“自上而下”构筑TiO2与Pt纳米簇之间的活性界面I: 再分散过程和机制

doi:10.1016/S1872-2067(23)64597-8

催化学报 ›› 2024, Vol. 58: 237-246.DOI: 10.1016/S1872-2067(23)64597-8

“自上而下”构筑TiO₂与Pt纳米簇之间的活性界面I: 再分散过程和机制

杜晓蕊^a^,^b^,¹, 黄一珂^a^,^c^,¹, 潘晓丽^a, 江训柱^a^,^d, 苏杨^a, 杨静怡^a, 郭亚琳^a^,^e, 韩冰^a^,^f, 文承彦^b, 王晨光^b^,^g,*(), 乔波涛^a^,^d,*()

^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
^b中国科学院广州能源研究所, 广东广州510640
^c北京科学智能研究院, 北京100000
^d中国科学院大学, 北京100049
^e重庆大学化学化工学院, 多尺度多孔材料研究中心, 重庆400044
^f中国石化大连石油化工研究院, 辽宁大连116023
^g中国科学院可再生能源重点实验室, 广东广州510640

收稿日期:2023-12-09 接受日期:2024-01-04 出版日期:2024-03-18 发布日期:2024-03-28
通讯作者: *电子信箱: bqiao@dicp.ac.cn (乔波涛),wangcg@ms.giec.ac.cn (王晨光).
作者简介:¹共同第一作者.
基金资助:
中国科学院稳定支持基础研究领域青年团队计划(YSBR-022);中国科学院稳定支持基础研究领域青年团队计划(YSBR-044);国家自然科学基金(22309185);国家重点研发计划项目(2021YFA1500503);辽宁省自由探索基金(2023020351-JH6/1005);国家自然科学基金中日合作交流项目(21961142006);国家自然科学基金单原子催化基础研究中心(22388102)

Top-down fabrication of active interface between TiO₂ and Pt nanoclusters. Part 1: Redispersion process and mechanism

Xiaorui Du^a^,^b^,¹, Yike Huang^a^,^c^,¹, Xiaoli Pan^a, Xunzhu Jiang^a^,^d, Yang Su^a, Jingyi Yang^a, Yalin Guo^a^,^e, Bing Han^a^,^f, Chengyan Wen^b, Chenguang Wang^b^,^g,*(), Botao Qiao^a^,^d,*()

^aCAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bGuangzhou Institute of Energy Conversion, Chinese Academy of Sciences, Guangzhou 510640, Guangdong, China
^cArtificial Intelligence for Science Institute, Beijing 100000, China
^dUniversity of Chinese Academy of Sciences, Beijing 100049, China
^eMulti-scale Porous Materials Center, Institute of Advanced Interdisciplinary Studies, School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China
^fSINOPEC Dalian Research Institute of Petroleum and Petrochemicals Co., Ltd. Dalian 116023, Liaoning, China
^gCAS Key Laboratory of Renewable Energy, Guangzhou Institute of Energy Conversion, Chinese Academy of Science, Guangzhou 510640, Guangdong, China

Received:2023-12-09 Accepted:2024-01-04 Online:2024-03-18 Published:2024-03-28
Contact: *E-mail: bqiao@dicp.ac.cn (B Qiao),wangcg@ms.giec.ac.cn (C. Wang).
About author:¹ Contributed equally to this work.
Supported by:
CAS Project for Young Scientists in Basic Research(YSBR-022);CAS Project for Young Scientists in Basic Research(YSBR-044);National Natural Science Foundation of China(22309185);National Key Project for Fundamental Research and Development of China(2021YFA1500503);Liaoning Province Free Exploration Fund(2023020351-JH6/1005);Natural Science Foundation of China and Japan Society for the Promotion of Science Cooperative Research Project(21961142006);National Natural Science Foundation of China(22388102)

摘要/Abstract

摘要：

负载型金属催化剂广泛应用于现代化学化工过程, 其中, 金属颗粒的尺寸通常对催化性能起着至关重要的作用. 尤其是, 那些粒径低于2 nm的高分散金属纳米簇, 不仅具有接近单原子催化剂的原子利用效率, 而且展现出协同活化底物的能力. 这使得它们在特定反应中能够兼具单原子和纳米催化剂的优势, 并逐渐受到关注. 然而, 制备高稳定负载型纳米簇催化剂仍然是一项挑战. 传统的“自下而上”制备策略存在成本高、产率低以及复杂配体难以去除等问题. 近年来, 通过“自上而下”的方法将金属纳米颗粒等聚集体再分散为单原子已经成为一种较普遍的单原子催化剂制备方法, 但利用类似策略合成纳米簇催化剂的报道较少.

本文通过对TiO₂负载的铂纳米颗粒或PtO₂粉末进行简单的煅烧, 成功制备了高分散且热稳定的铂纳米簇, 并通过系统表征和密度泛函理论(DFT)模拟深入研究了这一再分散过程和机制. 首先, 使用胶体沉淀法合成了TiO₂负载的铂纳米颗粒催化剂. 在400 °C空气中焙烧除去除保护剂后, 铂纳米颗粒平均粒径为3.4 nm. 然而, 当焙烧温度升高至550 °C时, Pt纳米颗粒消失, 转化为高度分散的纳米簇, 平均粒径约为1 nm. X射线光电子能谱和X射线吸收近边结构结果表明, 再分散后铂的价态从金属态转变为+4价为主的氧化态; 扩展X射线吸收精细结构的拟合结果进一步证实了再分散后铂的高价态和小尺寸. 值得注意的是, 与大部分金属再分散均形成单原子分散物种不同, 本工作中铂在TiO₂载体上的再分散以纳米簇为最终物种. 为了解释纳米簇的形成, 详细研究了金属再分散过程. 通过对照试验, 排除了表面活性剂的作用, 并证实形成氧化铂物种在再分散过程中起关键作用. 通过DFT计算评估了可能的氧化铂中间体的化学势, 结果表明铂的氧化单体, 尤其是Pt₁(O₂)/r110和气态PtO₂(g), 具有更低的化学势, 使得纳米颗粒的分解更有可能发生. 进一步通过DFT模拟排除了以Pt₁(O₂)/r110为中间体的表面扩散机理, 并指出对于气相捕获机制, PtO₂(g)是最可能的气态中间体. 模拟结果表明, PtO₂(g)分子优先被V_Ti5c空位捕获并形成Pt_ion-r110位点; 该位点可诱导更多的PtO₂(g)单体在其上聚集, 从而生长为纳米簇; 在550 °C下焙烧时, 其尺寸稳定分布在1 nm左右.

综上, 本工作提出一种“自上而下”的制备策略, 通过金属颗粒在载体表面的再分散过程, 成功合成了负载纳米簇催化剂. 该制备方法简单可行, 易于放大, 为实现宏量制备提供了有效途径. 同时, 深入研究了再分散过程, 揭示了纳米簇物种形成的原因和机理, 为金属再分散现象提供了新的理解和认识.

关键词: 多相催化, 纳米簇, 再分散, 金属-氧化物界面, 一氧化碳氧化

Abstract:

Supported metal nanoclusters (NCs) are regarded as the next generation of catalyst that bridge the nanocatalyst and single-atom catalyst. However, feasible fabrication of thermally stable NCs has remained a daunting challenge. In this paper, the first part of an extended work, we report a simple route to fabricate Pt NCs in size of around 1 nm through redispersion of Pt nanoparticles (NPs) or commercial PtO₂ by a calcination treatment. Combining control experiments and detailed DFT simulation, the whole redispersion process was described and evidenced to proceed via a gas-phase trapping way: Under promotion of oxygen atmosphere and high temperature, volatile oxidized Pt monomers were firstly generated and then trapped by surface defects, forming special sites that preferentially induce the growth of clusters on them. The growing clusters have both size- and temperature-dependent stability, resulting a most stable size distribution of around 1 nm when fabricated at 550 °C. This work provides a feasible top-down strategy to fabricate highly dispersed metal clusters.

Key words: Heterogeneous catalysis, Nanocluster, Redispersion, Metal-oxide interface, CO oxidation

杜晓蕊, 黄一珂, 潘晓丽, 江训柱, 苏杨, 杨静怡, 郭亚琳, 韩冰, 文承彦, 王晨光, 乔波涛. “自上而下”构筑TiO₂与Pt纳米簇之间的活性界面I: 再分散过程和机制[J]. 催化学报, 2024, 58: 237-246.

Xiaorui Du, Yike Huang, Xiaoli Pan, Xunzhu Jiang, Yang Su, Jingyi Yang, Yalin Guo, Bing Han, Chengyan Wen, Chenguang Wang, Botao Qiao. Top-down fabrication of active interface between TiO₂ and Pt nanoclusters. Part 1: Redispersion process and mechanism[J]. Chinese Journal of Catalysis, 2024, 58: 237-246.

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图/表 8

Fig. 1. Representative HAADF-STEM images and corresponding Pt size distributions of Pt/TiO2 (a,b), Pt/TiO2-400 (c,d), and Pt/TiO2-550 (e?h).

Fig. 2. (a) Pt 4f XPS of samples; The binding energy positions for Pt 4f7/2 of Pt0, Pt2+, and Pt4+ are at 71, 72.5, and 74.7 eV, respectively. The green peak represents the Ti 3s energy loss. (b) XANES spectra of samples, with Pt foil and PtO2 as references. (c) Fourier transforms of k3-weighted EXAFS spectra of samples.

Table 1 EXAFS fitting parameters at the Pt L3-edge various samples.

Sample	Shell	CN ^a	R (Å) ^b	σ²×10³(Å²) ^c	R factor
Pt foil	Pt‒Pt	12	2.76±0.002	5.0±0.2	0.003
Pt/TiO₂	Pt‒O	1.1±0.4	2.02±0.02	4.3±2.7	0.006
Pt/TiO₂	Pt‒Pt	6.7±0.6	2.76±0.01	5.4±0.4	—
Pt/TiO₂-400	Pt‒O	2.6±0.4	2.00±0.01	3.8±1.2	0.012
Pt/TiO₂-400	Pt‒Pt	4.0±0.7	2.76±0.01	5.2±0.7	—
Pt/TiO₂-550	Pt‒O	5.8±0.4	1.99±0.01	1.4±0.4	0.007
	Pt‒Pt	2.1±1.2	3.10±0.04	15.7±6.1	—
	Pt‒Ti (O bridged)	5.7±1.4	3.56±0.02	3.1±1.2	—
PtO₂	Pt‒O	5.2±0.4	2.02±0.01	2.6±0.5	0.004
	Pt‒Pt	5.4±0.8	3.10±0.01	3.6±0.5	—
	Pt‒O_sec	6.2±3.4	3.79±0.04	20.7±6.9	—

Fig. 3. Representative HAADF-STEM images and corresponding Pt size distributions of Pt/TiO2-550-N2 (a,b), PtO2/TiO2-grind (c,d), and PtO2/TiO2-grind-550 (e?h). The Pt/TiO2-550-N2 sample was obtained by calcining Pt/TiO2 under N2 flow at 550 °C for 3 h.

Fig. 4. Explore Pt NP redispersion mechanism by evaluating chemical potentials of intermediates (monomers) and size-dependent chemical potentials of metallic and di-oxidized clusters on perfect r110. (a) Chemical potentials of several Pt species at 450, 550 and 650 °C; Pt1(O2)/r110, and PtO2 (g) denotes oxygen-adsorbed Pt single atom on r110 surface and gaseous PtO2 molecule, respectively. (b,c) Optimized structures of possible surface diffusion species Pt1/r110 and Pt1(O2)/r110. Color code: O, red, Pt, white, Ti, ice blue. (d) Size-dependent chemical potentials of metallic and di-oxidized Pt clusters at different temperatures.

Fig. 5. Redispersion Gibbs free energy change ΔG at different temperatures for nanoparticle with 3 nm projected diameter (see Fig. S10), contact angle 60° with support. Because total number of Pt atoms is constant during redispersion, the boundary marked with dash line obeys relationship NPt~1/γ. ΔG values of conditions exceeding boundary are set as zero for color reference. (a) 450 °C; (b) 550 °C; (c) 650 °C.

Fig. 6. Representative HAADF-STEM images and corresponding size distributions of Pt/TiO2-550-10h (a?d), and the samples obtained by calcining Pt/TiO2-550-10h again at 600 (e?h) and 650 °C (i?l) for 10 h under air flow, denoted as Pt/TiO2-550-600 and Pt/TiO2-550-650, respectively.

Fig. 7. Scheme of redispersion from Pt NP to Pt NC on TiO2. Color code: O, red, Pt, white, Ti, ice blue.

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“自上而下”构筑TiO₂与Pt纳米簇之间的活性界面I: 再分散过程和机制

Top-down fabrication of active interface between TiO₂ and Pt nanoclusters. Part 1: Redispersion process and mechanism

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