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  • Editor: Christian Seassal
  • Vol. 21, Iss. S3 — May. 6, 2013
  • pp: A469–A474
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Effect of polymer morphology on P3HT-based solid-state dye sensitized solar cells: an ultrafast spectroscopic investigation

R. Sai Santosh Kumar, G. Grancini, A. Petrozza, A. Abrusci, H. J. Snaith, and G. Lanzani  »View Author Affiliations


Optics Express, Vol. 21, Issue S3, pp. A469-A474 (2013)
http://dx.doi.org/10.1364/OE.21.00A469


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Abstract

Solid-state dye sensitized solar cell devices are fabricated with poly(3-hexylthiophene) (P3HT) as the hole transporting layer. Upon annealing treatment we obtained ≈70% increase in the device efficiency compared to un-annealed devices. Our investigation, by means of ultrafast transient absorption spectroscopic characterization, correlates the increased device performances to a more efficient hole-transfer at the dye/polymer interface in the thermally treated P3HT.

© 2013 OSA

1. Introduction

Solid-state dye-sensitized solar cells (sDSC) are a potential alternative to liquid electrolyte based conventional DSCs as they promise to circumvent stability issues of DSC caused by several effects such as the evaporation and leakage of liquid and the corrosion of counter-electrode [1

1. A. Yella, H.-W. Lee, H. N. Tsao, C. Yi, A. K. Chandiran, M. K. Nazeeruddin, E. W. Guang Diau, C. Yu Yeh, S. M. Zakeeruddin, and M. Grätzel, “Porphyrin-sensitized solar cells with cobalt (II/III)–based redox electrolyte Exceed 12 percent efficiency,” Science 324, 634–639 (2011).

4

4. H. J. Snaith and L. Schmidt-Mende, “Advances in liquid-electrolyte and solid-State dye-sensitized solar cells,” Adv. Mater. 19(20), 3187–3200 (2007). [CrossRef]

], in addition to being easier to manufacture. As solid state hole transporter material (HTM) the most successfully employed is 2,2’,7,7’-tetrakis(N,N-di-4-methoxyphenylamino)-9,9’-spirobifluorene (spiro-OMeTAD) [5

5. M. Grätzel, U. Bach, D. Lupo, P. Comte, J. E. Moser, F. Weissörtel, J. Salbeck, and H. Spreitzer, “Solid-state dye-sensitized mesoporous TiO2 solar cells with high photon-to-electron conversion efficiencies,” Nature 395(6702), 583–585 (1998). [CrossRef]

] with a demonstrated power conversion efficiency (PCE) of 7.2% [6

6. J. Burschka, A. Dualeh, F. Kessler, E. Baranoff, N. L. Cevey-Ha, C. Yi, M. K. Nazeeruddin, and M. Grätzel, “Tris(2-(1H-pyrazol-1-yl)pyridine)cobalt(III) as p-type dopant for organic semiconductors and its application in highly efficient solid-state dye-sensitized solar cells,” J. Am. Chem. Soc. 133(45), 18042–18045 (2011). [CrossRef] [PubMed]

]. Although spiro-OMeTAD is among the first and longest standing organic HTM for sDSCs, it has some disadvantages such as low hole-mobility (≈10−4cm2V−1sec−1) [4

4. H. J. Snaith and L. Schmidt-Mende, “Advances in liquid-electrolyte and solid-State dye-sensitized solar cells,” Adv. Mater. 19(20), 3187–3200 (2007). [CrossRef]

,7

7. D. Poplavskyy and J. Nelson, “Nondispersive hole transport in amorphous films of methoxy-spirofluorenearylamine organic compounds,” J. Appl. Phys. 93(1), 341–346 (2003). [CrossRef]

] and relatively complex multistage synthesis [8

8. I.-K. Ding, J. Melas-Kyriazi, N.-L. Cevey-Ha, K. G. Chittibabu, S. M. Zakeeruddin, M. Grätzel, and M. D. McGehee, “Deposition of hole-transport materials in solid-state dye-sensitized solar cells by doctor-blading,” Org. Electron. 11(7), 1217–1222 (2010). [CrossRef]

]. Consequently, there is now a hot pursuit on the utility of conjugated polymers (CPs) as alternative HTMs due to their thermal stability, high conductivity, good solubility as well as tunable optoelectronic properties [9

9. G. K. Mor, S. Kim, M. Paulose, O. K. Varghese, K. Shankar, J. Basham, and C. A. Grimes, “Visible to near-infrared light harvesting in TiO2 nanotube array-P3HT based heterojunction solar cells,” Nano Lett. 9(12), 4250–4257 (2009). [CrossRef] [PubMed]

13

13. L. Yang, U. B. Cappel, E. L. Unger, M. Karlsson, K. M. Karlsson, E. Gabrielsson, L. Sun, G. Boschloo, A. Hagfeldt, and E. M. J. Johansson, “Comparing spiro-OMeTAD and P3HT hole conductors in efficient solid state dye-sensitized solar cells,” Phys. Chem. Chem. Phys. 14(2), 779–789 (2011). [CrossRef] [PubMed]

]. Additionally, they can also be used as cooperative light antenna to achieve panchromatic absorption in very thin films [14

14. G. Grancini, R. S. S. Kumar, M. Maiuri, J. Fang, W. T. S. Huck, M. Alcocer, G. Lanzani, A. Petrozza, G. Cerullo, and H. J. Snaith, “Panchromatic “dye-doped” polymer solar cells: from femtosecond energy relays to enhanced photo-response,” J. Chem Phys. Lett. 4(3), 442–447 (2013). [CrossRef]

]. We employ the ubiquitous semiconducting polymer in organic solar cells, poly(3-hexylthiophene) (P3HT), as the hole transport material for sDSC [13

13. L. Yang, U. B. Cappel, E. L. Unger, M. Karlsson, K. M. Karlsson, E. Gabrielsson, L. Sun, G. Boschloo, A. Hagfeldt, and E. M. J. Johansson, “Comparing spiro-OMeTAD and P3HT hole conductors in efficient solid state dye-sensitized solar cells,” Phys. Chem. Chem. Phys. 14(2), 779–789 (2011). [CrossRef] [PubMed]

].

2. Experimental details

The devices are fabricated using the procedure followed in our earlier work for optimized performances including the use of additives Li-TFSI and tBP [11

11. A. Abrusci, R. S. S. Kumar, M. Al-Hashimi, M. Heeney, A. Petrozza, and H. J. Snaith, “Influence of ion induced local coulomb field and polarity on charge generation and efficiency in poly (3-Hexylthiophene) -based solid-state dye-sensitized solar cells,” Adv. Funct. Mater. 21(13), 2571–2579 (2011).

]. The dye chosen for this work is the organic dye termed D131 [21

21. T. Horiuchi, H. Miura, and S. Uchida, “Highly efficient metal-free organic dyes for dye-sensitized solar cells,” J. Photochem. Photobiol. A 164(1-3), 29–32 (2004). [CrossRef]

] sensitized on 1μm thick mesoporous TiO2. We fabricated devices with region-random (RRa) and region-regular (RRe) P3HT as hole-transporter. We annealed the devices for 20 minutes at temperature of 140 °C. The current-voltage characteristics of all the devices under AM1.5 simulated sun light of 100 mWcm−2 have been measured using round metal mask to reduce the light piping [22

22. H. Snaith, “How should you measure your excitonic solar cells?” Energy Environ. Sci. 5(4), 6513–6520 (2012). [CrossRef]

]. To obtain repeatability 40 devices were fabricated and tested. During testing the active areas of the devices were defined by single aperture metal optical masks with a round aperture of 2.5 mm giving an area of 0.0491 cm2. We note that all light was excluded from entering the sides of the devices by having them in a “light-tight” sample holder, and the only light entering the solar cell substrate was through the single mask aperture. For the fs-TAS experiment, the laser source is an amplified mode locked Ti:sapphire laser (Clark-MXR Model CPA-1), delivering pulses at 1kHz repetition rate with 780 nm center wavelength, 150 fs duration. In the present work we used the second harmonic of fundamental centered at 390 nm as a pump pulse to excite the sample. Another small fraction of the Ti: sapphire amplified output is independently focused into a 1-mm-thick sapphire plate to generate a stable single-filament white-light supercontinuum which serves as a probe pulse. In a typical pump-probe experiment, the system under study is resonantly photoexcited by a short “pump” pulse and its subsequent dynamical evolution is detected by measuring the transmission (T) changes of a delayed “probe” pulse as a function of pump-probe delay τ given by the differential transmission ΔT/T[ = (Tpump-on-Tpump-off)/Tpump-off ]. The pump and probe beams are spatially and temporally overlapped on the sample, controlling the time delay by a motorized slit. The minimum detectable signal is ΔT/T ≈10−4 and the instrument response obtained is ≈200 fs time. The pump beam energy density used in the experiment is kept deliberately low (pump fluence = 10 μJ/cm2) to minimize bimolecular effects. All the measurements were taken with the samples in a vacuum chamber, to prevent any influence from oxygen or sample degradation.

3. Results and discussion

Figure 1(a)
Fig. 1 Normalized absorption spectra and molecular structure of D131, P3HT and the complete photovoltaic composite deposited on 1 μm TiO2. The shaded region represents the excitation pulse used for fs-TAS.
shows the absorption spectrum of the D131 sensitized TiO2 with (red circles) and without (black squares) RRe-P3HT. The dye shows a major absorption peak at 400 nm. Evidently the absorption spectra of P3HT (blue triangle) is complementary to the D131 absorption spectrum. From earlier reports, the HOMO levels of P3HT and D131 are assumed to be −5.10 eV [10

10. R. Zhu, C. Y. Jiang, B. Liu, and S. Ramakrishna, “Highly efficient nanoporous TiO2-polythiophene hybrid solar cells based on interfacial modification using a metal-free organic dye,” Adv. Mater. 21(9), 994–1000 (2009). [CrossRef]

] and −5.017 eV [23

23. R. Jose, A. Kumar, V. Thavasi, and S. Ramakrishna, “Conversion efficiency versus sensitizer for electrospun TiO2 nanorod electrodes in dye-sensitized solar cells,” Nanotechnology 19(42), 424004 (2008). [CrossRef]

] respectively, relative to vacuum. This energetic-landscape would favor hole-transfer from dye to P3HT making it a suitable candidate as a hole transporting layer. The design of the sDSC fabricated for the experiment is shown in Fig. 2(a)
Fig. 2 (a) Schematic design of the fabricated sDSC; (b) J-V characteristic for RRa P3HT (green empty dots), RRe P3HT (black full squares), thermal annealed RRe P3HT (red dotted line) and corresponding dark current in solid line. In the inset the table showing the device parameters
. The polymer is deposited on the D131-sensitized TiO2 mesoporous structure. The polymer infiltrates into the metal oxide pores and leaves a capping layer about of 200 nm thick. As a first attempt, we fabricated devices using regio-regular (RRe) P3HT and regio-random (RRa) P3HT. As seen from Fig. 2(b) devices with RRe-P3HT show better efficiency of 1.7% compared to 0.54% obtained with the RRa- P3HT. The photo-current density versus voltage traces for the sDSC were measured under AM 1.5G simulated sun light.

As a step forward, we annealed the RRe-P3HT devices at 140 °C for 20 minutes, before evaporating the top contact electrodes. The results (see dotted line in Fig. 2b) show an improved efficiency of 2.9%, leading to an increase of ≈70% compared to the un-annealed device. Significantly, Jsc increases from 3.2 mA/cm2 to 5.8 mA/cm2 upon thermal treatement suggesting an increase of ≈80% in the overall photo-generated charges reaching the electrodes upon annealing. No change in device performance is observed while annealing RRa-P3HT, suggesting annealing has no direct effect on it. The RRe-P3HT is known to have a planar backbone with respect to the twisted RRa-P3HT geometry (with inherent amorphous nature), leading to a higher crystallinity of the thin film, effect that is even more amplified upon annealing. This definitely affects the optoelectronic properties of the material [24

24. X. M. Jiang, R. Österbacka, O. Korovyanko, C. P. An, B. Horovitz, R. A. J. Janssen, and Z. V. Vardeny, “Spectroscopic studies of photoexcitations in regioregular and regiorandom polythiophene films,” Adv. Funct. Mater. 12(9), 587–597 (2002). [CrossRef]

29

29. Y. Kim, S. Cook, S. M. Tuladhar, S. A. Choulis, J. Nelson, J. R. Durrant, D. D. C. Bradley, M. Giles, I. McCulloch, C.-S. Ha, and M. Ree, “A strong regioregularity effect in self-organizing conjugated polymer films and high-efficiency polythiophene:fullerene solar cells,” Nat. Mater. 5(3), 197–203 (2006). [CrossRef]

]. For example, in P3HT: PCBM blend the hole-mobility in the P3HT phase is known to increase by more than three orders of magnitude upon annealing [27

27. V. D. Mihailetchi, H. Xie, B. de Boer, L. J. A. Koster, and P. W. M. Blom, “Charge transport and photocurrent generation in poly(3-hexylthiophene):methanofullerene bulk-heterojunction solar cells,” Adv. Funct. Mater. 16(5), 699–708 (2006). [CrossRef]

]. Therefore, upon annealing we conjecture improved device performances owing to change in morphology of the P3HT film itself. Additionally, we observe that open-circuit voltage (VOC) has slightly higher value upon annealing which can be surmised due to reduced charge-recombination pathways because of a different local morphology in the polymer for the annealed device. Also, contrary to our expectations we notice that the fill-factor (FF) obtained for the annealed device, though in agreement with data reported in literature [10

10. R. Zhu, C. Y. Jiang, B. Liu, and S. Ramakrishna, “Highly efficient nanoporous TiO2-polythiophene hybrid solar cells based on interfacial modification using a metal-free organic dye,” Adv. Mater. 21(9), 994–1000 (2009). [CrossRef]

, 11

11. A. Abrusci, R. S. S. Kumar, M. Al-Hashimi, M. Heeney, A. Petrozza, and H. J. Snaith, “Influence of ion induced local coulomb field and polarity on charge generation and efficiency in poly (3-Hexylthiophene) -based solid-state dye-sensitized solar cells,” Adv. Funct. Mater. 21(13), 2571–2579 (2011).

], has a slight reduction upon annealing. To this, we conjecture that the presence of additives might have an impact [2

2. A. Hagfeldt, G. Boschloo, L. Sun, L. Kloo, and H. Pettersson, “Dye-sensitized solar cells,” Chem. Rev. 110(11), 6595–6663 (2010). [CrossRef] [PubMed]

,10

10. R. Zhu, C. Y. Jiang, B. Liu, and S. Ramakrishna, “Highly efficient nanoporous TiO2-polythiophene hybrid solar cells based on interfacial modification using a metal-free organic dye,” Adv. Mater. 21(9), 994–1000 (2009). [CrossRef]

,11

11. A. Abrusci, R. S. S. Kumar, M. Al-Hashimi, M. Heeney, A. Petrozza, and H. J. Snaith, “Influence of ion induced local coulomb field and polarity on charge generation and efficiency in poly (3-Hexylthiophene) -based solid-state dye-sensitized solar cells,” Adv. Funct. Mater. 21(13), 2571–2579 (2011).

]. In particular, together with the different local morphology induced by annealing they can affect the charge dynamics thus resulting in minor variation of the FF. However, further investigations are needed to better address the variation in VOC and FF upon annealing.

In order to get insights on the effect of the nano-morphology on the photoexcited species and on their dynamics, we performed fs-TAS directly on samples which preserve the device configuration (without the top electrodes) before and after annealing. We tune the photoexcitation to 390 nm to predominantly excite the dye only. Upon photo-excitation, at the dye/TiO2 interface the exciton formed in the D131 dissociates and electrons are effectively injected into the metal oxide. Generally, the electron injection from an organic dye to TiO2 starts within the first 500 fs of the photo-excitation [11

11. A. Abrusci, R. S. S. Kumar, M. Al-Hashimi, M. Heeney, A. Petrozza, and H. J. Snaith, “Influence of ion induced local coulomb field and polarity on charge generation and efficiency in poly (3-Hexylthiophene) -based solid-state dye-sensitized solar cells,” Adv. Funct. Mater. 21(13), 2571–2579 (2011).

]. After the electron is injected, the hole is left in the dye, thus creating the oxidized dye species D131+ [30

30. W. H. Howie, F. Claeyssens, H. Miura, and L. M. Peter, “Characterization of solid-state dye-sensitized solar cells utilizing high absorption coefficient metal-free organic dyes,” J. Am. Chem. Soc. 130(4), 1367–1375 (2008). [CrossRef] [PubMed]

]. We identified the PA of D131+ species in the spectral region of 550-650 nm by performing the fs-TAS measurements of D131 adsorbed on TiO2 before depositing P3HT layer. In the device configuration after the deposition of P3HT as shown in Fig. 2(a) the dye is interfaced with P3HT. Due to the favorable HOMO level alignment of D131 and P3HT, the hole in D131 should transfer to P3HT thus forming P3HT+. Figure 3
Fig. 3 ΔT/T spectra of TiO2/D131/P3HT (a) un-annealed and (b) annealed devices by exciting the dye molecules at 390nm and probe in both the VIS spectral region.
shows the ΔT/T spectra of (a) un-annealed and (b) annealed samples. We can distinguish a positive band at shorter wavelength side of the spectrum that corresponds to the dye photobleaching (PB), in fair agreement with the ground-state absorption of the overall device material components. Though at 390 nm the dye molecules are resonantly excited, it should be noted that also P3HT partially absorbs at 390 nm (see Fig. 1) and hence the observation of a PB spectral band at 600 nm. In particular, we expect a contribution of the disordered P3HT phase for wavelengths shorter than 550nm. We assign the photo-induced absorption (PA) bands PA to D131+ partially overlapping with PA of P3HT+ species [31

31. E. V. Canesi, M. Binda, A. Abate, S. Guarnera, L. Moretti, V. D'Innocenzo, R. S. S. Kumar, C. Bertarelli, A. Abrusci, H. Snaith, A. Calloni, A. Brambilla, F. Ciccacci, S. Aghion, F. Moia, R. Ferragut, C. Melis, G. Malloci, A. Mattoni, G. Lanzani, and A. Petrozza, “The effect of selective interactions at the interface of polymer–oxide hybrid solar cells,” Energy Environ. Sci. 5(10), 9068–9076 (2012). [CrossRef]

] peaking at 750 nm.

4. Conclusions

We performed a systematic investigation on the effect of the polymer morphology of the P3HT used as hole-transport layer in solid-state dye sensitized solar cells (sDSC). Fabricated devices are tested before and after annealing and were observed to show ≈80% increase in Jsc and ≈70% in efficiency after annealing. We performed fs-TAS experiments to investigate the effect of morphology on the hole-transfer and recombination dynamics. We observed that upon annealing there is enhancement in the hole-transfer from dye to P3HT along with enhanced hole-mobility, thus being an effective way to increase the overall device performances.

Acknowledgments

Authors thank Mr. Andy Hey, University of Oxford, for his contribution to the illustration. We thank EPSRC for funding, and the Royal Society International Exchange Scheme 2012/R2 for supporting this collaboration.

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W. H. Howie, F. Claeyssens, H. Miura, and L. M. Peter, “Characterization of solid-state dye-sensitized solar cells utilizing high absorption coefficient metal-free organic dyes,” J. Am. Chem. Soc. 130(4), 1367–1375 (2008). [CrossRef] [PubMed]

31.

E. V. Canesi, M. Binda, A. Abate, S. Guarnera, L. Moretti, V. D'Innocenzo, R. S. S. Kumar, C. Bertarelli, A. Abrusci, H. Snaith, A. Calloni, A. Brambilla, F. Ciccacci, S. Aghion, F. Moia, R. Ferragut, C. Melis, G. Malloci, A. Mattoni, G. Lanzani, and A. Petrozza, “The effect of selective interactions at the interface of polymer–oxide hybrid solar cells,” Energy Environ. Sci. 5(10), 9068–9076 (2012). [CrossRef]

32.

W. C. Tsoi, S. J. Spencer, L. Yang, A. M. Ballantyne, P. G. Nicholson, A. Turnbull, A. G. Shard, C. E. Murphy, D. D. C. Bradley, J. Nelson, and J.-S. Kim, “Effect of crystallization on the electronic energy levels and thin film morphology of P3HT:PCBM Blends,” Macromolecules 44(8), 2944–2952 (2011). [CrossRef]

OCIS Codes
(040.5350) Detectors : Photovoltaic
(160.5470) Materials : Polymers
(320.7150) Ultrafast optics : Ultrafast spectroscopy
(350.6050) Other areas of optics : Solar energy

ToC Category:
Dye-Sensitized Solar Cells

History
Original Manuscript: February 12, 2013
Revised Manuscript: March 24, 2013
Manuscript Accepted: March 27, 2013
Published: April 22, 2013

Virtual Issues
Renewable Energy and the Environment (2013) Optics Express

Citation
R. Sai Santosh Kumar, G. Grancini, A. Petrozza, A. Abrusci, H. J. Snaith, and G. Lanzani, "Effect of polymer morphology on P3HT-based solid-state dye sensitized solar cells: an ultrafast spectroscopic investigation," Opt. Express 21, A469-A474 (2013)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-21-S3-A469


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  31. E. V. Canesi, M. Binda, A. Abate, S. Guarnera, L. Moretti, V. D'Innocenzo, R. S. S. Kumar, C. Bertarelli, A. Abrusci, H. Snaith, A. Calloni, A. Brambilla, F. Ciccacci, S. Aghion, F. Moia, R. Ferragut, C. Melis, G. Malloci, A. Mattoni, G. Lanzani, and A. Petrozza, “The effect of selective interactions at the interface of polymer–oxide hybrid solar cells,” Energy Environ. Sci.5(10), 9068–9076 (2012). [CrossRef]
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