钼酸根阴离子在增强聚苯胺包覆的镍钴层状氢氧化物的电容和析氧行为中的关键作用

doi:10.1016/S1872-2067(20)63724-X

催化学报 ›› 2021, Vol. 42 ›› Issue (6): 980-993.DOI: 10.1016/S1872-2067(20)63724-X

钼酸根阴离子在增强聚苯胺包覆的镍钴层状氢氧化物的电容和析氧行为中的关键作用

胡强^a, 王华^a, 向飞菲^a, 郑荞佶^a, 马新国^b, 霍瑜^a, 谢奉妤^a, 徐成刚^a, 赁敦敏^a^,^*(), 胡吉松^b^,^#()

^a四川师范大学化学与材料科学学院, 四川成都610066
^b湖北工业大学理学院, 湖北武汉430068

收稿日期:2020-08-17 接受日期:2020-10-09 出版日期:2021-06-18 发布日期:2021-01-30
通讯作者: 赁敦敏,胡吉松
基金资助:
四川省科学技术计划(2018JY0447)

Critical roles of molybdate anions in enhancing capacitive and oxygen evolution behaviors of LDH@PANI nanohybrids

Qiang Hu^a, Hua Wang^a, Feifei Xiang^a, Qiaoji Zheng^a, Xinguo Ma^b, Yu Huo^a, Fengyu Xie^a, Chenggang Xu^a, Dunmin Lin^a^,^*(), Jisong Hu^b^,^#()

^aCollege of Chemistry and Materials Science, Sichuan Normal University, Chengdu 610066, Sichuan, China
^bSchool of Science, Hubei University of Technology, Wuhan 430068, Hubei, China

Received:2020-08-17 Accepted:2020-10-09 Online:2021-06-18 Published:2021-01-30
Contact: Dunmin Lin,Jisong Hu
About author:^#E-mail: jisong.hu@yahoo.com
^*Tel/Fax: +86-28-84760802; E-mail: ddmd222@sicnu.edu.cn;
Supported by:
Sichuan Science and Technology Program(2018JY0447)

摘要/Abstract

摘要：

理论容量大且过电位低的层状氢氧化物(LDHs)是极有前景的超级电容电池和析氧反应的电极材料; 然而, 体相LDHs的低电导率和活性位点不足增加了电极的内阻, 降低了电极容量和产氧效率. 本文采用两步法制备了聚苯胺包覆的MoO₄^2-插层的镍钴层状双金属氢氧化物复合电极(M-LDH@PANI). 随着LDH中MoO₄^2-含量的增加, 针状的LDH微球逐渐演化为具有较高比表面积的片状M-LDH微球, 这为整个电极提供了更多的电化学位点. 此外, 非晶态的聚苯胺包覆提高了复合电极的电导率. 在引入适量MoO₄^2-插层离子时, M-LDH@PANI表现出显著强化的储能和催化性能. 所获得的M-LDH@PANI-0.5在析氧反应中表现出优越的电催化活性(10 mA cm^-2时的过电位为266 mV), 作为超级电容电池电极则具有864.8 C g^-1的高容量. 采用M-LDH@PANI-0.5作为正极及以活性炭作为负极组装的超级电容电池在功率密度为8,300.0 W kg^-1时能量密度为44.6 Wh kg^-1, 且具有优异的循环稳定性(10000次循环后保留83.9%的初始容量). 本文为LDH基材料的阴离子插层改性增强材料性能的机理提供了一个非传统的解释. 在上述研究基础上, 采用射线衍射(XRD)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、高分辨透射电镜(HRTEM)和比表面积测试(BET)等手段对样品进行了深入表征.
XRD结果表明, MoO₄^2-插层的LDH材料的层间晶面(003)的峰随着MoO₄^2-含量的增加而逐渐消失, 这是由于晶面间距越大越容易受到晶粒细化的影响, 间距大的晶格更容易受到破坏,导致晶格的展宽和弱化, 从而间接证明MoO₄^2-的成功插层. SEM、HRTEM和BET测试结果表明, MoO₄^2-的含量对材料的形貌和比表面积具有重大影响. 利用XPS对样品的价态进行了研究, 发现随着MoO₄^2-含量的增加, Co和Ni的价态没有明显变化. 电化学测试结果表明, 电极的储能和催化性能随MoO₄^2-含量的增加而先增加后减小. 利用理论计算分析了MoO₄^2-在LDH中的插层行为, 发现少量的MoO₄^2-有利于扩大LDH的层间间距, 而过量的MoO₄^2-则会与LDH的H原子结合, 从而与电解液中的OH^-竞争, 导致复合电极的电化学性能下降. 此外, MoO₄^2-插层的片状微球能有效调节材料的去质子化能, 大大加速电极表面的氧化还原反应. 因此, MoO₄^2-插层能够显著强化LDH基材料的超级电容电池电极和OER催化剂电化学性能.

关键词: 层状氢氧化物, 聚苯胺, 钼酸根离子, 插层分级结构, 超级电容电池, 电催化剂

Abstract:

Low-overpotential layered hydroxides (LDHs) with high theoretical capacity are promising electrodes for supercapaterry and oxygen evolution reaction; however, the low electronic conductivity and insufficient active sites of bulk LDHs increase the internal resistance and reduce the capacity and oxygen-production efficiency of electrodes. Herein, we prepared a polyaniline-coated NiCo-layered double hydroxide intercalated with MoO₄^2- (M-LDH@PANI) composite electrode using a two-step method. As the amount of MoO₄^2- in the LDH increases, acicular microspheres steadily evolve into flaky microspheres with a high surface area, providing more active electrochemical sites. Moreover, the amorphous PANI coating of M-LDH boosts the electronic conductivity of the composite electrode. Accordingly, the M-LDH@PANI at an appropriate level of MoO₄^2- exhibits significantly enhanced energy storage and catalytic performance. Experimental analyses and theoretical calculations reveal that a small amount of MoO₄^2- is conducive to the expansion of LDH interlayer spacing, while an excessive amount of MoO₄^2- combines with the H atoms of LDH, thus competing with OH^-, resulting in reduced electrochemical performance. Moreover, M-LDH flaky microspheres can efficiently modulate deprotonation energy, greatly accelerating surface redox reactions. This study provides an explanation for an unconventional mechanism, and a method for the modification of LDH-based materials for anion intercalation.

Key words: Layered hydroxide LDH, PANI, MoO₄^2-, Intercalated hierarchical structures, Supercapaterry, Electrocatalyst

胡强, 王华, 向飞菲, 郑荞佶, 马新国, 霍瑜, 谢奉妤, 徐成刚, 赁敦敏, 胡吉松. 钼酸根阴离子在增强聚苯胺包覆的镍钴层状氢氧化物的电容和析氧行为中的关键作用[J]. 催化学报, 2021, 42(6): 980-993.

Qiang Hu, Hua Wang, Feifei Xiang, Qiaoji Zheng, Xinguo Ma, Yu Huo, Fengyu Xie, Chenggang Xu, Dunmin Lin, Jisong Hu. Critical roles of molybdate anions in enhancing capacitive and oxygen evolution behaviors of LDH@PANI nanohybrids[J]. Chinese Journal of Catalysis, 2021, 42(6): 980-993.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63724-X

https://www.cjcatal.com/CN/Y2021/V42/I6/980

图/表 7

Fig. 1. Schematic representations of the two-step fabrication route for LDH, M-LDH and M-LDH@PANI architecture grown on NF.

Fig. 2. (a-c) SEM images of LDH, M-LDH-0.5 and M-LDH@PANI-0.5; (d,e) TEM and HRTEM images of LDH; (f,g) TEM and HRTEM images of M-LDH-0.5; (h-j) TEM and HRTEM images of M-LDH@PANI-0.5; (k) The corresponding element mappings images of M-LDH@PANI-0.5.

Fig. 3. (a) Schematic crystal structure of M-LDH; (b,c) XRD patterns of LDH, M-LDH-x and M-LDH@PANI-0.5; (d) FTIR spectra of LDH, M-LDH-0.5 and M-LDH@PANI-0.5; (e-i) High-resolution XPS spectra of Ni 2p, Co 2p, Mo 3d, O1s and N1s in LDH and M-LDH@PANI-0.5.

Fig. 4. (a) Comparative CV curves of LDH, M-LDH-x and M-LDH@PANI-0.5 electrodes at scan rate of 5 mV s-1; (b) CV curves of M-LDH@PANI-0.5 electrode at different scan rates; (c) Power law dependence of redox peak current on scan rate for LDH, M-LDH-x and M-LDH@PANI-0.5 electrodes; (d) GCD curves of M-LDH@PANI-0.5 electrode at different current densities; (e) Comparative GCD curves of LDH, M-LDH-x and M-LDH@PANI-0.5 electrodes at a current density of 1 A g-1; (f) Specific capacities of LDH, M-LDH-x and M-LDH@PANI-0.5 electrodes as function of current density; (g) Nyquist plots of LDH, M-LDH-0.5 and M-LDH@PANI-0.5 electrodes; (h) Cycling stability of M-LDH@PANI-0.5 electrode at a current density of 5 A g-1; (i) A comparison of improvement ability of our strategy with the values of previously reported similar electrodes.

Fig. 5. (a) Side views of pristine double-layer Co0.5Ni0.5-LDH; MoO42- (b) inside and (c) outside interface of Co0.5Ni0.5-LDH; (d) Stacked MoO42- inside interface of Co0.5Ni0.5-LDH; (e) MoO42- inside and outside interface of Co0.5Ni0.5-LDH; (f) The calculated deprotonation energy of pristine, one-layer MoO42- inside, one-layer MoO42- outside, MoO42- inside and outside the interface and two-layer MoO42- inside the interface of Co0.5Ni0.5-LDH, respectively; (g) Charge density difference isosurfaces for the deprotonation process on two-layer MoO42- inside the interface of Co0.5Ni0.5-LDH; yellow and blue areas indicate charge depletion and charge accumulation zones, respectively (isosurface value is 0.01 eV/?3).

Fig. 6. (a) Schematic of device fabrication; (b) Cyclic voltammetry curves of HSC at various voltage windows at 10 mV s-1; (c) GCD curves of HSC at various voltage windows at 1 A g-1; (d) CV curves of HSC at different scan rates; (e) GCD curves of HSC device at different current densities; (f) Specific capacity of HSC device at different current densities; (g) Comparison of the Ragone plots of the present and reported devices; and (h) cycling stability at a current density of 3 A g-1.

Fig. 7. (a) Polarization curves of LDH, M-LDH-x and M-LDH@PANI-0.5, respectively; (b) Tafel plots of LDH, M-LDH-x and M-LDH@PANI-0.5, respectively; (c) Free energy profiles for the OER over 2L MoO42- inside LDH at zero potential (U = 0), equilibrium potential for oxygen evolution (U = 1.23 V), and minimum potential (U = 1.61 V) where all steps run downhill; (d) Stability test of M-LDH@PANI-0.5 for 34 h in 1.0 M KOH.

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钼酸根阴离子在增强聚苯胺包覆的镍钴层状氢氧化物的电容和析氧行为中的关键作用

Critical roles of molybdate anions in enhancing capacitive and oxygen evolution behaviors of LDH@PANI nanohybrids

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