Harnessing electronic structure modulation of Cu2+-mediated layered double hydroxide towards selective C2 pathway in CO2 reduction and plastic upcycling

doi:10.1016/S1872-2067(26)65182-0

Abstract

Abstract:

The integration of CO₂ electroreduction with plastic upcycling offers a sustainable route to generate high-value C₂ products. This study presents a self-supported CuMgAl layered double hydroxide coupled with reduced graphene oxide (CMA-0.1-G) as a bifunctional electrocatalyst for both CO₂ reduction (CO₂RR) and polyethylene terephthalate (PET) oxidation (POR). The hierarchical 1D/3D nanoneedle structure enables abundant active sites, efficient charge transport, and high stability. CMA-0.1-G achieves a 51.98% Faradaic efficiency (FE) for C₂ products during CO₂RR, attributed to mixed Cu²⁺/Cu⁺/Cu⁰ oxidation states that promote *CO adsorption and C-C coupling. In-situ Raman spectroscopy confirms *CO intermediates and strong Cu-CO interactions. For POR, the catalyst demonstrates an impressive > 89% FE toward C₂ oxidation products, aided by redox-active M-OOH species. A two-electrode bifunctional system using CMA-0.1-G for both CO₂RR and POR is assembled and operates at 1.25 V for 10 mA cm^-2. In addition, the catalysts were tested using flow cell, demonstrating impressive performance for over 12 h under high voltage. Density functional theory analysis reveals the key intermediates formation, adsorption and desorption of the intermediates on key catalytic active sites, offering mechanistic insights into the optimum catalyst. Under simulated sunlight, the system achieves 5.68% solar-to-fuel efficiency for CO₂RR and 92% FE for oxalic acid. This work establishes a multifunctional, scalable platform for coupling CO₂RR and plastic upcycling, selectively generating C₂ products through coordinated redox reactions, offering a viable solution for carbon neutrality and circular chemical manufacturing.

Key words: CO₂ reduction reaction, Layered double hydroxide, Bifunctional, Polyethylene terephthalate, C₂ products

Jian Yiing Loh, Feng Ming Yap, Elton Song-Zhe Mah, Xianhai Zeng, Wee-Jun Ong. Harnessing electronic structure modulation of Cu²⁺-mediated layered double hydroxide towards selective C₂ pathway in CO₂ reduction and plastic upcycling[J]. Chinese Journal of Catalysis, 2026, 91: 103-121.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(26)65182-0

https://www.cjcatal.com/EN/Y2026/V91/I12/103

Figures/Tables 8

Fig. 1. (a) Schematic illustration of the synthesis of CMA-0.1-G. FESEM images of CMA-0.1-G on copper foam with elevating magnifications of 10 μm (b), 1 μm (c,d), and 200 nm (e). (f) STEM image with the corresponding EDX mapping of Cu, Mg, Al, C and O elements of CMA-0.1-G. (g) EDX spectrum of Cu, Mg, Al, C and O in CMA-0.1-G.

Fig. 2. (a) Low magnification TEM image of CMA-0.1-G, with the inset highlighting the CuMgAl-LDH. (b) HRTEM image of CMA-0.1-G with inset of FFT image. (c) Magnified TEM image of CMA-0.1-G. (d) HRTEM image of nanoneedles LDH. (e) XRD patterns of CMA-0.1 and CMA-0.1-G. (f) Raman spectra of CMA-0.1 and CMA-0.1-G.

Fig. 3. XPS spectra of C 1s (a), O 1s (b), Cu 2p (c), Cu LMM (d), Mg 1s (e), Mg 2p (f) and Al 2p (g). BET analysis (h) and pore size distribution (i) of CMA-0.1-G and CMA-0.1.

Fig. 4. Electrocatalytic CO2RR Performance. (a) LSV plots for different catalysts. Tafel plots (b), Nyquist plots (c), and Cdl (d) for the as-prepared catalysts. (e) FE values of C1 and C2 products at various applied potentials for CMA-0.1-G. (f) C2 partial current density plot of MA, CMA-0.1 and CMA-0.1-G. (g) Comparison plot of typical CO2RR electrocatalysts (e.g. MgAl-LDH/Cu [6], Ni/Cu [48], CuZn@Al-fum [49], CeO2-Cu2O/GA [50], Cu-N4/C [51], Ag-Cu2OPB [52], Cu-complex/Cu [10] and Cu@Ag-2 NPs [53]). (h) Chronopotentiometry test of CMA-0.1-G at 50 mA cm-2 for 100 h.

Fig. 5. (a) Graphical illustration of C2 product formation from electrocatalyst. In-situ Raman spectra for CO2RR for CMA-0.1 in the range of 400-780 cm-1 (b), 800-1100 cm-1 (c), 1900-2180 cm-1 (d) and CMA-0.1-G in the range of 400-800 cm-1 (e), 900-1150 cm-1 (f), and 1300-2200 cm-1 (g) at a potential range of -0.7 to -1.3 V vs. RHE. (h) Free energy profiles of CO2RR on MA and CMA-0.1 catalysts.

Fig. 6. Electrocatalytic PET oxidation performance. LSV plot (a), Tafel plot (b), Nyquist plot (c) and electrochemical double layer capacitance (Cdl) (d) for the as-prepared catalysts. (e) Chronopotentiometry test and FE of CMA-0.1-G at 50 mA cm-2 for 100 h.

Fig. 7. In-situ Raman spectra for CMA-0.1-G during OER (1 mol L-1 KOH) in the range of 350-750 cm-1 (a), 900-1300 cm-1 (b), 1400-1900 cm-1 (c) and PET oxidation at potential range of -0.7 to -1.3 V vs. RHE (d). (e) OER (1 mol L-1 KOH) and half-way injected PET under 1.7 V. (f) PET oxidation reaction network and free energy diagram for PET oxidation to oxalic acid on the surfaces of CMA-0.1 and MA.

Fig. 8. (a) LSV polarization curves of the integrated cell with and without PET hydrolysate. Flow-cell bifunctional electrolyzer: chronoamperometry stability test for POR-CO2RR. Chronoamperometry for CO2RR with product FE (b) and chronoamperometry for POR with product FE (c). CO2RR (d) and POR (e) stability during continuous illumination for 12 h, along with the inset displaying the solar-cell (light on and light off) bifunctional POR-CO2RR hybrid unit featuring CMA-0.1-G as the anode and cathode electrodes. (f) The ηSTF of the tested electrocatalysts in bifunctional solar-powered electrolysis at the 60th min.

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Harnessing electronic structure modulation of Cu²⁺-mediated layered double hydroxide towards selective C₂ pathway in CO₂ reduction and plastic upcycling

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