INFLUENCE OF SURFACTANTS ON Fe 2 O 3 NANOSTRUCTURE PHOTOANODE
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1 INFLUENCE OF SURFACTANTS ON Fe 2 O 3 NANOSTRUCTURE PHOTOANODE Amir Memar, Chi M. Phan, Moses O. Tade Department of Chemical Engineering, Curtin University, Bentley, WA 6102, Australia C.Phan@curtin.edu.au ABSTRACT Fe 2 O 3 nanostructures photoanodes were prepared via sol-gel spin-coating method onto Fluorine-doped Tin oxide (FTO) glass substrates using four different surfactants: Polyethylene glycol, Triton, F127 and Cetyltrimethylammonium bromide. The resulting films have thickness from 520±10 to 980±10 nm after calcinations at 450 C in the air. A comparative study of photocatalytic activity of thin films was performed. The photogenerated samples were determined by measuring the currents and voltages under illumination of UV vis light. The highest photocurrent density of 1.58 ma/cm 2 at 1 V/SCE, under illumination intensity of 100 mwcm -2 from a solar simulator with a global AM 1.5 filter, were produced by CTAB treated sample. The optical properties, morphology, surface roughness and structure of the films were also characterized by UV-Visible Spectroscopy, SEM, AFM and XRD. The results are consistent with photocatalytic performance: CTAB treated sample has the largest grain size and the highest optical absorption. The improved performance of this sample can be attributed to the crystallinity process of CTAB which leads to the larger grain size and highest photocatalytic activity. The study demonstrates that photoelectrochemical performance of metal oxide can be improved by simply changing surfactant. Further studies with another cationic surfactants are underway to optimize the nanostructure for water splitting process. Keywords: Fe 2 O 3 nanostructure, sol-gel method, surfactant, photoanode INTRODUCTION At present, approximately 88% of the world s energy supply is derived from fossil fuel (Mu et al., 2006). Combustion of fossil fuel brings about severe pollution and contributes to greenhouse effect. Hence, developing technologies utilizing renewable energies, such as solar energy, become an urgent priority. However, storage remains the main obstacle for solar energy. Therefore, an effective energy carrier is needed. At present, the only energy carrier that can be synthesized efficiently without material limitations is hydrogen. Furthermore, the combustion of hydrogen only produces water (Winter and Nitsch, 1988). Thus, hydrogen as an energy carrier is one of the most promising yet challenging prospects among several clean and sustainable energy systems (Zheng et al., 2009). In addition to thermolysis or biological processes, hydrogen can be directly produced by photocatalytic process, i.e. splitting water (Zheng et al., 2009). This process is the most attractive due to availability and sustainability of the energy source. Nevertheless, the process is far from being economically viable (Currao, 2007). As a result, new preparation techniques (Rajeshwar et al., 2008) and semiconductive oxides (Solarska et al., 2006) have been intensively studied to improve the efficiency of water splitting. Amongst these materials, Fe 2 O 3 is known as an n-type semiconductive oxide with a band gap of 2.2 ev and a flat band potential of 0.32 V which resulted in high theoretical efficiency of 12.9% (Murphy et al., 2006). Its absorption of solar spectrum is in the range of nm which comprises 38% of the photons of the solar spectrum (Komp, 1995). Although hematite possesses many favorable characteristics, the reported water splitting efficiencies in the literature for α-fe 2 O 3 are very low (Bolton, 1996) due to its low charge carrier mobility small hole diffusion length ( 2-4 nm < light penetration
2 depth 118 nm at λ=550 nm ) and fast recombination (Bird et al., 1983) and unfavorable bandedge positions (Dare-Edwards et al., 1983). Consequently, Fe 2 O 3 nanostructure have been used to improve photoelectrochemical performance (Wheeler et al., 2012). These nanostructures have large surface area, which provides a direct pathway for electrons to transfer (Memar et al., 2010). Metal oxide nanostructures can be prepared by sputtering, chemical vapor deposition or sol-gel. Among these methods, sol-gel technology for deposition of thin nanostructure has gained impetus in the last decade owing to the low capital cost and its adaptability towards large area deposition (Miyake and Kozuka, 2005). The sol-gel process often employs surfactants to enhance the quality of the nanostructures (Zhang et al., 2009, Liu et al., 2010). However, the influence of surfactants on the structural and photoelectric properties of resulting Fe 2 O 3 film is not well understood. This study investigates the effect of different surfactants on the optical absorption, morphology, surface roughness and photo-responses of Fe 2 O 3 nanostructures. Four different surfactants were used during sol-gel spin-coating method: Polyethylene glycol, Triton, F127 and Cetyltrimethylammonium bromide. Subsequently, the films were tested in a photoelectrochemical cell and characterized by UV-Visible spectroscopy, SEM, AFM and XRD. Ultimately, the study aims to improve the photoelectrochemical performance of Fe 2 O 3 nanostructures by simply varying surfactant. EXPERIMENTAL Materials Chemical and suppliers used for this study are listed in Table 1. Fluorine-doped Tin oxide (FTO) glass with a sheet resistance of R Ω < 15 Ω cm -1 was purchased from Pilkington glass (USA). Table 1: List of the chemicals used in the study Name Formula Grade (%) Supplier Iron (III) Nitrate Fe(NO 3 ) 3.9H 2 O 99.9 Chem. supply Co. Ethanol C 2 H 6 O 70 Sigma Aldrich PEG 300 (Polyethylene glycol 300) (C 2 H 4 O) n H 2 O 99 Sigma Aldrich T-100 (Triton X-100) (C 2 H 4 O) n C 14 H 22 O 99.9 Sigma Aldrich F127 (Pluronic F127) (C 3 H 6 O.C 2 H 4 O 2 ) x 99.9 Sigma Aldrich CTAB (Cetyltrimethylammonium bromide) C 19 H 42 BrN 98.5 AMRESCO Preparation of the electrodes The four FTO conductive glasses substrates mm (width/length/thickness), were cleaned and sonicated in solvents sequentially with acetone, ethanol, acetone. The FTO glasses were separately immersed into the solvents and treated in ultrasonic bath for 15 minutes. In the final stage after rinsing, the FTO glasses were dried using nitrogen gas. The solutions were prepared according to the followings: PEG-300. Iron nitrate 2.02 g was dissolved in 20 ml ethanol under ultrasonic irradiation; then 5 ml deionized water was added into the solution. 0.2 g concentrated PEG consisting of 30 g PEG 300 and 30 g water were added to the solution and stirred for 2 hrs at room temperature, and the 0.4 mol L -1 deep red solution (ph~2) was obtained. T-100. Iron nitrate (2.5 g) was added to 1 ml water. 0.4 g Triton (X-100) was added to 1 ml ethanol and stirred for 10 minutes. Both solutions were mixed together and stirred for 2 hrs. A light red solution (ph~1.7) was obtained. 2
3 F g F127 was added to 5 ml ethanol and stirred for 20 minutes. 2 g Fe 2 O 3 was added to 1 ml deionized water. Both solutions were mixed and stirred for 3 hrs. The resultant solution was dark brown solution with (ph~1.9). CTAB. 0.5 g CTAB was added to 4 ml distilled water. The solution was stirred for 30 minutes. Then 2 g Fe 2 O 3 was added to the solution. The mixture was stirred for 2 hrs and orange solution (ph~1.5) was obtained. Fe 2 O 3 nanostructures photoanodes were prepared via sol-gel spin coating method onto FTO glass substrate, and complied with the following deposition steps: 1. A spin coater (Laurell Tech., model WS-400-6NPP) at a two fixed rotation speed 5 s (500 rpm) and 25 s (5000 rpm) where used to deposit a few drops of the resulting solution into the FTO substrate. 2. The substrate was dried on a hot plate (~50 C) for 15 minutes. 3. To enhance the interconnectivity of the particles, samples were heated at 450 ± 1 C, for 2 hrs, in air, with fixed heating and a cooling rate of 5 C/min. Photoelectrochemical cell The photoelectrochemical installation (Fig. 1) encompasses two electrodes, which are wrapped up in an aqueous electrolyte in a vessel. In this case, either electrode can be photoactive (Minggu et al., 2010). The vessel, with a quartz optical window, is filled with an aqueous electrolyte. The quartz optical window allows light to reach the photoactive electrode. The photoelectrode absorbs photons with sufficient energy to inject electrons from the valence to the conduction band of the semiconductor, creating electron-hole pairs. Holes oxidize water in the semiconductor surface and gaseous oxygen evolves at the photoanode surface. Simultaneously, hydrogen ions migrate to the cathode through the aqueous electrolyte, resulting in the reduction of hydrogen ions into gaseous hydrogen. In a laboratory investigation such as in this study, a reference electrode is typically used (this method is commonly referred to as the three electrodes cell) for solar conversion efficiency measurement. The corresponding oxidation and reduction reactions are shown in Fig. 1. Water splitting will occur when the energetic requirements are met as shown in Table 2. In practice, the cell potential should be higher than the minimum requirement to overcome overpotential and other system losses. Fig. 1: Structure of the photo-electrochemical cell 3
4 Table 2: Main PEC water splitting requirements Conditions Main requirements PEC water splitting H 2 O (liquid) + 2hυ ½O 2(gas) + H 2(gas) Minimum potential requirement E H2O (25 C) min =1.229 ev For efficient utilization of sunlight UV> hυ (Vis)> IR hυ E bandgap Characterization of electrodes The films were characterized by X-ray diffraction (XRD, Bruker D8 Advance) with Cu Kα radiation (λ = nm) and for qualitative analysis, XRD diagrams were recorded in the interval 20 2θ 60 at scan rate of 0.01 s -1. The absorbance was measured by UV Visible Spectrophotometer (JASCO, V-670 spectrophotometer). Whereas the morphology of the thin films was obtained using field emission scanning electron microscopy (FESEM, Zeiss NEON 40 EsB CrossBeam) as well as atomic force microscope (Nanoscope (R) IIIa, Digital Instruments, Santa Barbara, CA). Photoelectrochemical measurements The photocurrent measurement was carried out on a model DEA 332 digital electrochemical analyzer by applying an external potential bias to the cell and measuring the generated photocurrent under 500 W xenon lamp (100 mwcm -2, 25 C) solar simulator (Abet Technologies Model 11016A Sun 3000). The light intensity was measured by a photodiode power meter, at a scan rate of 20 mv s -1 between -1.2 and 1.2 V RHE. All photoelectrochemical measurements were performed in a three-electrode setup. The prepared films were used as the working electrode and a Pt wire and Ag/AgCl electrode were used as the counter and reference electrode respectively. A 0.5 mol L -1 Na 2 SO 4 aqueous solution (ph ~ 7) was used as the electrolyte. In order to make an electrical connection, an uncoated area of the glass was attached to a copper wire by silver conductive glue. Subsequently, the copper wire was protected and supported by a glass tube. The edges and the back of the photoelectrode were covered with epoxy resin for insulation. The effective working area of the film was 1.34 ± 0.04 cm 2. RESULTS AND DISCUSSION Performance of the photo-electrochemical cell Figure 2 shows the current density voltage (J V) curves under illumination for the photoelectrochemical cell with Fe 2 O 3 nanostructures. The photo-responses of α-fe 2 O 3 films were evaluated by measuring photocurrent densities, J p. The results show distinctive influence of surfactants, with CTAB showing highest photo-generation. As shown in Table 3, the photocurrent density of CTAB treated sample was 1.58 ma/cm 2 at 1 V/SCE, under illumination intensity of 100 mwcm -2, which is significantly larger than the other samples (7 times more than PEG and almost 50% more than F127). It should be noted that PEG, the lowest sample, is often used in sol-gel method. The photocurrent density of Fe 2 O 3 /PEG at 1.23 V RHE was 0.65 macm -2, which is similar to reported value for the same sample in the literature (0.89 macm -2 ) (Lopes et al., 2010). 4
5 3.5 Photocurrent Density (ma/cm 2 ) Photocurrent Density at 1.00 V Vs RHE PEG-300 T-100 F127 CTAB Surfactant PEG-300 T-100 F127 CTAB Voltage (mv) Fig. 2: Photocurrent values of Fe 2 O 3 /PEG, Fe 2 O 3 /Triton, Fe 2 O 3 /F127 and Fe 2 O 3 /CTAB Optical characterization The optical properties of the surfactant treated hematite films (α-fe 2 O 3 ) produced by spin coating technique were measured by UV-visible absorption spectra and are displayed in Fig 3. Table 3 shows the UV-Visible absorption value for all samples between 320 and 670 nm. The UV-Vis analysis showed that both CTAB and Triton have higher optical absorption, covering both UV and visible spectrum. However, Triton sample diminished quickly with increasing wavelength. Again, the highest optical absorption observed in the ultraviolet and visible region for Fe 2 O 3 /CTAB sample (290 A.U.). The results agree with improved photocurrent performance and confirm that CTAB sample has larger numbers of electron hole pairs (Dare-Edwards et al., 1983). The bandgap of samples can be obtained from the absorption coefficient data, according to solid band theory (Tauc et al., 1966): (α h ν) = A (h ν - E g ) m [1] Where α is the absorption coefficient, hν is the energy of the incident photon, A is a constant related to the effective mass of the electrons and holes, E g represents the energy band gap of samples and m = 2 for allowed indirect transition. Analyzed onset region is at around 600 nm, which is in agreement with the bandgap of α-fe 2 O 3. The bandgap values were determined from the curves extrapolations. Fig. 4 presents the change in bandgap energy, E g, with treating Fe 2 O 3 by PEG and CTAB surfactants. It can be seen that the bandgap energy decreased slightly from indirect transition of 2.02 to 1.94 ev for PEG and CTAB treated of Fe 2 O 3, respectively. Similar values have already been reported in the literature, e.g ev (Souza et al., 2009) and 2 ev (Duret and Graetzel, 2005). The indirect transition has been identified as a spin-forbidden Fe 3+ 3d 3d excitation (Jitianu et al., 2002). Furthermore, it has been observed that the surfactant treated hematite film may not produce any intermediate level within the energy level of iron oxide. These results are in good agreement with XRD diffraction data (shown below), which did not show that any change in the structural parameters when different surfactant were added. The calculated band gaps are consistent with the optical absorption. Again, Fe 2 O 3 nanostructure treated with CTAB has the lowest band gap compared with the other samples. The lowest E g of 1.94 ev, it is expected to generate the highest number of electron hole pairs when illuminated with light. Moreover, with the lower band gap, it is easier for electrons to be excited from valence band to conduction band of Fe 2 O 3 (Cherepy et al., 1998). 5
6 1 PEG T-100 F127 CTAB Absorbance (a.u) Wavelength (nm) Fig. 3: Absorption spectra of Fe 2 O 3 /PEG, Fe 2 O 3 /Triton, Fe 2 O 3 /F127 and Fe 2 O 3 /CTAB 0.3 (α.hν) Indirect Transition PEG-300 CTAB Photon energy in ev Fig. 4: Calculation of the indirect electronic transition Table 3: Comparison of various parameters as a function of Fe 2 O 3 nanostructures treated with different type of surfactants Sample Photocurrent Absorption Open circuit Grain Surface density E g (A.U) Thickness potential size roughness (ma/cm 2 ) (ev) (nm) V (nm) R z (nm) aoc (V/SCE) At zero At nm V/SCE V/SCE PEG ± ± T ± ± F ± ± CTAB ± ±
7 Crystalline properties In order to investigate phase formation and crystalline properties of the films, XRD analysis was performed at room temperature. Similar hematite signature covered on FTO conducting glass substrate pattern was obtained from X-ray diffraction (XRD) experiments of surfactant treated hematite films (α-fe 2 O 3 ) produced by spin coating technique (Fig. 5). The diffraction peaks 24, 33, 34, 36, 41 and 55 at in Fig. 5a reveal the diffraction peaks of rhombohedral Fe 2 O 3. A similar prevalence of the peaks has also been observed for α-fe 2 O 3 nanostructure film in studies carried out by sol-gel method (Memar et al., 2010, Souza et al., 2009). The average crystallite size has been estimated from the Debye-Scherrer equation using (110) peak: D = 0.94 λ / β cos θ [2] where D is the crystalline dimension, λ is the wavelength of the X-ray radiation (which is nm), θ is the diffraction angle, and β is the full width at half maximum. From Table 3, it can be seen that surfactants can strongly influence the crystallite size, with CTAB being 4 times bigger than PEG sample. It can be seen that the grain size is directly correlated to the optical absorption and the photocurrent density, i.e. bigger grain size gives better optical and photo responses. This correlation is expected and consistent with previous study (Memar et al., 2010). Fig. 5: X-ray diffraction patterns of Fe 2 O 3 /PEG, Fe 2 O 3 /Triton, Fe 2 O 3 /F127 and Fe 2 O 3 /CTAB Surface morphology The surface morphology of the films was observed by field emission scanning electron microscopy (FESEM, Zeiss NEON 40 EsB CrossBeam) operating at 3 KV for both top and cross-sectional view using InLens mode. The SEM micrographs of four samples (Fig. 6) show distinctive features, which correspond well to the XRD results. The morphology of Fe 2 O 3 /PEG film shows a uniform, smooth and compact structure with worm-like grains in nanometric scale (Fig. 6 a). The Triton affects the grains size leading to a grain width reduction, (Fig. 6 b), which resulted in columnar tree structure. On the other hand, F127 7
8 treated Fe 2 O 3 thin films revealed the formation of a homogeneous and uniform surface (Fig. 6 c). Finally, CTAB treated sample (Fig. 6 d) comprises of small clusters of about 250 nm, which are consisted of much smaller primary particles in the range of nm. During the annealing process of CTAB sample, these smaller nanoparticles expectedly dispersed in the surface and form very compact layer. The SEM images are consistent with the grain size analysis. The film thickness was measured by FESEM, which ranged between 520±10 nm and 980±10 nm. Uncoated fluorine-doped thin oxide conductive layer with a thickness of about 820 nm was shown in Fig. 7, which highlights a good adherence in the FTO substrate. There is no clear correlation between film thickness and particle size nor grain size. Atomic force microscopy (AFM) images obtained for surfactant treated hematite thin films have been shown in Fig. 8. The estimated value of the average grain sizes are found to closely match the average particle/grain size obtained from XRD data. AFM photographs of surfactant treated hematite films show that Fe 2 O 3 /CTAB film was very rough with extensive granular structures extending over the film surface. This leads to large amounts of intergranular surfaces and higher possibilities of surface related effects. On the other hand, F127, Triton and PEG surfactants significantly reduced the surface roughness (Table 3). Amongst these samples, PEG treated film had the smoothest surface, 2 nm. The influence of surface roughness on photocurrent can be explained by considering the light absorption process. In general, a beam of radiation can be reflected, scattered and transmitted on a surface of sample. However, the diffuse reflection phenomena due to scattered light can increase the amount of absorption. On the other hand, a rough surface with large grain size can significantly increase the diffuse reflection in the visible light region. A rough surface also has higher electrode/electrolyte interfacial contact area for enhancing photocurrent and multiple scattering of UV vis light (Memar et al., 2010). As the results, the film with larger grain sizes and a higher surface roughness (CTAB) showed a better photocurrent. a b c d Fig. 6: SEM images of (a) Fe 2 O 3 /PEG, (b) Fe 2 O 3 /Triton, (c) Fe 2 O 3 /F127 and (d) Fe 2 O 3 /CTAB 8
9 Fig. 7: Cross sectional view of Fe 2 O 3 /PEG film Fig. 8: AFM image for (a) Fe 2 O 3 /PEG, (b) Fe 2 O 3 /Triton, (c) Fe 2 O 3 /F127, and (d) Fe 2 O 3 /CTAB It can be seen from the results that cationic surfactant has shown higher photocatalytic activity compare than non-ionic. The strong bonding forces between the positively charged amino-group of CTAB [CTA + ] and the Fe 2 O 3 particles probably prevented the aggregation of the molecules in solution and dispersed the particles evenly and increase the efficiency. The high photo current of CTAB sample is consistent with UV-vis optical absorption and the estimated band gap. The decrease in band gap is useful in obtaining higher electron hole pair generation, as electrons can transfer easily from valence bond to conduction band of the 9
10 semiconductor. Therefore, it can be concluded that CTAB treated sample can generate highest numbers of electron-hole pairs under illumination. The result is also supported by morphology characterization, in which CTAB produced larger grain size. On the other hand, the surface roughness plays an enhancing role in photocurrent yield due to large specific surface area (contact area) and strong light scattering effect (diffuse reflection). The results showed that surfactant treating of the film can release the internal stress, relax the distortion of the crystal lattice and improve the crystallinity, which increases the photocatalytic activity. On the other hand, with the decreasing particle size the surface tension increases and causes a crystal lattice distortion. Hence, the larger grain size effect can increase the photocatalytic activity of the Fe 2 O 3 thin film as demonstrated by CTAB sample. Further studies with other cationic surfactants are underway to confirm the phenomena. CONCLUSIONS Fe 2 O 3 nanostructures have successfully been prepared with surfactants (PEG, Triton, F127 and CTAB) on FTO substrate using the sol - gel spin coating technique. The surfactants distinguishingly altered morphology of the resulting Fe 2 O 3 nanoparticle layers. PEG, F127 and Triton surfactants produced smoother surface than CTAB. PEG produced the smoothest surface and the lowest photocurrent. More significantly, the surfactants significantly influence the photocurrent and optical absorption of Fe 2 O 3 layer. Amongst these four surfactants, CTAB revealed the best performance: highest current density (more than 7 times in comparison with PEG), lowest band gap (1.94 ev) and highest absorption (290 A.U.). These results indicated that CTAB treated sample had the highest number of electron-hole pairs under illumination, which is also supported by morphology characterization (largest grain size and roughest surface). The study demonstrates that the photo-electrochemical performance of Fe 2 O 3 nanostructures can be improved by simply varying surfactant. The results highlighted the superior performance of cationic surfactant over non-ionic surfactant in preparing photoanodes by sol-gel method. In comparison to PEG, a common surfactant used in sol-gel method, CTAB can increase the grain size by 4 times and increase photocurrent density by 7 times (at 1 V). The result can be attributed to crystallinity process of CTAB, which resulted in the larger grain size and highest photocatalytic activity. REFERENCES BIRD, R. E., HULSTROM, R. L. & LEWIS, L Terrestrial solar spectral data sets. Solar Energy, 30, BOLTON, J. R Solar photoproduction of hydrogen: A review. Solar Energy, 57, CHEREPY, N. J., LISTON, D. B., LOVEJOY, J. A., DENG, H. & ZHANG, J. Z Ultrafast studies of photoexcited electron dynamics in γ-and α-fe 2 O 3 semiconductor nanoparticles. The Journal of Physical Chemistry B, 102, CURRAO, A Photoelectrochemical water splitting. CHIMIA International Journal for Chemistry, 61, DARE-EDWARDS, M. P., GOODENOUGH, J. B., HAMNETT, A. & TREVELLICK, P. R Electrochemistry and photoelectrochemistry of iron (III) oxide. J. Chem. Soc., Faraday Trans. 1, 79, DURET, A. & GRAETZEL, M Visible light-induced water oxidation on mesoscopic α-fe 2 O 3 films made by ultrasonic spray pyrolysis. The Journal of Physical Chemistry B, 109,
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