This work was supported by the National Science Foundation, through the Nebraska MRSEC (Grant DMR-1420645), CHE-1565692, and CHE-145533 as well as the Nebraska Center for Energy Science Research.

CAUTION: Please consult the lab&#8217;s material safety data sheets (MSDS) before proceeding. The chemicals used in these synthesis protocols have associated health hazards. Additionally, nanomaterials have additional hazards compared to their bulk counterpart. Please use all appropriate safety practices when performing a nanocrystal reaction including the use of a fume hood or glovebox and the proper personal protective equipment (safety glasses, gloves, lab coat, pants, closed-toe shoes, etc.).
<p class="j...

<ol>
	<li>Weber, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=CH3NH3PbX3,+ein+Pb(II)-System+mit+kubischer+Perowskitstruktur+/+CH3NH3PbX3,+a+Pb(II)-System+with+Cubic+Perovskite+Structure.">CH3NH3PbX3, ein Pb(II)-System mit kubischer Perowskitstruktur / CH3NH3PbX3, a Pb(II)-System with Cubic Perovskite Structure.</a> Zeitschrift f&#252;r Naturforschung B. 33, 1443-1445 (1978).</li><li>Weber, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=(+x+=+0-3+),+ein+Sn+(+II+)+-System+mit+kubischer+Perowskitstruktur.">( x = 0-3 ), ein Sn ( II ) -System mit kubischer Perowskitstruktur.</a> Zeitschrift f&#252;r Naturforschung B. 33, 862-865 (1978).</li><li>Kojima, A., Teshima, K., Shirai, Y., Miyasaka, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Organometal+Halide+Perovskites+as+Visible-Light+Sensitizers+for+Photovoltaic+Cells.">Organometal Halide Perovskites as Visible-Light Sensitizers for Photovoltaic Cells.</a> Journal of the American Chemical Society. 131, 6050-6051 (2009).</li><li>. National Renewable Energy Laboratory NREL Best Research-Cell Efficiencies Available from: <a target="_blank" href="https://www.nrel.gov/pv/assets/images/efficiency-chart.png">https://www.nrel.gov/pv/assets/images/efficiency-chart.png</a> (2018)</li><li>Chen, Z., Wang, J. J., Ren, Y., Yu, C., Shum, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Schottky+solar+cells+based+on+CsSnI+3+thin-films.">Schottky solar cells based on CsSnI 3 thin-films.</a> Applied Physics Letters. 101 (9), 93901 (2012).</li><li>Sanehira, E. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Enhanced+mobility+CsPbI+3+quantum+dot+arrays+for+record-efficiency,+high-voltage+photovoltaic+cells.">Enhanced mobility CsPbI 3 quantum dot arrays for record-efficiency, high-voltage photovoltaic cells.</a> Science Advances. 3 (10), 4204 (2017).</li><li>Jia, Y., Kerner, R. A., Grede, A. J., Rand, B. P., Giebink, N. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Continuous-wave+lasing+in+an+organic-inorganic+lead+halide+perovskite+semiconductor.">Continuous-wave lasing in an organic-inorganic lead halide perovskite semiconductor.</a> Nature Photonics. 11 (12), 784-788 (2017).</li><li>Eaton, S. 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C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crystal+growth+of+the+perovskite+semiconductor+CsPbBr3:+A+new+material+for+high-energy+radiation+detection.">Crystal growth of the perovskite semiconductor CsPbBr3: A new material for high-energy radiation detection.</a> Crystal Growth and Design. 13 (7), 2722-2727 (2013).</li><li>Ilie, C. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inkjet+printable-photoactive+all+inorganic+perovskite+films+with+long+effective+photocarrier+lifetimes.">Inkjet printable-photoactive all inorganic perovskite films with long effective photocarrier lifetimes.</a> Journal of Physics Condensed Matter. 30 (18), (2018).</li><li>Shoaib, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Directional+Growth+of+Ultralong+CsPbBr3Perovskite+Nanowires+for+High-Performance+Photodetectors.">Directional Growth of Ultralong CsPbBr3Perovskite Nanowires for High-Performance Photodetectors.</a> Journal of the American Chemical Society. 139 (44), 15592-15595 (2017).</li><li>Swarnkar, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantum+dot-induced+phase+stabilization+of+a-CsPbI3+perovskite+for+high-efficiency+photovoltaics.">Quantum dot-induced phase stabilization of a-CsPbI3 perovskite for high-efficiency photovoltaics.</a> Science. 354 (6308), 92-96 (2016).</li><li>Kumar, M. H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lead-free+halide+perovskite+solar+cells+with+high+photocurrents+realized+through+vacancy+modulation.">Lead-free halide perovskite solar cells with high photocurrents realized through vacancy modulation.</a> Advanced Materials. 26 (41), 7122-7127 (2014).</li><li>Burschka, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sequential+deposition+as+a+route+to+high-performance+perovskite-sensitized+solar+cells.">Sequential deposition as a route to high-performance perovskite-sensitized solar cells.</a> Nature. 499 (7458), 316-319 (2013).</li><li>Dirin, D. N., Cherniukh, I., Yakunin, S., Shynkarenko, Y., Kovalenko, M. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solution-Grown+CsPbBr+3+Perovskite+Single+Crystals+for+Photon+Detection.">Solution-Grown CsPbBr 3 Perovskite Single Crystals for Photon Detection.</a> Chemistry of Materials. 28 (23), 8470-8474 (2016).</li><li>Zhou, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Vapor+Growth+and+Tunable+Lasing+of+Band+Gap+Engineered+Cesium+Lead+Halide+Perovskite+Micro/Nanorods+with+Triangular+Cross+Section.">Vapor Growth and Tunable Lasing of Band Gap Engineered Cesium Lead Halide Perovskite Micro/Nanorods with Triangular Cross Section.</a> ACS Nano. 11 (2), 1189-1195 (2017).</li><li>Teng, K. F., Vest, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+Ink+Jet+Technology+on+Photovoltaic+Metallization.">Application of Ink Jet Technology on Photovoltaic Metallization.</a> IEEE Electron Device Letters. 9 (11), 591-593 (1988).</li><li>Habas, S. E., Platt, H. a. S., van Hest, M. F. A. M., Ginley, D. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Low-Cost+Inorganic+Solar+Cells:+From+Ink+To+Printed+Device.">Low-Cost Inorganic Solar Cells: From Ink To Printed Device.</a> Chemical Reviews. 110 (11), 6571-6594 (2010).</li><li>Leenen, M. A. M., Arning, V., Thiem, H., Steiger, J., Anselmann, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Printable+electronics:+Flexibility+for+the+future.">Printable electronics: Flexibility for the future.</a> Physica Status Solidi (A) Applications and Materials Science. 206 (4), 588-597 (2009).</li><li>Koolyk, M., Amgar, D., Aharon, S., Etgar, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetics+of+cesium+lead+halide+perovskite+nanoparticle+growth;+focusing+and+de-focusing+of+size+distribution.">Kinetics of cesium lead halide perovskite nanoparticle growth; focusing and de-focusing of size distribution.</a> Nanoscale. 8 (12), 6403-6409 (2016).</li><li>Palazon, F., Di Stasio, F., Lauciello, S., Krahne, R., Prato, M., Manna, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evolution+of+CsPbBr+3+nanocrystals+upon+post-synthesis+annealing+under+an+inert+atmosphere.">Evolution of CsPbBr 3 nanocrystals upon post-synthesis annealing under an inert atmosphere.</a> Journal of Materials Chemistry C. 4 (39), 9179-9182 (2016).</li><li>Scherrer, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bestimmung+der+Gr&#246;&#223;e+und+der+inneren+Struktur+von+Kolloidteilchen+mittels+R&#246;ntgenstrahlen.+Nachrichten+von+der+Gesellschaft+der+Wissenschaften+zu+G&#246;ttingen.">Bestimmung der Gr&#246;&#223;e und der inneren Struktur von Kolloidteilchen mittels R&#246;ntgenstrahlen. Nachrichten von der Gesellschaft der Wissenschaften zu G&#246;ttingen.</a> Nachrichten von der Gesellschaft der Wissenschaften zu G&#246;ttingen, Mathematisch-Physikalische Klasse. 2, 98-100 (1918).</li><li>Shekhirev, M., Goza, J., Teeter, J., Lipatov, A., Sinitiskii, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+Cesium+Lead+Halide+Quantum+Dots.">Synthesis of Cesium Lead Halide Quantum Dots.</a> Journal of Chemical Education. 94 (8), 1150-1156 (2017).</li></ol>

The authors have no financial conflicts of interest and have nothing to disclose.

There are many parameters involved in the inkjet printing process that affect the final printed film. The discussion of all those parameters is beyond the scope of this protocol, but as this protocol focuses on a solution-based synthesis and deposition method, it is appropriate to give a short comparison to other well-known solution-based deposition methods: the spin-coating method and the doctor-blade method.
The spin-coating method is very fast, produces uniform films, and is low cost. The f...

Dieter Weber synthesized the first organic-inorganic hybrid&#160;halide&#160;perovskites in 19781,2. Roughly 30 years later in 2009, Akihiro Kojima and collaborators fabricated photovoltaic devices using the same organic-inorganic hybrid&#160;halide&#160;perovskites synthesized by Weber, namely, CH3NH3PbI3 and CH3NH3PbBr33. These experiments were the beginning of a subsequent tidal wave of research focusing on the photovoltaic properties of organic-inorganic hybrid halide perovskites. From 2009 to 2018, the device power conversion efficiency dramatically increased from 3.8%3 to over 23%4, making organic-inorganic hybrid&#160;halide perovskites comparable to Si-based solar cells. As with the organic-inorganic halide-based perovskites, the inorganic halide-based perovskites started gaining traction in the research community around 2012 when the first photovoltaic device efficiency was measured to be 0.9%5. Since 2012 the all inorganic halide-based perovskites have come a long way with some device efficiencies measured to be over 13% as in the 2017 study by Sanehira et al.6&#160;Both the organic-based and inorganic-based perovskites find applications related to lasers7,8,9,10, light emitting diodes11,12,13, high energy radiation detection14, photo detection15,16, and of course photovoltaic applications5,15,17,18. Over almost the past decade, many different synthesis techniques have emerged from scientists and engineers ranging from solution processed methods to vacuum vapor deposition techniques19,20,21. The halide&#160;perovskites synthesized using a solution-processed method are advantageous as they can easily be employed as inks for inkjet printing15.
In 1987, the first reported use of inkjet printing of solar cells was presented. Since then, scientists and engineers have sought ways to successfully print all inorganic solar cells with attractive performance properties and low implementation costs22. There are many advantages to inkjet printing solar cells, as compared to some of the common vacuum based fabrication methods. An important aspect of the inkjet printing method is that solution-based materials are used as inks. This opens the door for trials of many different materials, such as inorganic&#160;perovskite-based inks, which can be synthesized by facile wet chemical methods. In other words, inkjet printing of solar cell materials is a low-cost route to rapid prototyping. Inkjet printing also has the advantages of being able to print large areas on flexible substrates and print by design at low temperatures in atmospheric conditions. Furthermore, inkjet printing is highly suitable for mass production allowing for realistic low cost roll-to-roll implementation23,24.
In this article, we first discuss the steps involved with synthesizing inorganic&#160;perovskite quantum dot inks for inkjet printing. Then, we describe the additional steps for preparing inks for printing and the actual procedures for inkjet printing a photoactive film using a commercially available inkjet printer. Finally, we discuss the characterization of the printed films which is necessary to ensure the films are of proper chemical and crystal composition for high quality device performance.

<table>
	<tbody>
		<tr>
			<td>Oleic acid, 90%</td>
			<td>Sigma Aldrich</td>
			<td>364525</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>Oleylamine, 70%</td>
			<td>Sigma Aldrich</td>
			<td>O7805</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>1-octadecene, 90%</td>
			<td>Sigma Aldrich</td>
			<td>O806</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>Acetone, &#62;95%</td>
			<td>Fisher</td>
			<td>67641</td>
			<td>Certified ACS</td>
		</tr>
		<tr>
			<td>Cesium Carbonate, 99%</td>
			<td>Chem-Impex</td>
			<td>1955</td>
			<td>Assay</td>
		</tr>
		<tr>
			<td>Hexane, 98.5%</td>
			<td>Sigma Aldrich</td>
			<td>178918</td>
			<td>Mixture of isomers</td>
		</tr>
		<tr>
			<td>Cyclohexane, 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>110827</td>
			<td></td>
		</tr>
		<tr>
			<td>Lead(II) bromide, 98%</td>
			<td>Sigma Aldrich</td>
			<td>211141</td>
			<td></td>
		</tr>
		<tr>
			<td>Lead(II) iodide, 99%</td>
			<td>Sigma Aldrich</td>
			<td>211168</td>
			<td></td>
		</tr>
	</tbody>
</table>

inkjet printing all inorganic halide perovskite inks for photovoltaic applications

A method for synthesizing photoactive inorganic&#160;perovskite quantum dot inks and an inkjet printer deposition method, using the synthesized inks, are demonstrated. The ink synthesis is based on a simple wet chemical reaction and the inkjet printing protocol is a facile step by step method. The inkjet printed thin films have been characterized by X-ray diffraction, optical absorption spectroscopy, photoluminescent spectroscopy, and electronic transport measurements. X-ray diffraction of the printed quantum dot films indicates a crystal structure consistent with an orthorhombic room temperature phase with (001) orientation. In conjunction with other characterization methods, the X-ray diffraction&#160;measurements show high quality films can be obtained through the inkjet printing method.

Crystal Structure Characterization
Characterizing the crystal structure is vital regarding the synthesis of the inorganic&#160;perovskites. X-ray diffraction (XRD) was performed in air at room temperature on a diffractometer using a 1.54 &#197; wavelength Cu-K&#945; light source. Using the above protocols should lead to a room temperature orthorhombic crystal structure for the CsPbBr3 quantum dot inks as shown...

Watch this Scientific Journal Video about Inkjet Printing All Inorganic Halide Perovskite Inks for Photovoltaic Applications at JoVE.com

Inkjet Printing All Inorganic Halide Perovskite Inks for Photovoltaic Applications

A protocol for synthesizing inorganic-lead-halide hybrid perovskite quantum dot inks for inkjet printing and the protocol for preparing and printing the quantum dot inks in an inkjet printer with post characterization techniques are presented.

A method for synthesizing photoactive inorganic&#160;perovskite quantum dot inks and an inkjet printer deposition method, using the synthesized inks, are ...

The main advantages of this technique are that it is well suited for large area deposition, rapid prototyping and print by design, which suggests high potential for roll-to-roll manufacturing. Though this system can provide insight into inorganic photovoltaics it can also be applied to other systems such as organic photovoltaics or biophysics. Demonstrating the chemical synthesis procedure will be Mason McCormick, an undergraduate from the Sinitsky laboratory.An imprinting procedure will be demonstrated by Dylan Richmond from the Ilie laboratory. To prepare the cesium oleate precursor add 0.203 grams of cesium carbonate 10 milliliters of octadecene and 1.025 milliliters of oleic acid to a three neck round bottom flask containing 2.54 centimeter magnetic stir bar. Place a thermometer into one of the necks of the round bottom flask via a rubber septum.Next, place a rubber septum into one of the remaining necks of the round bottom flask and attach the third neck to the nitrogen gas line via a Schlenk line. Place the mixture under nitrogen atmosphere. Heat the mixture to 150 degrees celsius with constant stirring at a stirring speed of 399 millimeters per second until the cesium carbonate fully dissolves.Following this lower the temperature to 100 degrees celsius to avoid precipitation and decomposition of the cesium oleate and continue stirring at a stirring speed of 399 millimeters per second. To prepare the oleylamine lead bromide precursor add 1.35 millimoles of lead bromide 37.5 milliliters of octadecene 7.5 milliliters of olaylamine and 3.75 milliliters of oleic acid to a three neck round bottom flask containing a magnetic stir bar. Next place a thermometer into one of the necks of the round bottom flask and seal with polymer film.Place a rubber septum in one of the remaining necks of the round bottom flask and attach the third neck to the nitrogen gas line via a Schlenk line. Place mixture under nitrogen atmosphere. Heat the mixture to 100 degrees celsius with constant stirring at a stirring speed of 599 millimeters per second until the lead bromide is fully dissolved.Now, heat the mixture to 170 degrees celsius with constant stirring and observe the color change to dark yellow once the temperature reaches 170 degrees celsius. Continue stirring at 170 degrees celsius. Using a two milliliter glass syringe with a 10 centimeter long 18 gauge needle extract 1.375 milliliters of cesium oleate precursor from the three neck round bottom flask.Quickly inject this precursor into the three neck round bottom flask containing the oleylamine lead bromide precursor. After waiting five seconds remove the three neck round bottom flask from the heat and immerse it in an ice water bath. Separate the solution in the three neck round bottom flask equally into two test tubes.Add 25 milliliters of acetone to each of the supernatant solutions. Next, separate the quantum dots using a centrifuge at 2431.65G for five minutes at room temperature. Now dissolve the separated quantum dots in 10 to 25 milliliters of cyclohexane.To ensure that the inks print in the desired location draw a straight line at the edge of the disk and continue onto the CD disk tray. Place the desired substrate over the ink images printed on the disk and attach it to the disk using an adhesive such as double sided tape. Before filling the ink cartridges ensure the orange cover is installed correctly on the bottom of the ink cartridge to prevent ink from spilling out.Using a pipette inject the prepared quantum dot ink into the top of the ink cartridge. Once the cartridge is filled to the desired amount of ink plug the top with the rubber septum and carefully remove the orange cover. Next place the ink cartridge in the printer head and ensure that is snaps into place.Then insert the remaining cartridges before continuing to the next step. At this point the printer will accept the disk tray and print perovskites on the substrate. After printing is complete check that the inks actually printed onto the substrate as clogging is a common problem.Finally hold a UV lamp over the substrate to check if the printing was successful and a luminescing film is observed. Characterization of the synthesized inorganic perovskites is vital to confirm the crystal structure. The X Ray defraction results indicate that the crystalline cesium lead bromide quantum dot inks prepared using this protocol maintain an orthorhombic room temperature perovskite structure after the ink jet printing process.It is well known that the optical properties of these inorganic perovskite quantum dots are sensitive to quantum dot size and stoichiometry of the inorganic and halide atoms. The photoluminescence profile for cesium lead bromide shows a peak around 520 nanometers and the optical absorption profile shows an excitonic peak around 440 nanometers. Current voltage and capacitance voltage measurements were taken for the printed films under dark and light conditions as shown here.Under illumination the measured kind increased linearly and indicates that the films are photoactive. The films exhibit very low capacitance under dark conditions when no illumination is present. As can be seen here.Under light illumination the zero bias measured capacitance increases and is another indication that the films are photoactive. While attempting this procedure it's important to remember to keep both the printer head and gaskets as clean as possible. This will ultimately dictate successful printing.Following this procedure other methods like probe microscopy and time resolved luminescence can be performed in order to answer additional questions like what is the surface termination and surface morphology, and what are the exciton recombination dynamics. After it's development this technique paved the way for researchers in the fields of chemistry, physics and material science to explore roll-to-roll ready, photovoltaic systems composed of organic and inorganic semi conductor materials and the associated device interfaces. This technique proved to be a great educational tool as it was introduced in the upper level inorganic chemistry laboratory course at the University of Nebraska-Lincoln to introduce students to a variety of important concepts ranging from calyceal synthesis and quantum size affects to photovoltaics and renewable energy.Don't forget that working with lead based products and solvents like hexane, cyclohexane or acetone can be extremely hazardous and precautions such as using proper protective clothing and proper ventilation should always be taken when performing this procedure.

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Chemistry

10.9K Views.  State University of New York-Oswego. I principali vantaggi di questa tecnica sono che è adatta per la deposizione di grandi aree, la prototipazione rapida e la stampa per progettazione, il che suggerisce un alto potenziale per la produzione roll-to-roll. Sebbene questo sistema possa fornire informazioni sul fotovoltaico inorganico, può anche essere applicato ad altri sistemi come il fotovoltaico organico o la biofisica. A dimostrare la procedura di sintesi chimica sarà Mason McCormick, un laureato del laboratorio Sinitsky.