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Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters
Magnetite nanocrystal clusters are being investigated for their potential applications in catalysis, magnetic separation, and drug delivery. Controlling their size and size distribution is of paramount importance and often requires tedious trial-and-error experimentation to determine the optimal con...
Autores principales: | , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
MDPI
2021
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7912753/ https://www.ncbi.nlm.nih.gov/pubmed/33535568 http://dx.doi.org/10.3390/nano11020360 |
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author | Medinger, Joelle Nedyalkova, Miroslava Lattuada, Marco |
author_facet | Medinger, Joelle Nedyalkova, Miroslava Lattuada, Marco |
author_sort | Medinger, Joelle |
collection | PubMed |
description | Magnetite nanocrystal clusters are being investigated for their potential applications in catalysis, magnetic separation, and drug delivery. Controlling their size and size distribution is of paramount importance and often requires tedious trial-and-error experimentation to determine the optimal conditions necessary to synthesize clusters with the desired properties. In this work, magnetite nanocrystal clusters were prepared via a one-pot solvothermal reaction, starting from an available protocol. In order to optimize the experimental factors controlling their synthesis, response surface methodology (RSM) was used. The size of nanocrystal clusters can be varied by changing the amount of stabilizer (tribasic sodium citrate) and the solvent ratio (diethylene glycol/ethylene glycol). Tuning the experimental conditions during the optimization process is often limited to changing one factor at a time, while the experimental design allows for variation of the factors’ levels simultaneously. The efficiency of the design to achieve maximum refinement for the independent variables (stabilizer amount, diethylene glycol/ethylene glycol (DEG/EG) ratio) towards the best conditions for spherical magnetite nanocrystal clusters with desirable size (measured by scanning electron microscopy and dynamic light scattering) and narrow size distribution as responses were proven and tested. The optimization procedure based on the RSM was then used in reverse mode to determine the factors from the knowledge of the response to predict the optimal synthesis conditions required to obtain a good size and size distribution. The RSM model was validated using a plethora of statistical methods. The design can facilitate the optimization procedure by overcoming the trial-and-error process with a systematic model-guided approach. |
format | Online Article Text |
id | pubmed-7912753 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2021 |
publisher | MDPI |
record_format | MEDLINE/PubMed |
spelling | pubmed-79127532021-02-28 Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters Medinger, Joelle Nedyalkova, Miroslava Lattuada, Marco Nanomaterials (Basel) Article Magnetite nanocrystal clusters are being investigated for their potential applications in catalysis, magnetic separation, and drug delivery. Controlling their size and size distribution is of paramount importance and often requires tedious trial-and-error experimentation to determine the optimal conditions necessary to synthesize clusters with the desired properties. In this work, magnetite nanocrystal clusters were prepared via a one-pot solvothermal reaction, starting from an available protocol. In order to optimize the experimental factors controlling their synthesis, response surface methodology (RSM) was used. The size of nanocrystal clusters can be varied by changing the amount of stabilizer (tribasic sodium citrate) and the solvent ratio (diethylene glycol/ethylene glycol). Tuning the experimental conditions during the optimization process is often limited to changing one factor at a time, while the experimental design allows for variation of the factors’ levels simultaneously. The efficiency of the design to achieve maximum refinement for the independent variables (stabilizer amount, diethylene glycol/ethylene glycol (DEG/EG) ratio) towards the best conditions for spherical magnetite nanocrystal clusters with desirable size (measured by scanning electron microscopy and dynamic light scattering) and narrow size distribution as responses were proven and tested. The optimization procedure based on the RSM was then used in reverse mode to determine the factors from the knowledge of the response to predict the optimal synthesis conditions required to obtain a good size and size distribution. The RSM model was validated using a plethora of statistical methods. The design can facilitate the optimization procedure by overcoming the trial-and-error process with a systematic model-guided approach. MDPI 2021-02-01 /pmc/articles/PMC7912753/ /pubmed/33535568 http://dx.doi.org/10.3390/nano11020360 Text en © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Article Medinger, Joelle Nedyalkova, Miroslava Lattuada, Marco Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title | Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title_full | Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title_fullStr | Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title_full_unstemmed | Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title_short | Solvothermal Synthesis Combined with Design of Experiments—Optimization Approach for Magnetite Nanocrystal Clusters |
title_sort | solvothermal synthesis combined with design of experiments—optimization approach for magnetite nanocrystal clusters |
topic | Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7912753/ https://www.ncbi.nlm.nih.gov/pubmed/33535568 http://dx.doi.org/10.3390/nano11020360 |
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