Synthesis, Electrocatalytic and Gas Transport Characteristics of Pentagonally Structured Star-Shaped Nanocrystallites of Pd-Ag
Abstract
:1. Introduction
2. Materials and Methods
2.1. Synthesis of Bimetallic Pd–Ag Nanoparticles
- The classic palladium-black method or the “nanoparticle” method. The Pd–23%Ag alloy film was fixed in a holder, washed in 96% ethanol (Vecton, Saint-Petersburg, Russia), degreased by boiling for 30 min in a concentrated 6 M NaOH (Vecton, Saint-Petersburg, Russia) solution, then transferred for etching to a 60% HNO3 (Vecton, Saint-Petersburg, Russia) solution for 30 s, after which it was immediately transferred to a vessel with running distilled water for 10 min. Then, the film on an inert holder was transferred to an electrolytic cell for coating. The mass of the holder made of silver (LLC Research and Production company “Specialized metallurgy”, Yekaterinburg, Russia) with a purity of 99.99% was used as the current supply of the cathode. The contact was made with silver wire. Then, the palladium–silver alloy film was transferred to a cell with 0.1 M HCl (Vecton, Saint-Petersburg, Russia)and anodically polarized at a current density of 10–20 mA cm−2 using a potentiostat–galvanostat P-40X (Electrochemical Instruments, Chernogolovka, Russia), washed, cathodically polarized in 0.05 M H2SO4 (Vecton, Saint-Petersburg, Russia) at a current density of 10–20 mA cm−2, then filled with a 2% solution of H2PdCl4 (Vecton, Saint-Petersburg, Russia). Palladium black deposition was performed at a current density of 5–6 mA cm−2 for 30 min, after which it was washed with bidistillate and cathodically polarized in 0.05 M H2SO4 (Vecton, Saint-Petersburg, Russia).
- The difference of the “nanostar” method from the previous one is that, after washing with bidistillate, the cell was filled with a solution containing, along with H2PdCl4 (2%; Vecton, Saint-Petersburg, Russia), tetrabutylammonium bromide (0.01 mol L−1; Vecton, Saint-Petersburg, Russia) as a surfactant and AgNO3 (0.005 mol L−1; Vecton, Saint-Petersburg, Russia). Deposition was performed at a reduced current density, compared to the previous method, 3–4 mA cm−2 in stages with a step of 5 min for 30 min. In other words, in order to control changes in surface morphology during electrolytic deposition, a sample was selected after each stage for electron microscopy by cutting off part of the film. For this reason, the current density was adjusted over the area of the electrode for the further process.
2.2. Electrochemical Measurements
2.3. Measurement of Hydrogen Permeability
3. Results and Discussion
3.1. Morphology and Characteristics of Synthesized Nanoparticles
3.2. Cyclic Voltammetric Study of Methanol Oxidation in Alkaline
3.3. Chronoamperometric Study
3.4. Study of Hydrogen Permeability
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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Type of Modifying Coating | Palladium Black (Nanoparticles) | Nanostars |
---|---|---|
Average value, µm | 1.13074 | 1.00247 |
RMS roughness (Sq), nm | 223.578 | 315.565 |
Mean roughness (Sa), nm | 181.259 | 256.207 |
Coefficient of roughness | 12.27 | 20.53 |
Skew (Ssk) | −0.334003 | 0.27527 |
Excess kurtosis | −0.384457 | −0.34419 |
Projected area, µm2 | 12 | 12 |
Surface area, µm2 | 147.25 | 246.4 |
Volume, µm3 | 13.57 | 12.0297 |
Variation, µm2 | 164.14 | 269.66 |
Inclination θ, deg | 1.53 | 1.73 |
Inclination φ, deg | 20.50 | 143.9 |
Electrodes | Rf (Coefficient of Roughness) | EF, V | iF, µA cm−2 | EB, V | iB, µA cm−2 | iF/iB |
---|---|---|---|---|---|---|
Non-modified | 1.56 | −0.17 | 0.09 | −0.01 | −0.39 | 0.23 |
Nanoparticles | 12.27 | −0.09 | 10.66 | −0.34 | 4.13 | 2.58 |
Nanostars | 20.53 | −0.01 | 17.82 | −0.35 | 6.55 | 2.72 |
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Petriev, I.; Pushankina, P.; Lutsenko, I.; Shostak, N.; Baryshev, M. Synthesis, Electrocatalytic and Gas Transport Characteristics of Pentagonally Structured Star-Shaped Nanocrystallites of Pd-Ag. Nanomaterials 2020, 10, 2081. https://doi.org/10.3390/nano10102081
Petriev I, Pushankina P, Lutsenko I, Shostak N, Baryshev M. Synthesis, Electrocatalytic and Gas Transport Characteristics of Pentagonally Structured Star-Shaped Nanocrystallites of Pd-Ag. Nanomaterials. 2020; 10(10):2081. https://doi.org/10.3390/nano10102081
Chicago/Turabian StylePetriev, Iliya, Polina Pushankina, Ivan Lutsenko, Nikita Shostak, and Mikhail Baryshev. 2020. "Synthesis, Electrocatalytic and Gas Transport Characteristics of Pentagonally Structured Star-Shaped Nanocrystallites of Pd-Ag" Nanomaterials 10, no. 10: 2081. https://doi.org/10.3390/nano10102081