垂直自支撑式金属有机框架多级结构单晶用于锂定向沉积

doi:10.1016/S1872-2067(20)63755-X

催化学报 ›› 2021, Vol. 42 ›› Issue (9): 1553-1560.DOI: 10.1016/S1872-2067(20)63755-X

垂直自支撑式金属有机框架多级结构单晶用于锂定向沉积

贾晓敏^a^,^†, 李少雯^b^,^†, 孙凸^c^,^†, 王彦智^a^,^†, 范亚奇^c, 张超超^a, 徐杨^a, 梁作中^a, 雷海涛^a, 张伟^a, 周瑀烨^d, 马延航^c, 郑浩铨^a^,^*(), 马越^b^,^#(), 曹睿^a^,^$()

^a陕西师范大学化学化工学院, 应用表面与胶体化学教育部重点实验室, 陕西西安710119, 中国
^b西北工业大学材料学院, 凝固技术国家重点实验室, 纳米能源材料研究中心, 陕西西安710072, 中国
^c上海科技大学物质科学与技术学院, 上海201210, 中国
^d瑞典皇家理工学院化学生物技术和健康学院, 化学院, 应用物理化学系, 分析化学, 斯德哥尔摩, 瑞典

收稿日期:2020-12-11 接受日期:2021-01-11 出版日期:2021-09-18 发布日期:2021-05-16
通讯作者: 郑浩铨,马越,曹睿
作者简介:第一联系人：
^†共同第一作者.
基金资助:
国家自然科学基金(21975148);国家自然科学基金(51602261);国家自然科学基金(51711530037);国家自然科学基金(21773146);国家自然科学基金(21835002);国家自然科学基金(21875140);国家自然科学基金(21601118);教育部霍英东青年教师基金(21601118);中央高校基础研究基金(GK201903033);中央高校基础研究基金(3102019JC005);上海市自然科学基金(17ZR1418600)

Single crystal metal-organic framework constructed by vertically self-pillared nanosheets and its derivative for oriented lithium plating

Xiaomin Jia^a^,^†, Shaowen Li^b^,^†, Tu Sun^c^,^†, Yanzhi Wang^a^,^†, Yaqi Fan^c, Chaochao Zhang^a, Yang Xu^a, Zuozhong Liang^a, Haitao Lei^a, Wei Zhang^a, Yuye Zhou^d, Yanhang Ma^c, Haoquan Zheng^a^,^*(), Yue Ma^b^,^#(), Rui Cao^a^,^$()

^aKey Laboratory of Applied Surface and Colloid Chemistry, Ministry of Education, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi’an 710119, Shaanxi, China
^bCenter for Nano Energy Materials, State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi'an 710072, Shaanxi, China
^cSchool of Physical Science and Technology, ShanghaiTech University, Shanghai 201210, China
^dSchool of Engineering Sciences in Chemistry, Biotechnology and Health, Department of Chemistry, Division of Applied Physical Chemistry, Analytical Chemistry, KTH Royal Institute of Technology, SE-106 91, Stockholm, Sweden

Received:2020-12-11 Accepted:2021-01-11 Online:2021-09-18 Published:2021-05-16
Contact: Haoquan Zheng,Yue Ma,Rui Cao
About author:^$ E-mail: ruicao@snnu.edu.cn
^# E-mail: mayue04@nwpu.edu.cn;
^* E-mail: zhenghaoquan@snnu.edu.cn;
First author contact:
^† These authors contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21975148);National Natural Science Foundation of China(51602261);National Natural Science Foundation of China(51711530037);National Natural Science Foundation of China(21773146);National Natural Science Foundation of China(21835002);National Natural Science Foundation of China(21875140);National Natural Science Foundation of China(21601118);Fok Ying-Tong Education Foundation for Outstanding Young Teachers in University(21601118);Fundamental Research Funds for the Central Universities(GK201903033);Fundamental Research Funds for the Central Universities(3102019JC005);Shanghai Natural Science Fund(17ZR1418600)

摘要/Abstract

摘要：

金属有机框架材料(MOF)是由金属离子或簇和有机配体通过配位键自组装形成的多孔晶体材料. MOF及其衍生物具有开放金属位点和极大的比表面积, 广泛地应用在催化领域. 然而, MOF材料由于存在暴露活性位点较少, 传质受限或易发生不可控制的聚集等问题, 会导致活性位点的损失, 极大地限制了其在催化领域的应用. 多级结构不仅提供更多的暴露活性位点, 而且提升传质效率及稳定性. 因此, 设计和构造分层多级结构的MOF材料是解决上述问题的有效途径. 本文制备了一种垂直自支撑式MOF多级结构材料. 该多级结构材料由相互垂直自支撑式纳米片所构成; 通过三维电子衍射表征显示, 单个垂直自支撑式MOF多级结构颗粒显示单晶特性. 因此, 可以确定垂直自支撑式MOF多级结构是ZIF-67的单晶. 本文也对这种结构的形成机理进行了初步探究, 两种具有结构相关性ZIF在混合溶液中的相互转化是主要驱动力. 这种垂直穿插的多级结构具有优异的传质/传荷能力和增强反应动力学的特性, 扩展了传统多孔晶体材料的应用领域.
本文通过温和的溶液硫化法, 制备了保留垂直穿插结构的硫化钴, 并进一步将这种垂直穿插结构的硫化钴应用在锂金属电池中. 这类材料显示出多个优点: (1)具有高比表面积, 提升了离子通量和传质; (2)锂离子的结合将硫化钴物种还原为钴金属颗粒; (3)垂直穿插结构引导金属沿着二维纳米片的方向沉积, 避免树枝状晶体的生成. 将这种垂直自支撑式硫化钴多级结构材料用作电极材料时, 所组装的锂金属电池显示出有效的电流密度、高库伦效率(99%)、低成核过电位(30 mV于5 mA cm^-2)和较好的稳定循环性(510 h). 本文对于垂直穿插结构材料的设计及研究其在金属电池中的应用具有重大意义.

关键词: 垂直自支撑式结构, 金属有机框架材料, 催化剂前驱体, 锂定向沉积, 金属电池

Abstract:

This vertically self-pillared (VSP) structure extends the application range of traditional porous materials with facile mass/ion transport and enhanced reaction kinetics. Here, we prepare a single crystal metal-organic framework (MOF), employing the ZIF-67 structure as a proof of concept, which is constructed by vertically self-pillared nanosheets (VSP-MOF). We further converted VSP-MOF into VSP-cobalt sulfide (VSP-CoS₂) through a sulfidation process. Catalysis plays an important role in almost all battery technologies; for metallic batteries, lithium anodes exhibit a high theoretical specific capacity, low density, and low redox potential. However, during the half-cell reaction (Li⁺+e=Li), uncontrolled dendritic Li penetrates the separator and solid electrolyte interphase layer. When employed as a composite scaffold for lithium metal deposition, there are many advantage to using this framework: 1) the VSP-CoS₂ substrate provides a high specific surface area to dissipate the ion flux and mass transfer and acts as a pre-catalyst, 2) the catalytic Co center favors the charge transfer process and preferentially binds the Li⁺ with the enhanced electrical fields, and 3) the VSP structure guides the metallic propagation along the nanosheet 2D orientation without the protrusive dendrites. All these features enable the VSP structure in metallic batteries with encouraging performances.

Key words: Vertically self-pillared structure, Metal organic framework, Pre-catalyst preparation, Lithium plating orientation, Metallic battery

贾晓敏, 李少雯, 孙凸, 王彦智, 范亚奇, 张超超, 徐杨, 梁作中, 雷海涛, 张伟, 周瑀烨, 马延航, 郑浩铨, 马越, 曹睿. 垂直自支撑式金属有机框架多级结构单晶用于锂定向沉积[J]. 催化学报, 2021, 42(9): 1553-1560.

Xiaomin Jia, Shaowen Li, Tu Sun, Yanzhi Wang, Yaqi Fan, Chaochao Zhang, Yang Xu, Zuozhong Liang, Haitao Lei, Wei Zhang, Yuye Zhou, Yanhang Ma, Haoquan Zheng, Yue Ma, Rui Cao. Single crystal metal-organic framework constructed by vertically self-pillared nanosheets and its derivative for oriented lithium plating[J]. Chinese Journal of Catalysis, 2021, 42(9): 1553-1560.

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图/表 4

Fig. 1. Illustrating house-of-cards structure (a), selected area electron diffraction (SAED) pattern (b) and corresponding TEM image (c) along [111] of VSP-MOFs. Projection of reconstructed reciprocal lattice from 3D EDT data along [100] (d), [010] (e), [001] (f) directions, respectively. The crystal structural mode (g), experimental PXRD patterns (h) and N2 adsorption/desorption isotherm (i) of VSP-MOF and reference materials.

Fig. 2. TEM (a), HRTEM (b) images, EDS mapping (c), PXRD pattern (d), high-resolution XPS of Co 2p (e) and S 2p (f) of VSP-CoS2.

Fig. 3. Electrochemical characterization of the metallic batteries assembled by the VSP-CoS2 composite anodes. The discharge/charge profiles of (a) VSP-CoS2 electrode at the selected cycles between 0 and 3 V; (b) Voltage-time profiles of the Li plating/stripping of VSP-CoS2||VSP-CoS2 and Li||Li@1 mA cm-2 with the predetermined capacity of 1 mAh cm-2 for 510 h in symmetric cells; (c) The enlarged view of the voltage-time curve of the VSP-CoS2||VSP-CoS2 and Li||Li cells during 0 to 5 h symmetric cycling; (d) Voltage pro?les of the VSP-CoS2 electrode after activation process for different cycles with the upper cutoff voltage of 1.0 V at 5 mA cm-2; The inset in Fig. 3(d) presents the enlarged voltage pro?le. (e) CE of the VSP-CoS2 composite and the bare Cu foil for 100 cycles@0.5, 1, and 2 mA cm-2; (f) Galvanostatic discharge-charge curves of LMO||VSP-CoS2 full cell during different cycles.

Fig. 4. Schematic illustration of the Li plating in the VSP-CoS2 composite at different cycling states.

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垂直自支撑式金属有机框架多级结构单晶用于锂定向沉积

Single crystal metal-organic framework constructed by vertically self-pillared nanosheets and its derivative for oriented lithium plating

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