Advanced Energy Materials - 2023 - Oh - Activity Restoration of PT Ni Octahedron Via Phase Recovery For Anion Exchange

RESEARCH ARTICLE
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Activity Restoration of Pt–Ni Octahedron via Phase

Recovery for Anion Exchange Membrane-Unitized
Regenerative Fuel Cells
Cheoulwoo Oh, Man Ho Han, Young-Jin Ko, Jun Sik Cho, Min Wook Pin, Peter Strasser,
Jae-Young Choi, Hansung Kim,* Chang Hyuck Choi,* Woong Hee Lee,*
and Hyung-Suk Oh*
1. Introduction
Unitized regenerative fuel cells (URFCs) offer a cost-effective solution for
energy conversion by functioning as both fuel cells and electrolyzers. Unitized regenerative fuel cells (URFCs)
have gained significant attention as
Anion-exchange membrane-based URFCs (AEM-URFCs) require bifunctional
promising energy conversion systems
electrocatalysts, such as Pt–Ir alloys, for the oxygen evolution reaction (water that can function as both fuel cells and
electrolysis mode) and oxygen reduction reaction (fuel cell mode). However, electrolyzers in a single device.[1] In
the low stability of Pt in alkaline media and the high cost of Ir remain particular, proton exchange membrane
challenges for the widespread application of these URFCs. In this study, a (PEM)-based URFCs (PEM-URFCs)
Pt–Ni octahedral alloy is synthesized to replace Ir with Ni as the oxygen using Nafion membrane and Pt–Ir alloys
as the ion exchange membrane and
evolution reaction catalyst. The alloying effect of Pt–Ni inhibits the dissolution
oxygen electrocatalysts, respectively, have
of Pt and transforms PtOx to metallic Pt via a recovery process, thereby been actively investigated.[2] However,
providing a new operational strategy for improving the durability of the high cost of platinum group met-
AEM-URFCs. Remarkably, the performance of the AEM-URFC single cell is als, such as Pt and Ir, severely limits
maintained over ten cycles after the recovery process, demonstrating the their commercialization.[3] To address
this issue, anion exchange membrane
viability of this approach for long-term operations. These findings pave the
(AEM)-based URFCs (AEM-URFCs),
way for broader applications and advancements of AEM-URFCs. which can utilize transition metals as
oxygen electrode catalysts, have emerged
C. Oh, M. H. Han, Y.-J. Ko, W. H. Lee, H.-S. Oh P. Strasser

Clean Energy Research Center Department of Chemistry
Korea Institute of Science and Technology (KIST) Chemical Engineering Division
Seoul 02792, Republic of Korea Technical University Berlin
E-mail: abcabac@kist.re.kr; hyung-suk.oh@kist.re.kr 10623 Berlin, Germany
J. S. Cho, C. H. Choi J.-Y. Choi, H.-S. Oh
Department of Chemistry School of Advanced Materials Science and Engineering
Pohang University of Science and Technology (POSTECH) Sungkyunkwan University (SKKU)
Pohang 37673, Republic of Korea Suwon 16419, Republic of Korea
E-mail: chchoi@postech.ac.kr J.-Y. Choi, H.-S. Oh
M. W. Pin KIST-SKKU Carbon-Neutral Research Center
Analysis and Assessment Group Sungkyunkwan University (SKKU)
Research Institute of Industrial Science and Technology (RIST) Suwon 16419, Republic of Korea
Pohang 37673, Republic of Korea H. Kim
Department of Chemical and Biomolecular Engineering
Yonsei University
The ORCID identification number(s) for the author(s) of this article Seoul 03722, Republic of Korea
can be found under https://doi.org/10.1002/aenm.202302971 E-mail: elchem@yonsei.ac.kr
© 2023 The Authors. Advanced Energy Materials published by C. H. Choi
Wiley-VCH GmbH. This is an open access article under the terms of the Institute for Convergence Research and
Creative Commons Attribution-NonCommercial-NoDerivs License, Education in Advanced Technology (I-CREATE)
which permits use and distribution in any medium, provided the original Yonsei University
work is properly cited, the use is non-commercial and no modifications Seoul 03722, Republic of Korea
or adaptations are made.
DOI: 10.1002/aenm.202302971
Adv. Energy Mater. 2024, 14, 2302971 2302971 (1 of 10) © 2023 The Authors. Advanced Energy Materials published by Wiley-VCH GmbH
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as promising candidates. The recent technological advances in of 0.216 nm (Figure 1b). The presence of the (111) facet of PtNi-
AEM-based fuel cells and water-splitting systems further en- octa was confirmed by the XRD spectrum (Figure 1c), where its
hance this possibility.[4] However, there has been little research peak was located between the peaks of the (111) lattice planes of
on AEM-URFCs because of the challenges arising from the poor Pt (JCPDS card no. 65–2868) and Ni (JCPDS card No. 65–2865).
catalytic activity and stability of the oxygen electrode. Additional diffraction peaks corresponding to the (200), (220),
Generally, oxygen electrodes require a bifunctional electro- and (311) facets of PtNi-octa were observed (JCPDS card no. 65–
catalyst because they are the site for two reactions: the oxygen 2797), while the broad peak at 25° was attributed to the carbon
evolution reaction (OER; water electrolysis mode) and the oxy- support. HR-TEM images (Figure S1, Supporting Information)
gen reduction reaction (ORR; fuel cell mode).[5] In alkaline envi- revealed the sub-10 nm octahedral shape and uniform dispersion
ronments, transition metal oxides (e.g., NiOx , NiFeOx , CoFeOx, of the Pt–Ni alloy. This was confirmed by the EELS line scans of Pt
etc.) and Pt have been widely used for the OER and ORR, and Ni (Figure 1d) and the EDS mapping image (Figure 1e). ICP-
respectively.[6] That is, transition metals can replace Ir as OER OES analysis showed that PtNi-octa had a Pt-based weight com-
catalysts, thereby reducing the cost. Moreover, the combination position of 47.06% and Ni-based weight composition of 14.09%
of Pt and transition metals has been widely utilized as alloy cata- with an atomic ratio of 1:1.
lysts for the ORR under acidic conditions. Alloying Pt with a tran- The electrochemical activity of PtNi-octa was evaluated using
sition metal having a smaller lattice constant, such as Ni, can be an RDE in the three-electrode system. Initially, RDE measure-
an effective way of controlling surface strains.[7] The octahedral- ments were conducted in O2 -saturated 0.1 m KOH to compare
shaped Pt3 Ni single-crystal surface with an exposed (111) facet is the ORR performance of PtNi-octa with those of Pt/C, Pt black,
currently considered the best electrocatalyst for the ORR.[8] and the Pt/C-Ni/C mixture (denoted as Pt-Ni/C), which was phys-
Although PtNi is a promising catalyst for the ORR, the poor ically mixed at the same composition. This is because Pt atoms
stability of Pt in alkaline electrolytes remains a severe limitation are basically associated with the ORR and Ni atoms with the OER
for the fabrication of efficient AEM-URFCs. The poor stability of in PtNi-octa (Figure S2, Supporting Information). Usually, alloy-
Pt is mainly attributable to PtOx formation and Ptn+ dissolution ing with Ni can enhance the ORR activity of an electrocatalyst
during the OER, which lower the ORR catalytic activity and de- because alloying Pt with 3d-transition metal, Ni could downshift
crease the catalytic active surface area, respectively.[9] During the the d-band center compared to pure Pt, reducing the adsorp-
OER, oxide monolayers are formed on the Pt surface, and Pt─Pt tion energy of oxygen intermediates.[13] Consequently, PtNi-octa
bonds are broken, with O atoms exchanging their positions with had the lowest onset potential with the highest current density
Pt in the Pt crystal lattice.[10] In this process, the uncoordinated (Figure 2a), which was confirmed by this catalyst having the high-
Pt atoms are exposed to the electrolyte and are dissolved.[11] The est mass activity based on Pt weight at 0.8 VRHE (Figure 2b). Deter-
dissolution of the metal can be influenced by passivation effects mination of the selectivity of the ORR using an RRDE confirmed
and changes in the electronic structure.[12] For example, Ko et al. that H2 O was mainly produced instead of H2 O2 (Figure S3, Sup-
reported that antimony-doped tin oxide (ATO) could be utilized porting Information). Subsequently, the OER activity of PtNi-octa
as a metal oxide support to control the electronic structures of Pt in N2 -saturated 0.1 m KOH was compared with those of Ni black,
and Ir to inhibit their dissolution.[5] Ni/C, and Pt–Ni/C. PtNi-octa had a higher current density than
Herein, we report a Pt–Ni octahedron (PtNi-octa) as an oxygen the reference materials (Figure 2c). The OER activity of PtNi-octa
electrocatalyst in an AEM-URFC. PtNi-octa could effectively re- was also compared with that of IrO2 (Figure S4, Supporting Infor-
duce Pt dissolution, resulting in improved durability. To restore mation). When Pt/C was physically mixed with Ni/C, its current
the activity of the oxidized Pt and preserve the performance of density was lower than that of the bare Ni/C. However, it showed
PtNi-octa as a bifunctional oxygen electrode, an electrochemical higher mass activity based on Ni weight (Figure 2d). Pt can en-
recovery procedure was conducted after every cycle. The oxidized hance the OER activity when it is mixed well as an alloy to form an
Pt on the outer surface of the PtNi-octa was removed after the re- octahedral shape,[14] which was induced by the synergetic effect
covery process and examined. The mechanism of activity restora- between the intrinsic activity of Ni and the high conductivity of
tion in terms of changes in the structure and oxidation state of Pt.[14b] It was shown that PtNi-octa has the highest current den-
PtNi-octa during the URFC cycles was also investigated. Notably, sity among the catalysts. The Tafel plots showed that PtNi-octa
the AEM-URFC single cell could be operated for 10 cycles after had the lowest Tafel slope of 48.19 mV dec‒1 (Figure S5, Support-
the recovery process. To the best of our knowledge, this is the ing Information).
first example of an AEM-URFC exhibiting device-level durability. In addition, it had the highest mass activity based on Ni weight
We expect that such electrochemical recovery treatments can be at 1.6 VRHE (Figure 2d). This high activity was maintained even
potentially applied to catalysts other than Pt-based alloys to over- at low loading amounts, as shown by a comparison of its perfor-
come the stability challenges in AEM-URFCs. mance with those of reported bifunctional electrocatalysts at over-
potentials of 10 mA cm‒2 for the OER and −3 mA cm‒2 for the
2. Results and Discussion ORR (Table S1, Supporting Information). These results suggest
that PtNi-octa is a promising bifunctional electrocatalyst. Fur-
PtNi-octa with an exposed (111) facet is a promising efficient elec- thermore, the TEM images of the references sample exhibited
trocatalyst that has shown high mass activity toward the ORR and that Pt black and Pt/C samples have nano-sized particles which
OER. PtNi-octa nanoparticles were synthesized on Vulcan carbon is displayed in Figure S6 (Supporting Information). Even with
black by an N,N-dimethylformamide-based solvothermal method similar particle size of Pt in samples, PtB–NiB (metal black mix-
at 200 °C. An octahedral-shaped Pt–Ni alloy was successfully syn- ture) had the lowest electrochemical surface area (ECSA) due to
thesized on the carbon support (Figure 1a) with a lattice distance the absence of carbon (Figure S7, Supporting Information). In
Figure 1. Morphology of Pt–Ni octahedron (PtNi-octa). a) HR-TEM image, b) HAADF-STEM image, c) XRD pattern, d) HAADF-STEM image with EELS
line scans, and e) EDS mapping image of PtNi-octa. Red, green, blue, and cyan colors indicate Pt, Ni, C, and O, respectively.
addition, PtNi-octa had the largest ECSA calculated from CV, nearly 35 cycles (see the full range of the cycle test in Figure S8,
but the difference between the ECSA of PtNi-octa and Pt–Ni/C Supporting Information) before undergoing a sharp decline and
(carbon-supported metal mixture) was not huge. However, PtNi- eventually reaching the same working potential as that of PtB–
octa had higher activity toward ORR and OER because of its alloy NiB. The polarization curves for the ORR performance of the
effect with Ni. catalysts (Figure S9, Supporting Information) followed a simi-
To further investigate the electrochemical performance of the lar trend to the cycle test results, with PtB-NiB and Pt–Ni/C un-
catalysts used in URFCs, cycle tests consisting of the ORR–OER– dergoing complete degradation and PtNi-octa only partial degra-
recovery series were conducted in O2 -saturated 0.1 m KOH. In dation. During the cycle tests of PtB-NiB and Pt–Ni/C, the cat-
general, after carrying out a URFC cycle with PtNi-octa, oxygen alyst deposited on the RDE began to detach as the overpoten-
molecules form on the catalyst surface, especially on Pt atoms, tial increased, resulting in the degradation of both the ORR and
which can be oxidized in alkaline media when the applied po- OER performances. Notably, this behavior differed from that of
tential is above 0.7 VRHE .[9a,15] A catalyst passivated by oxidation PtNi-octa, which could maintain its overpotential. In general, the
cannot maintain its bifunctional ability, especially for the ORR, degradation of the ORR performance can be attributed to Pt dis-
because the diffusion of oxygen toward the catalyst is hindered. solution during the OER, particularly as transient corrosion can
Because Ni oxides have superior OER activity to Pt,[14a,16] the OER easily occur when an oxide layer is repeatedly formed and re-
primarily occurs on Ni during the URFC process. Thus, even if moved during oxidation and reduction.[9a,10a,17] To investigate this
the activity of Pt is reduced by passivation, the overall OER ac- phenomenon, in situ/operando ICP-MS analysis was conducted
tivity is maintained. The degradation of the ORR performance to monitor the dissolution of Pt and Ni during the URFC cycles
of PtNi-octa was confirmed by a half-cell cycle test of 50 cycles. (Figure 2f). Ni was stable and unlike Pt, did not undergo signifi-
As illustrated in Figure 2e, the ORR activity initially occurred cant dissolution during the ORR and OER. Notably, PtB–NiB ex-
at 0.81 V but gradually decreased to 0.68 V after 50 cycles of hibited more severe dissolution during the OER than PtNi-octa
URFC without recovery. PtB-NiB (black metal mixture) and Pt– and Pt–Ni/C, indicating that the carbon support effectively re-
Ni/C (carbon-supported metal mixture) were also subjected to the duced Pt dissolution. In addition, the alloy (PtNi-octa) was more
same cycle test. Both the OER and ORR performances of PtB– stable than the physical mixture (Pt–Ni/C), suggesting that the
NiB degraded rapidly after only a few cycles. On the other hand, presence of Ni in the alloy mitigated Pt dissolution. Ni, which
the activity of Pt–Ni/C was comparable to that of PtNi-octa for can easily form oxides, can prevent Pt dissolution by passivating
Figure 2. Electrochemical characterization and in situ/operando properties. a) Polarization curves and b) mass activities for the oxygen reduction
reaction (ORR; at 0.8 VRHE ) in 0.1 m KOH. c) Polarization curves and d) mass activities for the oxygen evolution reaction (OER; at 1.6 VRHE ) in 0.1 m KOH.
e) Chronopotentiometry curves in unitized regenerative fuel cell mode at 2 mA cm−2 for 50 cycles without recovery. f) In situ/operando electrochemical
dissolution of Pt and Ni in 0.1 m KOH. g) Fourier transformation of the in situ/operando EXAFS spectra under various operation conditions (OCV: open
circuit voltage). The blue dashed lines indicate the metal–metal bond distances.
the alloy surface. Indeed, Ni is known to be soluble and stable spectra during the ORR and OER (Figure 2g). Furthermore, PtNi-
during redox reactions in alkaline electrolytes, which is due to octa, a metal alloy, had a shorter metal–metal bond distance than
the formation of Ni(OH)2 through the dissolution precipitation the physical mixtures (Pt–Ni/C and PtB–NiB).
mechanism.[10a] This was also confirmed by a comparison of the Subsequently, electrochemical recovery was included in the cy-
EDS mapping images of PtNi-octa in the pristine state (Figure 1e) cle test (Figure 3a). The details of the recovery process are de-
and after the URFC cycles (Figure S10, Supporting Information), scribed in the experimental section, and the potential applied
which revealed Ni atoms primarily occupying the alloy surface. for this process is presented in Figure S11 (Supporting Infor-
The passivation of Ni in PtNi-octa and the change in electronic mation). Interestingly, in contrast to the results of the cycle tests
structure due to alloying effects have reduced the dissolution of without recovery (Figure 2e), all catalysts showed a stable perfor-
Pt, [9a,18] but small amounts still occur. This could be attributed to mance. Although the ORR activities of PtB–NiB and Pt–Ni/C de-
the exposure of Pt atoms at the edges of PtNi-octa, which could creased, the applied working potentials were higher than those
not be fully covered by Ni oxides. Pt oxidation was observed for observed without recovery, and the OER performance was essen-
all catalysts, as indicated by the increase in the peak intensity tially maintained. Thus, the recovery process can be applied to
of Pt─O (associated with a shoulder peak at ≈1.7 Å) in the in physical mixtures and not only to alloys. Previous studies indi-
situ/operando extended X-ray absorption fine structure (EXAFS) cated that the activity of the Pt/C electrocatalyst is regenerated
Figure 3. Electrochemical properties and electrochemical state changes during the unitized regenerative fuel cell (URFC) cycles. a) Chronopotentiometry
curves in the URFC mode with recovery at 2 mA cm−2 for 50 cycles in 0.1 m KOH. b) Polarization curves before and after the URFC cycles with recovery.
c) Peak ratios of PtO/Pt (black) and NiO/Ni (green) in pristine PtNi-octa and after the reaction steps [oxygen reduction reaction (ORR), oxygen evolution
reaction (OER), and recovery]. d) HR-TEM image of pristine Pt–Ni octahedron (PtNi-octa). STEM images of PtNi-octa e) after the URFC cycles and
f) after recovery. The yellow circle in (e) indicates oxidized Pt.
by stripping carbonaceous species from the interface between PtNi-octa maintained its shape after 50 cycles. Similar to the cy-
the carbon substrate and Pt.[19] However, this explanation cannot cle test results shown in Figure 2e, PtB–NiB and Pt–Ni/C showed
fully account for the effect of recovery since it was also observed degradation but still had higher current densities than those ob-
for the PtB–NiB catalyst without carbon support. The polarization served without recovery (Figure S9, Supporting Information).
curves after the long-term URFC cycle tests with recovery were The effect of recovery was investigated by conducting IL-
further studied. As shown in Figure 3b, the polarization curve of TEM to monitor the changes in the morphology and surface
properties of PtNi-octa after undergoing the URFC cycles and re- the Ni oxides. The change in the PtO/Pt peak ratio indicated that
covery process. The HAADF-STEM images revealed the presence Pt was oxidized after the OER and reduced after recovery. Inter-
of oxidized Pt on the outer surface of PtNi-octa after the URFC estingly, the NiO/Ni peak ratio increased after recovery because
cycles, which disappeared after recovery (Figure 3d–f). some Ni atoms were oxidized by accepting the oxygen detached
The surface properties of each element after each step of the from Pt. Even after recovery, the oxidized Ni was not reduced.
cycle (ORR, OER, recovery, and OCV) were further examined by These results are consistent with those from half-cell cycle tests
XPS. First, the chemical oxidation of Ni was observed in pristine (Figure 3a). Although the ORR performance deteriorated with-
PtNi-octa even before the URFC cycles when it was immersed in out the recovery process, the OER performance was maintained
an alkaline electrolyte.[20] This was supported by the XPS spec- because oxidized Ni was still present on the surface. Thus, the re-
trum (Figure S12, Supporting Information), which suggested an covery mostly contributed to the reduction of oxidized Pt atoms
increase in the peak ratio of Ni oxide to Ni metal. A comparison so that the change in the NiO/Ni peak ratio was smaller than that
of the in situ/operando XANES spectrum of the OCV state and in the PtO/Pt peak ratio. The PtO/Pt peak ratio increased after
the ex situ XANES spectrum (Figure S13, Supporting Informa- the OER because of Pt oxidation and decreased after recovery
tion) also indicated an evident shift in the oxidation state. The owing to Pt oxide reduction, while Ni maintained its oxidation
metallic Ni content, as estimated by linear combination fitting, state (Figure S14, Supporting Information). A comparison of the
was ≈33.2% in as-prepared PtNi-octa and ≈30.7% at the OCV IL-TEM images before and after the URFC process with recov-
state immersed in the electrolyte. ery (Figures S20 and S21, Supporting Information) showed that
To investigate the change of oxidation state of Pt and Ni during there was no significant shape change or degradation. As men-
URFC operation with recovery, peak ratios of Pt oxides and Ni ox- tioned above, Ni atoms were mostly located on the facets and Pt
ides to Pt and Ni metal were exhibited in Figure 3c and Figure S14 atoms at the edges.
(Supporting Information). Ni further underwent electrochemical To summarize, Ni atoms were easily oxidized upon immer-
oxidation during the ORR because the operational potential re- sion in an alkaline electrolyte and then dealloyed into the sur-
gion was above 0.6 VRHE (Figure 3f).[21] To determine the atomic face, turning the (111) facets into Ni-oxide-rich facets and passi-
ratio at the surface, the change in the peak ratio of PtO to NiO vating the Pt atoms on these facets. The Pt atoms at the edges
was calculated (Figure S14, Supporting Information) from the could be oxidized and reduced during the URFC and recovery
deconvoluted Ni 3p and Pt 4f spectra taken after each URFC step process, which could restore their catalytic performance. The se-
(Figures S15 and S16, Supporting Information). The Ni 3p spec- ries of morphological and structural changes during each step
tra were chosen to calculate the atomic ratio because they were of the URFC cycles with recovery are schematically illustrated in
obtained under the same conditions as the Pt 4f spectra.[22] Dur- Figure 3c.
ing the URFC process, Ni atoms diffused to the surface via deal- Finally, PtNi-octa was utilized in an AEM-URFC single-cell sys-
loying, and the ratio of surface Ni atoms to Pt atoms increased. tem, which could be operated in two modes: water electrolysis
The peak ratio of PtO to NiO sharply decreased after the ORR (Figure 4a) and fuel cell (Figure 4b). Using a MEA-type cell, polar-
(Figure 3c), suggesting that Ni atoms moved from the interior to ization curves were obtained to compare the ORR and OER per-
the surface, especially the (111) facets of PtNi-octa.[14a,23] The ox- formances of the catalysts. PtNi-octa had much higher ORR and
idizing of Ni had started when it immersed in the electrolyte as OER activities than PtB–NiB and Pt–Ni/C, having current densi-
shown in Figures S12 and S13 (Supporting Information). Con- ties of −0.5 A cm−2 at 0.3 V (cell voltage) and 0.5 A cm−2 at 2.0 V
sequently, the (111) facets became Ni-oxide-rich facets, thereby (cell voltage) (Figure 4c). At a current density of 100 mA cm−2 ,
passivating the Pt atoms on these facets. Consequently, these PtNi-octa showed 46% round trip efficiency, while PtB-NiB had a
Pt atoms formed PtNiO, in which oxygen is bonded to both Ni lower efficiency of 37%. It is difficult to compare the single-cell
and Pt. The XRD spectrum taken after the ORR step showed the performance of the catalysts with those obtained in other stud-
appearance of an additional peak at ≈42.5° attributed to PtNiO ies because of differences in MEA fabrication parameters and
(JCPDS card no. 01-076-1245) (Figure S17, Supporting Informa- operating conditions, such as the loading amount, membrane
tion). Additionally, the dealloying of Ni was confirmed by the shift type, binder type and ratio, and operating temperature, which
of the peaks of the (111) and (200) facets of PtNi-octa, attributed all directly affect cell performance. However, only a few stud-
to the Pt and Ni metals, respectively, from 40.05° and 46.45° to ies have conducted the single-cell procedure for AEM-URFCs.
39.82° and 44.36°, respectively.[14a,23c,d] As references of Pt and Ni Even when bifunctional electrocatalysts were applied to the sin-
metal peaks, the XRD spectra of the black and carbon-supported gle cell, their catalytic performance was too low and could not be
mixtures are shown in Figures S16 and S17 (Supporting Infor- maintained over a few cycles.[4c,25] By utilizing PtNi-octa with a
mation). recovery process, long-term operation of the AEM-URFC single
Because the synthesis of PtNi-octa was initiated by the con- cell over 10 cycles could proceed without cell potential degrada-
struction of the frames of the alloy (i.e., edges) with Pt atoms, fol- tion (Figure 4e). Pt–Ni/C also maintained its performance with-
lowed by the filling of the facets with Ni and Pt atoms,[24] the Pt out severe degradation. On the other hand, without a recovery
atoms at the edges were not covered by Ni oxides. Thus, they were treatment, the potential driving the ORR of PtNi-octa decreased
oxidized during the OER in the alkaline electrolyte (Figure 3c). gradually, then rapidly after 5 cycles. Unlike in the half-cell sys-
Without recovery, they remained in the oxidized state after the tem, PtB–NiB could not maintain its performance in the single-
OER, leading to hindered oxygen diffusion by their oxides and cell system since this system is affected by several factors. In the
a decrease in the ORR activity. However, after recovery, oxygens case of black mixtures such as PtB–NiB, the low conductivity of
were detached from the Pt atoms at the edges, whereas the Pt on a metal alloy without a substrate could cause more damage to
the (111) facets could not be reduced because of passivation by the membrane, resulting in severe losses in performance and
Figure 4. Unitized regenerative fuel cell (URFC) performance and durability of Pt–Ni octahedron (PtNi-octa). Schematic diagrams of a) water electrolysis
and b) fuel cell modes. c) URFC performance of PtNi-octa, PtB-NiB, and Pt-Ni/C. d) URFC performance of PtNi-octa after durability tests with and without
recovery. e) Long-term-operation URFC performance at 10 mA cm‒2 for 200 min. The operation comprised ten cycles of the URFC and recovery process,
with each cycle performed for 10 min.
stability after only 3 cycles, as confirmed by the polarization curve decrease the OER performance of Pt–Ni/C. Finally, we demon-
after the URFC process (Figure S22, Supporting Information). strated that the single-cell system could also operate at a high
Notably, its OER performance had slightly increased after the current density of 100 mA cm‒2 for 5 cycles with a duration of
URFC process because Ni was oxidized after URFC which had 100 min (Figure S24, Supporting Information).
better activity for OER. Similar to the results of the half-cell test,
the ORR polarization curve of PtNi-octa maintained its shape af- 3. Conclusion
ter the URFC process with recovery, although the catalyst per-
formance completely degraded without recovery (Figure 4d). Al- In summary, we studied the effect of electrochemical recovery
though Pt–Ni/C could preserve its activity at low current density treatment on a PtNi-octa alloy as a bifunctional catalyst for AEM-
during the URFC cycles, its polarization curve showed degrada- URFCs. Pt and Ir/Ni mixtures usually have the problem of Pt
tion similar to that in the half-cell test (Figure S23, Supporting dissolution during the OER. To solve this problem, PtNi-octa was
Information). Compared to the polarization curve after URFC of synthesized and applied to the oxygen electrode, which achieved
PtB–NiB and PtNi-octa, Pt–Ni/C showed degradation of OER per- low Pt dissolution and high mass activity due to Ni passiva-
formance (Figure S23, Supporting Information). This can be ex- tion and electronic structure change. However, because Pt oxides
plained by the carbon corrosion of Ni/C that recovery process was formed after the OER, degradation of the ORR activity of Pt was
applied to Pt/C and Pt atoms in PtNi-octa where Ni/C was not observed. The ORR performance was restored through electro-
treated. Therefore, carbon corrosion from Ni/C could possibly chemical recovery, involving the removal of oxygen atoms from
the Pt atoms. The AEM-URFC single cell with PtNi-octa showed of anion ionomer (Sustainion XA-9, Dioxide Materials) solution were fully
a stable performance over 10 cycles. Further studies, including dispersed in 4 mL of isopropyl alcohol. To prepare the Pt–Ni/C ink, Pt/C,
the optimization of the potential region for the recovery process and Ni/C were mixed at the same weight ratio as that used for PtNi-octa. To
be specific, 26.1 mg of Pt/C, 20 mg of Ni/C, and 307 mg of anion ionomer
and investigating the effect of recovery on other single-cell com-
(Sustainion XA-9, Dioxide Materials) solution were fully dispersed in 8 mL
ponents such as the membrane and anode, are required to better of isopropyl alcohol. The prepared inks were deposited on the GDL using a
understand Pt-based catalysts and the applicability of the recov- spray at 70 °C. The area of the substrate was 5 cm2 with loading densities
ery treatment to other non-noble metal catalysts for AEM-URFCs. of 1mgPt+Ni cm−2 and 0.4 mgPt cm−2 for oxygen electrode and hydrogen
This recovery method offers a new direction for the development electrode, respectively.
of AEM-URFCs. Electrochemical Measurements: A three-electrode system consisting of
a Hg/HgO electrode as the reference electrode and a graphite rod as the
counter electrode was utilized for all electrochemical measurements. The
catalyst inks were composed of 2.49 mL of isopropyl alcohol, 2.49 mL of
deionized water, and 20 μL of Nafion solution with 5 mg of the catalyst.
4. Experimental Section They were fully dispersed by ultrasonication for 30 min, dropped onto
Preparation of Octahedral PtNi (PtNi-Octa) Catalyst: To synthesize a rotating disk electrode (RDE; area = 0.196 cm2 , Pine Instruments) or
PtNi-octa, 4 mm of platinum(II) acetylacetonate (Pt(acac)2 ; 98%, Acros rotating ring-disk electrode (RRDE; area = 0.241 cm2 , Pine Instruments)
Organics) and 4 mm of nickel acetylacetonate (Ni(acac)2 ; 96%, Acros at a loading density of 50 μgmetal cm−2 , and dried. Electrochemical mea-
Organics) were dissolved in 50 mL of N,N-dimethylformamide solution surements (VSP-3e, BioLogic SAS) were conducted in O2 -saturated 0.1 m
(>99.8%, Sigma–Aldrich), and the solution was vigorously stirred for KOH. Linear sweep voltammetry (LSV) was performed at the potential re-
30 min. Subsequently, the as-prepared solution was transferred to the gions of 1.2–0.2 VRHE for the ORR and 1.2–2.0 VRHE for the OER at a scan
glass liner of an autoclave. The glass-lined stainless-steel autoclave was rate of 10 mV s−1 and rotation rate of 1600 rpm. All the LSV measure-
heated and maintained at 200 °C for 12 h with magnetic stirring. After ments were based on three times experiments. The RRDE voltammograms
cooling the solution to room temperature, 32.45 mg of Vulcan XC72 car- were obtained by applying a ring potential of 1.23 VRHE . Recovery cyclic
bon black was dispersed in the solution by strong ultrasonication and vig- voltammetry (CV) was performed under the same conditions as those for
orous stirring for 60 min. The final catalyst was filtered and washed with the LSV measurements at the negative potential range from −0.1 to −0.8
a mixture of deionized water and ethanol. After drying, carbon-supported VRHE . For the half-cell URFC test, chronoamperometry was conducted at
PtNi-octa was obtained. 2 mA cm−2 for the OER and −2 mA cm−2 for the OER using the RDE.
Material Characterizations: The structure and morphology of the pre- The same potential region for the ORR was used, and a ring potential of
pared electrocatalysts were observed by TEM (Titan 300 keV, FEI) and 1.23 VRHE was applied. The prepared electrodes were used for the XRD and
high-angle annular dark-field scanning transmission electron microscopy XPS measurements. Under the same conditions as those for the LSV mea-
(HAADF-STEM; Titan 300 keV, FEI) with electron energy loss spectroscopy surements, 0.8 VRHE was applied for 1 h to prepare the post-ORR sample.
(EELS). The atomic distributions of Pt and Ni were investigated by energy- To prepare the post-OER sample, the ORR step was performed, followed
dispersive X-ray spectroscopy (EDS; Talos F200X, FEI). Structural changes by the application of 1.7 VRHE for 1 h. After preparing the post-OER sam-
after the experiments were studied by IL-TEM (Titan 300 keV, FEI). The ple, the recovery step was conducted by CV for 50 cycles at a scan rate of
crystalline structure of carbon-supported PtNi-octa was confirmed by X-ray 100 mV s−1 .
diffraction (XRD; SmartLab, Rigaku) using Cu K𝛼 radiation. The surface URFC Single-Cell Measurement: URFC single-cell measurements of
properties of the catalysts were investigated by XPS (Nexsa G2, Thermo the as-prepared electrodes and AEM (Fumasep FAA-3-50, Fuelcellstore)
Scientific). The ratio of each metal configuration was measured by induc- in a membrane–electrode assembly (MEA) were performed in an alka-
tively coupled plasma optical emission spectroscopy (ICP-OES; iCAP 7000 line electrolyte using a potentiostat (VSP-3e, BioLogic SAS). Before the
series, Thermo Scientific). Changes in the electronic structures of the cata- single-cell experiments, the alkaline electrolyte was sufficiently bubbled
lysts during the experiments were investigated by XAS using the 1D beam- with high-purity nitrogen gas (>99.99%) for 1 h to prevent degradation
line in the Pohang Accelerator Laboratory (Pohang, South Korea). The dis- by carbon dioxide. To activate the ionomer used in electrode fabrication,
solution of Pt and Ni was monitored by ICP-MS (iCAP RQ, Thermo Scien- all electrodes were immersed in 1 m KOH for 1 h before the tests. In the
tific). fuel cell mode, hydrated oxygen and hydrogen were supplied at a constant
Electrodes Preparation: The synthesized and commercial metal cata- rate of 150 mL min−1 at 50 °C with a 1.5 bar back pressure applied. In the
lysts were deposited on the gas diffusion layer (GDL; Sigracet 39BB, SGL water electrolysis mode, a N2 -saturated alkaline electrolyte (0.1 m KOH)
Carbon) to be used as the cathode and anode in half-cell and URFC single- flowed at 15 mL min−1 without back pressure. During the recovery CV,
cell systems. For XPS and XRD measurements, 10 mg of PtNi-octa pow- humidified hydrogen gas was supplied to the hydrogen compartment and
der was dispersed in 2 mL of isopropyl alcohol (>99.7%, Sigma–Aldrich) the alkaline electrolyte to the oxygen compartment to eliminate the overpo-
with 66.7 mg of Nafion solution (5 wt%, Sigma–Aldrich) by ultrasonica- tential at the hydrogen compartment. The URFC experiments proceeded
tion to prepare a catalyst ink. The prepared ink was sprayed directly on in the order of the ORR, OER, and recovery CV for one cycle. Chronopo-
the GDL with an area of 1 cm2 and a loading density of 1 mgPt+Ni cm−2 . tentiometry was conducted at −10 mA cm−2 for the ORR step and
For the URFC single-cell system, a Sustainion XA-9 solution (Dioxide Ma- 10 mA cm−2 for the OER step. Subsequently, recovery CV was performed
terials) was used instead of the Nafion solution for delivering hydroxide in the potential range from −0.1 to −0.8 VRHE for 10 cycles.
ions in an alkaline electrolyte. Pt black and Ni black mixture (denoted as In Situ/Operando XAS and ICP-MS: In situ/operando XAS was per-
PtB–NiB) consisting of commercial Pt black (Thermo Scientific) and Ni formed using a homemade electrochemical flow cell. The set-up details
black (99.99%, Sigma–Aldrich), Pt supported on carbon (Pt/C) and Ni were reported in a previous paper.[26] The OER electrocatalysts were de-
supported on carbon (Ni/C) mixture (denoted as Pt–Ni/C) consisting of posited on the surface of a thin carbon film in contact with O2 -saturated
Pt/C (46 wt%, TKK) and Ni/C (20 wt%, Premetek), and PtNi-octa were 0.1 m KOH. Graphite and Ag/AgCl electrodes were installed on the back
used as bifunctional oxygen electrodes, and commercial Pt/C (46 wt%, of the flow cell. Potentials of 0.8 VRHE and 1.7 VRHE were applied for the
TKK) was used as a hydrogen bifunctional electrode. The same composi- ORR and OER experiments, respectively. The potential region from −0.1
tion of ink was used to manufacture the PtNi-octa electrode. To prepare to −0.8 VRHE was used for the recovery CV.
the PtB-NiB ink, Pt black and Ni black were mixed at the same weight ra- The dissolution of Pt and Ni in the catalysts was detected by online
tio as that used for PtNi-octa. To be specific, 15 mg of Pt black, 5 mg of ICP-MS. An electrochemical flow cell with three electrodes was equipped
Ni black, and 22.23 mg of anion ionomer (Sustainion XA-9, Dioxide Ma- with a U-shaped channel with a diameter of 1 mm and an opening for
terials) solution were dispersed in 2 mL of isopropyl alcohol by ultrasoni- possible contact with a glassy carbon working electrode (disk diameter =
cation. To prepare the Pt/C ink, 20 mg of commercial Pt/C and 133.4 mg 1 mm, GC-3155, EC Frontier). A catalyst ink was prepared by dispersing
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Activity Restoration of Pt–Ni Octahedron via Phase

C. Oh, M. H. Han, Y.-J. Ko, W. H. Lee, H.-S. Oh P. Strasser

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