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L Chu (2017)
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TiO, ZrO and layer-by-layer T iO –ZrO films were prepared by doctor blade method followed by sensitization with natural 2 2 2 2 dye for dye-sensitized solar cell application. The structural and optical, morphological and compositional properties were investigated by X-ray diffraction and UV–Vis spectroscopy, scanning electron microscopy, BET, surface profilometer and energy-dispersive X-ray analyzer, respectively. Dye-sensitized solar cells were fabricated using the prepared electrodes of TiO, ZrO and layer-by-layer TiO –ZrO films sensitized with natural dye extracted from Pandan leaves (Pandanus ama- 2 2 2 2 ryllifolius). The J–V characteristics were recorded to measure photo-response of fabricated devices and electrochemical impedance spectroscopy to study the electron behavior, series resistance and lifetime. Photovoltaic parameter like short- circuit current, open-circuit voltage, fill factor, and power conversion efficiency were evaluated for fabricated solar cell under −2 artificial light supplied from white LED (15 mW·cm ). The average values of power conversion efficiency of DSSCs fabri- cated with TiO, ZrO and layer-by-layer TiO –ZrO photoanodes were found to be 0.65%, 3.04% and 3.13%, respectively. 2 2 2 2 Keywords TiO –ZrO · Layer by layer · Pandan leaves · Natural dye-sensitized solar cells · EIS 2 2 Introduction along with moderated efficiency. In general, TiO and/or ZnO are used as a wide band gap semiconductor material in Today, due to the increasing global warming and energy DSSCs [1–3]. Still there is a need to search for alternative crisis worldwide, it is important to find renewable and green materials towards the enhancement in device efficiency. In energy source, which are cost effective and reliable. Solar this direction, one can look for alternative semiconductor energy is one of the most gifted sources for producing envi- such as ZrO and its bilayered structure with routine T iO . 2 2 ronmentally friendly energy. Compared to first- and second- ZrO is a wide band gap semiconductor with direct band generation solar cells, dye-sensitized solar cells (DSSCs) gap values ranging from 2.5 to 3.8 eV [4], which may be an can be considered as one of the most favorable photovoltaic attractive candidate for dye-sensitized solar cell application devices because of the low-cost, simplicity in fabrication [5]. Doping in T iO can modified optical and electrical properties leads to increase the performance by providing * Prashant K. Baviskar more active sites on the surface that can play a significant pkbaviskar@physics.unipune.ac.in role for adsorption of dye molecules, improvement in light * Habib M. Pathan absorption, and also enhance the electron collection in the habib.pathan@gmail.com conduction band [6, 7]. On the contrary, one can enhance Advanced Physics Laboratory, Department of Physics, the performance of DSSC using multi-layered or composite Savitribai Phule Pune University, Pune 411007, India photoanodes [8, 9]. Recently, Mohamed et al. reported the Department of Chemistry, Savitribai Phule Pune University, improvement in efficiency from 1.61 to 4.51% of DSSC fab- Pune 411007, India ricated with doping of ZrO in TiO nanofibers photoanode 2 2 Department of Chemistry, Faculty of Science, King sensitized using N719 dye [7]. Jin et al. observed that the Abdulaziz University, Jeddah 21589, Saudi Arabia efficiency of DSSCs with a TiO –ZrO composite electrode 2 2 Department of Botany, Savitribai Phule Pune University, was 6.2%, an increase of 26.5% than pure T iO electrode Pune 411007, India Vol.:(0123456789) 1 3 12 Page 2 of 9 Materials for Renewable and Sustainable Energy (2019) 8:12 (4.9%) for N719 dye as sensitizer. This is because, the addi- using Zn-doped T iO –ZrO prepared by hydrothermal 2 2 tion of ZrO in TiO increased dye loading, thereby improv- method with juice of pomegranate as natural sensitizer. The 2 2 ing the electron recombination times than for a pure TiO efficiency of DSSC fabricated with TiO –ZrO is 1.97% 2 2 2 electrode results in the decreased electron recombination at and that of the Zn-doped T iO –ZrO nanocomposites were 2 2 the TiO /electrolyte interface, increasing electron transfer found 4.58%. The enhancement in efficiency is because the [10]. The highest efficiency of 6.5% was achieved for N719 Zn doping has introduced new energy levels and lowered the dye-sensitized ZrO nanofiber-doped TiO photoelectrode recombination [22]. 2 2 prepared by squeeze printing [11]. Furthermore, the sig- From literature survey including recent reports, very few nificant enhancement in power conversion efficiency can be reports are available on sensitization of chlorophyll dye ascribed for TiCl-treated TiO nanosheets film coated with with different metal oxides for dye-sensitized solar cell. The 4 2 ZrO and the highest efficiency of 7.33% is achieved for comparison of photovoltaic performance of chlorophyll dye- N719 dye [12]. sensitized photoanodes for DSSC application under different Usually, Ru-metal complexes and metal-free organic light intensities with reported literature is summarized in dyes are used as sensitizer due their good stability and light Table 1 [21, 23–36]. harvesting property with high molar extinction coefficient In this article, we promote to use natural dyes as sen- [13, 14]. However, application of these types of sensitizers sitizer towards the development of attractive, colorful and also faced problems regarding complicated synthetic routes low-cost DSSCs. Hence, attempt has been focused in this and most importantly use of environmentally non-benign direction to develop the low cost and eco-friendly source of chemicals [15]. Hence, dyes obtained from nature having green energy by using inexpensive and naturally available similar characteristic were used with the advantages such dye extracted from Pandan leaves as sensitizer over TiO , as availability, low-cost, environmental friendliness and as ZrO and layer-by-layer T iO –ZrO photoelectrodes towards 2 2 2 a green alternative to commercially available dyes [16–20]. the fabrication of DSSCs. To the best of our knowledge; it is observed that not many reports are available on natural dye-sensitized TiO –ZrO 2 2 bilayer electrode for DSSC application. Win et al. reported Experimental sensitization of Rose extract over T iO –ZrO film prepared 2 2 by rolling method of DSSC and observed 0.23% efficiency Material and chemicals [21]. DSSC fabricated using nanocrystalline ZrO –TiO 2 2 film prepared by doctor blade method and sensitized with Fluorine-doped tin oxide (FTO)-coated glass with a sheet −2 the bioorganic dye, chlorophyll extracted from green leaves resistance of ~ 15 Ω cm was used as substrate. Nanocrys- of Chromolaena odorata shows 0.1% efficiency. Recently, talline powder of T iO (particle size ~ 7 nm with anatase Tomar et al. reported improvement in efficiency of DSSC phase), zirconium oxide powder (particle size ~ 45 nm from Table 1 Summary of Photoanode Source Intensity of light PEC (%) References photovoltaic performance of −2 (mW cm ) chlorophyll dye-sensitized with various photoanodes for DSSC TiO –ZrO Rose dye – 0.23 [21] 2 2 application TiO Pandan leaves 100 0.1 [23] TiO Anthocyanin:chlorophyll 100 0.062 [24] TiO Pandan leaves 100 0.35 [25] TiO Papaya leaves 100 0.36 [26] TiO Rosella extract 100 0.57 [27] TiO Chlorophyll derivative 100 2.25 [28] TiO /ZnO Papaya leaves 100 0.07 [29] TiO Papaya leaves 100 0.094 [30] TiO Chlorophyll – 0.049 [31] TiO Pandan leaves 100 0.0006 [32] TiO –ZrO Chromolaena odorata 10 0.1 [33] 2 2 TiO Shisonin leaves 100 0.59 [34] TiO Chlorophyllin (Cu-Chl-e6) 100 1.81 [35] TiO Undaria pinnatifida (Wakame) 100 4.6 [36] TiO –ZrO Pandan leaves 15 15 Present work 2 2 1 3 Materials for Renewable and Sustainable Energy (2019) 8:12 Page 3 of 9 12 SRL Chem. India), ethyl cellulose (SDFCL, India), etha-and TiO –ZrO bilayered structure were air annealed at 2 2 nol (AR, 99.9%, Changshu Yangyuan Chemical, China), 450 °C for 1 h to remove the organic solvents as well as α-terpineol (LR, 98%, HPLC, India), acetyl acetone (98%, to improve the crystallinity of the film and the interfacial Merck, India), potassium iodide (99.8%, SRL, India), iodine structures. (99.5%, Fisher Scientific, UK), t -butyl pyridine (96%, Acros organics, USA), acetonitrile (AR, 99.5%, SDFCL, India) Preparation of natural dye were used as it is without any further purification. Firstly, natural chlorophyll dye was prepared from 3 g fresh Substrate cleaning leaves of fragrant screwpine (Pandanus amaryllifolius) or locally known as Pandan leaves. The leaves were cleaned Prior to deposition FTO substrates were cleaned by using with distilled water, rinsed with ethanol, and were cut into soap solution followed by double distilled water and then small pieces and immersed in 5 ml ethanol followed by with acetone in ultrasonic bath for 10–15 min. grinding in mixer for 10 min and the same was repeated at least for 3–4 times. Again 5 ml of ethanol was then added Preparation of TiO and ZrO paste 2 2 in the above mixture and kept on a magnetic stirrer at room temperature for 1 h. Finally, the above mixture is kept for In detail, 0.5 g TiO nanoparticles powder was ground in around 24 h in a closed bottle in dark at room temperature. mortar pestle with addition of 7 ml ethanol and kept in The filtrate of the above solution was used as natural dye ultrasonic bath for 15–20 min. Afterwards 0.3 g ethyl cel- for sensitization of photoelectrodes towards the fabrication lulose was ground in same mortar pestle in 2 ml ethanol. of DSSCs. Then the sonicated paste of TiO was subsequently added and ground with ethyl cellulose in mortar pestle for uni- Sensitization of photoelectrodes form mixing. Then the mix solution was transferred in the borosilicate glass bottle for sonication with the addition of The annealed films of pristine TiO, ZrO and TiO –ZrO 2 2 2 2 1.3 g α-terpineol for 3 h followed by addition of 3 drops of bilayered structure were then immersed in naturally prepared acetyl acetone to the above mixture and allowed to sonicate dye for 72 h at room temperature. Subsequently, the films for another 1 h. Finally, for the evaporation of ethanol; the were dipped in ethanol for 5–10 s to remove the excess of prepared solution was placed in incubator at 60 °C till it dye, followed by drying at room temperature. becomes more viscous. Similar procedure was repeated for the preparation of ZrO paste. Characterizations Preparation of photoelectrodes The structural and optical analysis was carried out using Pre-cleaned FTO substrate was covered at the edges by using X-ray diffractometry (XRD) (model: XRD, Rigaku ‘‘D/B scotch tape of ~ 30 μm thickness and layer of prepared T iO max-2400’’, CuK with λ = 1.54 Å) and UV–Vis spectro- 2 α paste was then coated on FTO substrates using doctor blade photometer (model: JASCO V-670) was used to record method at room temperature. The as-prepared films of pris- optical absorption spectra of photoelectrodes using diffused tine TiO were dried at 60 °C in incubator for 10–15 min. reflectance (DRS) mode in wavelength range 310–800 nm The above procedure was repeated four times to get opti- at room temperature, respectively. Surface profilometer mized thickness of ~ 12 μm measured by using surface pro- (Dektak 150) was used for the measurement of thickness of filometer. Similar route is employed for the preparation of annealed photoelectrodes. The morphological properties and ZrO films followed by drying at 60 °C for 10–15 min. elemental composition was done by using scanning electron Layer-by-layer approach was utilized for the preparation microscopy (SEM) and energy-dispersive X-ray spectros- of TiO –ZrO bilayered films. Briefly, pre-cleaned FTO copy (EDS) (model: JEOL-JSM 6360-A), respectively. The 2 2 substrate was covered at the edges by using scotch tape and BET method was used for the measurement of surface area first layer of prepared TiO paste was coated on FTO using of all samples using Quantachrome Autosorb-iQ unit. The doctor blade method. Then the as-prepared film was dried at cell performance was measured by a semiconductor char- 60 °C for 15 min followed by the coating of second layer of acterization unit (Keithley 2420 source meter) under illu- −2 ZrO on putting scotch tape over T iO in similar way. Again mination of artificial LED light (15 mW cm ). The elec- 2 2 the as-prepared bilayered film was dried at 60 °C for 15 min. trochemical impedance spectroscopy (EIS) measurements The above procedure was repeated one more times to get for DSSCs were carried out using potensiostat/galvanostat optimized thickness of ~ 12 μm for layer-by-layer TiO –ZrO (IVIUM:Vertex) in the frequency range of 1 MHz to 1 Hz 2 2 films. Finally, all the prepared films of pristine TiO, ZrO under dark. 2 2 1 3 12 Page 4 of 9 Materials for Renewable and Sustainable Energy (2019) 8:12 Results and discussion Structural studies XRD patterns of the T iO, ZrO and T iO –ZrO bilayered 2 2 2 2 −1 films were recorded using X-ray diffractometer with 0.1° s step size and scan rate of 1 s/step as shown in Fig. 1. The characteristic along (101) and (004) peaks at 25.27° and 37.8°, respectively, were clearly observed and confirm the growth of tetragonal structure (JCPDF card No. 21-1272) of TiO having anatase phase (a) on FTO substrate. XRD pattern of ZrO on FTO substrate by doctor blade method is depicted as (b). The strong diffraction peaks along ( 111 ) and (111 ) were indexed to monoclinic structure (JCPDF card No. 37-1484). The XRD pattern (c) for T iO –ZrO layer-by-layer 2 2 film represents the combination of two sets of patterns: one from TiO and the other originating from the ZrO . Thus 2 2 Fig. 2 Optical absorption spectra of TiO (−), ZrO (−), TiO –ZrO the formation of layer-by-layer TiO with ZrO is confirmed 2 2 2 2 2 2 (−) films and ethanolic solution of dye (−) from the XRD. Asterisk (*) shown in the pattern assigned to the FTO-coated glass substrate. spectrum. Usually, TiO shows the characteristic spectrum Optical absorption spectroscopy with its fundamental absorption of Ti–O bond in UV region between 320 and 400 nm [37] with characteristic peak A UV–Vis spectrophotometer (model: JASCO V-670) was around 350 nm (band edge) for TiO [38]. Whereas naturally used to record optical absorption spectra of photoelectrodes prepared chlorophyll dye exhibits maximum absorption at in diffused reflectance (DRS) mode and ethanolic solution 413 and 665 nm in visible region. Chlorophylls, which act of dye under transmission mode in the wavelength range as an effective photo-sensitizer in photosynthesis of green 310–800 nm at room temperature. Figure 2 shows the plant, has absorption maximum at 670 nm, thus, it is an absorption spectra of pristine TiO, ZrO, TiO –ZrO films, 2 2 2 2 attractive potential compound as a photo-sensitizer in the and chlorophyll dye solution. It is observed that all the films visible region [39]. The values for amount of dye adsorbed exhibit low absorbance in the visible region of the solar over different photoelectrodes used for the fabrication of DSSCs along with the thickness of photoanodes are summa- rized in Table 2. Chu et al. reported the enhancement of dye absorption for layer-by-layer photoelectrode and observed the improvement in performance of DSSC [40]. Surface morphology and elemental analysis The top-view of pristine TiO, ZrO and TiO –ZrO bilayer 2 2 2 2 films was examined using SEM to analyze the surface morphology (Fig. 3). The SEM results clearly illustrated nanoporous surface nature of T iO, ZrO and T iO –ZrO 2 2 2 2 films which is the basic requirement of photoelectrode in DSSC. At high resolution (inset), it is observed that the samples were granular in structure and porous in nature. Figure 3c shows the TiO –ZrO film has uniform surface 2 2 area than the pristine ZrO and TiO which leads to bet- 2 2 ter dye adsorption and results in enhancing the overall performance of the DSSC for T iO –ZrO bilayered pho- 2 2 toanode. The layer-by-layer structure of TiO –ZrO bilay- 2 2 ered photoanode exhibit moderate surface area compared Fig. 1 XRD pattern of pristine TiO (a), ZrO (b) and layer-by-layer 2 2 TiO –ZrO (c) films with the pristine bulk materials positive sign for amount of 2 2 1 3 Materials for Renewable and Sustainable Energy (2019) 8:12 Page 5 of 9 12 dye adsorption and also leads to the shortened collection length for charges results into increasing efficiency [41]. The values of surface area measure by BET technique for all the samples are summarized in Table 2 and found to be in accordance with the previously reported results [42]. The energy-dispersive X-ray (EDS) spectrum of TiO –ZrO bilayer film is shown in Fig. 3d. EDS con- 2 2 firmed that the presence of titanium, zirconium and oxy - gen. The atomic percentages of elements are tabulated in the inset of Fig. 3d. Solar cell assembly The dye-sensitized photoanodes and platinum counter electrode was separated by spacer of 10 μm thickness over photoanodes and assembled into a sandwich-type open cell using binder clip. The active cell area for DSSC was regu- lated to 0.25 cm using stainless steel mask covered from back side of photoanode over the glass side of the FTO. The mask is designed in such a way that it allowed enter- ing the light through aperture and remains opaque for light over the remaining part of the cell. Figure 4a shows the schematic of device for chlorophyll dye-sensitized layer- by-layer TiO –ZrO photoanode-based DSSC. A drop of 2 2 prepared liquid electrolyte was introduced between the sensitizer and the counter electrode in such a way that no air bubble is formed. An electrolyte composed of 0.5 M potassium iodide (KI); 0.1 M iodine (I ) and 0.5 M t-butyl pyridine (C H N) in an acetonitrile solvent was used. 13 21 Photovoltaic study Photovoltaic measurements of the fabricated DSSCs using natural dye as sensitizers were performed by meas- uring the J–V measurement as shown in Fig. 4b. In pre- sent study we have measured the J–V characteristics of each DSSCs device 3 times for 2 sets of photoanodes to check the repeatability along with the reproducibility of the device and the average values of photovoltaic perfor- mance was reported. The cell performance was recorded by a semiconductor characterization unit (Keithley 2420 source meter) under illumination of artificial light (15 mW −2 cm ) supplied from white LED source. The current den- sity–voltage (J–V) characteristics under illumination con- ditions were measured at room temperature (27 °C). The output photovoltaic parameters of natural dye-sensitized solar cell, i.e., the short-circuit current density (J ), open- sc circuit voltage (V ), fill factor (FF) and power conversion oc efficiency (PEC) of the devices with standard deviation are summarized in Table 2. 1 3 Table 2 Structural and morphological properties of TiO, ZrO and TiO –ZrO photoelectrodes and their photovoltaic and electrochemical output parameters with natural dye-sensitized solar 2 2 2 2 cells −2 Photoanode Surface area multi- Thickness (μm) Crystallite Amount of dye τ (ms) R (Ω) V (mV) J (mA cm ) FF PCE (%) e ct oc sc 2 −1 −2 BET (m g ) size (nm) adsorbed (nmole cm ) TiO 72.26 2.8 37 4.18 0.53 648 340 ± 3 1.69 ± 0.07 0.170 ± 0.008 0.65 ± 0.04 ZrO 25.80 3.2 158 69.5 3.33 1184 341 ± 1 7.03 ± 0.14 0.190 ± 0.004 3.04 ± 0.02 TiO –ZrO 33.39 12.5 50 82.4 1.32 1340 530 ± 5 4.80 ± 0.11 0.185 ± 0.006 3.13 ± 2 2 0.03 ±, standard deviation 12 Page 6 of 9 Materials for Renewable and Sustainable Energy (2019) 8:12 Fig. 3 Surface morphologies of a pristine TiO , b ZrO and b TiO –ZrO bilayered films. Corresponding inset shows the images at high resolu- 2 2 2 2 tion. d EDS spectra of TiO –ZrO bilayered film and inset shows elemental constituent in tabulated form 2 2 photoanode. The values of τ found to increase from bare Electrochemical impedance spectroscopy (EIS) TiO to TiO –ZrO photoanode-based DSSC. The substan- 2 2 2 tial increase in the values of electron lifetime indicates the Figure 4c shows the Nyquist plots and Fig. 4d represents the ee ff ctive suppression of back reaction between the photogen - Bode phase plots for all three devices sensitized with natural erated electrons. Superior value for τ was recorded for the chlorophyll dye. It is observed that the radius of distorted TiO –ZrO photoanode-based device as compare to the bare semicircles increases as TiO < ZrO < TiO –ZrO which 2 2 2 2 2 2 metal oxide-based devices, demonstrating the reduced indicate the highest charge recombination resistance was charge recombination. This may be the reason towards get- observed for TiO –ZrO photoanode-based DSSC. The elec- 2 2 ting higher efficiency with layer-by-layer TiO –ZrO photo- tron lifetime (τ ) can be calculated by the peak frequency at 2 2 anode-based DSSC. The value of charge recombination the minimum phase angle (f ) from Bode phase plots peak resistance (R ) was measured from Nyquist plots using sec- using the relationship [τ = ] [43]. The shift in the phase ct 2f peak ond distorted semicircle in mid frequency region. Table 2 angle maxima has been observed towards the low-frequency summarizes the values for τ and R for all the three devices. e ct range as we move from the T iO to ZrO to T iO –ZrO 2 2 2 2 As per literature, the larger value of R is leads to the ct 1 3 Materials for Renewable and Sustainable Energy (2019) 8:12 Page 7 of 9 12 Fig. 4 a Schematic of device, b current density–voltage (J–V) characteristics curve, c Nyquist plot and d bode phase plot for TiO (open square), ZrO 2 2 (open circle), TiO –ZrO (open 2 2 triangle) photoanodes-sensitized with natural dye reduction in charge recombination rate which is favorable photoanode-based DSSCs leads to the effective suppression towards the enhancement in device efficiency [44]. The of photo-injected electron recombination with the excited highest current density value is observed for ZrO -based dye and I in the electrolyte resulted in the enhancement in DSSCs which is may be due to the highest value of electron efficiency for layer-by-layer TiO –ZrO photoanode-based 2 2 life time (τ ) compared to other two devices. DSSC. This opens the window for use of ZrO as photo- e 2 electrode instead of routine metal oxides used as wide band gap materials and natural dye in spite of Ru-metal-based Conclusion expensive dyes as sensitizer towards the fabrication of cost- effective and eco-friendly DSSC. Dye-sensitized solar cells (DSSCs) were assembled using Acknowledgements Authors are thankful to University with Potential extracts from fragrant screwpine (P. amaryllifolius) leaves for Excellence (UPE)—II for partial financial support. PKB is thank - as sensitizers with pristine T iO, ZrO and TiO –ZrO 2 2 2 2 ful to University Grants Commission, New Delhi, India, for the award photoelectrodes. Photovoltaic parameters of the fabricated of Dr. D.S. Kothari Postdoctoral Fellowship and financial assistance DSSCs were determined under illumination. It is found that (PH/16-17/0074). the natural dye-sensitized layer-by-layer T iO –ZrO pho- 2 2 Open Access This article is distributed under the terms of the Crea- toanode exhibits maximum power conversion efficiency of tive Commons Attribution 4.0 International License (http://creat iveco 3.13% than pristine ZrO (3.04%) and TiO (0.65%) which 2 2 mmons.or g/licenses/b y/4.0/), which permits unrestricted use, distribu- suggest that the anchoring of chlorophyll dye goes well with tion, and reproduction in any medium, provided you give appropriate ZrO as compared to T iO . The improvement in efficiency credit to the original author(s) and the source, provide a link to the 2 2 Creative Commons license, and indicate if changes were made. is observed for T iO –ZrO bilayered structure, which is due 2 2 to the high surface area available for dye adsorption. From EIS studies it is observed that the electron lifetime values References for layer-by-layer photoanode-based DSSC is in between pristine photoanode-based DSSC. On the other hand, the 1. Mathew, S., Yella, A., Gao, P., Humphry-Baker, R., Curchod, charge recombination resistance for layer-by-layer photo- B.F.E., Ashari-Astani, N., Tavernelli, I., Rothlisberger, U., anode is significantly greater than pristine ZrO and TiO 2 2 1 3 12 Page 8 of 9 Materials for Renewable and Sustainable Energy (2019) 8:12 Nazeeruddin, M.K., Gratzel, M.: Dye-sensitized solar cells with 19. 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