重塑位于火山曲线右支的弱吸附金属单原子位点的配位环境及电子结构

doi:10.1016/S1872-2067(23)64460-2

催化学报 ›› 2023, Vol. 50: 352-360.DOI: 10.1016/S1872-2067(23)64460-2

重塑位于火山曲线右支的弱吸附金属单原子位点的配位环境及电子结构

贡立圆^a^,^b^,^c^,¹, 王颖^d^,¹, 刘杰^a^,^b^,^c^,¹, 王显^a^,^b^,^c, 李阳^a^,^b^,^c, 侯帅^a^,^c, 武志坚^d, 金钊^a^,^c^,^*(), 刘长鹏^a^,^b^,^c, 邢巍^a^,^b^,^c^,^*(), 葛君杰^a^,^b^,^e^,^*()

^a中国科学院长春应用化学研究所, 吉林省低碳化学电源重点实验室, 电分析化学国家重点实验室, 吉林长春 130022
^b中国科学技术大学, 安徽合肥 230026
^c中国科学院长春应用化学研究所, 先进电源实验室, 吉林长春 130022
^d中国科学院长春应用化学研究所, 稀土资源利用国家重点实验室, 吉林长春 130022
^e中国科学院洁净能源创新研究院, 辽宁大连 116023

收稿日期:2023-04-05 接受日期:2023-05-08 出版日期:2023-07-18 发布日期:2023-07-25
通讯作者: *电子信箱: zjin@ciac.ac.cn (金钊), xingwei@ciac.ac.cn (邢巍), gejunjie@ustc.edu.cn (葛君杰).
作者简介:
¹共同第一作者.
基金资助:
国家重点研发计划(2022YFB4004100);国家自然科学基金(21875243);国家自然科学基金(21733004);中国科学院科技服务网络倡议(KFJ-STS-ZDTP-088);吉林省科技开发项目(20190201270JC);吉林省科技开发项目(20190201300JC);吉林省科技开发项目(20200201001JC);中央财政引导地方科技发展专项资金(2020JH6/10500021);中国科学院洁净能源国家实验室研究创新基金(DNL202010)

Reshaping the coordination and electronic structure of single atom sites on the right branch of ORR volcano plot

Liyuan Gong^a^,^b^,^c^,¹, Ying Wang^d^,¹, Jie Liu^a^,^b^,^c^,¹, Xian Wang^a^,^b^,^c, Yang Li^a^,^b^,^c, Shuai Hou^a^,^c, Zhijian Wu^d, Zhao Jin^a^,^c^,^*(), Changpeng Liu^a^,^b^,^c, Wei Xing^a^,^b^,^c^,^*(), Junjie Ge^a^,^b^,^e^,^*()

^aState Key Laboratory of Electroanalytical Chemistry, Jilin Province Key Laboratory of Low Carbon Chemical Power Sources, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, Jilin, China
^bUniversity of Science and Technology of China, Hefei 230026, Anhui, China
^cLaboratory of Advanced Power Sources, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, Jilin, China
^dState Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, Jilin, China
^eDalian National Laboratory for Clean Energy, Dalian 116023, Liaoning, China

Received:2023-04-05 Accepted:2023-05-08 Online:2023-07-18 Published:2023-07-25
Contact: *E-mail: zjin@ciac.ac.cn (Z. Jin), xingwei@ciac.ac.cn (W. Xing), gejunjie@ustc.edu.cn (J. Ge).
About author:
¹ Contributed to this work equally.
Supported by:
National Key R&D Program of China(2022YFB4004100);National Natural Science Foundation of China(21875243);National Natural Science Foundation of China(21733004);Science and Technology Service Network Initiative of CAS(KFJ-STS-ZDTP-088);Jilin Province Science and Technology Development Program(20190201270JC);Jilin Province Science and Technology Development Program(20190201300JC);Jilin Province Science and Technology Development Program(20200201001JC);Special Funds for Guiding Local Scientific and Technological Development by the Central Government(2020JH6/10500021);Dalian National Laboratory for Clean Energy (DNL), CAS, the Research Innovation Fund(DNL202010)

摘要/Abstract

摘要：

金属单原子位点独特的电子结构使其在燃料电池阴极氧还原催化反应(ORR)的应用引起广泛兴趣. 金属单原子中心作为催化剂的活性位点遵循Sabatier原则, 即位于火山型曲线右侧的金属中心与ORR中间产物的结合能力弱, 使中间产物难以被位点活化, 与之相反, 左侧的位点则与中间产物的结合力太强, 使中间产物难以脱附. 因此, 构建中间产物结合强度适中的位点可以提高催化剂活性. 研究表明, 通过改变金属中心的配位环境可以调控金属的电子结构, 进而调节对ORR中间产物的吸附能力, 提高催化剂活性. 例如, 对于位于火山曲线左侧的FeN₄位点, 通过在配位原子中引入高电负性的基团, 如OH, S, Cl, 减弱其对ORR中间产物的结合强度, 使其活性向右侧活性顶点移动. 然而, 目前还没有提出有效的策略来改善火山曲线右侧位点的弱吸附能力. 例如, Pd和Pt的纳米催化剂具有较高的ORR活性, 而其单原子MN₄位点却对ORR呈惰性, 原因为高电负性的N使M具有较高的电荷密度, 使其对中间产物的吸附能力太弱而位于火山曲线的最右边, 具有较差的本征活性. 为了缓解此类金属与配位N之间的不匹配的问题, 我们提出通过利用电负性低的C (χ_p = 2.55)代替N (χ_p= 3.04)配位, 以提升弱吸附位点的本征活性.

本文制备了Ir-N-C, Pd-N-C, Pt-N-C, Ir-C, Pd-C和Pt-C六种催化剂; X射线衍射、透射电极和球差电镜结果表明, 催化剂不含金属颗粒; 同步辐射结果表明, 催化剂呈M-N/C配位形式存在, 且价态为氧化态. 飞行时间二次离子质谱法(ToF-SIMS)测试可以检测到MN_XC_Y和MC_X的位点结构, 结合同步辐射结果, 认为活性位点分别是IrN_XC_(4‒_X₎, IrC₄, PdN₂C_X和PdN₃C_X, PdC₄, PtN₃C₁和PtN₄, PtC₄. 电化学结果表明, 相比N配位的催化剂, C配位的催化剂具有更高的半波电位、起始电位及本征活性, 表明C配位更适合配位金属Ir, Pd和Pt, 证明本文策略的可行性.

为了进一步研究催化活性提升的原因, 本文采用密度泛函理论计算探究催化机理, 根据实验结果(X射线吸附光谱和ToF-SIMS)模拟了催化剂的活性位点结构, 并计算反应中间产物的吸附能ΔG_OH*. 将ΔG_OH*作为横坐标, 反应的起始电位即催化活性作为纵坐标, 绘制图谱得到火山型曲线. 结果表明, 相比N配位的金属位点, C配位的金属位点向强吸附端移动并靠近活性顶点, 与实验结果一致, 说明催化活性的提升是因为配位环境的改变改善了位点吸附能力. 随后, 通过计算活性位点的Bader电荷密度探究配位环境对电子结构的调控. 结果显示, 低电负性的C由于吸电子能力弱于高电负性的N, 使MC_X位点具有较低的Bader电荷密度, 从而具有较强的中间产物吸附能力, 进而提高催化活性. 综上, 本文提出了一个普遍性的原则, 通过利用低电负性的元素配位调节具有弱结合能的金属(不仅是Ir, Pd, Pt)位点活性, 为不同性质的金属匹配合适的配位环境, 以实现高催化活性.

关键词: 氧还原反应, 单原子催化剂, 配位环境, 电子结构, 反应中间产物吸附能

Abstract:

The coordination environment of atomic metal sites in single atom catalysts is of vital significance in tailoring the d-orbital states and thus the catalytic behavior towards oxygen reduction reaction (ORR), thereby offering great promise to boost activity via regulating the local chelation structure. Herein we designed a carbon coordination environment for the atomic M sites reside on the right leg of the volcano plot, to effectively counter balance the low adsorption energy of the metal center to oxygen species. Combining time-of-flight secondary ion mass spectrometry and density functional theory calculations, we unveiled the M-C coordination structure and the thus induced changes in electronic structure and ORR catalytic behavior. The reshape in coordination structure, i.e., the replacement of typical nitrogen coordination by low electronegativity carbon coordination, gives rise to exceptional intrinsic activity towards ORR. This work brings a new perspective to boost the activity of single atom catalysts on the weak bonding leg, with exceptional ORR activity being further expected through advancing the chelation structure.

Key words: Oxygen reduction reaction, Single atom catalyst, Coordination environment, Electronic structure, Adsorption energy of reaction intermediate

贡立圆, 王颖, 刘杰, 王显, 李阳, 侯帅, 武志坚, 金钊, 刘长鹏, 邢巍, 葛君杰. 重塑位于火山曲线右支的弱吸附金属单原子位点的配位环境及电子结构[J]. 催化学报, 2023, 50: 352-360.

Liyuan Gong, Ying Wang, Jie Liu, Xian Wang, Yang Li, Shuai Hou, Zhijian Wu, Zhao Jin, Changpeng Liu, Wei Xing, Junjie Ge. Reshaping the coordination and electronic structure of single atom sites on the right branch of ORR volcano plot[J]. Chinese Journal of Catalysis, 2023, 50: 352-360.

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https://www.cjcatal.com/CN/Y2023/V50/I7/352

图/表 5

Fig. 1. (a) Synthetic scheme for the preparation of M-C and M-N-C samples; the HAADF-STEM image of Ir-N-C (b), Ir-C (c), Pd-N-C (d), Pd-C (e), Pt-N-C (f), and Pt-C (g).

Fig. 2. EXAFS and XANES spectra of Ir-N-C (a,b), Pd-N-C (c,d), Pt-N-C (e,f), Ir-C (g,h), Pd-C (i,j) and Pt-C (k,l) and reference samples.

Fig. 3. Characteristic fragment of varied catalysts detected by ToF-SIMS. IrN4 (a), IrC4 (b), PdN2 (c) of M-N-C catalysts, and PdC4 (d), PtN4 (e), PtC4 (f) of M-C catalysts.

Fig. 4. (a) The LSV curves of Ir SACs. (b) Comparison of E1/2 of Ir based catalysts. (c) The LSV curves of Pd SACs catalysts. (d) Comparison of the Eonset of Pd SACs. (e) The LSV curves of Pt SACs. (f) Comparison of the Eonset of Pt SACs. RDE and RRDE measurements were conducted by CV in 0.1 -1.1 V at a scan rate of 10 mV s-1 at 1600 r min-1 in O2 saturated 0.1 mol L-1 HClO4.

Fig. 5. (a-c) Gibbs free energy diagrams on various sites. (d-f) ORR theoretical onset potential (fitting) versus ΔGOH* on various sites. (g-i) ΔGOH* and ORR theoretical onset potential (exact) versus Bader charge for various sites. The blue symbols are corresponding to ΔGOH* and the red symbols correspond to theoretical onset potential. The circular symbols represent the MCX site and the star symbols represent the MNX site. The insert picture is charge density difference, cyan and yellow areas represent charge density increase and decrease, respectively.

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重塑位于火山曲线右支的弱吸附金属单原子位点的配位环境及电子结构

Reshaping the coordination and electronic structure of single atom sites on the right branch of ORR volcano plot

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