钙钛矿介导强化的铁基氧载体脱合金-脱溶循环及其太阳能热化学CO2裂解性能

doi:10.1016/S1872-2067(21)63857-3

催化学报 ›› 2021, Vol. 42 ›› Issue (11): 2049-2058.DOI: 10.1016/S1872-2067(21)63857-3

钙钛矿介导强化的铁基氧载体脱合金-脱溶循环及其太阳能热化学CO₂裂解性能

胡月^a^,^b,†, 吴坚^a^,^c,†, 韩宇佳^a^,^b,†, 徐维斌^a^,^b, 张立^a, 夏雪^a^,^c, 黄传德^a^,^#(), 朱燕燕^c, 田鸣^a, 苏杨^a, 李林^a, 侯宝林^a, 林坚^a, 刘汶^d^,^$(), 王晓东^a^,^*()

^a中国科学院大连化学物理研究所, 中国科学院应用催化科技重点实验室, 辽宁大连116023, 中国
^b中国科学院大学, 北京100049, 中国
^c西北大学化工学院, 陕西西安710069, 中国
^d南洋理工大学化学与生物医药工程学院, 新加坡

收稿日期:2021-04-19 修回日期:2021-04-19 接受日期:2021-06-03 出版日期:2021-11-18 发布日期:2021-06-09
通讯作者: 黄传德,刘汶,王晓东
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(21706254);国家自然科学基金(21676269);国家自然科学基金(21676266);国家自然科学基金(21878283);国家自然科学基金(21978239);国家自然科学基金(22022814);中国科学院先导专项(XDB17020100);大连化学物理研究所基金(DICP I201916);中国科学院科学研究基金(CXJJ-20S034);国家重点研发项目(2016YFA0202-801)

Intensified solar thermochemical CO₂ splitting over iron-based redox materials via perovskite-mediated dealloying-exsolution cycles

Yue Hu^a^,^b,†, Jian Wu^a^,^c,†, Yujia Han^a^,^b,†, Weibin Xu^a^,^b, Li Zhang^a, Xue Xia^a^,^c, Chuande Huang^a^,^#(), Yanyan Zhu^c, Ming Tian^a, Yang Su^a, Lin Li^a, Baolin Hou^a, Jian Lin^a, Wen Liu^d^,^$(), Xiaodong Wang^a^,^*()

^aCAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cCollege of Chemical Engineering, Northwest University, Xi’an 710069, Shannxi, China
^dSchool of Chemical and Biomedical Engineering, Nanyang Technological University 637459, Singapore

Received:2021-04-19 Revised:2021-04-19 Accepted:2021-06-03 Online:2021-11-18 Published:2021-06-09
Contact: Chuande Huang,Wen Liu,Xiaodong Wang
About author:^$E-mail: wenliu@ntu.edu.sg
^#E-mail: huangchuande@dicp.ac.cn;
^*E-mail: xdwang@dicp.ac.cn;
First author contact:^†These authors contributed equally.
Supported by:
National Natural Science Foundation of China(21706254);National Natural Science Foundation of China(21676269);National Natural Science Foundation of China(21676266);National Natural Science Foundation of China(21878283);National Natural Science Foundation of China(21978239);National Natural Science Foundation of China(22022814);Strategic Priority Research Program of the Chinese Academy of Sciences(XDB17020100);Dalian Institute of Chemical Physics, CAS(DICP I201916);Scientific Research Foundation of Chinese Academy of Sciences(CXJJ-20S034);National Key R&D Program of China(2016YFA0202-801)

摘要/Abstract

摘要：

大气中CO₂含量的增加已对气候和环境造成巨大影响, 要实现碳中和的目标, 目前迫切需要开发CO₂高效利用技术. 太阳能热化学循环CO₂裂解可充分利用太阳全光谱能量将CO₂转化为CO, 从而实现太阳能到化学能的存储. 进一步引入CH₄作为氧载体的还原气体, 不仅能有效降低反应温度、提高氧载体供氧能力, 还能联产高质量合成气, 为生产甲醇和乙酸及费托合成提供原料, 达到一举多得的效果. 铁基材料因其成本低、环境友好等优点受到广泛关注, 但普通铁氧化物(如Fe₃O₄, FeO)催化甲烷活化性能差, 且受热力学限制, CO₂分解转化率较低.
本文制备了一种FeNi合金修饰的钙钛矿复合材料为氧载体(FeNi-LFA), 其在两步法太阳能热化学CO₂裂解反应中展现出较好的反应活性和循环稳定性. 在反应温度为850^oC时, CO₂分解速率达到381 mL g^‒1 min^‒1(STP), 转化率达到99%, 氧化后材料可在恒温条件下经甲烷还原再生, 合成气收率达96%以上, 30次循环性能无明显下降. 本文还结合高分辨透射电子显微镜(HRTEM), 原位X射线衍射(XRD), 原位扫描透射电镜(STEM)和⁵⁷Fe穆斯堡尔谱等表征深入研究了热化学循环反应中氧载体的结构演变, 并借助密度泛函理论(DFT)计算, 研究其构效关系.
HRTEM及EDS结果表明, FeNi-LFA中FeNi合金颗粒尺寸为20~50 nm, 且合金颗粒部分嵌入到钙钛矿基体中, 从而显著增强了金属-载体间相互作用. 为了研究FeNi-LFA氧载体动态构造演化过程, 采用XRD对氧载体反应中衍射峰变化进行研究. 当FeNi-LFA暴露于CO₂中, FeNi合金的特征衍射峰向高角度偏移, 同时, La₂O₃衍射峰减弱. 钙钛矿衍射峰增强, 说明氧化气氛中, FeNi合金发生Fe脱合金过程, 而氧化后的铁离子能与La₂O₃快速反应生成钙钛矿氧化物. 当反应气氛切换成CH₄后, 钙钛矿衍射峰强度降低, La₂O₃信号相应增强, 说明钙钛矿中铁离子脱溶析出, 使材料在恒温条件下完成再生. 进一步利用STEM对FeNi-LFA的结构演变中的元素迁移进行研究发现, 新鲜样品中, FeNi合金与钙钛矿载体接触密切, FeNi合金周围仅有少量铁分布, 在FeNi合金与氧化物载体的界面处, Fe信号强度有所下降, 表明FeNi合金嵌入在富含La₂O₃的钙钛矿载体中, 这与HRTEM表征结果一致. 在CO₂裂解过程中, FeNi合金中的Fe信号明显降低, 并出现金属Ni颗粒, 说明Fe原子从合金中脱出. 此外, 在Ni颗粒表面没有出现FeO_x等钝化层, 说明氧化后的Fe可与载体快速反应, 抑制了钝化层的形成, 从而有利于提高CO₂裂解转化率. 相应⁵⁷Fe穆斯堡尔谱结果表明, FeNi合金中的Fe与La₂O₃反应转化为LaFeO₃, 与XRD结果一致. 对反应过程进行DFT计算, 发现FeNi/La₂O₃界面很容易发生CO₂吸附和活化, 其反应活性远高于FeNi合金. 同样地, 氧化后形成的Ni/LaFeO₃(110)界面有利于CH₄吸附和C‒H键解离, 有利于Fe离子还原和FeNi合金再生. 两步法太阳能热化学CO₂裂解工艺经济可行性的一个关键指标是太阳能利用效率, 热力学分析结果表明, 即使在没有热回收的情况下, 该过程的理论太阳能利用效率可达58%, 当显热回收效率为90%时, 太阳能利用效率可达78%.
综上, 本文发展了一种新型高效CO₂热化学裂解氧载体, 实现铁在钙钛矿-合金中的定向可逆迁移, 通过勒沙特列原理显著提高了CO₂分解转化率及反应活性, 同时可产生高质量合成气. 通过构建复合氧载体, 实现Fe离子的原位稳定作为一种新型的氧载体设计策略, 可推广应用至其他氧载体的设计开发, 从而有效提高太阳能燃料生产效率.

关键词: CO₂裂解, FeNi合金, 钙钛矿, 甲烷, 太阳能利用效率

Abstract:

Solar thermochemical CO₂-splitting (STCS) is a promising solution for solar energy harvesting and storage. However, practical solar fuel production by utilizing earth-abundant iron/iron oxides remains a great challenge because of the formation of passivation layers, resulting in slow reaction kinetics and limited CO₂ conversion. Here, we report a novel material consisting of an iron-nickel alloy embedded in a perovskite substrate for intensified CO production via a two-step STCS process. The novel material achieved an unprecedented CO production rate of 381 mL g^-1 min^-1 with 99% CO₂ conversion at 850 °C, outperforming state-of-the-art materials. In situ structural analyses and density functional theory calculations show that the alloy/substrate interface is the main active site for CO₂ splitting. Preferential oxidation of the FeNi alloy at the interface (as opposed to forming an FeO_x passivation shell encapsulating bare metallic iron) and rapid stabilization of the iron oxide species by the robust perovskite matrix significantly promoted the conversion of CO₂ to CO. Facile regeneration of the alloy/perovskite interfaces was realized by isothermal methane reduction with simultaneous production of syngas (H₂/CO = 2, syngas yield > 96%). Overall, the novel perovskite-mediated dealloying-exsolution redox system facilitates highly efficient solar fuel production, with a theoretical solar-to-fuel efficiency of up to 58%, in the absence of any heat integration.

Key words: CO₂ splitting, Iron-nickel alloy, Perovskite, Methane, Solar-to-fuel efficiency

胡月, 吴坚, 韩宇佳, 徐维斌, 张立, 夏雪, 黄传德, 朱燕燕, 田鸣, 苏杨, 李林, 侯宝林, 林坚, 刘汶, 王晓东. 钙钛矿介导强化的铁基氧载体脱合金-脱溶循环及其太阳能热化学CO₂裂解性能[J]. 催化学报, 2021, 42(11): 2049-2058.

Yue Hu, Jian Wu, Yujia Han, Weibin Xu, Li Zhang, Xue Xia, Chuande Huang, Yanyan Zhu, Ming Tian, Yang Su, Lin Li, Baolin Hou, Jian Lin, Wen Liu, Xiaodong Wang. Intensified solar thermochemical CO₂ splitting over iron-based redox materials via perovskite-mediated dealloying-exsolution cycles[J]. Chinese Journal of Catalysis, 2021, 42(11): 2049-2058.

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图/表 8

Fig. 1. Schematic of CO2 splitting process. (a) Traditional two-step STCS process with temperature swing; (b) isothermal two-step STCS process utilizing CH4 as reducing gas; (c) CO2 splitting over metallic Fe induces formation of FeOx passivation layer. Note: ox and red are abbreviations for oxidation and reduction; Tred and Tox represent the reduction and oxidation temperature.

Fig. 2. Local structure and elemental distribution analysis. (a) HRTEM image of a typical particle of FeNi-LFA catalyst. (b) Enlarged view of zone 1 in image (a). La (c), Ni (d), Fe (e), Al (f) and O (g) EDS maps of the same region of image (a). (h) EDS line-scan taken across the particle, as indicated by red dashed arrow in image (a). White dashed circles in (c) represent the areas with relatively low concentration of La.

Fig. 3. CO2 splitting performance. Gas composition during CO2 pulse reaction over FeNi-LFA (a) and corresponding CO2 conversion and CO yield in the reaction (b). (c) Transient CO evolution rate during CO2 splitting half-cycle of two-step STCS process. Pulse reaction conditions: 64 μmol CO2 g-1 of FeNi-LFA was injected in each pulse reaction at 850 °C. STCS reaction conditions: 385 mL CO2 min-1 g-1 (STP) of FeNi-LFA at 850 °C during CO2 splitting half-cycle. The dashed line in (c) gives the average CO productivity during 10 sequential redox cycles.

Fig. 4. CO2 splitting and methane partial oxidation performance over FeNi-LFA under optimized redox conditions. Reaction conditions: 850 °C, total flow = 150 mL min-1 g-1, PCO2 = 0.05, PCH4 = 0.05.

Fig. 5. In-situ structural analysis. (a) In situ XRD measurement under CO2 and CH4 atmosphere at 850 °C. (b1-b6) Representative HAADF image of fresh FeNi-LFA and corresponding element maps of Fe, Ni, La, O and Al. (b7) Line-scan results along the red dashed arrow in image (b1). (c1-c6) HAADF image of FeNi-LFA after CO2 treatment at 850 °C and corresponding element maps of Fe, Ni, La, O and Al. (c7) Line-scan results along the red dashed arrow in image (c1). White dashed area in (b2) contains relatively low iron concentration. White dash arrowed and area in (c2) show the iron migration direction.

Fig. 6. Structural analysis of FeNi-LFA after CO2 splitting. (a) Room temperature 57Fe Mössbauer spectra. The spectrum of LaFeO3 is added as a reference. Representative HAADF image (b1) and corresponding element maps of La (b2), Fe (b3), Ni (b4), Al (b5) and O (b6). White dashed areas in (b2) and (b3) show the LaFeO3 layer.

Fig. 7. Schematic of heat flows for the two-step solar thermochemical CO2 splitting. Note: T0 is ambient temperature and TR is the reaction temperature.

Fig. 8. DFT calculation results. (a) CO2 splitting (CO2 (g) → CO*+O*) on FeNi alloy and FeNi/La2O3 interface, (b) CH4 dissociation (CH4 (g) → CH3*+H*) on Ni and Ni/LaFeO3 interface. Inset: top views of the reaction intermediates: Ni (green), La (blue), Fe (purple), O of redox material (red), C (gray), O of CO2 (pink), and H (orange).

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钙钛矿介导强化的铁基氧载体脱合金-脱溶循环及其太阳能热化学CO₂裂解性能

Intensified solar thermochemical CO₂ splitting over iron-based redox materials via perovskite-mediated dealloying-exsolution cycles

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