基于聚(两性离子液体)功能化聚吡咯/氧化石墨烯的独特MoS2-SnS2异质纳米片及其改善的氮还原电活性

doi:10.1016/S1872-2067(21)63944-X

催化学报 ›› 2022, Vol. 43 ›› Issue (5): 1341-1350.DOI: 10.1016/S1872-2067(21)63944-X

基于聚(两性离子液体)功能化聚吡咯/氧化石墨烯的独特MoS₂-SnS₂异质纳米片及其改善的氮还原电活性

茆卉^a, 杨浩然^a, 柳金池^a, 张帅^a, 刘大亮^a, 吴琼^a, 孙文平^c, 宋溪明^a(), 马天翼^b()

^a辽宁大学化学院, 辽宁沈阳110036, 中国
^b斯威本科技大学埃米材料转化中心, 霍索恩, 澳大利亚
^c浙江大学材料科学与工程学院, 洁净能源利用国家重点实验室, 浙江杭州310027, 中国

收稿日期:2021-08-13 接受日期:2021-09-13 出版日期:2022-05-18 发布日期:2022-03-23
通讯作者: 宋溪明,马天翼
基金资助:
国家自然科学基金(51773085);国家自然科学基金(52071171);辽宁省“兴辽英才计划”项目-攀登学者(XLYC1802005);辽宁省百千万人才项目(LNBQW2018B0048);辽宁省自然科学基金优秀青年基金(2019-YQ-04);辽宁省教育厅重点研发项目(LZD201902);澳大利亚研究委员会未来学者(FT210100298);辽宁省教育厅青年科技人才“育苗”项目(LQN201903);辽宁省“兴辽英才计划”项目(XLYC2007132);辽宁大学本科教学改革项目(JG2020YBXM115)

Improved nitrogen reduction electroactivity by unique MoS₂-SnS₂ heterogeneous nanoplates supported on poly(zwitterionic liquids) functionalized polypyrrole/graphene oxide

Hui Mao^a, Haoran Yang^a, Jinchi Liu^a, Shuai Zhang^a, Daliang Liu^a, Qiong Wu^a, Wenping Sun^c, Xi-Ming Song^a(), Tianyi Ma^b()

^aInstitute of Clean Energy Chemistry, Key Laboratory for Green Synthesis and Preparative Chemistry of Advanced Materials, College of Chemistry, Liaoning University, Shenyang 110036, Liaoning, China
^bCentre for Translational Atomaterials, Swinburne University of Technology, Hawthorn, VIC 3122, Australia
^cSchool of Materials Science and Engineering, State Key Laboratory of Clean Energy Utilization, Zhejiang University, Hangzhou 310027, Zhejiang, China

Received:2021-08-13 Accepted:2021-09-13 Online:2022-05-18 Published:2022-03-23
Contact: Xi-Ming Song, Tianyi Ma
Supported by:
National Natural Science Foundation of China(51773085);National Natural Science Foundation of China(52071171);Liaoning Revitalization Talents Program - Pan Deng Scholars(XLYC1802005);Liaoning BaiQianWan Talents Program(LNBQW2018B0048);Natural Science Fund of Liaoning Province for Excellent Young Scholars(2019-YQ-04);Key Project of Scientific Research of the Education Department of Liaoning Province(LZD201902);Australian Research Council (ARC) Future Fellowship(FT210100298);Scientific Research Fund of Liaoning Provincial Education Department(LQN201903);Liaoning Revitalization Talents Program(XLYC2007132);Undergraduate Teaching Reform Project of Liaoning University(JG2020YBXM115)

摘要/Abstract

摘要：

NH₃是一种重要的化工原料, 广泛应用于合成各种化工产品. 然而, 传统还原N₂制备NH₃的Haber-Bosch工艺执行条件苛刻, 在消耗大量化石能源的同时产生严重环境污染. 在环境条件下的电化学氮还原反应(NRR)是一种最具前景的可持续、清洁生产NH₃的能源技术, 其实际应用的核心是开发高效、价格低廉和易制备的NRR电催化剂. 过渡金属二硫族化合物(TMDCs)储量丰富并且价格低廉, 具有多变的晶体结构和相组成、可控的形貌、缺陷设计可调节等特点, 呈现出优异的电催化活性, 是用来替代贵金属的理想选择. MoS₂和SnS₂都可作为电催化剂应用于NRR. 由于金属1T-MoS₂和1T’-MoS₂对与NRR竞争的析氢反应(HER)具有极好的电化学活性, 其NRR法拉第效率较低; 尽管具有半导体特性的SnS₂能够通过限制表面电子可及性来抑制HER, 但是高过电位和较低氨产率仍不能令人满意. 据报道, 在碳布上原位生长Mo掺杂SnS₂具有丰富的S空位, 由于杂原子掺杂和空位工程形成了Mo-Sn-Sn三元催化位点, 其NRR活性显著增强.

因此, 为了抑制竞争反应以提高NRR的法拉第效率, 本文设计并制备了一种独特的无机/有机分级纳米结构用于电催化NRR. 选用一种独特的聚两性离子液体, 即侧链同时含有咪唑盐和磺酸基团的聚1-乙烯基-3-丙烷磺酸基咪唑盐(PVIPS), 作为界面诱导剂, 利用离子交换作用吸附作为前驱体的Mo₇O₂₄^6‒和Sn⁴⁺, 诱导1T’-MoS₂和2T型六方SnS₂同时生长, 形成独特的MoS₂-SnS₂异质纳米片负载于PVIPS功能化的聚吡咯/氧化石墨烯(PVIPS/PPy/GO)表面. 由于各组分的协同效应, 得到的MoS₂-SnS₂/PVIPS/PPy/GO纳米片表现出较好的NRR活性, 其在‒0.5 V (vs. RHE)时氨产率最佳, 为16.74 μg h^‒1 mg^‒1_act., 其相应的法拉第效率为4.07%. 具有半导体特性的SnS₂能够限制表面电子的可及性, 进而抑制1T’-MoS₂的HER过程, 而具有金属性的1T’-MoS₂可与SnS₂形成Mo-Sn-Sn三元催化活性位点, 进而提高SnS₂的NRR电催化活性. 此外, 高分辨透射电镜, X射线衍射和X射线光电子能谱结果表明, MoS₂-SnS₂/PVIPS/PPy/GO在NRR使用前后存在显著差异, 这主要归因于在NRR过程中MoS₂-SnS₂异质纳米片发生了不可逆的晶体相变. 部分1T’-MoS₂和SnS₂与N₂发生电化学反应形成Mo‒N和Sn‒N键, 不可逆地相转变为Mo₂N和Sn_xN_z; 部分SnS₂由于电化学体系中电源的还原作用而不可逆地演化为SnS. 本文为优化TMDCs的制备方法及其电催化活性提供了新的设计思路.

关键词: MoS₂, SnS₂, 聚1-乙烯基-3-磺酸丙基咪唑盐功能化的聚吡咯/氧化石墨烯, 氮还原反应, 不可逆晶体相变

Abstract:

Unique MoS₂-SnS₂ heterogeneous nanoplates have successfully in-situ grown on poly(3-(1-vinylimidazolium-3-yl)propane-1-sulfonate) functionalized polypyrrole/ graphene oxide (PVIPS/PPy/GO). PVIPS can attract heptamolybdate ion (Mo₇O₂₄^6-) and Sn⁴⁺ as the precursors by the ion-exchange, resulting in the simultaneous growth of 1T’-MoS₂ and the berndtite-2T-type hexagonal SnS₂ by the interfacial induced effect of PVIPS. The obtained MoS₂-SnS₂/ PVIPS/PPy/GO can serve as electrocatalysts, exhibiting good NRR performance by the synergistic effect. The semi-conducting SnS₂ would limit the surface electron accessibility for suppressing HER process of 1T’-MoS₂, while metallic 1T’-MoS₂ might efficiently improve the NRR electroactivity of SnS₂ by the creation of Mo-Sn-Sn trimer catalytic sites. Otherwise, the irreversible crystal phase transition has taken place during the NRR process. Partial 1T’-MoS₂ and SnS₂ have electrochemically reacted with N₂, and irreversibly converted into Mo₂N and Sn_xN_z due to the formation of Mo-N and Sn-N bonding, meanwhile, partial SnS₂ has been irreversibly evolved into SnS due to the reduction by the power source in the electrochemical system. It would put forward a new design idea for optimizing the preparation method and electrocatalytic activity of transition metal dichalcogenides.

Key words: MoS₂, SnS₂, Poly(3-(1-vinylimidazolium-3-yl)propane-1-sulfonate), functionalized polypyrrole/graphene oxide, Nitrogen reduction reaction, Irreversible crystal phase transition

茆卉, 杨浩然, 柳金池, 张帅, 刘大亮, 吴琼, 孙文平, 宋溪明, 马天翼. 基于聚(两性离子液体)功能化聚吡咯/氧化石墨烯的独特MoS₂-SnS₂异质纳米片及其改善的氮还原电活性[J]. 催化学报, 2022, 43(5): 1341-1350.

Hui Mao, Haoran Yang, Jinchi Liu, Shuai Zhang, Daliang Liu, Qiong Wu, Wenping Sun, Xi-Ming Song, Tianyi Ma. Improved nitrogen reduction electroactivity by unique MoS₂-SnS₂ heterogeneous nanoplates supported on poly(zwitterionic liquids) functionalized polypyrrole/graphene oxide[J]. Chinese Journal of Catalysis, 2022, 43(5): 1341-1350.

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图/表 8

Fig. 1. XRD patterns (a), EDS spectra (b), survey (c), Mo 3d (d), Sn 3d (e), and S 2p (f) XPS spectra of MoS2/PVIPS/PPy/GO (1), SnS2/PVIPS/PPy/GO (2), and MoS2-SnS2/PVIPS/PPy/GO (3).

Fig. 2. SEM (a), TEM (b), HRTEM (c), the SAED pattern (d) and high-angle annular dark field image (e) of MoS2-SnS2/PVIPS/PPy/GO, with the corresponding elemental mapping of C, N, O, Mo, Sn, S.

Fig. 3. The NH3 yield and FE of MoS2/PVIPS/PPy/GO (a), SnS2/PVIPS/PPy/GO (b), MoS2-SnS2/PVIPS/PPy/GO (c) for NRR under electrolysis for 2 h in 0.1 mol/L Na2SO4 at different potentials (vs. RHE); (d) The NH3 yield and FE obtained by different electrocatalysts at ?0.5 V (vs. RHE) under electrolysis for 2 h in 0.1 mol/L Na2SO4: (1) MoS2-SnS2, (2) MoS2-SnS2/GO, (3) MoS2-SnS2/PPy/GO, (4) MoS2/PVIPS/PPy/GO, (5) SnS2/PVIPS/PPy/GO and (6) MoS2-SnS2/PVIPS/PPy/GO.

Table 1 Different electrocatalysts synthesized by different supporters with their Mo and Sn content determined by ICP and calculated MoS2+SnS2 loading content.

Electrocatalyst	Mo content by ICP (wt%)	Sn content by ICP (wt%)	MoS₂+SnS₂ loading (wt%)
MoS₂-SnS₂	—	—	100.00
MoS₂-SnS₂/GO	7.97	13.22	33.63
MoS₂-SnS₂/PPy/GO	5.75	5.21	17.59
MoS₂/PVIPS/PPy/GO	17.46	0	29.10
SnS₂/PVIPS/PPy/GO	0	7.51	11.56
MoS₂-SnS₂/PVIPS/PPy/GO	5.16	6.03	17.88

Fig. 4. (a) Linear sweep voltammograms of MoS2-SnS2/PVIPS/PPy/GO under saturated Ar and N2 in 0.1 mol/L Na2SO4; (b) The NH3 yield and FE of MoS2-SnS2/PVIPS/PPy/GO with alternating 2 h cycles at ?0.5 V between Ar and N2 atmosphere; (c) Recycling test for MoS2-SnS2/PVIPS/PPy/GO at ?0.5 V under electrolysis for 2 h performed six times; (d) XRD patterns of MoS2-SnS2/PVIPS/PPy/GO before (1) and after (2) NRR for 30 h.

Fig. 5. SEM (a), TEM (b), HRTEM (c), the SAED pattern (d) and high-angle annular dark field image (e) of MoS2-SnS2/PVIPS/PPy/GO after NRR for 30 h, with the corresponding elemental mapping of C, N, O, Mo, Sn, S.

Fig. 6. XPS spectra of MoS2-SnS2/PVIPS/PPy/GO before (1) and after (2) electrocatalysis, performed by chronoamperometry for 30 h under saturated N2 in 0.1 mol/L Na2SO4. (a) C 1s; (b) O 1s; (c) N 1s; (d) Mo 3d; (e) Sn 3d; (f) S 2p.

Scheme 1. The irreversible crystal phase transition of MoS2-SnS2 heterogeneous nanoplates with the corresponding electrode reactions on MoS2-SnS2/PVIPS/PPy/GO in 0.1 mol/L Na2SO4 solution containing saturated N2.

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基于聚(两性离子液体)功能化聚吡咯/氧化石墨烯的独特MoS₂-SnS₂异质纳米片及其改善的氮还原电活性

Improved nitrogen reduction electroactivity by unique MoS₂-SnS₂ heterogeneous nanoplates supported on poly(zwitterionic liquids) functionalized polypyrrole/graphene oxide

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