Name: Electrospinning of Photocatalytic Electrodes for Dye-sensitized Solar Cells (Video) | JoVE Journal
Uploaded: 2017-06-28T13:00:00.000+00:00
Duration: 9 min 30 s
Description: Learn electrospinning to fabricate photocatalytic photoanodes for dye-sensitized solar cells using one-dimensional inorganic nanofibres. This method enhances device performance through improved directionality and charge transport.

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5 minutes

The authors have no acknowledgements.

1. Precursor Solution Preparation
NOTE: Please consult all relevant material safety data sheets (MSDS) before use. Several of the chemicals used in this procedure are harmful and/or toxic to humans. Nanomaterials may have additional hazards compared to their bulk counterpart. Please use the appropriate safety measures and personal protective equipment.
<ol>
	<li>Place 5 g of titanium(IV) n-butoxide, 1 g of polyvinylpyrrolidone (PVP), 1 mL of glacial acetic acid, and 10 mL of absolute ethanol into a sample vial.</li>
	<li>Use a magnetic stirring plate to mix the solution until it has become homogeneous and no bubbles can be observed.</li>
</ol>
2. Electrospinning and Calcination of the Nanofibers
<ol>
	<li>Prepare the needle used for the electrospinning process by cutting off the tip of a 21 G needle and sanding it down using moderate-grade sandpaper until the tip is completely flat.</li>
	<li>Mount the needle on a disposable 10 mL syringe.</li>
	<li>Load some of the precursor solution into the syringe and place it on the syringe pump.</li>
	<li>Wrap the collector plate in aluminum foil and place it directly in front of the needle tip. 
	NOTE: The distance from the needle to the plate should be 20 cm.</li>
	<li>Connect the collector plate to the ground and the needle to the high-voltage power source.</li>
	<li>Place the protective shield around the setup.</li>
	<li>Set the flow rate on the syringe pump to 1 mL/h and begin pumping.</li>
	<li>As soon as some solution appears at the tip of the needle, turn on the high-voltage source and set it to 15 kV. 
	NOTE: At this point, fibers are going to collect on the plate. The setup be left running for as long as necessary to achieve the desired thickness of the fiber mat.</li>
	<li>After the spinning is completed, turn off the high-voltage source and syringe pump. Remove the foil from the collector plate.</li>
	<li>Let the fibers rest overnight and then peel them off the aluminum foil.</li>
	<li>Place the peeled-off fibers in a crucible and place that into a muffle furnace.</li>
	<li>Calcinate the fibers by setting up a temperature ramp of 5&#176;/min up to 500 &#176;C and holding for 2 h to remove the PVP and to produce pure TiO2 nanofibers.</li>
	<li>Once the calcination process is completed, leave the furnace closed until the temperature reaches below 80 &#176;C to avoid any thermal shock, which may damage the fibers.</li>
</ol>
3. Electrode Fabrication
<ol>
	<li>Preparation of the slurries
	<ol>
		<li>Add 500 mg of titanium dioxide paste to 20 mL of ethanol in a round-bottomed flask.</li>
		<li>In a separate flask, mix 500 mg of the electrospun TiO2-NFs with another 20 mL of ethanol.</li>
		<li>Sonicate the solutions for 2 h using a bath sonicator.</li>
		<li>Once uniform mixtures are obtained, add 2 mL of terpineol to each flask and sonicate for another 15 min.</li>
		<li>Evaporate the solvent from both flasks using a rotary evaporator to obtain the slurries.</li>
	</ol>
	</li>
	<li>Doctor blading and sintering
	<ol>
		<li>Using a diamond glass cutter, cut an FTO-conductive glass slide into a 2 cm x 2 cm square.</li>
		<li>Secure the FTO slide to the work area by placing adhesive tape on the glass slide, leaving a 0.4-cm2 area exposed in the center. To avoid an irregular coating, place the tape on two parallel sides first and then on the other two.</li>
		<li>Deposit a few drops of the TiO2-NP slurry on the exposed center of the slide.</li>
		<li>Use a razor blade to spread the slurry evenly over the exposed area.</li>
		<li>Once a uniform coating is achieved, carefully remove the adhesive tape.</li>
		<li>Place the coated slide in a furnace and sinter at 500 &#176;C for 2 h.</li>
		<li>Repeat steps 3.2.2-3.2.6 on the same FTO slide, this time using the TiO2-NF slurry instead of the nanoparticles, to obtain the photoanode.</li>
	</ol>
	</li>
</ol>
4. NF Characterization
<ol>
	<li>SEM characterization
	<ol>
		<li>Prepare the sample for SEM by attaching a strip of adhesive carbon tape to a microscope stub. Carefully place a small quantity of nanofibers on the tape.</li>
		<li>Mount the stub onto a sample holder and load it into the exchange chamber of the instrument.</li>
		<li>Set up the instrument conditions and parameters: set the accelerating voltage to 20 kV and the working distance to 10 mm.</li>
		<li>Collect images of the sample, making sure that they display the overall morphology of the material.</li>
	</ol>
	</li>
	<li>XRD characterization
	<ol>
		<li>Gently grind some nanofibers into a fine powder and spread them evenly on an XRD stage.</li>
		<li>Load the sample into the diffractometer.</li>
		<li>Set up the acquisition parameters: use a start angle of 10&#176;, an end angle of 80&#176;, and a step size of 0.015&#176;.</li>
		<li>Start the acquisition of the XRD data.</li>
	</ol>
	</li>
</ol>
5. Solar-cell Fabrication
<ol>
	<li>Treat the photoanode with an aqueous solution of TiCl4 at 75 &#176;C for 45 min. After treatment, wash it with deionized water and dry it.</li>
	<li>Sensitize the photoanode by submerging it in a 0.5-mM solution of ruthenium dye N719 in absolute ethanol for 24 h under dark conditions.</li>
	<li>Place a sheet of sealing film on top of the sensitized photoanode to serve as a thermoplastic gasket between the photoanode and the counter-electrode.</li>
	<li>Place a Pt-coated FTO counter-electrode with a pre-drilled hole in the center, on top of the sealing film, such that both sides face each other.</li>
	<li>Heat the assembled cell to 100 &#176;C for 15 min to seal the gasket.</li>
	<li>Deposit a few drops of a redox mediator, consisting of a solution of 1-propyl-3-methylimidazolium iodide (0.8 M), iodine (0.1 M), and benzimidazole (0.3 M) in 3-methoxypropionitrile, on top of the pre-drilled hole of the counter-electrode.</li>
	<li>Place the cell in a vacuum desiccator to let the redox mediator fill the internal space of the assembled cell.</li>
</ol>
6. J-V Curve Characterization
<ol>
	<li>Acquire the J-V curves using a digital source meter under 100 mW/cm2 illumination from a xenon-arc source passed through an AM1.5G filter.</li>
</ol>

<ol><li>O'Regan, B., Grätzel, M. <a target="_blank" href="http://www.nature.com/nature/journal/v353/n6346/abs/353737a0.html">A low-cost, high-efficiency solar cell based on dye-sensitized colloidal TiO2 films.</a> Nature. 353 (6346), 737-740 (1991).</li>
<li>Lee, C. H., Chiu, W. H., Lee, K. M., Hsieh, W. F., Wu, J. M. <a target="_blank" href="http://pubs.rsc.org/en/Content/ArticleLanding/2011/JM/C0JM04099A#!divAbstract">Improved performance of flexible dye-sensitized solar cells by introducing an interfacial layer on Ti substrates.</a> J Mat Chem. 21 (13), 5114-5119 (2011).</li>
<li>Burschka, J., Pellet, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Sequential+deposition+as+a+route+to+high-performance+perovskite-sensitized+solar+cells%5BTitle%5D)+AND+%22Nature%22%5BJournal%5D)">Sequential deposition as a route to high-performance perovskite-sensitized solar cells.</a> Nature. 499 (7458), 316-319 (2013).</li>
<li>Ohsaki, Y., Masaki, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Dye-sensitized+TiO2+nanotube+solar+cells%3A+fabrication+and+electronic+characterization%5BTitle%5D)+AND+%22Phys+Chem+Chem+Phys%22%5BJournal%5D)">Dye-sensitized TiO2 nanotube solar cells: fabrication and electronic characterization.</a> Phys Chem Chem Phys. 7 (24), 4157-4163 (2005).</li>
<li>Mor, G. K., Shankar, K., Paulose, M., Varghese, O. K., Grimes, C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Enhanced+Photocleavage+of+Water+Using+Titania+Nanotube+Arrays%5BTitle%5D)+AND+%22Nano+Letters%22%5BJournal%5D)">Enhanced Photocleavage of Water Using Titania Nanotube Arrays.</a> Nano Letters. 5 (1), 191-195 (2005).</li>
<li>Feng, X., Shankar, K., Varghese, O. K., Paulose, M., Latempa, T. J., Grimes, C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Vertically+Aligned+Single+Crystal+TiO2+Nanowire+Arrays+Grown+Directly+on+Transparent+Conducting+Oxide+Coated+Glass%3A+Synthesis+Details+and+Applications%5BTitle%5D)+AND+%22Nano+Letters%22%5BJournal%5D)">Vertically Aligned Single Crystal TiO2 Nanowire Arrays Grown Directly on Transparent Conducting Oxide Coated Glass: Synthesis Details and Applications.</a> Nano Letters. 8 (11), 3781-3786 (2008).</li>
<li>Roy, P., Berger, S., Schmuki, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((TiO2+Nanotubes%3A+Synthesis+and+Applications%5BTitle%5D)+AND+%22Angewandte+Chemie+International+Edition%22%5BJournal%5D)">TiO2 Nanotubes: Synthesis and Applications.</a> Angewandte Chemie International Edition. 50 (13), 2904-2939 (2011).</li>
<li>Macdonald, T. J., Xu, J., et al. <a target="_blank" href="http://www.mdpi.com/2079-4991/4/2/256">NiO Nanofibers as a Candidate for a Nanophotocathode.</a> Nanomaterials. 4 (2), 256-266 (2014).</li>
<li>Chuangchote, S., Sagawa, T., Yoshikawa, S. <a target="_blank" href="http://aip.scitation.org/doi/abs/10.1063/1.2958347?journalCode=apl">Efficient dye-sensitized solar cells using electrospun TiO2 nanofibers as a light harvesting layer.</a> Appl Phys Lett. 93 (3), 033310(2008).</li>
<li>Li, D., Xia, Y. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1002/adma.200400719/abstract">Electrospinning of Nanofibers: Reinventing the Wheel?</a> Adv Mat. 16 (14), 1151-1170 (2004).</li>
<li>Li, W. J., Laurencin, C. T., Caterson, E. J., Tuan, R. S., Ko, F. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Electrospun+nanofibrous+structure%3A+A+novel+scaffold+for+tissue+engineering%5BTitle%5D)+AND+%22J+Biomed+Mat+Res%22%5BJournal%5D)">Electrospun nanofibrous structure: A novel scaffold for tissue engineering.</a> J Biomed Mat Res. 60 (4), 613-621 (2002).</li>
<li>Jia, H., Zhu, G., Vugrinovich, B., Kataphinan, W., Reneker, D. H., Wang, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Enzyme-Carrying+Polymeric+Nanofibers+Prepared+via+Electrospinning+for+Use+as+Unique+Biocatalysts%5BTitle%5D)+AND+%22Biotechnol+Prog%22%5BJournal%5D)">Enzyme-Carrying Polymeric Nanofibers Prepared via Electrospinning for Use as Unique Biocatalysts.</a> Biotechnol Prog. 18 (5), 1027-1032 (2002).</li>
<li>Mai, L., Xu, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Electrospun+Ultralong+Hierarchical+Vanadium+Oxide+Nanowires+with+High+Performance+for+Lithium+Ion+Batteries%5BTitle%5D)+AND+%22Nano+Letters%22%5BJournal%5D)">Electrospun Ultralong Hierarchical Vanadium Oxide Nanowires with High Performance for Lithium Ion Batteries.</a> Nano Letters. 10 (11), 4750-4755 (2010).</li>
<li>Cai, J., Niu, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((High-Performance+Supercapacitor+Electrode+Materials+from+Cellulose-Derived+Carbon+Nanofibers%5BTitle%5D)+AND+%22ACS+Appl+Mat+Interfaces%22%5BJournal%5D)">High-Performance Supercapacitor Electrode Materials from Cellulose-Derived Carbon Nanofibers.</a> ACS Appl Mat Interfaces. 7 (27), 14946-14953 (2015).</li>
<li>Joshi, P., Zhang, L., et al. <a target="_blank" href="http://pubs.rsc.org/en/Content/ArticleLanding/2010/EE/c0ee00068j#!divAbstract">Composite of TiO2 nanofibers and nanoparticles for dye-sensitized solar cells with significantly improved efficiency.</a> Energ Environ Sci. 3 (10), 1507-1510 (2010).</li>
<li>Macdonald, T. J., Tune, D. D., Dewi, M. R., Gibson, C. T., Shapter, J. G., Nann, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((A+TiO2+Nanofiber-Carbon+Nanotube-Composite+Photoanode+for+Improved+Efficiency+in+Dye-Sensitized+Solar+Cells%5BTitle%5D)+AND+%22ChemSusChem%22%5BJournal%5D)">A TiO2 Nanofiber-Carbon Nanotube-Composite Photoanode for Improved Efficiency in Dye-Sensitized Solar Cells.</a> ChemSusChem. 8 (20), 3396-3400 (2015).</li>
<li>Teo, W. E. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aTeo%2C+WE+%22Electrospinning+parameters+and+fiber+control%22">Electrospinning parameters and fiber control</a>. , 
 <a target="_blank" href="http://electrospintech.com/hb-espinparameters.html ">http://electrospintech.com/hb-espinparameters.html </a> (2015).</li>
</ol>

The authors have nothing to disclose.

The methods presented in this work describe the fabrication of efficient nanofibrous photoanodes for photocatalytic devices such as DSSCs. Electrospinning is a very versatile technique for the fabrication of nanofibers, but a certain level of skill and knowledge is required to obtain materials with optimal morphologies. One of the most critical aspects to obtaining good nanofibers is the preparation of the precursor solution: there are some key factors, such as the concentration of the carrier polymer and the choice of t...

Dye-sensitized solar cells (DSSCs) are an interesting alternative to silicon-based solar cells1 thanks to their low cost, relatively simple manufacturing process, and ease of large-scale production. Another benefit is their potential to be incorporated into flexible substrates, a distinct advantage over silicon-based solar cells2. A typical DSSC utilizes: (1) a nanoparticulate TiO2 photoanode, sensitized with a dye, as a light-harvesting layer; (2) a Pt-coated FTO, used as a counter electrode; and (3) an electrolyte containing a redox couple, such as I-/I3-, placed between the two electrodes, working as a &#34;hole-conducting medium.&#34;
Although DSSCs have surpassed efficiencies of 15%3, the performance of nanoparticle-based photoanodes is still still hindered by a number of limitations, including slow electron mobility4, poor absorption of low-energy photons5, and charge recombination6. The electron collection efficiency strongly depends upon the rate of electron transport through the TiO2 nanoparticle layer. If the charge diffusion is slow, the probability of recombination with I3- in the electrolyte solution increases, resulting in a loss of efficiency.
It has been shown that replacing nanoparticulate TiO2 with one-dimensional (1D) TiO2 nanoarchitectures can improve charge transport by reducing the scattering of free electrons from the grain boundaries of the interconnected TiO2 nanoparticles7. As 1D nanostructures provide a more direct pathway for charge collection, we can expect that electron transport in nanofibers (NFs) would be significantly faster than in nanoparticles8,9.
Electrospinning is one of the most commonly used methods for the fabrication of fibrous materials with sub-micron diameters10. This technique involves the use of high voltage to induce the ejection of a polymer solution jet through a spinneret. Due to bending instability, this jet is subsequently stretched many times to form continuous nanofibers. In recent years, this technique has been extensively used to fabricate polymeric and inorganic materials, which have been used for numerous and diverse applications, such as tissue engineering11, catalysis12, and as electrode materials for lithium ion batteries13 and supercapacitors14.
The use of electrospun TiO2-NFs as the scattering layer in the photoanode can increase the performance of DSSCs. However, photoanodes with nanofibrous architectures tend to have poor dye absorption due to surface-area limitations. One of the possible solutions to overcome this is to mix NFs and nanoparticles. This has been shown to result in additional scattering layers, improving light absorption and overall efficiency15.
The protocol presented in this video provides a facile method to synthesize ultralong TiO2 nanofibers through a combination of electrospinning and sol-gel techniques, followed by a calcination process. The protocol then illustrates the use of the TiO2-NFs in combination with nanoparticulate TiO2 for the fabrication of a dual-layer photoanode with enhanced light-scattering capability using doctor blading techniques, as well as the subsequent assembly of a DSSC using such a photoanode.

<table><tbody><tr><td>titanium(IV) n-butoxide</td><td>Sigma-Aldrich</td><td>244112</td><td></td></tr><tr><td>Polyvinylpyrrolidone</td><td>Sigma-Aldrich</td><td>437190</td><td></td></tr><tr><td>glacial acetic acid</td><td>Sigma-Aldrich</td><td>A6283</td><td></td></tr><tr><td>Ethanol, absolute</td><td>Fisher Scientific</td><td>E/0650DF/17</td><td></td></tr><tr><td>20 mL Sample vials</td><td>(any)</td><td></td><td>(or larger volume)</td></tr><tr><td>disposable 21G needle</td><td>(any)</td><td></td><td></td></tr><tr><td>P150 grit sandpaper</td><td>(any)</td><td></td><td></td></tr><tr><td>disposable 10mL syringe</td><td>(any)</td><td></td><td>(or larger volume)</td></tr><tr><td>magnetic stirrer + stirring bar</td><td>(any)</td><td></td><td></td></tr><tr><td>PHD 2000 syringe pump</td><td>Harvard Apparatus</td><td>71-2002</td><td>(or any other syringe pump capable of outputting a 1mL/hr flow</td></tr><tr><td>Aluminium foil</td><td>(any)</td><td></td><td></td></tr><tr><td>Stainless steel collector plate</td><td>(custom built)</td><td></td><td></td></tr><tr><td>High Voltage Power Source</td><td>Gamma High Voltage Research, Inc</td><td>ES30P-10W</td><td>(or any other power supply capable of outputting +15 kV</td></tr><tr><td>Polycarbonate protective shield</td><td>(custom built)</td><td></td><td></td></tr><tr><td>Ceramic crucible</td><td>(any)</td><td></td><td></td></tr><tr><td>Muffle furnace</td><td>(any)</td><td></td><td></td></tr><tr><td>Titanium dioxide, nanopowder</td><td>Sigma-Aldrich</td><td>718467</td><td></td></tr><tr><td>50 mL 1-neck round bottom flasks</td><td>(any)</td><td></td><td></td></tr><tr><td>bath sonicator</td><td>(any)</td><td></td><td></td></tr><tr><td>Terpineol</td><td>Sigma-Aldrich</td><td></td><td></td></tr><tr><td>Rotary evaporator</td><td>(any)</td><td></td><td></td></tr><tr><td>FTO glass</td><td>Solaronix</td><td>TCO30-10/LI</td><td></td></tr><tr><td>Adhesive tape</td><td>(any)</td><td></td><td></td></tr><tr><td>razor blade</td><td>(any)</td><td></td><td></td></tr><tr><td>SEM</td><td>JEOL</td><td>6500F</td><td></td></tr><tr><td>XRD</td><td>PANalytical&amp;nbsp;</td><td>X&#039;pert Pro</td><td></td></tr><tr><td>Titanium Tetrachloride</td><td>Sigma-Aldrich</td><td>89545</td><td></td></tr><tr><td>Ruthenizer&amp;nbsp; 535-bisTBA</td><td>Solaronix</td><td>N719</td><td></td></tr><tr><td>sealing film</td><td>Dyesol</td><td>Meltonix 1170-25</td><td></td></tr><tr><td>Pt-coated FTO</td><td>Solaronix</td><td>TCO30-10/LI</td><td></td></tr><tr><td>1-propyl-3-methylimidazolium iodide</td><td>Sigma-Aldrich</td><td>49637</td><td></td></tr><tr><td>Iodine</td><td>Sigma-Aldrich</td><td>207772</td><td></td></tr><tr><td>benzimidazole</td><td>Sigma-Aldrich</td><td>194123</td><td></td></tr><tr><td>3-Methoxypropionitrile</td><td>Sigma-Aldrich</td><td>65290</td><td></td></tr><tr><td>Digital source meter</td><td>Keithley</td><td>2400</td><td></td></tr><tr><td>Solar Simulator</td><td>Abet technologies</td><td>10500</td><td></td></tr></tbody></table>

electrospinning of photocatalytic electrodes for dye-sensitized solar cells

Electrospinning of Photocatalytic Electrodes for Dye-sensitized Solar Cells

This work demonstrates a protocol to fabricate a fiber-based photoanode for dye-sensitized solar cells, consisting of a light-scattering layer made of electrospun titanium dioxide nanofibers (TiO2-NFs) on top of a blocking layer made of commercially available titanium dioxide nanoparticles (TiO2-NPs). This is achieved by first electrospinning a solution of titanium (IV) butoxide, polyvinylpyrrolidone (PVP), and glacial acetic acid in ethanol to obtain composite PVP/TiO2 nanofibers. These are then calcined at 500 &#176;C to remove the PVP and to obtain pure anatase-phase titania nanofibers. This material is characterized using scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). The photoanode is prepared by first creating a blocking layer through the deposition of a TiO2-NPs/terpineol slurry on a fluorine-doped tin oxide (FTO) glass slide using doctor blading techniques. A subsequent thermal treatment is performed at 500 &#176;C. Then, the light-scattering layer is formed by depositing a TiO2-NFs/terpineol slurry on the same slide, using the same technique, and calcinating again at 500 &#176;C. The performance of the photoanode is tested by fabricating a dye-sensitized solar cell and measuring its efficiency through J-V curves under a range of incident light densities, from 0.25-1 Sun.

The TiO2 nanofibers were characterized using SEM, X-ray photoelectron spectroscopy (XPS), and XRD. The nanostructure of the photoanode was characterized using SEM. The performance of the assembled DSSC was tested using a solar simulator and a source measure unit.
The SEM image in Figure 1A shows that the nanofibers synthesized using this protocol have a porous structure and a high aspect ...

The overall goal of this project was to use electrospinning to fabricate a photoanode with improved performance for dye-sensitized solar cells.

This work demonstrates a protocol to fabricate a fiber-based photoanode for dye-sensitized solar cells, consisting of a light-scattering layer made of ...

The overall goal of this work is to fabricate a photoanode for dye-sensitized solar cells with improved performance using electrospinning. Nanomaterials are great. They show chemical and physical properties that you cannot find in the corresponding bulk materials.However, if you try to make a device using nanomaterials, this become, can become quite difficult. In this video, we show how to fabricate one-dimensional inorganic nanofibres, and using them for a solar cell device. The directionality in the nanofibres causes the devices to have a much better performance compared with devices that just use nanocrystalline materials.To make the precursor solution, place 10 milliliters of absolute ethanol, one milliliter of glacial acetic acid, five grams of Titanium(II)oxide, and one gram of PVP into a sample vial. Mix the solution until it has become homogeneous and no bubbles can be observed. In order to obtain a one-dimensional nanoarchitecture, we're going to use electrospinning.A simple yet rather clever technique which allows us to obtain nanofibres with several micrometers in length and only few hundred nanometers in diameter. To prepare the needle used for the electrospinning process, cut the tip of a 21 gauge needle and sand it down using moderate grade sandpaper until the tip is completely flat. Load the precursor solution into the syringe and place it on the syringe pump.Wrap the collector plate with aluminum foil and place the protective shield around the setup. The distance between the needle and the collector plate should be 20 centimeters. Connect the collector to the ground and the needle to the power source.Set the flow rate of the syringe pump to one milliliter per hour, and begin pumping. As soon as some solution appears on the tip of the needle, turn on the high voltage source and set it to 15 kilovolts. At this point, fibers are going to collect on the plate.This can be left running for as long as necessary to achieve the desired thickness of the fiber mat. After the spinning is completed, turn off the high voltage source and remove the foil from the collector plate. Letting the fibers rest overnight makes it easier to peel them off the collector plate.Place the peeled off fibers in a crucible and place them in a furnace with a temperature ramp of five degrees per minute, up to 500 degrees for two hours to remove the PVP and produce pure TiO2 nanofibres. Fabrication of the photoanode requires that the position of a light-scattering layer consisting of titanium dioxide nanofibres on top of a blocking layer made of commercially available titanium dioxide nanoparticles. This is essential for preventing charge accumulation with a substrate.Start by adding 500 milligrams of titanium dioxide nanoparticles to 20 mils of ethanol in a round-bottom flask. In a separate flask, mix 500 milligrams of the electrospun titanium dioxide nanofibres with another 20 mils of ethanol. Sonicate the solutions for two hours using a bath sonicator.Once uniform mixtures are obtained, add 2 mils of terpineol to each flask, and sonicate for another 15 minutes. Finally, evaporate the solvent using a rotary evaporator to obtain the slurries. Using a diamond glass cutter, cut an FTO slide into a two by two centimeter square.Place adhesive tape on the glass slide, leaving a 0.4 square centimeter area, exposing the center. Deposit a few drops of the titanium dioxide nanoparticle slurry on the center of the glass slide. Use a razor blade to spread the slurry evenly on the exposed area.Once a uniform coating is achieved, carefully remove the adhesive tape. Photoanodes are then placed in a furnace and centered at 500 degrees for two hours. Repeat the process on the same glass slide, this time using the nanofibre slurry to deposit the light scattering layer.The composite photoanode is again centered at 500 degrees for two hours. To characterize our nanofibres, we are going to use SEM and XRD, and then to test the performance of our nanofibres, we are going to implement them in a dye-sensitized solar cell. To prepare the sample for scanning electron microscoping, attach a strip of adhesive carbon tape on the microscope stub.And then carefully place a small quantity of nanofibres on the tape. Mount the stub onto a sample holder and lower it into the exchange chamber of the instrument. Set up the instrument conditions and parameters accordingly.Collect images of the sample, making sure that they display the overall morphology of the material. The SEM images show that the fibers are porous in structure and have a high aspect ratio. To prepare the material for X-ray diffraction characterization, gently grind some nanofibres into a fine powder and spread them evenly on an XRD stage.Load the sample into the diffractometer. Set up the acquisition parameters and start collecting the data. The diffractogram shows a series of peaks corresponding to the anatase phase of titanium dioxide.To prepare the solar cell, first treat the TiO2 photoanodes with an aqueous solution of TiCl4 at 75 degrees C for 45 minutes. After treatment, wash the photoanodes with the ionized water. Dry them, and insensitize them in a solution of Ruthenizer N719 and absolute ethanol for 24 hours under dark conditions.The sensitized photoanodes will wash with ethanol to remove excess dye molecules from the TiO2 photoanode surface. Sealing film is used as a thermoplastic gasket between the counter electrode and the photoanodes. Counter electrodes of platinum-coated FTO are used for all solar cells.The assembled solar cells are heated to 100 degrees C for 15 minutes to seal the gasket. A redox mediator is added to the internal space of the solar cells by vacuum filling. J-V curves are acquired using a Keithley 2400 Digital SourceMeter under a 100 milowatt per centimeter square illumination from a xenon arc source passed through an AM 1.5 G filter.The illumination plane for the light source is calibrated with a monocrystalline silicon reference cell. In this video, we have shown you how to fabricate a dye-sensitized solar cells using inorganic nanofibres. On top of this application, there are many other possibilities.For example, batteries, transparent electrodes, active filters, and others. If you want to know more details, please have a look at our publications. I hope you enjoyed and learned from this video, and please contact us if you've got question or want to give any feedback.

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Research

JoVE Journal

Engineering

The process of electrospinning polymers for tissue engineering and cell culture is addressed in this article.  Specifically, the electrospinning of photoreactive macromers with additional processing capabilities of photopatterning and multi-polymer electrospinning is described.

Electrospinning Fibrous Polymer Scaffolds for Tissue Engineering and Cell Culture

Electrospinning techniques can create a variety of nanofibrous scaffolds for tissue engineering or other applications.  We describe here a procedure to optimize the parameters of the electrospinning solution and apparatus to obtain fibers with the desired morphology and alignment.  Common problems and troubleshooting techniques are also presented.

Electrospinning Fundamentals: Optimizing Solution and Apparatus Parameters

An integrated device, incorporating a dye-sensitized solar cell and triplet-triplet annihilation up-conversion unit was produced, affording enhanced light harvesting, from a wider section of the solar spectrum. Under modest irradiation levels a significantly enhanced response to low energy photons was demonstrated, yielding a record figure of merit for dye-sensitized solar cells.

Integrating a Triplet-triplet Annihilation Up-conversion System to Enhance Dye-sensitized Solar Cell Response to Sub-bandgap Light

This paper investigates the suitability of inkjet printing for the manufacturing of dye-sensitized solar cells. A binder-free TiO2 nanoparticle ink was formulated and printed onto a FTO glass substrate. The printed layer was fabricated into a cell with an active area of 0.25 cm2 and an efficiency of 3.5%.

Digital Printing of Titanium Dioxide for Dye Sensitized Solar Cells

This protocol demonstrates how to achieve femto molar detection sensitivity of proteins in 10 µL of whole blood within 30 min. This can be achieved by using electrospun nanofibrous mats integrated in a lab-on-a-disc, which offers high surface area as well as effective mixing and washing for enhanced signal-to-noise ratio.

Fully Automated Centrifugal Microfluidic Device for Ultrasensitive Protein Detection from Whole Blood

We have directly incorporated a stilbene-based organic dye into a cobaloxime core to generate a photosensitizer-catalyst dyad for photocatalytic H2 production. We have also developed a simple experimental setup for evaluating the light-driven H2 production by photocatalytic assemblies.

Developing Photosensitizer-Cobaloxime Hybrids for Solar-Driven H2 Production in Aqueous Aerobic Conditions

This paper describes a simple technique for coating electrospun PAN nanofibers with electroactive polymers using vapor deposition. The effects of the oxidant FeCl₃ on the deposition of poly(3,4-ethylenedioxythiophene) coatings on PAN were investigated to understand and optimize polymer growth, fiber diameter, and overall mechanical strength of the nanofiber mats.

Vapor Phase Deposition of Electroactive Poly(3,4-ethylenedioxythiophene) onto Electrospun Commodity Polymer Nanofibers

A synthesis technique to prepare the visible-light-responsive ZnCoS/ZnCdS with twin crystal structure photocatalyst and the photoredox reaction testing technique of its photocatalytic activity and selectivity in H2 evolution and benzaldehyde production is presented.

Synthesis and Performance Evaluations of ZnCoS/ZnCdS with Twin Crystal Structure for Multifunctional Redox Photocatalysis in Energy Applications

This protocol guides the fabrication and electrochemical analysis of MXene-supported CuZn and NiCo bi-metallic electrocatalysts for green fuel production from carbon dioxide and water using solar energy.

Solar-Driven Electrochemical Green Fuel Production from CO2 and Water Using Ti3C2Tx MXene-Supported CuZn and NiCo Catalysts

Polycrystalline silicon thin-film solar cells on glass are fabricated by deposition of boron and phosphorous doped silicon layers followed by crystallisation, defect passivation and metallisation. Plasmonic light-trapping is introduced by forming Ag nanoparticles on the silicon cell surface capped with a diffused reflector resulting in ~45% photocurrent enhancement.

Polycrystalline Silicon Thin-film Solar cells with Plasmonic-enhanced Light-trapping

Learn electrospinning to fabricate photocatalytic photoanodes for dye-sensitized solar cells using one-dimensional inorganic nanofibres. This method enhances device performance through improved directionality and charge transport.

Electrospinning of Photocatalytic Electrodes for Dye-sensitized Solar Cells

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