Ultrasmall palladium nanoparticles supported on zirconium phosphate for electrochemical CO₂ reduction to ethanol

Abstract

The electrochemical CO₂ reduction reaction (CO₂RR) provides a promising approach to mitigate the global greenhouse effect by converting CO₂ into high-value chemicals or fuels. Noble metal-based nanomaterials are widely regarded as efficient catalysts for CO₂RR due to their high catalytic activity and excellent stability. However, these catalysts typically favor the formation of C1 products, which have relatively low economic value. Moreover, the high cost and limited availability of noble materials necessitate strategies to reduce their usage, often by dispersing them on suitable support materials to enhance catalytic performance. In this study, a novel metal-based support, zirconium phosphate Zr₃(PO₄)₄, was used to anchor ultrasmall palladium nanoparticles (pre-ZrP-Pd). Compared to the reversible hydrogen electrode, the pre-ZrP-Pd achieved a maximum Faradaic efficiency (FE) of 92.1% for ethanol at –0.8 V versus RHE, along with a peak ethanol current density of 0.82 mA/cm². Density functional theory (DFT) calculations revealed that the strong metal-support interactions between the ZrP support and Pd nanoparticles lead to an upward shift of the Pd d-band center, enhancing the adsorption of CO* and promoting the coupling of CO and CO to produce ethanol.

Graphical abstract

Keywords

electrochemical CO₂ reduction reaction (CO₂RR) / noble metal-based nanocatalysts / zirconium phosphate (Zr₃(PO₄)₄) support / ethanol selectivity / density functional theory (DFT) calculations

1 Introduction

The extensive use of fossil fuels has dramatically increased atmospheric CO₂ emissions, exacerbating the greenhouse effect and posing serious environmental threats globally. Using CO₂ as a feedstock to synthesize high-value chemicals is gaining increasing attention as a sustainable solution. Among various CO₂ conversion technologies, electrochemical CO₂ reduction reaction (CO₂RR) conducted in aqueous media, particularly when powered by renewable energy for carbon-neutral energy conversion, is a promising strategy. CO₂RR can yield a broad spectrum of products, ranging from C1 to C₂₊ hydrocarbons and oxygenates [1–6]. In particular, liquid C₂₊ alcohols, due to their high energy density, market demand, and ease of storage and transportation, have garnered significant attention in practical production and daily life [7,8]. For example, ethanol (C₂H₅OH) serves as both a fuel and a commodity chemical, with a global market value of approximately $75 billion and a volumetric energy density of 24 MJ/L.

To date, copper-based catalysts have been the most extensively studied materials for catalyzing CO₂RR to produce C₂₊ products. However, the formation of C–C bonds via *CO intermediates on copper surfaces remains energetically demanding and complex, resulting in limited selectivity for ethanol as a single product [9–11]. Moreover, the lack of a comprehensive understanding of the CO₂ to C₂₊ alcohol pathway has hindered the development of efficient catalysts for selective CO₂ to C₂₊ alcohol conversion. As a result, extensive efforts have been directed toward non-copper catalytic systems. Metals such as Co, Mo, Fe, Sn, Ir, Ni, and Pd-based metals, their alloys, oxides, phosphides, sulfides, and molecular complexes have been explored, though most have achieved limited success in selectively producing C₂₊ alcohols [12–19]. Among them, palladium-based catalysts are particularly notable due to their unique C–C coupling behavior and distinct CO₂RR performance, which differ from those of copper-based catalysts. For example, Zhang et al. [20] have demonstrated that In₂O₃ catalysts doped with a small amount of Pd exhibit high activity for CO₂RR to ethanol at low overpotentials, along with a high Faradaic efficiency (FE) of 50.7%.

In this work, zirconium phosphate-supported ultrasmall palladium nanoparticles (pre-ZrP-Pd) have been developed as an efficient catalyst for the selective electrochemical reduction of CO₂ to C₂H₅OH. Zirconium phosphate with a surface enriched in oxygen vacancies is employed to anchor Pd species (pre-ZrP-1.5Pd, pre-ZrP-2.5Pd). The developed pre-ZrP-1.5Pd catalyst achieved a FE of 87.6% for C₂H₅OH at –0.8 V versus RHE, ranking among highest reported for both copper and non-copper systems. Density functional theory (DFT) calculations demonstrate the strong metal-support interaction between the Pd nanoparticles and the ZrP substrate induces an upward shift in the Pd d-band center toward the Fermi level. This electronic shift enhances CO* adsorption, suppresses CO* desorption, and promotes CO–CO coupling, thereby facilitating ethanol formation. The findings suggest that tailoring metal-support interactions provides a promising strategy for advancing non-copper CO₂RR catalysts with improved selectivity toward C₂₊ alcohols.

2 Experiment

2.1 Chemicals

H₃PO₄ (99.9%), zirconium(IV) oxychloride octahydrate (ZrClO₂·8H₂O, 99.9%), ethanol (99.5%), and N,N-dimethylformamide (DMF, 99.9%) were purchased from Innochem Co., Ltd, China. Tetrabutylammonium hydroxide (25 wt% in H₂O) was obtained from Aladdin, Co., Ltd., China. Sodium tetrachloropalladate (II) hydrate (99.95%) was supplied by Alfa Co., Ltd., China. Ultrapure water (resistivity > 18 MΩ) was obtained using a Milli-Q purification system and used in all experiments. All gases were sourced from Linde Co., Ltd., China.

2.2 Synthesis

Zirconium phosphate was synthesized via a hydrothermal method using phosphoric acid, deionized water, and zirconium oxychloride octahydrate as precursors. First, 20 mL of deionized water was added to a hydrothermal synthesis reactor (Anhui Chem-n Instrument Co. Ltd., China), followed by 3 g of zirconium oxychloride octahydrate. The mixture was stirred until completely dissolved. Subsequently, 18 mL of phosphoric acid (18 mL) was slowly added under continuous stirring until the solution became clear. The mixture was then sealed and heated in a blast drying oven at 180 °C for 24 h. The resulting precipitate was collected by centrifugation, washed with deionized water until the supernatant reached neutral pH, and dried in a vacuum oven at 60 °C for 12 h to yield zirconium phosphate.

Next, 500 mg of the finely ground zirconium phosphate was placed in a mixture of 40 mL deionized water and 10 mL of tetrabutylammonium hydroxide in a 50 mL centrifuge tube. The suspension was sonicated in an ice-water bath for 1 h, followed by washing with ethanol via centrifugation, and drying under vacuum for 12 h to obtain tetrabutylammonium hydroxide-intercalated zirconium phosphate. This material was then calcined at 400 °C in air for 1 h to produce zirconium phosphate with a surface enriched in oxygen vacancies (pre-ZrP) [21].

Finally, 30 mg of pre-ZrP was mixed with 3 and 5 mL of 0.5 mg/mL chloropalladic acid solution in DM and stirred for 12 h. The mixture was vacuum filtered and dried for 12 h, then calcined at 400 °C under a nitrogen atmosphere in a tube furnace for 1 h, resulting in the formation of the catalysts pre-ZrP-1.5Pd and pre-ZrP-2.5Pd, respectively.

2.3 Characterization

The crystal structures were determined by X-ray powder diffraction (XRD using a Bruker D8 Advance diffractometer with Cu Kα (λ =1.5406 Å). Data were collected over a 2θ range of 5° to 45° at a scanning speed of 2 (° )/min with operating conditions of 40 kV and 40 mA. Crystalline phases were analyzed and confirmed using the Jade software package. X-ray photoelectron spectroscopy (XPS) was performed on a K-Alpha photoelectron spectrometer equipped with a monochromatic Al Kα X-ray source (1486.6 eV). All spectra were calibrated using the C 1s peak at 284.8 eV.

Morphology and structural characterization of the catalysts was conducted using field-emission transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS) on an FEI Talos F200i instrument. Scanning electron microscope (SEM) images were obtained using a Nova NanoSEM 230 field-emission SEM. X-ray absorption fine structure (XAFS) measurements were performed at the BL11B beamline of Shanghai Synchrotron Radiation Facility (SSRF) operating at 3.5 GeV and 250 mA maximum current, with Si (311) crystals used for monochromatization.

Electron paramagnetic resonance (EPR) spectra were recorded using a Bruker Elexsys E580 X-band EPR spectrometer. Proton nuclear magnetic resonance (¹H-NMR) measurements were conducted using a Bruker AVANCE NEO 600 MHz spectrometer. Thermogravimetric analysis (TGA) was conducted using a TGA 8000 thermogravimetric analyzer.

2.4 CO₂RR measurements

CO₂RR performance was evaluated using a CHI 760e electrochemical workstation in a typical three-electrode setup in an H-type cell. The cathode and anode chambers were separated by a Nafion 117 proton exchange membrane. Hydrophobic carbon paper (YLS-30T) loaded with the catalytic material served as the working electrode, with a geometric area of 0.5 cm × 1 cm. A carbon rod and an Ag/AgCl electrode (saturated KCl solution) were used as the counter and reference electrodes, respectively. Linear sweep voltammetry (LSV) and chronoamperometry were performed at different potentials in a 0.1 mol/L CO₂-saturated KHCO₃ electrolyte (pH 6.8). All potentials were converted to the reversible hydrogen electrode (RHE) scale according to

E(\mathrm{v}\mathrm{s}\mathrm{R}\mathrm{H}\mathrm{E})=E (\mathrm{v}\mathrm{s}\mathrm{A}\mathrm{g}/\mathrm{A}\mathrm{g}\mathrm{C}\mathrm{l}) +0.197 \mathrm{V}+0.059\times \mathrm{p}\mathrm{H}.

The catalyst ink was prepared by dispersing 2.5 mg of the prepared catalyst and 1.5 mg of commercial carbon black (XC 72) in 0.5 mL of an isopropanol-water mixture (3:1, v/v), followed by the addition of 10 µL of a 5 wt% Nafion solution (D520). Then, 80 µL of the catalyst ink was drop-cast onto carbon paper to fabricate the working electrode. Both the cathode and anode chambers were filled with 20 mL of 0.1 mol/L KHCO₃ electrolyte. Prior to electrochemical measurements, CO₂ gas was bubbled continuously through the electrolyte for 30 min to ensure saturation.

Gas-phase products, mainly CO and H₂, were analyzed online by a gas chromatograph (GC, Shimadzu 2014) directly connected to the electrochemical cell outlet. Except for the first 600 seconds of electrolysis at each potential, gas samples were collected every 300 s for analysis. Liquid-products were quantified using proton nuclear magnetic resonance (¹H-NMR) spectroscopy.

3 Result and discussion

3.1 Characterization of catalysts

The schematic illustration of the synthesis is shown in Fig.1. Various characterizations were conducted on ZrP, pre-ZrP, and pre-ZrP-xPd (x = 1.5, 2.5) catalysts to investigate their defects, crystallinity, thermal stability, and composition. The EPR spectrum (Fig. S1, Electronic Supplementary Material) shows a distinct signal at g = 2.003 for the pre-ZrP sample, indicating the presence of oxygen vacancies on the ZrP surface, which provides anchoring sites for the adsorption of chloropalladic acid anions. TG analysis curves (Fig. S2) reveal similar weight loss trends for pre-ZrP materials in both nitrogen and oxygen atmospheres. A weight loss peak around 170 °C corresponds to the removal of crystallization water, around 300 °C to the elimination of tetrabutylammonium hydroxide, and around 600 °C to the loss of phosphate groups. Notably, the total weight loss at 800 °C is approximately 13%, indicating that pre-ZrP does not undergo oxidation to form ZrO₂ in the oxygen atmosphere and possesses excellent thermal stability.

XRD patterns (Fig. S3) show that pre-ZrP retains diffraction peaks similar to those of ZrP but with reduced intensities, particularly for the (002) plane. Normalization analysis (Fig. S4), reveals that the intensity of the (110) plane peak in pre-ZrP is higher than in ZrP, accompanied by a broader half-peak width, suggesting that the intercalated and calcined ZrP has a thin-layer or few-layer structure. Additionally, the XRD patterns of pre-ZrP-xPd correspond to those of zirconium phosphate (PDF#28-1498), with no observable diffraction peak corresponding to the Pd (100) plane, indicating that the pre-ZrP-xPd remains intact and that Pd likely exists as ultrasmall Pd nanoclusters.

EDS elemental mapping images show a uniform distribution of Zr, O, and P elements (Fig.2(a)). TEM, SEM, and high-angle annular dark-field scanning TEM (HAADF-STEM) images reveal that pre-ZrP-xPd exhibits a layered hexagonal prism morphology (Fig.2(c) and Fig.2(d)) with edge lengths of approximately 0.1 µm. Notably, the surface of the prepared pre-ZrP-xPd displays numerous pores, and no distinct Pd particles are observed, suggesting that the Pd is present as ultrasmall nanoparticles dispersed within the structure.

High-resolution Pd 3d XPS spectra pre-ZrP-xPd (x = 1.5, 2.5) samples display characteristic peaks (Fig.3(a) and Fig.3(b)). Two distinct peaks at 333.55 and 334.42 eV correspond to Pd²⁺ and Pd⁰ species, respectively, accompanied by satellite peaks. A strong metal-support interaction is evident between the Pd particles and the ZrP support, with partial electrons from Pd to the ZrP substrate. The high-resolution O 1s XPS spectra show that a surface is rich in oxygen vacancies on ZrP, which act as anchoring sites to enhance the adsorption of Pd species.

Extended X-ray absorption fine structure (EXAFS) analysis at the Pd K-edge (Fig.3(c)) was performed via Fourier transform to study the atomic coordination environment of pre-ZrP-xPd. The first bridge-layer peak at approximately 2.2 Å is consistent with Pd particles, confirming the presence of Pd nanoparticles in pre-ZrP-xPd. Additionally, the coordination number of Pd in pre-ZrP-xPd is significantly lower than that of bulk Pd foil, suggesting the formation of ultrasmall Pd particles (Table S1).

3.2 CO₂RR performance

The CO₂RR performance was evaluated in 0.1 mol/L KHCO₃ electrolyte using an H-cell configuration. The electrocatalytic behavior of pre-ZrP-xPd (x = 1.5, 2.5) varies with applied potential. The hydrogen evolution reaction (HER) FE for pre-ZrP-1.5Pd increases from 8% at –0.8 V versus RHE to 41.8% at –1 V versus RHE, while the CO₂RR FE correspondingly decreases (Fig.4(a)). In contrast, pre-ZrP-2.5Pd shows an increase in HER FE from 0.8% at –0.8 V to 24% at –1 V versus RHE (Fig.4(b)). These results suggest a competition between HER and CO₂RR, with pre-ZrP-1.5Pd effectively catalyzing CO₂ reduction to ethanol predominantly at potentials more positive than –0.9 V versus RHE. Notably, at –0.8 V versus RHE for both catalysts, the ethanol current density (Fig.4(c) and Fig.4(d)) followed by a decline at more negative potentials.

Fig.4(e) and Fig.4(f) show the current density curves for pre-ZrP-1.5Pd and pre-ZrP-2.5Pd across different potentials. As the bias voltage increases from –0.5 to –1 V versus RHE, the ethanol current density for pre-ZrP-1.5Pd increases from 0.43 to 0.82 mA/cm² before dropping to 0.11 mA/cm². For pre-ZrP-2.5Pd, the current density increases from 0.42 to 0.75 mA/cm² and then drops moderately to 0.51 mA/cm². A comparison of pre-ZrP-xPd catalysts with different Pd loadings (x = 1.5, 2.5) reveals that pre-ZrP-2.5Pd, with a higher Pd content, exhibits a broader working potential range for high ethanol selectivity, demonstrating that Pd is the active site for ethanol production.

Pre-ZrP-xPd catalysts show strong suppression of HER and effectively steer the CO₂ reduction pathway toward C₂H₅OH formation, achieving selectivity similar to or even surpassing that of some of the optimized Cu-based catalysts [22–28] (Fig. S13). The comparison of ethanol FE between copper-based and non-copper-based catalysts, as reported in the literature, can be seen from Fig. S13. However, it is worth noting that the current densities for pre-ZrP-xPd remains similar to those of reported Pd-based catalysts, but much lower than those of Cu-based catalysts.

3.3 Reaction mechanism

The reaction mechanism for ethanol production over ultrasmall Pd nanoparticles supported on ZrP was further investigated using DFT. Reaction pathways involving CO₂—*COOH—*CO and H⁺—½ H₂ were calculated to simulate the competition between CO₂RR and the HER (Fig.5(a) and Fig.5(b)). The calculation shows that the Gibbs free energy of hydrogen adsorption (∆G_H) on Pd (111) is 0.03 eV, indicating that Pd facilitates both H⁺ adsorption and H₂ desorption, resulting in excellent HER activity, which can significantly suppress CO₂RR. In contrast, for pre-ZrP-xPd, ∆G_H decreases to –0.77 eV, suggesting that hydrogen desorption is greatly suppressed, inhibiting HER and promoting CO₂RR.

Additionally, for Pd (111), the energy barrier for CO formation is 1.9 eV, while for pre-ZrP-xPd, it increases to 2.01 eV, indicating that CO desorption, which leads to CO formation, is greatly suppressed on pre-ZrP-xPd. This strong suppression of CO desorption allows for the abundant adsorption of *CO, which can further couple to form ethanol. Partial density of states (PDOS) analysis shows that, compared to Pd (111) (Fig.5(c) and Fig.5(d)), the d-band center of pre-ZrP-xPd shifts upward from –1.98 to –1.38 eV, which significantly enhances CO adsorption [29]. Charge difference density analysis further confirms electron transfer from ZrP support to Pd, confirming that the metal-support interactions between Pd and ZrP strengthen *CO adsorption and promote further CO–CO coupling.

4 Conclusions

This study presents a novel non-copper-based catalyst composed of ultrasmall palladium nanoparticles supported on layered zirconium phosphate for CO₂RR to ethanol. The zirconium phosphate support, rich in oxygen vacancies, was synthesized via a hydrothermal method, followed by loading of ultrasmall Pd nanoparticles. The results demonstrate that the catalyst achieves a FE of 92.1% for ethanol at −0.8 V versus RHE, with a peak current density of 0.82 mA/cm², outperforming many copper-based catalysts and offering a promising strategy for high-value CO₂ conversion. XPS and EXAFS analyses reveal strong metal-support interactions between Pd and the support, leading to an upward shift in the Pd d-band center, which enhances *CO intermediate adsorption while suppressing CO desorption and HER. Although the current density (< 1 mA/cm²) remains lower than that of copper-based catalysts, this work opens new avenues for CO₂ utilization and carbon-neutral fuel synthesis.

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