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

物理化学学报 >> 2020, Vol. 36 >> Issue (9): 1912005.doi: 10.3866/PKU.WHXB201912005

所属专题：精准纳米合成

单层类水滑石纳米片的可控合成及规模生产展望

李天, 郝晓杰, 白莎, 赵宇飞(), 宋宇飞()

北京化工大学，化工资源有效利用国家重点实验室，北京 100029

收稿日期:2019-12-02 录用日期:2019-12-30 发布日期:2020-02-14
通讯作者: 赵宇飞,宋宇飞 E-mail:songyf@mail.buct.edu.cn;zhaoyufei@mail.buct.edu.cn
作者简介:赵宇飞，出生于1985年。于2007年获得山西大学双学士学位。2011–2012年，于牛津大学Dermot O’Hare教授实验室交流学习。2013年于北京化工大学获得博士学位。现为北京化工大学化工资源有效利用国家重点实验室教授。主要研究方向为二维插层材料的可控合成及精细结构表征，LDHs基纳米材料的拓扑结构转变，面向高值精细化学品的光/电催化合成
宋宇飞，出生于1976年。于1997年和2002年获得山西大学学士学位和山西大学分子科学研究所博士学位。2002年至2004年在荷兰莱顿大学化学系做博士后研究；2004年至2005年在德国马普生物无机所做博士后研究；2005年至2008年博在英国格拉斯哥大学化学系做博士后研究。现为北京化工大学化工资源有效利用国家重点实验室教授。主要研究方向为多酸基先进功能材料、插层结构组装与催化、以能源与环保为导向的功能材料的设计与制备
基金资助:
国家重点基础研究发展计划(2017YFB0307303);国家重点基础研究发展规划项目(973)(2014CB932104);国家自然科学基金(U1707603);国家自然科学基金(21878008);国家自然科学基金(21625101);国家自然科学基金(20190816);国家自然科学基金(21601195);国家自然科学基金(21922801);北京自然科学基金(2182047);北京自然科学基金(2202036);中央高校基金(ZY1709)

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

Tian Li, Xiaojie Hao, Sha Bai, Yufei Zhao(), Yu-Fei Song()

State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, P. R. China

Received:2019-12-02 Accepted:2019-12-30 Published:2020-02-14
Contact: Yufei Zhao,Yu-Fei Song E-mail:songyf@mail.buct.edu.cn;zhaoyufei@mail.buct.edu.cn
About author:Emails: zhaoyufei@mail.buct.edu.cn, +86-10-64431832 (Y.S.)
Emails:songyf@mail.buct.edu.cn, Tel.: +86-10-64431832 (Y.Z.)
Supported by:
The project was supported by the National Key Basic Research Development Program of China(2017YFB0307303);the National Key Basic Research Program of China (973)(2014CB932104);the National Natural Science Foundation of China(U1707603);the National Natural Science Foundation of China(21878008);the National Natural Science Foundation of China(21625101);the National Natural Science Foundation of China(20190816);the National Natural Science Foundation of China(21601195);the National Natural Science Foundation of China(21922801);the Beijing Natural Science Foundation, China(2182047);the Beijing Natural Science Foundation, China(2202036);the Central University Fund, China(ZY1709)

摘要/Abstract

摘要：

水滑石(LDHs)是一种阴离子黏土材料，由于其主体层板厚度的可调性，使其在光/电催化、电池、超级电容器、传感器以及生物医药等领域都具有广泛应用。降低层厚至单层可使材料的物理化学性质发生根本改变，从而优化催化性能。近期研究表明，利用自上而下，自下而上的方法，可以实现单层LDHs类材料的合成，但是受限于产量(g级)以及成本设备等问题，目前规模化制备高质量单层LDHs类材料还没有工业案例。成核晶化隔离法是目前唯一规模化合成纳米LDHs的工业化方法，具有成本低，产量可吨级放大等优点。本综述从合成方法、表征手段、应用三个角度讨论了单层及超薄LDHs的精准调控，详细论述了近期关于单层及超薄LDHs合成突破以及LDHs的规模化生产进展，并对其性能进行了总结，为后续设计高性能单层LDHs提供思路。

关键词: 水滑石, 厚度, 单层, 超薄, 缺陷, 规模化制备

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

李天, 郝晓杰, 白莎, 赵宇飞, 宋宇飞. 单层类水滑石纳米片的可控合成及规模生产展望[J]. 物理化学学报, 2020, 36(9), 1912005. doi: 10.3866/PKU.WHXB201912005

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

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB201912005

https://www.whxb.pku.edu.cn/CN/Y2020/V36/I9/1912005

图/表 13

表1

单层及超薄LDH合成方法"

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

表1

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单层类水滑石纳米片的可控合成及规模生产展望

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

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