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Integrated Photoelectrolysis of Water Implemented On Organic Metal Halide Perovskite Photoelectrode Minh Tam Hoang, Ngoc Duy Pham, Ji Hun Han, James M. Gardner, and Ilwhan Oh ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.6b03478 • Publication Date (Web): 27 Apr 2016 Downloaded from http://pubs.acs.org on May 5, 2016

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Integrated Photoelectrolysis of Water Implemented On Organic Metal Halide Perovskite Photoelectrode Minh Tam Hoang†, Ngoc Duy Pham†, Ji Hun Han†, James M. Gardner┴, and Ilwhan Oh†,∗

†

Department of Applied Chemistry, Kumoh National Institute of Technology, Gumi, 730-701, Republic of

Korea ┴

Department of Chemistry, Division of Applied Physical Chemistry, School for Chemical Sciences, KTH

Royal Institute of Technology, Teknikringen 30, SE-114 28 Stockholm, Sweden

Corresponding author: *E-mail: [email protected] (I.O.)

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Abstract

Herein we report on integrated photoelectrolysis of water employing organic metal halide (OMH) perovskite material. Generic OMH perovskite material and device architecture are highly susceptible to degradation by moisture and water. We found that decomposition of perovskite devices proceeds by water ingress through pinholes in upper layers and is strongly affected by applied bias/light and electrolyte pH. It was also found that a pinholefree hole transport layer (HTL) could significantly enhance the stability of the perovskite photoelectrode, thereby extending the photoelectrode lifetime to several tens of minutes, which is an unprecedented record-long operation. Furthermore, a carbon nanotube (CNT)/polymer composite layer was developed that can effectively protect the underlying perovskite layer from electrolyte molecules.

Keywords: Perovskite, water photolysis, photocathode, solar energy, photoelectrochemistry.


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In the 2015 Paris Climate Conference, leaders from around the world emphasized the ever increasing threat of global warming to mankind.1 Carbon emission from fossil fuels should be reduced substantially by replacing conventional energy technology with sustainable ones, such as solar cells. Even though the cost of solar energy reduced remarkably in the last decade, further cost reduction is required to reach grid parity with the conventional energy.

Additionally, development of energy storage system (ESS) is

required, which can produce electricity only during daytime. In recent years, organic metal halides (OMH) perovskites have emerged as promising materials for solar energy conversion, and have galvanized the solar cell community2-7. With a generic chemical formula of CH3NH3PbI3 (MAPbI3), this exciting material can be synthesized at low temperature via low-cost solution processing. Unlike other semiconductor materials synthesized at low temperature, the OMH perovskite materials exhibit excellent optoelectronic properties including large absorption coefficient and a long carrier diffusion length. Even though the current worldwide research activities on OMH perovskites are mostly focused on photovoltaics, solar water splitting is another relevant field that might benefit from the emerging OMH perovskite materials. Due to the intermittent nature of solar energy, storing solar energy in chemical fuels is necessary to compliment photovoltaics. Although some studies are already reported on perovskite-based water splitting,

8-9

they can be categorized into the photovoltaic-electrolyzer configuration, where

perovskite cells are separated from the fuel-generating electrolyzer. On the other hand, the integrated photoelectrolysis is an alternative configuration, which involves intimate contact between the photoelectrode and electrolyte with the merits of simplified wiring and saved space10.

A detailed

comparison between the integrated photoelectrolysis and the series-connected PV-electrolyzer system have shown that the integrated system can leverage enhanced kinetics and mass transport at elevated temperature and outperform the PV-electrolyzer device on the basis of annual hydrogen yield11-12. In a more recent report, a breakthrough was reported that perovskite cells can be directly immersed in electrolyte and electrolysis can be performed at least for a short period.13 However, in order to realize unassisted H2 generation, a sacrificial agent (sulfide) was utilized; the electrolysis will stop after the sacrificial agent is completely consumed. Overall, although the pioneering studies involved light-driven



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water splitting by OMH perovskites, integrated photoelectrolysis of water employing perovskite photoelectrodes is yet to be investigated. Here in this report, we have demonstrated for the first time that integrated photoelectrolysis of water is possible with OMH perovskite materials. We have observed that minimizing pinholes in the upper layer can substantially stabilize the perovskite photoelectrode in aqueous electrolyte (for an hour). Furthermore, we have found that a carbon nanotube (CNT)/polymer composite layer provides enhanced protection to the perovskite photoelectrode, significantly extending the lifetime of the perovskite photoelectrode. We first fabricated photoelectrodes from a generic perovskite device and constructed an integrated photoelectrolysis cell. Figure 1A depicts the photoelectrolysis cell employed in this work, which is composed of perovskite photoanode directly in contact with liquid electrolyte, a hydrogen-evolving Pt counter electrode, and a reference electrode. Following the previously reported fabrication method for high-performance perovskite solar cells,14 we made the perovskite photoanode having the most widely adapted device structure for perovskite solar cells. Our perovskite photoanode was composed of mesoporous (mp) TiO2 layer as electron transport layer (ETL), MAPbI3 perovskite material infiltrating the mp-TiO2, spiro-MeOTAD as hole transport layer (HTL) and finally a thin gold layer as the electrode (Details of cell fabrication are in Supporting Information). In addition to this generic perovskite device structure, a thin layer of Ni was deposited which functioned as a catalyst for OER. In Figure 1B is shown a cross-sectional SEM image of the perovskite photoelectrode. Smooth and clear interfaces between different layers are evident. Under sunlight illumination, photons pass through the transparent FTO glass and ETL (TiO2) before they are absorbed by the perovskite layer and generate electron-hole pairs. Due to the electric field at the junction, the photo-generated electrons move to the ETL and then flow toward the Pt counter electrode through the external circuit. At the same time, the photo-generated holes are collected by the HTL and drawn toward the catalyst/electrolyte interface where the OER occurs.


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Figure 1. (A) Schematic illustration of integrated photoelectrolysis cell with perovskite photoelectrode; (B) SEM crosssectional image of the perovskite device employed; (C) X-ray diffraction spectrum for the perovskite film formed on porous TiO2/FTO glass substrate. (D) J-V curve for the solid-state perovskite cell under standard AM1.5 illumination (100 mW/cm2)

In order to confirm the formation of the MAPbI3 perovskite layer, x-ray diffraction (XRD) was carried out. The XRD pattern of MAPbI3 thin film on TiO2/FTO glass is shown in Figure 1C. The sharp diffraction peaks corresponded to the (110), (112), (202), (220), and (310) lattice planes belonging to tetragonal crystal structure of MAPbI3, which was consistent with the literature. 15 Prior to assessment in photoelectrolysis cell, the performance of the solid-state perovskite cell was measured. As the current density-voltage (J-V) graph in Figure 1D shows, our solid-state solar cell exhibited a decent cell performance metrics (open-circuit voltage of 1.06V, short-circuit current density of 18.3 mA/cm2, and power conversion efficiency (PCE) of 14.4%). We found that adding an ultra-thin Ni layer had little effect on the



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performance of the solid-state cells. However, the Ni catalyst layer had a large effect on the photoelectrochemistry of the perovskite photoanode, as discussed below. Performance of the perovskite photoanodes in integrated photoelectrolysis was examined in a three-electrode configuration, as depicted in Fig 1A. The perovskite photoanode was immersed in electrolyte, and bias voltage and simulated sunlight were applied to the perovskite photoanode. In the J-V graph for the OER reaction (Figure 2A), the perovskite photoelectrode produced a substantial photocurrent (red curve), which corresponded to light-driven water oxidation to O2 (refer to Eq. 2). The photographic image in Figure 2B displays O2 bubbles emerging from the active area of photoanode (see Supporting Information for a video of gas evolution). As control experiments, the dotted line in Figure 2A corresponds to the perovskite photoanode without illumination and exhibits a very small dark current, which proves that the current observed upon illumination was photon-generated. The perovskite photoanode without Ni (bare Au; blue curve) exhibited smaller current (9.2 mA/cm2 at 1.23V) than the one with the Ni layer (red curve; 17.4 mA/cm2), which reflected the well-known electrocatalytic effect of Ni toward OER reaction.16 Note that the current density level of the J-V graph corresponds well with the short-circuit current density for the solid-state solar cell in Figure 1D. As a reference, a potential sweep curve of bare Ni is also shown (black curve in Figure 2A). The early peak at 1.08 V can be attributed to oxidation of Ni to nickel oxide (see the potential cycling measurement in Figure S1). It is well known that nickel oxide can function as an active catalyst for water oxidation.16 The potential difference between the perovskite photoanode and the bare Ni electrode was about ~0.8V, which is the photovoltage gained by the perovskite photoanode. Note that the observed photovoltage is close to the open-circuit voltage of the solid-state cell in Figure 1D.


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Figure 2. (A) Voltammogram of perovskite photoanodes with uppermost thin Ni catalyst (red curve), with no Ni catalyst (bare Au electrode; blue curve) under simulated illumination (0.7 sun). For comparison, voltammogram under dark condition (dotted curve) and on metallic Ni electrode (black) is also shown. (B) Photographic image of active area on photoanode surface with oxygen bubbles emerging from surface. (circle diameter = 5 mm)

Now that it had been demonstrated that perovskite electrodes could drive light-driven photoelectrolysis, the next important pending task was to assess and enhance the stability of the perovskite photoanode in aqueous electrolyte. The MAPbI3 perovskite material is notoriously sensitive toward moisture and water. In working perovskite devices, however, the perovskite material is covered with several upper layers, such as HTL and metal layers, which can provide additional protection against moisture and water. So the key to development of practical perovskite-based integrated photoelectrolysis is to build and optimize the upper layers that can effectively block electrolyte molecules from attacking the underlying perovskite layer. We first examined the stability of the perovskite photoanode having the conventional device structure in aqueous electrolyte. As shown in Figure 3A, when an anodic potential of ~1.0V was applied, the perovskite photoanode maintained a substantial current level for a few hundreds of seconds. Considering the extreme sensitivity of perovskites toward water and the fact that the perovskite photoanode is in direct contact with aqueous electrolyte, even this duration of stability was remarkable. Note that the current is slightly increased at the initial stage. In

solid-state perovskite solar cells, this phenomenon is commonly observed in the I-t measurements and is attributed to slow ion migration and electronic charge traps in the perovskite film.17 However, after photoelectrolysis for about 10 min, the activity of the perovskite electrode declined to near zero, indicating that the perovskite was completely decomposed by the electrolyte. Examination of our perovskite layer after photoelectrolysis for 5 min clearly showed degradation in the perovskite layer (Figure 3B). A population of macro-sized yellow dots were observed, which suggested existence of pinholes through which electrolyte molecules could penetrate and decompose MAPbI3 to yellow PbI2. Compared to the decomposition in the absence of applied light and potential, we found that decomposition of the perovskite was faster when potential and light were applied. (Figure S2) This observation was in accordance with previous report that light and bias can accelerate the decomposition of perovskite.18 In addition, we found that the decomposition of the perovskite was strongly affected by the pH of the solution (Figure S3). In either strongly acidic (pH 1) or strongly alkaline (pH 14) electrolyte, the perovskite ACS Paragon Plus Environment


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photoanode decomposed quite fast (decomposed area ~47% after 5 min immersion), whereas in neutral electrolyte (pH 7.0 − 9.2) the decomposition was much slower (Figure S3). These results were also consistent with the stability trends in photoelectrolysis. In photoelectrolysis measurements, the photocurrent from perovskite photoanodes quickly diminished in either acidic or alkaline electrolyte (Figure S4). This phenomenon can be understood considering that all precursor molecules for OMH perovskite (CH3NH2, HI, PbI2) were either weak base or weak acid (PbI2 is a Lewis acid). Thus strong acid or strong base from electrolyte would replace the weak acid or base, thereby decomposing the perovskite material.

Figure 3. (A) Current vs. time graph of perovskite photoanode under illumination (0.7 sun) and bias (1.0V vs. SHE) in a buffer solution (pH 9.2) (B) Photograph of degraded perovskite layer after 5 min photoelectrolysis. The yellow boundary was artificially added to highlight the degraded area.

So far, it has been shown that integrated photoelectrolysis can be performed on the conventional perovskite materials and devices architecture for at least a few minutes. However, novel perovskite materials and device architectures are needed that can extend the stability. For this purpose, several approaches have been taken to achieve sustained photoelectrolysis for a longer period. Literature reported that mixed halide perovskite solar cells showed improved stability toward atmospheric humidity.19 In this regard, perovskite photoanodes made of mixed halide perovskite MAPb(I1−xBrx)3 (x=0.12) was fabricated and tested in integrated photoelectrolysis. However, no improvement was achieved with respect to long-term stability (Figure S5). This indicated that the degradation rate ACS Paragon Plus Environment

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of the perovskite photoelectrode is determined by how fast electrolyte molecules penetrate through pinholes rather than the kind of perovskite materials used, unless the material stability is significantly improved.

Figure 4. (A) Performance of solid state perovskite solar cells with pinhole-free spiro-MeOTAD layer (red curve) and with CNT/PMMA composite film (blue curve); (B) Long-term stability measurement of the modified perovskite photoanodes; (C,D) SEM images showing top view and cross section of the CNT/PMMA composite film.

These results suggested that the best strategy to enhance the stability of perovskite photoelectrode is to engineer the upper layers to reduce pinholes and block the penetration of electrolyte molecules. Indeed, it was previously reported that the spiro-MeOTAD hole transport layer contains a high density of pinholes.20 Thus we tried to reduce the number of pinholes by switching the solvent for spiro-MeOTAD (from chlorobenzene to chloroform). The perovskite photoanode with a pinhole-free HTL showed a significantly enhanced stability compared with the



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conventional device (Figure 4B). Now the perovskite photoanode can continuously operate for tens of minutes. The slow decay in activity was probably related to the fact that the spiro-MeOTAD layer contained ionic dopant (Li-TFSI), which made the spiro-MeOTAD slightly hygroscopic. Effect of the thickness of the HTL layer on stability was investigated (Figure S7), which is consistent with the expectation that thicker HTL layer would generated longer pathway of water penetration, providing better protection of the underlying perovskite layer.

In another engineering of upper layers to enhance the photoanode stability, we introduced a protection layer that can effectively block electrolyte molecules from attacking the underlying perovskite layer and at the same time can conduct charge carriers and perform electrochemical reaction. Among several promising candidates, we found that CNT/polymer composite film serves this purpose well.21 The carbon nanotubes in this composite became functionalized with poly(3-hexyl thiophene), a hole transport material,22 and deposited on perovskite layer together with poly(methyl methacrylate) (PMMA) in a simple one-step procedure (see Supporting Information for details). As shown in Figure 4C, D, the resultant film contained a functionalized CNT scaffold embedded in a PMMA water-proof layer. Note that the P3HT-functionalized CNT/polymer composite film functioned not only as interconnect between the perovskite layer and the upper catalyst layer, but also as a hole transport layer that selectively collected photo-generated holes from the perovskite layer. The solid-state device with the CNT/polymer HTL gave a decent J-V response (the blue line in Figure 4A). Voltammogram of the perovskite photoanode with the CNT/polymer layer is similar to the photoelectrode without the CNT/polymer layer (Figure S8).

Most

importantly, we found that the long-term stability of the perovskite photoanode with the CNT/polymer protective layer is significantly enhanced compared to the conventional device (blue line in Figure 4B). When the thickness of the CNT/polymer layer was changed, it was found that thicker film provides better protection of the underlying perovskite film (Figure S6). This result demonstrated that adding a water-proof protective layer is a promising method to enhance the perovskite photoanode stability. In conclusion, we have successfully demonstrated that OMH perovskite material can be employed in integrated photoelectrolysis of water into hydrogen and oxygen. The conventional OMH perovskite material and device architecture were susceptible to degradation by electrolyte molecules. The decomposition of perovskite photoanode occurred due to water ingress through pinholes and is strongly affected by applied bias/light and electrolyte pH. It was found that the pinhole-free HTL layer deposited in appropriate solvent could significantly enhance the stability ACS Paragon Plus Environment

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of the perovskite photoelectrode, extending the photoelectrode lifetime to close to one hour. In addition, a novel device structure with CNT/polymer composite layer could provide effective protection for the underlying perovskite layer and exhibited an unprecedented record-long operation. This demonstration was especially remarkable considering the fact that the photoelectrode was placed in a harsh oxidative environment. In this regard, a relevant future research will be to fabricate perovskite-based photocathodes, which can operate in a more benign reductive environment and might show even higher stability. We believe that this proof-of-concept report will pave the way to a relevant and important area of research for OMH perovskite materials.

Supporting Information.

Materials & methods, additional cyclic voltammogram, photographs of degraded

perovskite layers, additional stability data.

Acknowledgements I.O. acknowledges the support from the Korea-Sweden Collaborative Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Science, ICT and Future Planning (NRF2014K1A3A1A47067328).

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