Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions
The advantages of microwave technology over conventionally conducted experiments are numerous. Some of them are reduction in reaction time, a higher degree of process control, repeatability, and work safety. Microwave synthesis routes require a complete description of the experimental details, instr...
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MDPI AG
2021-04-01
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| Series: | Crystals |
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| Online Access: | https://www.mdpi.com/2073-4352/11/4/383 |
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| author | Ivana Mitar Lucija Guć Željka Soldin Martina Vrankić Andrea Paut Ante Prkić Stjepko Krehula |
| author_facet | Ivana Mitar Lucija Guć Željka Soldin Martina Vrankić Andrea Paut Ante Prkić Stjepko Krehula |
| author_sort | Ivana Mitar |
| collection | DOAJ |
| description | The advantages of microwave technology over conventionally conducted experiments are numerous. Some of them are reduction in reaction time, a higher degree of process control, repeatability, and work safety. Microwave synthesis routes require a complete description of the experimental details, instrumentation, and design program of a microwave oven used in the experiments. In this work, microwave-assisted hydrothermal synthesis of hematite (α-Fe<sub>2</sub>O<sub>3</sub>) particles from 0.1 M FeCl<sub>3</sub> solution in highly alkaline media with heating in a microwave oven at continuous microwave emission of 800 W at 150 °C, 200 °C, and 250 °C for 20 min are presented. Also, the influence of the percentage of the addition of a cationic surfactant, cetyltrimethylammonium bromide (CTAB) on the composition, size, and shape of the final product was investigated. The samples precipitated at 150 °C formed a final product consisting of goethite (α-FeOOH) and hematite particles in contrast to the those precipitated at 200 °C and 250 °C where pure hematite phase was obtained. In these synthesis routes, the CTAB caused to slow down the rate of the goethite-to-hematite transformation process at temperatures at 200 °C but did not affect the transformation at 250 °C. |
| first_indexed | 2024-03-10T12:34:21Z |
| format | Article |
| id | doaj.art-f5f8de1235544e21831cd10314e3a15e |
| institution | Directory Open Access Journal |
| issn | 2073-4352 |
| language | English |
| last_indexed | 2024-03-10T12:34:21Z |
| publishDate | 2021-04-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Crystals |
| spelling | doaj.art-f5f8de1235544e21831cd10314e3a15e2023-11-21T14:24:03ZengMDPI AGCrystals2073-43522021-04-0111438310.3390/cryst11040383Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific ConditionsIvana Mitar0Lucija Guć1Željka Soldin2Martina Vrankić3Andrea Paut4Ante Prkić5Stjepko Krehula6Faculty of Science, University of Split, Ruđera Boškovića 33, 21000 Split, CroatiaUniversity of Split, Ruđera Boškovića 31, 21000 Split, CroatiaDepartment of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, 10000 Zagreb, CroatiaDivision of Materials Physics and Center of Excellence for Advanced Materials and Sensing Devices, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb, CroatiaFaculty of Chemistry and Technology, University of Split, Ruđera Boškovića 35, 21000 Split, CroatiaFaculty of Chemistry and Technology, University of Split, Ruđera Boškovića 35, 21000 Split, CroatiaDivision of Materials Chemistry, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb, CroatiaThe advantages of microwave technology over conventionally conducted experiments are numerous. Some of them are reduction in reaction time, a higher degree of process control, repeatability, and work safety. Microwave synthesis routes require a complete description of the experimental details, instrumentation, and design program of a microwave oven used in the experiments. In this work, microwave-assisted hydrothermal synthesis of hematite (α-Fe<sub>2</sub>O<sub>3</sub>) particles from 0.1 M FeCl<sub>3</sub> solution in highly alkaline media with heating in a microwave oven at continuous microwave emission of 800 W at 150 °C, 200 °C, and 250 °C for 20 min are presented. Also, the influence of the percentage of the addition of a cationic surfactant, cetyltrimethylammonium bromide (CTAB) on the composition, size, and shape of the final product was investigated. The samples precipitated at 150 °C formed a final product consisting of goethite (α-FeOOH) and hematite particles in contrast to the those precipitated at 200 °C and 250 °C where pure hematite phase was obtained. In these synthesis routes, the CTAB caused to slow down the rate of the goethite-to-hematite transformation process at temperatures at 200 °C but did not affect the transformation at 250 °C.https://www.mdpi.com/2073-4352/11/4/383microwave-assisted synthesishematiteα-Fe<sub>2</sub>O<sub>3</sub> particlesgoethiteα-FeOOH particlescetyltrimethylammonium bromide |
| spellingShingle | Ivana Mitar Lucija Guć Željka Soldin Martina Vrankić Andrea Paut Ante Prkić Stjepko Krehula Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions Crystals microwave-assisted synthesis hematite α-Fe<sub>2</sub>O<sub>3</sub> particles goethite α-FeOOH particles cetyltrimethylammonium bromide |
| title | Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions |
| title_full | Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions |
| title_fullStr | Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions |
| title_full_unstemmed | Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions |
| title_short | Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions |
| title_sort | rapid microwave method for synthesis of iron oxide particles under specific conditions |
| topic | microwave-assisted synthesis hematite α-Fe<sub>2</sub>O<sub>3</sub> particles goethite α-FeOOH particles cetyltrimethylammonium bromide |
| url | https://www.mdpi.com/2073-4352/11/4/383 |
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