Comparative Physicochemical and Electrochemical Characterization of the Structure and Composition of Thin Pd Binary and Ternary Codeposits with Pt, Ru, and Rh
Abstract
:1. Introduction
2. Materials and Methods
3. Results and Discussion
3.1. Structural Characterization
- (1)
- In most cases, lattice parameters of fresh deposits are close to those predicted by Vegard’s law;
- (2)
- Under hydrogen atmosphere, the lattice parameter for Pd-rich samples considerably increases, while for the samples poorer in Pd, it almost does not alter, or even slightly decreases;
- (3)
- Lattice parameter in vacuum or in helium before or after exposure to hydrogen is often slightly smaller than that in air.
- (1)
- The good agreement with Vegard’s law suggests that the alloy phase is the only one present in the samples, i.e., that the deposits are highly homogeneous. However, the literature data show that such a conclusion should be drawn with care (see Januszewska et al. [65] and the references therein). In particular, there are evidences that even in homogenous systems, the deviations from Vegard’s law are observed, and vice versa, Vegard’s law can be very well fulfilled in the case of heterogeneous materials.
- (2)
- The magnitude of changes in lattice parameter under hydrogen atmosphere depends on the fact whether a given sample can absorb hydrogen or not. This is illustrated in Figure 1c,d, comparing XRD patterns for two Pd-Pt-Ru samples with different abilities to absorb hydrogen. While for a Pd-rich (ca. 95% Pd in the bulk) Pd-Pt-Ru sample, lattice parameter increases under hydrogen atmosphere and the diffraction lines are shifted negatively, in the case of the sample containing ca. 36% Pd in the bulk, no expansion of the crystal lattice occurs, as mirrored by no alterations of XRD spectrum. The constant position of signals in XRD spectra during the exposure to gaseous hydrogen is typical of those Pd-based deposits which contain too little Pd in the bulk for hydrogen absorption in the β-phase to occur [9]. In the presence of only negligible amounts of hydrogen absorbed in the α-phase, the lattice parameter increases very weakly in comparison to that of a non-hydrogenated material [31,32], and therefore its slight change is not detected by XRD. It should be added that lattice parameter for the hydride phase in the Pd-Rh alloys containing ca. 92 at % Pd in the bulk (4.028–4.043 Å) is even greater than that for Pd hydride (4.025 Å), which is consistent with the literature [31].
- (3)
- The small decrease in lattice parameter after pumping out the air and then after contact with hydrogen could indicate changes in the composition of the alloy phases. For instance, using Vegard’s law, one obtains the alloy bulk composition as ca. 92% Pd-Rh for the fresh alloy, and ca. 86% Pd-Rh after hydrogen absorption/desorption. The former value is in a very good agreement with atomic emission spectroscopy data. The small decrease in lattice parameter, converted via Vegard’s law into the apparent alloy enrichment with Rh, can be explained taking into account the following possibilities [64]: (i) An irreversible surface segregation accelerated by superabundant vacancy formation (SAV) [66] that may accompany hydrogen absorption, and (ii) an additional reduction of small amounts of Rh and/or Ru surface oxides (present on the surface after contact with the deposition bath) to the metallic form by atomic hydrogen taking part in the absorption process.
3.2. Characterization by Spectroscopic Techniques
- (1)
- In the case of Pd-rich (>85% Pd in the bulk) binary Pd-Ru deposits, it is difficult to find a distinct, unequivocal tendency in the relation between bulk and surface/subsurface content of the metals. For individual Pd-Ru samples, a rather large scatter of data is observed within ±4%, and the mean difference between the metal contents derived from XPS and EDS does not exceed ±0.5 at %;
- (2)
- In case of Pd-rich (>90% Pd in the bulk) binary Pd-Rh deposits, XPS detected ca. 1.5–4% less Rh than EDS (a difference mean value ca. −2.7 at %);
- (3)
- A systematic excess of Pd content in XPS vs. EDS data (a difference mean value ca. +5 at %) at the expense of Rh and Ru is observed in the case of Pd-rich (>80% in the bulk) Pd-Rh-Ru deposits;
- (4)
- Ru content determined from XPS data is smaller than that obtained by EDS for Pd-Pt-Ru and Pd-Rh-Ru electrodes. For individual Pd-Pt-Ru samples, the depletion with Ru visible by XPS becomes greater with increasing Ru bulk content, reaching ca. −8.7 at % for a sample containing 65% Ru in the bulk. The mean differences between both sets of data are ca. −3.7 at % (and almost −6 at % for Pd-Pt-Ru samples containing more than 25% Ru and less than 65% Pd in the bulk) and −2.5 at %, respectively;
- (5)
- In the case of Pd-Pt-Ru samples, much more Pt is indicated by XPS than by EDS, i.e., by up to +11 at % individually and ca. +4 at % on the average (and even +6 at % for Pd-Pt-Ru samples containing less than 65 at % Pd in the bulk).
3.3. Electrochemical Characterization
- (1)
- Rh content determined by EDS is usually higher than those derived from XPS or AES measurements, and at the same time Rh content originating from AES data is higher than that from XPS. For Pd-Rh samples in the composition range examined in this study, Rh concentration determined by CV is similar to or lower than that obtained by EDS (differences up to −5.7 at % for the individual samples, and ca. −2.4 at % on average). This is in line with our earlier data on the electrochemistry of the Pd-Rh system [79,80]. However, according to the results of the experiments performed with Pd-Rh electrodes in a much wider composition range, for Pd-Rh electrodeposits containing more than ca. 20% Rh in the bulk, the surface becomes more and more enriched with Rh [79,80];
- (2)
- For individual Pd-Ru samples, the differences in Ru contents determined by CV and EDS vary within the range ±4 at %, but the mean differences do not exceed +1 at %;
- (3)
- For Pd-Pt-Ru electrodes, the analysis of CV curves gives a systematically smaller Ru content with respect to EDS data (to −3.5 at % for the individual samples and ca. −2 at % on average);
- (4)
- The differences in Ru or Rh contents determined by CV and XPS/AES are opposite to CV vs. EDS-derived values. In particular, for Pd-Pt-Ru alloys with increasing bulk Ru content (>25%), more Ru (by up to +8 at % individually and ca. +4 at % on average) is detected by CV than by XPS, while for the same samples, CV data are closer to EDS data. A similar situation occurs for CV vs. AES data for Pd-rich Pd-Rh alloys, while for Pd-rich Pd-Ru alloys CV analysis gives a smaller Ru content (to −4 at % individually and ca. −1.5 at % on average) than that based on XPS analysis.
3.4. Comparison of Data Obtained by Various Analytical Techniques
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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Hubkowska, K.; Łukaszewski, M.; Soszko, M.; Koss, U.; Hamankiewicz, B.; Czerwiński, A. Comparative Physicochemical and Electrochemical Characterization of the Structure and Composition of Thin Pd Binary and Ternary Codeposits with Pt, Ru, and Rh. Materials 2018, 11, 798. https://doi.org/10.3390/ma11050798
Hubkowska K, Łukaszewski M, Soszko M, Koss U, Hamankiewicz B, Czerwiński A. Comparative Physicochemical and Electrochemical Characterization of the Structure and Composition of Thin Pd Binary and Ternary Codeposits with Pt, Ru, and Rh. Materials. 2018; 11(5):798. https://doi.org/10.3390/ma11050798
Chicago/Turabian StyleHubkowska, Katarzyna, Mariusz Łukaszewski, Michał Soszko, Urszula Koss, Bartosz Hamankiewicz, and Andrzej Czerwiński. 2018. "Comparative Physicochemical and Electrochemical Characterization of the Structure and Composition of Thin Pd Binary and Ternary Codeposits with Pt, Ru, and Rh" Materials 11, no. 5: 798. https://doi.org/10.3390/ma11050798