Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials

Core-shell Zinc Oxide/Layered Double Hydroxide (ZnO@LDH) composite nanomaterials have been produced by a one-step continuous hydrothermal synthesis process, in an attempt to further enhance the application potential of layered double hydroxide (LDH) nanomaterials. The synthesis involves two hydrothe...

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Main Authors: Ian Clark, Jacob Smith, Rachel L. Gomes, Edward Lester
Format: Article
Language:English
Published: MDPI AG 2020-10-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/10/10/2052
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author Ian Clark
Jacob Smith
Rachel L. Gomes
Edward Lester
author_facet Ian Clark
Jacob Smith
Rachel L. Gomes
Edward Lester
author_sort Ian Clark
collection DOAJ
description Core-shell Zinc Oxide/Layered Double Hydroxide (ZnO@LDH) composite nanomaterials have been produced by a one-step continuous hydrothermal synthesis process, in an attempt to further enhance the application potential of layered double hydroxide (LDH) nanomaterials. The synthesis involves two hydrothermal reactors in series with the first producing a ZnO core and the second producing the Mg<sub>2</sub>Al-CO<sub>3</sub> shell. Crystal domain length of single phase ZnO and composite ZnO was 25 nm and 42 nm, respectively. The ZnO@LDH composite had a specific surface area of 76 m<sup>2</sup> g<sup>−1</sup>, which was larger than ZnO or Mg<sub>2</sub>Al-CO<sub>3</sub> when produced separately (53 m<sup>2</sup> g<sup>−1</sup> and 58 m<sup>2</sup> g<sup>−1</sup>, respectively). The increased specific surface area is attributed to the structural arrangement of the Mg<sub>2</sub>Al-CO<sub>3</sub> in the composite. Platelets are envisaged to nucleate on the core and grow outwards, thus reducing the face–face stacking that occurs in conventional Mg<sub>2</sub>Al-CO<sub>3</sub> synthesis. The Mg/Al ratio in the single phase LDH was close to the theoretical ratio of 2, but the Mg/Al ratio in the composite was 1.27 due to the formation of Zn<sub>2</sub>Al-CO<sub>3</sub> LDH from residual Zn<sup>2+</sup> ions. NaOH concentration was also found to influence Mg/Al ratio, with lower NaOH resulting in a lower Mg/Al ratio. NaOH concentration also affected morphology and specific surface area, with reduced NaOH content in the second reaction stage causing a dramatic increase in specific surface area (> 250 m<sup>2</sup> g<sup>−1</sup>). The formation of a core-shell composite material was achieved through continuous synthesis; however, the final product was not entirely ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub>. The product contained a mixture of ZnO, Mg<sub>2</sub>Al-CO<sub>3</sub>, Zn<sub>2</sub>Al-CO<sub>3</sub>, and the composite material. Whilst further optimisation is required in order to remove other crystalline impurities from the synthesis, this research acts as a stepping stone towards the formation of composite materials via a one-step continuous synthesis.
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spelling doaj.art-d73cbb292198461dbdd041465dcc9b652023-11-20T17:26:19ZengMDPI AGNanomaterials2079-49912020-10-011010205210.3390/nano10102052Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite NanomaterialsIan Clark0Jacob Smith1Rachel L. Gomes2Edward Lester3Advanced Materials Research Group, Faculty of Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, UKAdvanced Materials Research Group, Faculty of Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, UKFood, Water, Waste Research Group, Faculty of Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, UKAdvanced Materials Research Group, Faculty of Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, UKCore-shell Zinc Oxide/Layered Double Hydroxide (ZnO@LDH) composite nanomaterials have been produced by a one-step continuous hydrothermal synthesis process, in an attempt to further enhance the application potential of layered double hydroxide (LDH) nanomaterials. The synthesis involves two hydrothermal reactors in series with the first producing a ZnO core and the second producing the Mg<sub>2</sub>Al-CO<sub>3</sub> shell. Crystal domain length of single phase ZnO and composite ZnO was 25 nm and 42 nm, respectively. The ZnO@LDH composite had a specific surface area of 76 m<sup>2</sup> g<sup>−1</sup>, which was larger than ZnO or Mg<sub>2</sub>Al-CO<sub>3</sub> when produced separately (53 m<sup>2</sup> g<sup>−1</sup> and 58 m<sup>2</sup> g<sup>−1</sup>, respectively). The increased specific surface area is attributed to the structural arrangement of the Mg<sub>2</sub>Al-CO<sub>3</sub> in the composite. Platelets are envisaged to nucleate on the core and grow outwards, thus reducing the face–face stacking that occurs in conventional Mg<sub>2</sub>Al-CO<sub>3</sub> synthesis. The Mg/Al ratio in the single phase LDH was close to the theoretical ratio of 2, but the Mg/Al ratio in the composite was 1.27 due to the formation of Zn<sub>2</sub>Al-CO<sub>3</sub> LDH from residual Zn<sup>2+</sup> ions. NaOH concentration was also found to influence Mg/Al ratio, with lower NaOH resulting in a lower Mg/Al ratio. NaOH concentration also affected morphology and specific surface area, with reduced NaOH content in the second reaction stage causing a dramatic increase in specific surface area (> 250 m<sup>2</sup> g<sup>−1</sup>). The formation of a core-shell composite material was achieved through continuous synthesis; however, the final product was not entirely ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub>. The product contained a mixture of ZnO, Mg<sub>2</sub>Al-CO<sub>3</sub>, Zn<sub>2</sub>Al-CO<sub>3</sub>, and the composite material. Whilst further optimisation is required in order to remove other crystalline impurities from the synthesis, this research acts as a stepping stone towards the formation of composite materials via a one-step continuous synthesis.https://www.mdpi.com/2079-4991/10/10/2052continuous hydrothermal synthesislayered double hydroxidecompositenano hybrid structuresUltraviolet (UV) properties
spellingShingle Ian Clark
Jacob Smith
Rachel L. Gomes
Edward Lester
Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
Nanomaterials
continuous hydrothermal synthesis
layered double hydroxide
composite
nano hybrid structures
Ultraviolet (UV) properties
title Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
title_full Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
title_fullStr Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
title_full_unstemmed Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
title_short Towards the Continuous Hydrothermal Synthesis of ZnO@Mg<sub>2</sub>Al-CO<sub>3</sub> Core-Shell Composite Nanomaterials
title_sort towards the continuous hydrothermal synthesis of zno mg sub 2 sub al co sub 3 sub core shell composite nanomaterials
topic continuous hydrothermal synthesis
layered double hydroxide
composite
nano hybrid structures
Ultraviolet (UV) properties
url https://www.mdpi.com/2079-4991/10/10/2052
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AT rachellgomes towardsthecontinuoushydrothermalsynthesisofznomgsub2subalcosub3subcoreshellcompositenanomaterials
AT edwardlester towardsthecontinuoushydrothermalsynthesisofznomgsub2subalcosub3subcoreshellcompositenanomaterials