Preparation and electro-catalytic performance of SBA15 modified carbon- supported PtNi catalyst

doi:10.21203/rs.3.rs-3774373/v1

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Preparation and electro-catalytic performance of SBA15 modified carbon- supported PtNi catalyst

https://doi.org/10.21203/rs.3.rs-3774373/v1

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Maximizing catalyst activity and stability while minimizing costs remains a formidable challenge. In this study, we employed the straightforward and easily executed ethylene glycol reduction method to synthesize highly active and stable Pt-Ni alloy catalysts, utilizing SBA15-modified carbon as the supporting material. Subsequent meticulous examinations delved into their physicochemical properties and electrocatalytic activities.Transmission electron microscopy (TEM) analyses unveiled a uniform distribution of PtNi particles on the support, showcasing a narrow particle size distribution centered around approximately 1.91 nm with minimal aggregation. Electrochemical assessments demonstrated that Pt3Ni/SBA15-C outperforms Pt/C, exhibiting 50 and 150 mV higher half-wave potentials (E_1/2) and onset potential (E_onset), respectively. Furthermore, our meticulously prepared Pt3Ni/SBA15-C, featuring a cage structure, displayed remarkable stability while sustaining superior catalytic durability under an applied potential of + 0.7 V. These findings underscore the effectiveness of the cage structure catalyst, comprising porous nanoparticles, in ensuring both catalytic activity and stability. The results collectively contribute to advancing our understanding of catalyst design and performance optimization in electrochemical applications.

fuel cell

SBA15 molecular sieve

PtNi nanoparticles

electrocatalytic activity

stability

In response to the growing demand for clean energy in both daily life and industry, significant attention has been directed toward proton exchange membrane fuel cells (PEMFCs) characterized by the imperative for secure, reliable, renewable, and sustainable energy source ^[1–10]. PEMFCs stand out as a promising alternative energy solution due to their advantageous attributes, including straightforward operation, high efficiency, environmental friendliness, and excellent stability ^[11–16]. Furthermore, the substantial conversion of chemical energy into electrical energy at a notably high efficiency renders PEMFCs suitable for diverse applications such as distributed generation, transportation power, and portable power for numerous electronic devices ^[17–24].

As widely recognized, the pivotal and prerequisite element within PEMFCs is the cathodic catalyst ^[25–30], exerting a direct impact on the overall performance of the fuel cell ^{[31, 32]}. Consequently, identifying a stable and efficient catalyst represents a formidable challenge. Currently, platinum (Pt)-based catalysts are the most widely adopted and essential choice, acknowledged for their distinctive catalytic activity and promising stability ^[33–35]. Nevertheless, the utilization of PEMFCs is hindered by issues such as high costs, scarcity, and suboptimal performance, particularly in the context of the oxygen reduction reaction (ORR), posing a significant impediment to achieving large-scale commercial viability. Addressing these concerns presents substantial challenges in the development of Pt-based catalysts for practical applications. Novel and innovative approaches to creating highly efficient fuel-cell catalysts are urgently required, ones that can sustain superior catalytic properties and maintain stability under demanding operating conditions, such as surface structure modification or Pt alloying ^[36–42].

Henceforth, diverse strategies have been employed to mitigate these challenges. Alloying, specifically with Pt-M alloy catalysts where M represents transition metals, stands out as the most extensively utilized and straightforward approach, effectively enhancing electrocatalytic activities while substantially reducing Pt consumption ^[43–48]. Numerous investigations have demonstrated that the introduction of transition metal doping induces alterations in the electron density and structure of the D-band state and the Fermi energy, thereby influencing the electronic properties of the Pt cluster through the so-called strain and ligand effect ^{[44, 46, 49]}. Noteworthy among these alloy catalysts are Pt-Ni catalysts, which have garnered considerable attention due to their commendable catalytic activity. Pt-Ni catalysts exhibit favorable oxygen reduction reaction (ORR) activity and enhanced stability against electrochemical oxidation. The incorporation of Ni induces electron transfer from Ni to Pt, resulting in a downward shift in the Pt 4f binding energy. This phenomenon weakens the adsorption of O2 molecules onto the Pt surface, providing an effective strategy for enhancing the reactivity of Pt-based catalysts through synergistic effects ^[47–52]. Additionally, this approach serves as a means to mitigate costs through the increased utilization of nanostructured platinum particles, leveraging bifunctional mechanisms and electronic effects [44,53].

Support material is widely recognized for its pivotal role in catalyst performance ^[54–55]. Achieving a uniform catalyst deposition on the support not only ensures a large surface area but also enhances electrical conductivity. Among the various support options, zeolite stands out as a promising choice due to its distinctive properties, such as a large specific surface area, ion exchange capacity, rich and uniform pore structure, and superior electronic conductivity. Notably, its microchannels facilitate the highly dispersed and stabilized distribution of Pt particles ^[57–61].

In this study, we opted for SBA15 modified carbon as the support for depositing Pt-Ni nanoparticles (Pt-Ni/SBA15-C) through a simple ethylene glycol reduction technique. Subsequently, an array of physicochemical tests was conducted to comprehensively characterize the catalysts. Finally, we delved into the electrocatalytic behavior of these catalysts toward the oxygen reduction reaction (ORR) using the rotating disk electrode (RDE) in an alkaline (potassium hydroxide) medium.

2.1. Preparation of Pt-based alloys catalysts

Firstly, 10ml H₂PtCl₆·6H₂O (20mg Pt/mL) and 0.03g of NiCl₂, 50 mg Fe-SBA15 and 500 mg carbon black were added to 50 mL ethylene glycol (EG), respectively. Then, the solution is stirred magnetically until the solution was evenly dispersed. The PH was adjusted to (10.0 ± 0.1) with 0.1mol/l NaOH glycol solution. Then appropriate polyvinylpyrrolidone (PVP) was added and stirred for 1 h. The solution is then dried at 150℃ for 8 h to ensure complete reduction of Pt precursors, and then cooled to ambient temperature. Then the sample is dried at 90 ℃ overnight and thoroughly ground. Finally, the samples were calcined at 500℃ for 4 h to obtain alloy Pt3Ni/SBA15-C, and stored in a glass vial for further experiments.

2.2. Structural characterization of Electrocatalyst

For the structure characterization, X-ray diffraction analysis (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectra (XPS) were performed. The mean particle size was calculated by determining the diameter of more than 100 particles. The average particle diameters and size distributions of Pt were also measured from the HRTEM images.

2.3. Electrochemical characterization

We performed RDE tests with a three-electrode system at 25 ℃, where a Pt foil, an Ag/AgCl electrode (3 M KCl), and GC electrode coated with catalyst (diameter = 4.0 mm, surface area = 0.1256 cm²) were used as working electrode, the counter electrode, and the reference electrode, respectively.

Before use, a series of pretreatment procedures are performed. Firstly, the GC electrode was polished with 0.3 µm alumina powder (Al₂O₃), then washed with deionized water, and polished again with 0.05 µm Al₂O₃. Finally, the polished GC electrode is repeatedly rinsed with deionized water. Then, it was ultrasonic treated in deionized water for 30s, and dried with nitrogen gas for use.

The catalyst ink was prepared by dispersion of 4 mg catalyst powder in a mix-solution of 20µl 5% Nafion solution and 980µl ethyl alcohol in an ultrasonic bath for 2 h to obtain a homogeneous slurry. Then 20 µl catalyst ink was deposited onto the glassy carbon disk (the GC electrode is rotated at a certain speed in order to be evenly coated) and dry at room temperature for subsequent testing.

High-purity O₂ (99.99%) was continuously blown into the electrolyte solution for 30 minutes before the experimental test to get a stable curve and sweep away excess impurities. An aqueous solution of 0.1mol/l KOH was used as the electrolyte in all the electrochemical measurements and was saturated with High purity O₂ for at least 0.5 h. The electrodes need to be cycled several times before each electrochemical measurement to produce clean surfaces between − 1.0-0.2 V (vs. SCE).

We carried cyclic voltammetry (CV) in 0.1 M KOH solution at a scan rate of 50 mV·s^− 1 between − 1.0V to 0.2 V, and evaluated the electrochemically active surface areas (ECSA) from the CV curve. LSV test is used to study the activity of the ORR and obtained in O₂ saturated 0.1mol/l KOH electrolyte from − 1.0V to 0.2V at a scanning rate of 10mV·s^− 1.

ORR polarization curves were conducted from − 1.0 V to 0.2 V with different rotation speeds (400–1600 r·min^− 1) at the rate of 10 mV·s^− 1. The Koutecky-Levich equation is used to study the the number of transferred electrons, as shown in Eq. (2 − 1)^{[17, 21, 25]}:

$\frac{1}{i}=\frac{1}{{i}_{k}}+\frac{1}{{i}_{d}}$ (2 − 1)

where i is the current used in the test, i_k is the kinetic current, i_d is the limiting diffusion current, which can be obtained from the Levich Eq. (2–2):

${i}_{d}=0.62nFA{D}^{\raisebox{1ex}{$2$}\!\left/ \!\raisebox{-1ex}{$3$}\right.}{v}^{\raisebox{1ex}{$-1$}\!\left/ \!\raisebox{-1ex}{$6$}\right.}{\omega }^{\raisebox{1ex}{$1$}\!\left/ \!\raisebox{-1ex}{$2$}\right.}{C}_{{O}_{2}}$ (2–2)

where n is the number of transferred electrons, and F is the Faraday constant (96485 C·mol^− 1), A is thearea of the GC electrode (0.196 cm²), D is the diffusion coefficient of O₂ in 0.1 M KOH solution (1.9×10^− 5 cm²·s^− 1), v is the dynamic viscosity of the electrolyte (1.13×10^− 2 cm²·s^− 1), and w is the angular frequency of rotation (rpm/min). C_O2 is the oxygen concentration of molecules (1.2×10^− 3 mol·cm^− 3).

In O₂-saturated 0.1M KOH solutions, CA (i-t) was tested at 0.6V constant voltage at a speed of 1600r, and the current change with time was recorded. The test time was 6 h, and the change in current density was recorded to analyze the stability of the catalyst.

3.1 Structural characterization

In Fig. 1a, a schematic representation illustrates the X-ray diffraction (XRD) patterns of our meticulously prepared catalysts, revealing characteristic diffraction peaks at (111), (200), (220), (311), and (222) for Pt, indicative of its face-centered cubic (FCC) structure (JCPDS#04-0802). These findings affirm the successful loading of Pt onto the support. Intriguingly, no discernible Ni diffraction peaks are evident, implying the successful incorporation of Ni atoms into the Pt lattice, existing in an alloyed form. Notably, for Pt3Ni/SBA15-C, the diffraction peaks exhibit increased sharpness, underscoring that alloying contributes significantly to the enhancement of crystallinity.

As depicted in Fig. 1b, the (111) peak of the PtNi catalysts exhibits a subtle shift towards higher diffraction angles. This shift is primarily attributed to the variance in the atomic radius between Ni and Pt^{[43, 48]}.

3.2 Morphology characterization (TEM)

The TEM, HRTEM and size distribution histograms are presented in Fig. 2. The discernible light and dark parallel lines in the micrographs are a result of the alternating arrangements of internal channels and pore walls within the SBA15 carrier, characterized by a uniform size of approximately 7 nm (Fig. 2a).

In Fig. 2b, a distinct hexagonal honeycomb arrangement is observed, showcasing the exemplary structural characteristics of SBA15. These features unequivocally underscore the high degree of order in the SBA15 structure, resulting in a notably expansive active area. The HRTEM image, detailed in the inset, reveals well-defined and ordered lattice fringes corresponding to Pt nanoparticles. The lattice spacing of 0.226 nm aligns consistently with the Pt (111) crystal plane. Numerous studies have consistently highlighted that precise control over the morphology of Pt-based alloy nanoparticles with exposed (111) crystal faces significantly enhances ORR performance ^{[45, 47, 62]}. Furthermore, Pt nanoparticles exhibit a uniform distribution on the grain of SBA15, with a particle size measuring approximately 7 ± 0.5 nm. This distribution is visually confirmed in the EDS results, validating the successful loading of Pt onto the SBA15 support.

As illustrated in Fig. 3(a-e), the SBA15 channels exhibit a uniform distribution on the carbon carrier, maintaining a characteristic hexagonal honeycomb structure. High-Resolution Transmission Electron Microscopy (HRTEM) analysis reveals a lattice spacing of 0.238 nm, aligning consistently with the Pt (111) crystal plane. Furthermore, the nanoparticles are evenly dispersed on the SBA15-C carrier, exhibiting a particle size of approximately 1.91 nm, which is smaller than that observed in Pt3Ni/SBA15. These findings collectively suggest potential advantages for enhancing catalytic activity.

3.3 Elemental composition analysis (XPS)

XPS further explored the surface composition and chemical oxidation state. Figure 4(a) is the XPS survey spectra of the Pt3Ni/SBA15-C and Pt/C catalyst, respectively, involving the signals of C 1s, O 1s, Pt 4f, Pt 4d, Pt 4p, and Ni 2p.

Gaussian peaks were employed for fitting the Pt 4f peak, decomposing it into four distinct peaks: Pt 4f7/2 and Pt 4f5/2, as depicted in Fig. 4. The presence of different peaks signifies the existence of distinct Pt oxidation states. The binding energies of 71.3 eV and 75.5 eV correspond to the metal Pt0 (4f 7/2) and Pt0 (4f 5/2), respectively. Peaks observed at 72.1 eV and 74.6 eV are attributed to Pt^+ 2 (4f 7/2) and Pt + 2 (4f 7/2), potentially arising from sample oxidation during annealing processes ^{[11, 12, 31]}. Additionally, the sample is susceptible to oxidation when exposed to air before X-ray Photoelectron Spectroscopy (XPS) measurements.

These findings suggest that the Pt2 + species in the samples are primarily PtO. Calculations based on the relative areas of these peaks reveal that the percentages of Pt0 and Pt + 2 species are 66.7% and 33.3%, respectively. This analysis indicates that the predominant form of surface Pt is metallic, favoring high electrochemical activity ^[63].

3.4 Electrochemical performance of Pt3Ni/SBA15-C

To assess the catalytic activity for ORR, CV test was employed to evaluate the electrochemically active surface areas (ECSA), as illustrated in Fig. 5a. Both curves exhibit characteristic peaks related to hydrogen adsorption/desorption within the potential range of -0.5 to 1.3 V. During the positive sweep, the oxidation peak beyond 0.50 V corresponds to the oxidation of precious metals into PtO. In the negative sweep, the reduction peak represents the reduction of the corresponding metal oxide. Notably, for Pt3Ni/SBA15-C, the peak current intensity of the catalyst increases, indicating its enhanced catalytic activity. The ECSA of Pt3Ni/SBA15-C is approximately 2.13 times larger than that of Pt/C, as depicted in Fig. 5, underscoring the superior electrochemical activity of Pt3Ni/SBA15-C.

As indicated in the literature, superior catalytic performance in ORR is associated with higher values of onset potential (E_onset), limiting current (I_lim), and half-wave potential (E_1/2). Analyzing the LSV curves provides insights into peak current, peak potential, and E_1/2 values for assessing ORR activity.

Figure 5b illustrates the ORR polarization curves of Pt3Ni/SBA15-C, revealing E1/2 and Eonset values of 0.88 and 1.05 V, respectively, surpassing those of commercial Pt/C^[50]. The enhanced ORR performance of Pt3Ni/SBA15-C can be primarily attributed to two factors. First, the exposure of (111) crystal faces, known to enhance ORR reaction activity, while (100) or (110) crystal faces may impede ORR reaction activity ^{[62, 64]}. Second, Pt3Ni/SBA15-C features numerous hollow channels and inner walls, indicative of a typical cage morphology, thereby increasing active sites in comparison to Pt/C.

Then we calculated the electron-transfer number, which is given in section 2. The calculated n values on Pt3Ni/SBA15-C were close to 4, which indicated that the reduction of oxygen on Pt3Ni/SBA15-C follows 4 electron transfer pathways.

The Pt3Ni/SBA15-C also demonstrated enhanced stability with negligible activity decay following the Chronoamperometry (CA) test. Examining the current-time (i-t) curve in Fig. 7 reveals that the current density of Pt/C reduced to 0.152 A after 60,000 s, whereas that of Pt3Ni/SBA15-C remained at 0.278 A. Even after the 370,000 s test, the current density of the Pt3Ni/SBA15-C electrode persisted at 0.25 A, surpassing that of Pt/C. This sustained performance can be attributed to the uniform distribution of nanoparticles and the unique pore structure on the surface of Pt3Ni/SBA15-C.

Primarily, the heightened electrocatalytic activity and stability stem from the synergistic effect between Ni and Pt. Additionally, the widespread distribution of Pt nanoparticles, coupled with the large hollow channels and available inner walls of SBA15-C, contributes to an increased number of active sites for the Oxygen Reduction Reaction (ORR) compared to traditional carbon. This aspect plays a pivotal role in enhancing both ORR activity and stability.

The innovative Pt3Ni/SBA15-C catalysts were synthesized using a sophisticated method, ensuring well-dispersed PtNi nanoparticles. Electrochemical measurements underscore the exceptional and enduring electrocatalytic performance of Pt3Ni/SBA15. This remarkable performance can be ascribed to the alteration in electronic structure induced by the synergistic effect between Pt and Ni. Furthermore, Pt3Ni/SBA15-C exhibits superior stability, surpassing that of commercial Pt/C by a factor of 5.6. Collectively, these outcomes establish the novel Pt3Ni/SBA15 as a compelling choice for PEMFC, particularly in applications such as portable electronic devices and power supply.

Author Contribution

Xia Li was responsible for the testing and sorting of articles, experimental content and experimental data,and wrote the main manuscript. All authors reviewed the manuscript.

Acknowledgments

This work was supported by Artificial intelligence vision chip development (2022D022).

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No competing interests reported.

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Preparation and electro-catalytic performance of SBA15 modified carbon- supported PtNi catalyst

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Abstract

Figures

1. Introduction

2. Experiment

2.1. Preparation of Pt-based alloys catalysts

2.2. Structural characterization of Electrocatalyst

2.3. Electrochemical characterization

3. Result and discussion

3.1 Structural characterization

3.2 Morphology characterization (TEM)

3.3 Elemental composition analysis (XPS)

3.4 Electrochemical performance of Pt3Ni/SBA15-C

4. Conclusions

Declarations

Author Contribution

Acknowledgments

References

Additional Declarations

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