Upscaling the urea method synthesis of CoAl layered double hydroxides

Camilo Jaramillo-Hernández, Víctor Oestreicher, Martín Mizrahi and Gonzalo Abellán

Beilstein J. Nanotechnol. 2023, 14, 927–938. https://doi.org/10.3762/bjnano.14.76

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Upscaling the urea method synthesis of CoAl layered double hydroxides

Camilo Jaramillo-Hernández, Víctor Oestreicher, Martín Mizrahi and Gonzalo Abellán

Beilstein J. Nanotechnol. 2023, 14, 927–938. https://doi.org/10.3762/bjnano.14.76

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Jaramillo-Hernández, C.; Oestreicher, V.; Mizrahi, M.; Abellán, G. Beilstein J. Nanotechnol. 2023, 14, 927–938. doi:10.3762/bjnano.14.76

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TY  - JOUR
A1  - Jaramillo-Hernández, Camilo
A1  - Oestreicher, Víctor
A1  - Mizrahi, Martín
A1  - Abellán, Gonzalo
T1  - Upscaling the urea method synthesis of CoAl layered double hydroxides
JF  - Beilstein Journal of Nanotechnology
PY  - 2023///
VL  - 14
SP  - 927
EP  - 938
SN  - 2190-4286
DO  - 10.3762/bjnano.14.76
PB  - Beilstein-Institut
JA  - Beilstein J. Nanotechnol.
UR  - https://doi.org/10.3762/bjnano.14.76
KW  - Co-based hydroxides
KW  - layered double hydroxide
KW  - layered materials
KW  - scale-up process
KW  - synthesis
KW  - two-dimensional materials
N2  - Research on two-dimensional materials is one of the most relevant fields in materials science. Layered double hydroxides (LDHs), a versatile class of anionic clays, exhibit great potential in photocatalysis, energy storage and conversion, and environmental applications. However, its implementation in real-life devices requires the development of efficient and reproducible large-scale synthesis processes. Unfortunately, reliable methods that allow for the production of large quantities of two-dimensional LDHs with well-defined morphologies and high crystallinity are very scarce. In this work, we carry out a scale-up of the urea-based CoAl-LDH synthesis method. We thoroughly study the effects of the mass scale-up (25-fold: up to 375 mM) and the volumetric scale-up (20-fold: up to 2 L). For this, we use a combination of several structural (XRD, TGA, and N2 and CO2 isotherms), microscopic (SEM, TEM, and AFM), magnetic (SQUID), and spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the alkalinization rates and, concomitantly, the precipitation, even under recrystallization at high temperatures. In contrast, for the tenfold mass scale-up, similar morphological features were observed and assigned to changes in nucleation and growth. However, at higher concentrations, simonkolleite-like Co-based layered hydroxide impurities are formed, indicating a phase competition during the precipitation related to the thermodynamic stability of the growing phases. Overall, this work demonstrates that it is possible to upscale the synthesis of high-quality hexagonal CoAl-LDH in a reproducible manner. It highlights the most critical synthesis aspects that must be controlled and provides various fingerprints to trace the quality of these materials. These results will contribute to bringing the use of these 2D layered materials closer to reality in different applications of interest.
ER  -

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Scholarly Works

Jaramillo‐Hernández, C.; Seijas‐Da Silva, A.; Abellán, G. Crystallographic Phase‐Dependent Electrochemical Properties of Layered Hydroxides for Energy Applications. European Journal of Inorganic Chemistry 2025, 28. doi:10.1002/ejic.202400754
Bai, S.; Liu, G.; Shen, T.; Wu, Z.; Chen, W.; Song, Y.-F. Controllable synthesis of layered double hydroxides: From macroscopic morphology to microscopic coordination at the atomic level. Coordination Chemistry Reviews 2025, 529, 216437. doi:10.1016/j.ccr.2025.216437
Mahmoud, M. E.; El-Sharkawy, R. M.; Allam, E. A.; Nabil, G. M.; Louka, F. R.; Sillanpää, M.; Elsayed, S. M. Layered double hydroxide nanocomposites as promising nanomaterials for removal of inorganic pollutants from aquatic systems: A review. Journal of Solid State Chemistry 346, 125289. doi:10.1016/j.jssc.2025.125289

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