Electronic enrichment on Ni atoms at Ni-CeO2 interfaces: Unraveling the catalytic role in CO methanation and its volcano-type relation with the CeO2 content

doi:10.1016/S1872-2067(25)64688-2

Abstract

Abstract:

Tuning the metal-oxide interface to achieve optimal catalytic performance represents a classic yet fast-growing area in catalysis research. This work demonstrated that the decoration of CeO₂ clusters onto Ni particles creates electron-enriched Ni sites at the Ni-CeO₂ interface with highly efficient CO methanation, by kinetics, chemical titration, and a series of in situ/operando spectroscopic characterizations. These electron-enriched Ni atoms facilitate the back-donation of electrons into the orbital of CO and thus reduce the reaction barrier of CH₄ formation, but do not alter the catalytic steps and their kinetic relevance as well as the evolution of surface intermediates during CO methanation. The amount of electron-enriched Ni atoms increases significantly to a maximum value and then decreases as the content of CeO₂ increases, leading the formation rates of CH₄ to increase in a volcano-type relation with CeO₂ contents in xCeNi/Al₂O₃ catalysts. These insights provide a comprehensive understanding of the nature and the role of the metal-oxide interface and could potentially guide the rational design of highly efficient oxide-supported catalysts for CO methanation.

Key words: CO methanation, Ni catalyst, Interfacial sites, Active sites, In-situ and operando spectroscopy

Xinli Li, Xiaonan Zhang, Zhenzhen Du, Feixue Han, Zhihui Fan, Shaokang Zhang, Zhenzhou Zhang, Weifeng Tu, Yi-Fan Han. Electronic enrichment on Ni atoms at Ni-CeO₂ interfaces: Unraveling the catalytic role in CO methanation and its volcano-type relation with the CeO₂ content[J]. Chinese Journal of Catalysis, 2025, 74: 177-190.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64688-2

https://www.cjcatal.com/EN/Y2025/V74/I7/177

Figures/Tables 12

Table 1 Physical properties of Ni/Al2O3 and xCeNi/Al2O3 catalysts.

Sample	Mole ratio^a Ce/(Ce+Ni)	BET surface areas^b (m² g^-1)	Mean Ni crystalline size ^c (nm)	Mean Ni particle size^d (nm)	Mean CeO₂ particle^d size (nm)	Dispersion of Ni^e (%)
Ni/Al₂O₃	—	203.7	13.1	13.2	—	7.6
0.01CeNi/Al₂O₃	0.013	244.9	14.1	—	—	7.1
0.02CeNi/Al₂O₃	0.022	225.4	15.4	—	—	6.5
0.05CeNi/Al₂O₃	0.038	229.7	15.1	14.9	3.1	6.6
0.07CeNi/Al₂O₃	0.071	224.1	15.2	—	—	6.6
0.10CeNi/Al₂O₃	0.091	205.3	14.1	15.5	4.4	7.1
0.13CeNi/Al₂O₃	0.123	189.0	14.2	15.8	5.2	7.0

Fig. 1. XRD patterns of xCeNi/Al2O3 catalysts (x = 0.00-0.13) after treated in H2/Ar (10 kPa H2 and 90 kPa Ar) at 873 K for 4 h.

Fig. 2. HRTEM images and particle size distribution of the reduced Ni/Al2O3 (a1,a2), 0.05CeNi/Al2O3 (b1,b2), 0.1CeNi/Al2O3 (c1,c2) and 0.13CeNi/Al2O3 (d1,d2) catalysts.

Fig. 3. Effect of Ce content on the rate (rCH?, per total weight of Ni atoms) and TOF (per surface Ni atoms) of CH4 formation (a, 50 kPa CO, 700 kPa H2, Ar balance, 753 K) and the turnover frequencies of CH4 formation on CO pressure (b, 753 K), H2 pressure (c, 753 K), and temperature (d, 50 kPa CO, 700 kPa H2, Ar balance, 733-773 K) during CO-H2 reactions over Ni/Al2O3 and xCeNi/Al2O3 catalysts (weight hourly space velocity (WHSV) of 2.9×107 cm3 g-1 h-1, 1 MPa).

Fig. 4. H2-TPR profiles (a), Ni 2p XPS spectra (b), and Ce 3d XPS spectra (c) of Ni/Al2O3 and xCeNiAl2O3 catalysts with different Ce contents (Ce/(Ce + Ni) = 0.01, 0.02, 0.05, 0.07, 0.1 and 0.13).

Fig. 5. The fraction of Ni0 in Ni species (a), the fraction of Ce3+ in Ce species (b), CO-TPD profiles (c) of Ni/Al2O3 and xCeNiAl2O3 catalysts with different Ce contents (Ce/(Ce + Ni) = 0.01, 0.02, 0.05, 0.07, 0.1 and 0.13), and the apparent barriers of CH4 formation versus the downshift of Ni0 binding energy (d) and the desorption temperature of CO (e) over these catalysts.

Fig. 6. H2-TPD profiles (a), the fraction of surface Ni atoms and interfacial Ce atoms (b), and the amounts (normalized by the total weight of Ni atoms) of surface Ni atoms and interfacial Ce atoms (c) on Ni/Al2O3 and xCeNi/Al2O3 catalysts with different Ce contents (Ce/(Ce + Ni) = 0.01, 0.02, 0.05, 0.07, 0.1, and 0.13).

Fig. 7. The adsorption of CO (determined from the CO-TPD profiles in Fig. 5(c), normalized by total weight of Ni atoms) (a), the in-situ CO-DRIFTS spectra (b), and the fraction of interfacial CO (c) on Ni/Al2O3 and xCeNi/Al2O3 catalysts with different Ce contents (Ce/(Ce + Ni) = 0.01, 0.02, 0.05, 0.07, 0.1, and 0.13).

Fig. 8. Rates of CH4 formation (per total weight of Ni atoms) versus the amount of the H2 adsorption on interfacial Ni-CeO2 sites (a) and the amount of the CO adsorption on the interfacial Ni-CeO2 sites (b).

Fig. 9. Operando DRIFTS spectra of Ni/Al2O3 (a) and 0.05CeNi/Al2O3 (b) catalysts during CO-H2 (5 vol% CO, 70 vol% H2 and Ar balance) reaction at different temperatures (548-673 K).

Fig. 10. Transient DRIFTS spectra of Ni/Al2O3 and 0.05CeNi/Al2O3 catalysts in 5 vol% CO/Ar for 15 min (a,d), followed by Ar flow (b,e) and 70 vol% H2/Ar (c,f) at 573 K.

Scheme 1. Plausible mechanisms of CO methanation over Ni/Al2O3 and CeNi/Al2O3 catalysts.

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Electronic enrichment on Ni atoms at Ni-CeO₂ interfaces: Unraveling the catalytic role in CO methanation and its volcano-type relation with the CeO₂ content

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