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Adjusting the Anisotropy of 1D Sb2se3 Nanostructures for Highly Efficient Photoelectrochemical Water Splitting

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Adjusting the Anisotropy of 1D Sb2se3 Nanostructures for Highly Efficient Photoelectrochemical Water Splitting FULL PAPER Water Splitting www.advenergymat.de Adjusting the Anisotropy of 1D Sb2Se3 Nanostructures for Highly Efficient Photoelectrochemical Water Splitting Wooseok Yang, Jihoon Ahn, Yunjung Oh, Jeiwan Tan, Hyungsoo Lee, Jaemin Park, Hyeok-Chan Kwon, Juran Kim, William Jo, Joosun Kim, and Jooho Moon* in a single device.[2] Semiconductor mate- Sb2Se3 has recently spurred great interest as a promising light-absorbing rials in a PEC device transform absorbed material for solar energy conversion. Sb2Se3 consists of 1D covalently linked photons into excited electronic states that nanoribbons stacked via van der Waals forces and its properties strongly drive the electrochemical reaction at the semiconductor–electrolyte interface. To depend on the crystallographic orientation. However, strategies for adjusting date, numerous semiconductors have the anisotropy of 1D Sb2Se3 nanostructures are rarely investigated. Here, a been reported as photoelectrodes for PEC [3,4] novel approach is presented to fabricate 1D Sb2Se3 nanostructure arrays with water splitting, including Si, III–V different aspect ratios on conductive substrates by simply spin-coating Sb-Se group elements,[5,6] metal oxides,[7,8] Cu- [9,10] [11] solutions with different molar ratios of thioglycolic acid and ethanolamine. chalcogenides, and polymers. How- A relatively small proportion of thioglycolic acid induces the growth of short ever, until now, a nontoxic and low-cost material that can be obtained with scalable Sb2Se3 nanorod arrays with preferred orientation, leading to fast carrier processing is not available and therefore, transport and enhanced photocurrent. After the deposition of TiO2 and Pt, there is ongoing intensive research for an appropriately oriented Sb2Se3 nanostructure array exhibits a significantly exploring new absorber materials. enhanced photoelectrochemical performance; the photocurrent reaches Antimony triselenide (Sb2Se3), com- 12.5 mA cm−2 at 0 V versus reversible hydrogen electrode under air mass posed of comparatively abundant and low-toxic constituents, is an attractive 1.5 global illumination. p-type semiconductor for PEC hydrogen production owing to its narrow band gap of 1.0–1.3 eV, high absorption coefficient 5 −1 [12] 1. Introduction (>10 cm ), and high hole mobility. Moreover, Sb2Se3 is a simple binary compound with uniquely a thermodynamically Inspired by natural photosynthesis, storing solar energy in the stable orthorhombic phase, which allows avoiding the com- form of chemical fuels via artificial photosynthesis is one of plexities associated with phase- and defect-control, as encoun- the most promising ways to realize sustainable energy. Among tered in other p-type semiconductors such as Cu(In,Ga)(S,Se)2 the available chemical fuels, hydrogen produced from water is and Cu2ZnSn(S,Se)4. With its promising properties, Sb2Se3 has attractive because of the ubiquitous availability of water and been applied in diverse optoelectronic and energy conversion its low-carbon footprint.[1] Solar hydrogen production can be devices such as solar cells,[13] thermoelectric devices,[14] photo- accomplished by a photoelectrochemical (PEC) system, which detectors,[15] PEC cells,[16] and lithium/sodium ion batteries.[17] simultaneously functions as a light harvester and electrolyzer Recently, efficient photocathodes for PEC water splitting based [18,19] on Sb2Se3 have been reported. Our group also reported a novel method to fabricate Sb Se nanoneedle arrays, to serve as W. Yang, Dr. J. Ahn, Y. Oh, J. Tan, H. Lee, J. Park, H.-C. Kwon, 2 3 Prof. J. Moon a photocathode for PEC water splitting, by facile spin-coating Department of Materials Science and Engineering of a precursor solution without any complicated processes.[20] Yonsei University Despite the unique growth behavior of the Sb2Se3 nanostruc- 50 Yonsei-ro, Seodaemun-gu, Seoul 03722, Republic of Korea tures, the growth mechanism and the chemistry of the Sb-Se E-mail: [email protected] precursor solution has not yet been elucidated. To establish a J. Kim, Prof. W. Jo Department of Physics reliable strategy to control the Sb2Se3 nanostructures, under- Ewha Womans University standing the molecular structure of the involved precursor spe- Ewhayeodae-gil 50, Seodaemun-gu, Seoul 03760, Republic of Korea cies and their interactions in the solvent is imperative. Dr. J. Kim Controlling the shapes of semiconductor nanomaterials has High-Temperature Energy Materials Research Center been of great interest because their optical and electrical proper- Korea Institute of Science and Technology ties are significantly influenced by the structures of their constit- Seoul 02792, Republic of Korea uent materials.[21] In particular, Sb Se consists of accumulated The ORCID identification number(s) for the author(s) of this article 2 3 can be found under https://doi.org/10.1002/aenm.201702888. [Sb4Se6]n nanoribbons stacked through van der Waals forces along the [100] and [010] axes, whereas strong covalent bonds DOI: 10.1002/aenm.201702888 exist along the [001] axis, resulting in a preferred anisotropic Adv. Energy Mater. 2018, 8, 1702888 1702888 (1 of 11) © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.advancedsciencenews.com www.advenergymat.de [12] growth of Sb2Se3. This anisotropy leads to anisotropic car- toward the positive direction likely results from reduced elec- rier mobility depending on the transport direction, with the tron density on the sulfur atom owing to the deprotonation of hole mobilities in a single grain along the [100], [010], and [001] the carboxylic acid group.[32] Simultaneously, the peak intensi- directions being 1.17, 0.69, and 2.59 cm2 V−1 s−2, respectively.[22] ties of CCOOH stretching (≈907 cm−1) and CO stretching −1 − −1 Thus, the efficiencies of thermally evaporated Sb2Se3 thin films (≈1725 cm ) decrease, whereas that of CCOO (≈930 cm ) solar cells are reportedly strongly dependent on their crystallo- increases with increasing mixing ratio of EA (Figure 1b,c), graphic orientation.[23,24] Although some studies on synthesis indicating that the carbonyl group (CO) disappears as the car- [25,26] [33] of Sb2Se3 nanowires have been reported; however, the boxylate anion is produced. When the molar ratio of TGA: influence of varying the 1D Sb2Se3 nanostructure on the photo- EA is 40:60, the peaks of CCOOH and CO stretching even- electrode performance is rarely investigated. tually disappear with the concomitant appearance of the NH2 Here, we demonstrate a novel molecular solution approach stretching band at 3100–3500 cm−1 (Figure 1b–d). In addition, −1 for implementing the Sb2Se3 nanostructure arrays as photo- the SH stretching band at 2573 cm diminishes in intensity cathodes for PEC water splitting. Shape-controlled Sb2Se3 with increasing ratio of EA, simply due to the reduced propor- nanostructures were obtained by simply adjusting the sol- tion of TGA, and rather not owing to the intersolvent interac- vent ratio of thioglycolic acid (TGA) and ethanolamine tion, because significant amount of the thiol group (SH) still (EA). A mixture of thiol-amine, the so-called “alkahest,” is remained in TGA: EA = 40:60 (Figure 1e). Our liquid Raman known to be a strong solvent system capable of dissolving analysis clearly shows that by mixing TGA and EA, amine diverse compounds, including metals, oxides, and chalcoge- deprotonates the carboxylic acid (Figure 1f), releasing the car- nides.[27] High-quality metal chalcogenide thin films could boxylate anions (CCOO−), without producing thiolate (CS−) be obtained by a recovering process involving a sequence of that has been commonly observed in other thiol-amine sys- dissolving a precursor powder, followed by coating the solu- tems.[34] Although the use of TGA/EA has been already reported tion and annealing. Although numerous chalcogenide thin as a solvent for preparing chalcogenide thin films,[35,36] deproto- films such as CdS, CuInS2, CuZnSnS4, SnS, and V2VI3 have nation of the carboxylic acid group in a mixture of TGA and EA been prepared,[28–30] nanostructuring strategies through the is confirmed for the first time. This is in accordance with lower thiol-amine system have been elusive. For the first time, pKa of the carboxylic acid group (3.83) than that of the thiol we elucidate the role of the carboxylate nucleophile in dis- group (9.3) in TGA, indicating that the deprotonation of the solving the chalcogen materials, whereas studies on the pre- carboxylic acid is preferred over that of the thiol. The formed viously developed alkahest solution-derived chalcogenide carboxylate anion is expected to play a unique role in the prepa- materials focused on the role of the thiolate nucleophile. The ration of the chalcogen precursor solution in TGA/EA mixture, chemistry of the Sb-Se precursor solution is elucidated by which is clearly different from the previously reported thiolate- liquid Raman spectroscopy, and the possible growth mecha- mediated dissolution of the chalcogenide species because the nism is proposed. Deposition of TiO2 and Pt on the shape- carboxylate anion is a much weaker nucleophile than the thi- controlled Sb2Se3 nanostructures enabled us to demonstrate olate anion. a remarkable device performance, reaching a photocurrent After analyzing the molecular structures of the TGA-EA mix- of 12.5 mA cm−2 at 0 V versus reversible hydrogen electrode ture solvent, we prepared three different Sb-Se precursor solu- under air mass 1.5 global (AM 1.5 G) illumination. tions. Three different Se solutions were prepared by adding Se powders into TGA/EA mixtures of varying molar ratios (TGA: EA = 5:95, 20:80, and 40:60). The Sb solutions were pre- 2. Results pared by dissolving SbCl3 in 2-methoxyethanol (2ME). Note that except for the TGA: EA molar ratio, all other parameters 2.1. Preparation and Analysis of Sb-Se Precursor Solution including the concentration of Sb and Se were fixed. Three different Sb-Se precursor solutions were obtained by mixing Identification of the growth mechanism of solution-derived the individual Sb and Se solutions, which are referred hereafter 1D nanostructures requires an in-depth understanding of the as TGA 5, TGA 20, and TGA 40 Sb-Se solutions, respectively.
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