated temperature carbon dioxide (epet-CO2) nanoparticle deposition process where silver nanoparticles were deposited directly from an organometallic precursor in the fluid phase onto a silicon wafer surface. A target mean nanoparticle size of 40 nm was chosen, with surface enhanced Raman spectroscopy (SERS) as the motivating application. Using the LoE/ACD method, it was possible to find the process optimum for the epet-CO2 process and build a reliable model using only 12 experiments conducted in two sequential layers. With temperature as the design variable, the first layer of experiments was conducted in the region [60 °C, 150 °C], while the second layer was conducted in the region [98 °C, 128 °C], indicating that the LoE/ACD algorithm reduced the size of the design region by 60 °C while building a reliable model for statistical inference. In the first layer, a purely space-filling design was used since the model structure was unknown; in the second layer, the ACD approach yielded a design weighted between space-filling and D-optimal, favoring the D-optimal design. The optimized temperature for fabricating 40 nm diameter silver nanoparticles in this system was 117 °C. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie2028574#cor1

Synthesis of optically active ZnS – carbon nanotube nanocomposites in supercritical carbon dioxide via a single source diethyldithiocarbamate precursor / Michael J. Casciato in Industrial & engineering chemistry research, Vol. 51 N° 36 (Septembre 2012) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 51 N° 36 (Septembre 2012) . - pp. 11710-11716 Titre : Synthesis of optically active ZnS – carbon nanotube nanocomposites in supercritical carbon dioxide via a single source diethyldithiocarbamate precursor Type de document : texte imprimé Auteurs : Michael J. Casciato, Auteur ; Galit Levitin, Auteur ; Dennis W. Hess, Auteur Année de publication : 2012 Article en page(s) : pp. 11710-11716 Note générale : Industrial chemistry Langues : Anglais (eng) Mots-clés : Precursor  Supercritical  state  Carbon  dioxide  Nanocomposite Résumé : Zinc sulfide nanoparticles (ZnS NPs) have been deposited on carbon nanotubes (CNTs) from a single source precursor, zinc(II) bis(diethyldithiocarbamate), using a one-step batch supercritical carbon dioxide (sc-CO2) process. By eliminating the need for an additional sulfur source while simultaneously employing CO2 as the solvent, this method replaces environmentally unfriendly chemicals commonly used in ZnS―CNT nanocomposite synthesis such as ethylene glycol, thiourea, and hydrogen sulfide. ZnS NP morphology displayed large clusters (209 ± 24 nm) that were comprised of smaller particles (16.9 ± 1.9 nm). Photoluminescence spectroscopy demonstrated broad band fluorescence of the ZnS―CNT nanocomposite at 440 nm (2.82 eV) and fluorescence of a Mn doped ZnS-CNT nanocomposite at 445 nm (2.79 eV) and 602 nm (2.07 eV), also in agreement with previous studies. The ZnS―CNT nanocomposite was compared to ZnS NPs synthesized in the absence of a substrate; results indicated that the ZnS―CNT nanocomposite was formed by a heterogeneous reaction mechanism in the sc-CO2 system. ISSN : 0888-5885 En ligne : http://cat.inist.fr/?aModele=afficheN&cpsidt=26350339 [article] Synthesis of optically active ZnS – carbon nanotube nanocomposites in supercritical carbon dioxide via a single source diethyldithiocarbamate precursor [texte imprimé] / Michael J. Casciato, Auteur ; Galit Levitin, Auteur ; Dennis W. Hess, Auteur . - 2012 . - pp. 11710-11716. Industrial chemistry Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 51 N° 36 (Septembre 2012) . - pp. 11710-11716 Mots-clés : Precursor  Supercritical  state  Carbon  dioxide  Nanocomposite Résumé : Zinc sulfide nanoparticles (ZnS NPs) have been deposited on carbon nanotubes (CNTs) from a single source precursor, zinc(II) bis(diethyldithiocarbamate), using a one-step batch supercritical carbon dioxide (sc-CO2) process. By eliminating the need for an additional sulfur source while simultaneously employing CO2 as the solvent, this method replaces environmentally unfriendly chemicals commonly used in ZnS―CNT nanocomposite synthesis such as ethylene glycol, thiourea, and hydrogen sulfide. ZnS NP morphology displayed large clusters (209 ± 24 nm) that were comprised of smaller particles (16.9 ± 1.9 nm). Photoluminescence spectroscopy demonstrated broad band fluorescence of the ZnS―CNT nanocomposite at 440 nm (2.82 eV) and fluorescence of a Mn doped ZnS-CNT nanocomposite at 445 nm (2.79 eV) and 602 nm (2.07 eV), also in agreement with previous studies. The ZnS―CNT nanocomposite was compared to ZnS NPs synthesized in the absence of a substrate; results indicated that the ZnS―CNT nanocomposite was formed by a heterogeneous reaction mechanism in the sc-CO2 system. ISSN : 0888-5885 En ligne : http://cat.inist.fr/?aModele=afficheN&cpsidt=26350339