单层类水滑石纳米片的可控合成及规模生产展望

doi:10.3866/PKU.WHXB201912005

Abstract

Abstract:

As a type of layered material, layered double hydroxides (LDHs) exhibit high development potential and application prospects, and have been used widely in adsorbents, catalysts, ion exchangers, flame retardants, biology, sensing, medicine, and other fields. With the continued development in nanoscience and nanotechnology, it has been established that monolayer LDHs contain an abundance of exposed highly unsaturated coordination sites, and so display unexpected functionality. However, due to the higher charge density of the LDHs layers, the strong interactions between the layers, and the hydroxyl groups on the surface of the layers, the result is a compact stacking of the layers. Consequently, it is still a great challenge to synthesize high-quality monolayer LDHs. Despite various methods of preparing monolayer LDHs having been developed, which can generally be divided into top-down and bottom-up strategies, most of these approaches have used organic solvents, which take a long time to achieve the exfoliation of LDHs, or require special equipment. Furthermore, high costs and the low yields have prevented large-scale production of monolayer LDHs. With the rapid development of the national economy, the industrial preparation of monolayer LDHs has become an inescapable trend. The separate nucleation and ageing method for the preparation of nanostructured LDHs is a feasible method, the key features of which are a very rapid mixing and nucleation process in a colloid mill, followed by a separate ageing process. This method has been successfully applied to a pilot plant in China for the industrial-scale synthesis of LDHs materials. It should be noted that the particle size distribution of LDHs obtained by this method can be well controlled. Moreover, the synthesis operation is simple, and quick (with a short duration of only several minutes). Through new in-depth technology studies on two-dimensional layered materials, large-scale preparation, and industrial application of monolayer LDHs will certainly be increasingly realized, and ultimately transformed into economic benefits. In this review, we summarize the synthesis method of monolayer LDHs, describe the necessary characterization technologies that have been used to study monolayers LDHs nanosheets, such as X-ray diffraction, transmission electron microscopy, and atomic force microscopy. Then we discuss the applications in various fields, such as photocatalysis, electrocatalysis, batteries, supercapacitors, membrane materials, and biomedical fields. We further discuss the recent breakthroughs in the synthesis of monolayer and ultrathin LDHs and the advance of production scale-up of LDHs. Finally, the performance of monolayer/ultrathin LDHs is summarized to provide a basis for the ensuing design of high-performance monolayer LDHs.

Key words: Layered double hydroxides, Thickness, Monolayer, Ultrathin, Defect, Scale-up production

Tian Li, Xiaojie Hao, Sha Bai, Yufei Zhao, Yu-Fei Song. Controllable Synthesis and Scale-up Production Prospect of Monolayer Layered Double Hydroxide Nanosheets[J]. Acta Phys. -Chim. Sin. 2020, 36(9), 1912005. doi: 10.3866/PKU.WHXB201912005

Figures/Tables 13

Table 1

Monolayer or ultrathinLDH synthesis method."

Number	Method	Thickness	Solvent	Remarks	Ref.
1	Organic solvent exfoliation		DDS, butanol	Organic LDH compounds are delaminated in vacuum drying at room temperature	6
2	Formamide exfoliation		Amino acids, formamide	The characteristic peak of LDH in XRD disappears, The strong hydrogen bond between the anion and the polar solvent in the intercalation leads to the penetration of a large number of solvents in the intercalation, thus promoting exfoliation	36
3	Formamide exfoliation	0.8 nm	Formamide	No prior modification of amino acids or surfactants is required, requiring approximately 2.5 d and excess formamide	37
4	Formamide exfoliation	0.7–1.4 nm	Formamide	The samples were dispersed in formamide and treated with ultrasonic water bath at continuous intervals of 30 min	41
5	Liquid exfoliation at low temperature	0.6 nm	Sodium hydroxide/ urea solution	At low temperature, the exfoliation degree was larger, the thickness was reduced to 0.6 nm at -10 ℃	42
6	Temperature shock method	~0.18 nm	H₂O	The LDH solution was frozen in liquid nitrogen and then melted in 80 water bath with a delamination rate of 61%	44
7	Ostwald ripening driven exfoliation	4–9 nm	H₂O, DMF	While, the as-exfoliated nanosheets are still vertically aligned on the electrode and possess a good structural integrity, which exhibits good electrical contact and effectively avoids the restacking of the exfoliated nanosheets	43
8	Aqueous miscible organic solvent treatment method		H₂O, acetone	LDH wet samples were re-dispersed in acetone and stirred for 1 h, then washed with acetone. Dry samples were kept in monolayer	45
9	Amino acid reconstruction method	~0.8–1.5 nm	Amino acids	LDH was calcination in air and then reconstruct in aqueous solution of amino acid	46
10	Water-Plasma-Enabled Exfoliation	1.54 nm	H₂O	The as-obtained pristine CoFe LDHs were subjected to water-plasma treatment in a dielectric barrier discharge (DBD) plasma reactor for 5 min to obtain ultrathin CoFe LDHs nanosheets	47
11	Dry Exfoliation	0.6 nm		Ar dry exfoliation is a clean, time-saving, non-toxic method and avoids the adsorption of solvent molecules	48
12	Reverse microemulsion method	1.5 nm	H₂O, iso-octane, DDS, 1-butanol	Particle size in diameter and thickness can be effectively controlled by the ratio of water to surfactant, but surfactant residues are unavoidable	49
13	One step synthesis by formamide	0.8 nm	H₂O, formamide	The monolayer LDH was synthesized by adding formamide directly during the reaction	52
14	One-step synthesis by ethylene glycol	0.85 nm	Ethylene glycol	It remains stable when dispersed in water or dried into powder	56
15	One step synthesis by H₂O₂	1.44 nm	H₂O, H₂O₂	LDHs catalyzes the rapid decomposition of H₂O₂ and releases a large amount of O₂, which causes the layers to move violently, resulting in the separation of LDHs layers	57
16	One step synthesis by NH₃·H₂O	0.8 nm	H₂O	The gel was synthesized by co-precipitation, washed and re-dispersed by ultrasound in water, and the sample remained stable for 20 d at -4 ℃	58

Table 1

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Controllable Synthesis and Scale-up Production Prospect of Monolayer Layered Double Hydroxide Nanosheets

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