Two-dimensional magnetic behaviour in hybrid NiFe-layered double hydroxides by molecular engineering

Silva, Álvaro Seijas-Da; Carrasco, Jose A.; Vieira, Bruno; Waerenborgh, J.C.; Coronado, Eugenio; Abellán, Gonzalo

doi:10.1039/d2dt03804h

Cited by 3 publications

(1 citation statement)

References 42 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…A n− symbolizes a constituent ranging from (in)organic anions to macromolecules, and Sv stands for solvent molecules. This general composition leads to a plethora of highly tunable systems [12][13][14][15][16] with relevance in environmental applications [17], photocatalysis [18], energy storage and conversion [19][20][21], quantum materials [22,23], and others [24]. This wide range of potential applications makes the development of reliable scaling processes crucial.…”

Section: Introductionmentioning

confidence: 99%

Upscaling the urea method synthesis of CoAl layered double hydroxides

Jaramillo-Hernández,

Oestreicher,

Mizrahi

et al. 2023

Beilstein J. Nanotechnol.

Self Cite

View full text Add to dashboard Cite

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.

show abstract