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

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

Chinese Journal of Catalysis ›› 2024, Vol. 58: 237-246.DOI: 10.1016/S1872-2067(23)64597-8

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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)

Abstract

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

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

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