Towards the Continuous Hydrothermal Synthesis of ZnO@Mg2Al-CO3 Core-Shell Composite Nanomaterials
Abstract
:1. Introduction
2. Materials and Methods
2.1. Reagents and Chemicals
2.2. Preparation of Composite Nanomaterials
2.3. Materials Characterisation
3. Results and Discussion
3.1. Crystal Characterisation of Composite and Single-Phase Materials
3.2. Specific Surface Area Analysis
3.3. Chemical Characterisation
3.4. Thermal Stability
3.5. Electronic Structure Characterisation
3.6. The Impact of Reactor 1 vs. Reactor 2
3.7. LDH Formation in Reactor 1 and in Reactor 2
3.8. The Impact of Residual Ions from ZnO Synthesis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
References
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Sample | Reactor | Material | [NaOH] (mol L−1) | Down-Flow (mL min−1) | [MII + MIII] (mol L−1) | Up-Flow (mL min−1) |
---|---|---|---|---|---|---|
ZnO | 1 | ZnO | 0.050 | 20 | 0.05 | 10 |
LDHinitial | 1 | Mg2Al-CO3 | 0.125 | 20 | 0.10 | 10 |
† LDHmix | - | mixture of ZnO and LDHinitial | - | - | - | - |
ZnO-LDH | 1 - 2 | ZnO - Mg2Al-CO3 | 0.05 - 0.15 | 40 | 0.05 - 0.05 | 20 |
LDH-only experiments | ||||||
LDH3 | 2 | Mg2Al-CO3 | 0.25 | 40 | 0.05 | 20 |
* LDH4 | 2 | Mg2Al-CO3 | 0.15 | 40 | 0.05 | 20 |
LDH5 | 2 | Mg2Al-CO3 | 0.15 | 40 | 0.05 | 20 |
LDH6 | 2 | Mg2Al-CO3 | 0.25 | 40 | 0.05 | 20 |
LDH7 | 2 | Mg2Al-CO3 | 0.15 | 40 | 0.05 | 20 |
LDH8 | 2 | Mg2Al-CO3 | 0.25 | 40 | 0.05 | 20 |
Sample | Miller Indices | a Lattice Parameter a (nm) | Miller Indices | a Lattice Parameter c (nm) |
---|---|---|---|---|
ZnO | 010 | 0.33 | 002 | 0.52 |
LDHinitial | 110 | 0.30 | 003 | 2.32 |
ZnO-LDH | 010 110 | 0.32 a 0.31 b | 002 003 | 0.52 a 2.28 b |
Sample | XRD | TEM | |||
---|---|---|---|---|---|
CDL (012) (nm) | CDL (003) (nm) | CDL (110) (nm) | b Particle Size (nm) | b Particle Size (nm) | |
ZnO | 25 | - | - | 22 ± 14 | - |
LDHinitial | - | 8 | 25 | - | 34 ± 34 |
ZnO-LDH | 42 | 12 | 27 | 53 ± 40 | 51 ± 22 |
Sample | SBET (m2 g−1) | Pore Diameter (nm) | Pore Volume (cm−3 g−1) |
---|---|---|---|
ZnO | 53.0 ± 0.1 | 17.6 | 0.3 |
LDHinitial | 58.2 ± 0.3 | 4.0 | 0.1 |
LDHmix | 39.6 ± 0.1 | 7.2 | 0.1 |
ZnO-LDH | 76.2 ± 0.1 | 17.0 | 0.7 |
Sample | Band Gap (eV) |
---|---|
ZnO | 3.21 |
LDHinitial | 5.24 |
LDHmix | 3.22 |
ZnO-LDH | 3.31 |
Sample | Reactor | Flow Rate (mL min−1) | Re | CDL (003) (nm) | CDL (110) (nm) |
---|---|---|---|---|---|
LDHinitial | 1 | 30 | 235 | 8 | 25 |
LDH3 | 2 | 60 | 297 | 7 | 30 |
Sample | SBET (m2 g−1) | BJH (Barrett, Joyner, and Halenda) Pore Diameter (nm) | BJH Pore Volume (cm3 g−1) |
---|---|---|---|
LDHinitial | 58.2 ± 0.3 | 3.5 | 0.07 |
LDH3 | 20.1 ± 0.1 | 4.2 | 0.04 |
Sample | CDL (003)/nm | CDL (110)/nm |
---|---|---|
LDH4 | 6 | 25 |
LDH5 | 6 | 26 |
LDH6 | 7 | 25 |
LDH7 | 5 | 27 |
LDH8 | 8 | 27 |
Sample | SBET (m2 g−1) | Pore Diameter (nm) | Pore Volume (cm3 g−1) |
---|---|---|---|
LDH4 | 266.8 ± 0.4 | 16.85 | 1.36 |
LDH5 | 270.2 ± 0.5 | 15.87 | 1.29 |
LDH6 | 22.6 ± 0.1 | 3.89 | 0.06 |
LDH7 | 271.7 ± 0.5 | 14.55 | 1.20 |
LDH8 | 26.1 ± 0.2 | 4.42 | 0.05 |
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Clark, I.; Smith, J.; Gomes, R.L.; Lester, E. Towards the Continuous Hydrothermal Synthesis of ZnO@Mg2Al-CO3 Core-Shell Composite Nanomaterials. Nanomaterials 2020, 10, 2052. https://doi.org/10.3390/nano10102052
Clark I, Smith J, Gomes RL, Lester E. Towards the Continuous Hydrothermal Synthesis of ZnO@Mg2Al-CO3 Core-Shell Composite Nanomaterials. Nanomaterials. 2020; 10(10):2052. https://doi.org/10.3390/nano10102052
Chicago/Turabian StyleClark, Ian, Jacob Smith, Rachel L. Gomes, and Edward Lester. 2020. "Towards the Continuous Hydrothermal Synthesis of ZnO@Mg2Al-CO3 Core-Shell Composite Nanomaterials" Nanomaterials 10, no. 10: 2052. https://doi.org/10.3390/nano10102052