Name: synthesis of platinum-nickel nanowires and optimization for oxygen reduction performance
Uploaded: 2018-04-27T12:30:00
Description: Watch this Scientific Journal Video about Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance at JoVE.com

Financial support was provided by the U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy under contract number DE-AC36-08GO28308 to NREL.

1. Synthesis of Pt-Ni Nanowires
<ol>
	<li>To begin the displacement process, suspend the nickel nanowire template in water and heat it to 90 &#176;C.
	<ol>
		<li>Add 40 mg of commercially available, nickel nanowires to 20 mL of deionized water in a 50 mL centrifuge tube. Sonicate it for 5 min. 
		&#8203;NOTE: The nanowires are approximately 150-250 nm in diameter and 100-200 &#181;m in length.</li>
		<li>Transfer the suspended nanowires to a 250 mL glass round bottom flask and add 60 mL of deionized water. Heat th...

<ol>
	<li>Bregoli, L. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+Platinum+Crystallite+Size+on+Electrochemical+Reduction+of+Oxygen+in+Phosphoric-Acid.">Influence of Platinum Crystallite Size on Electrochemical Reduction of Oxygen in Phosphoric-Acid.</a> Electrochim. Acta. 23 (6), 489-492 (1978).</li><li>Debe, M. K., Parsonage, E. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+electrode+membranes.">Nanostructured electrode membranes.</a> US patent. , (1994).</li><li>Papandrew, A. B., 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=Oxygen+Reduction+Activity+of+Vapor-Grown+Platinum+Nanotubes.">Oxygen Reduction Activity of Vapor-Grown Platinum Nanotubes.</a> ECS Trans. 50 (2), 1397-1403 (2013).</li><li>Alia, S. M., Yan, Y. S., Pivovar, B. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Galvanic+displacement+as+a+route+to+highly+active+and+durable+extended+surface+electrocatalysts.">Galvanic displacement as a route to highly active and durable extended surface electrocatalysts.</a> Cat. Sci. Tech. 4 (10), 3589-3600 (2014).</li><li>Alia, S. 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=Platinum-Coated+Nickel+Nanowires+as+Oxygen-Reducing+Electrocatalysts.">Platinum-Coated Nickel Nanowires as Oxygen-Reducing Electrocatalysts.</a> ACS Cat. 4 (4), 1114-1119 (2014).</li><li>Alia, S. 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=Exceptional+Oxygen+Reduction+Reaction+Activity+and+Durability+of+Platinum-Nickel+Nanowires+through+Synthesis+and+Post-Treatment+Optimization.">Exceptional Oxygen Reduction Reaction Activity and Durability of Platinum-Nickel Nanowires through Synthesis and Post-Treatment Optimization.</a> ACS Omega. 2 (4), 1408-1418 (2017).</li><li>Norskov, 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=Origin+of+the+Overpotential+for+Oxygen+Reduction+at+a+Fuel-Cell+Cathode.">Origin of the Overpotential for Oxygen Reduction at a Fuel-Cell Cathode.</a> J. Phys. Chem. B. 108 (46), 17886-17892 (2004).</li><li>Sha, Y., Yu, T. H., Merinov, B. V., Shirvanian, P., Goddard, W. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanism+for+Oxygen+Reduction+Reaction+on+Pt3Ni+Alloy+Fuel+Cell+Cathode.">Mechanism for Oxygen Reduction Reaction on Pt3Ni Alloy Fuel Cell Cathode.</a> J. Phys. Chem. C. 116 (40), 21334-21342 (2012).</li><li>Paulus, U. 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=Oxygen+reduction+on+high+surface+area+Pt-based+alloy+catalysts+in+comparison+to+well+defined+smooth+bulk+alloy+electrodes.">Oxygen reduction on high surface area Pt-based alloy catalysts in comparison to well defined smooth bulk alloy electrodes.</a> Electrochim. Acta. 47 (22-23), 3787-3798 (2002).</li><li>Stamenkovic, V., 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=Changing+the+activity+of+electrocatalysts+for+oxygen+reduction+by+tuning+the+surface+electronic+structure.">Changing the activity of electrocatalysts for oxygen reduction by tuning the surface electronic structure.</a> Angew. Chem. 118 (18), 2963-2967 (2006).</li><li>Cui, C., Gan, L., Heggen, M., Rudi, S., Strasser, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Compositional+segregation+in+shaped+Pt+alloy+nanoparticles+and+their+structural+behaviour+during+electrocatalysis.">Compositional segregation in shaped Pt alloy nanoparticles and their structural behaviour during electrocatalysis.</a> Nat Mater. 12 (8), 765-771 (2013).</li><li>Chen, 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=Highly+Crystalline+Multimetallic+Nanoframes+with+Three-Dimensional+Electrocatalytic+Surfaces.">Highly Crystalline Multimetallic Nanoframes with Three-Dimensional Electrocatalytic Surfaces.</a> Science. 343 (6177), 1339-1343 (2014).</li><li>Alia, S., 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=Porous+Platinum+Nanotubes+for+Oxygen+Reduction+and+Methanol+Oxidation+Reactions.">Porous Platinum Nanotubes for Oxygen Reduction and Methanol Oxidation Reactions.</a> Adv. Funct. Mater. 20 (21), 3742-3746 (2010).</li><li>Alia, S. 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=Platinum+Coated+Copper+Nanowires+and+Platinum+Nanotubes+as+Oxygen+Reduction+Electrocatalysts.">Platinum Coated Copper Nanowires and Platinum Nanotubes as Oxygen Reduction Electrocatalysts.</a> ACS Cat. 3 (3), 358-362 (2013).</li><li>Alia, S. 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=Platinum-Coated+Cobalt+Nanowires+as+Oxygen+Reduction+Reaction+Electrocatalysts.">Platinum-Coated Cobalt Nanowires as Oxygen Reduction Reaction Electrocatalysts.</a> ACS Cat. 4 (8), 2680-2686 (2014).</li><li>Alia, S. M., Duong, K., Liu, T., Jensen, K., Yan, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Palladium+and+Gold+Nanotubes+as+Oxygen+Reduction+Reaction+and+Alcohol+Oxidation+Reaction+Catalysts+in+Base.">Palladium and Gold Nanotubes as Oxygen Reduction Reaction and Alcohol Oxidation Reaction Catalysts in Base.</a> ChemSusChem. , (2014).</li><li>Alia, S. M., Pylypenko, S., Neyerlin, K. C., Kocha, S. S., Pivovar, B. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Platinum+Nickel+Nanowires+as+Methanol+Oxidation+Electrocatalysts.">Platinum Nickel Nanowires as Methanol Oxidation Electrocatalysts.</a> J. Electrochem. Soc. 162 (12), 1299-1304 (2015).</li><li>Alia, S. 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These protocols have been used to produce extended surface electrocatalysts with both high surface areas and specific activities in the oxygen reduction reaction8. By depositing Pt onto nanostructured templates, the nanowires avoided low coordinated sites and minimize particle size effects, producing specific activities more than 12 times greater than carbon-supported Pt nanoparticles. Using galvanic displacement as the synthesis approach also produced an approximate coating on the Ni template<sup...

Proton exchange membrane fuel cells are partially limited by the amount and cost of platinum required in the catalyst layer, which can account for half of fuel cell costs1. In fuel cells, nanomaterials are typically developed as oxygen reduction catalysts, since the reaction is kinetically slower than hydrogen oxidation. Carbon-supported Pt nanoparticles are often used as oxygen reduction electrocatalysts due to their high surface area; however, they have specific selective activity and are prone to durability losses.
Extended thin films offer potential benefits to nanoparticles by addressing these limitations. Extended Pt surfaces typically produce specific activities an order of magnitude greater than nanoparticles, by limiting less active facets and particle size effects, and have been shown to be durable under potential cycling2,3,4. While high mass activities have been achieved in extended surface electrocatalysts, improvements have been made primarily through increases in specific activity, and the catalyst type has been limited to Pt with a low surface area (10 m2 gPt-1)3,4,5.
Spontaneous galvanic displacement combines the aspects of corrosion and electrodeposition6. The process is generally governed by the standard redox potentials of the two metals, and the deposition typically occurs when the metal cation is more reactive than the template. The displacement tends to produce nanostructures that match the template morphology. By applying this technique to extended nanostructures, Pt-based catalysts can be formed that take advantage of the high specific oxygen reduction activity of extended thin films. Through partial displacement, small amounts of Pt have been deposited, and have produced materials with high surface areas (&#62; 90 m2 gPt-1)7,8.
These protocols involve hydrogen annealing to mix Pt and Ni zones and improve oxygen reduction activity. A number of studies have theoretically established the mechanism and experimentally confirmed an alloying effect in Pt oxygen reduction. Modeling and correlating Pt-OH and Pt-O binding to oxygen reduction activity suggest that Pt improvements can be made through lattice compression9,10. Alloying Pt with smaller transition metals has confirmed this benefit, and Pt-Ni has been investigated in a number of forms, including polycrystalline, faceted electrodes, nanoparticles, and nanostructures11,12,13,14.
Galvanic displacement has been used in Pt-oxygen reduction catalyst development with a variety of other templates, including silver, copper, and cobalt nanostructures15,16,17. The synthesis technique has also been used in the deposition of other metals and has produced electrocatalysts for fuel cells, electrolyzers, and the electrochemical oxidation of alcohols18,19,20,21. Similar protocols can also be adapted for the synthesis of nanomaterials with a wider range of electrochemical applications.

<table border="0" cellpadding="0" cellspacing="0" style="width:681px;" width="680">
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	<tbody>
		<tr height="40">
			<td height="40" style="height:40px;width:215px;">Nickel nanowires</td>
			<td style="width:300px;">Plasmachem GmbH</td>
			<td style="width:167px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">250 mL round bottom flask</td>
			<td>Ace Glass</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Hot plate</td>
			<td>VWR International</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Mineral oil</td>
			<td>VWR International</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Potassium tetrachloroplatinate</td>
			<td>Sigma Aldrich</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Syringe pump</td>
			<td>New Era Pump Systems</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Rotator</td>
			<td>Arrow Engineering</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Teflon paddle</td>
			<td>Ace Glass</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Glass shaft</td>
			<td>Ace Glass</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Split hinge tubular furnace</td>
			<td>Lindberg</td>
			<td></td>
			<td>Customized in-house</td>
		</tr>
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			<td height="40" style="height:40px;">Schlenk line</td>
			<td>Ace Glass</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Condensers</td>
			<td>VWR International</td>
			<td></td>
			<td></td>
		</tr>
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			<td height="40" style="height:40px;">Nitric acid</td>
			<td>Fisher Scientific</td>
			<td></td>
			<td></td>
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			<td height="40" style="height:40px;">2-propanol</td>
			<td>Fisher Scientific</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Nafion ionomer (5 wt. %)</td>
			<td>Sigma Aldrich</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Glassy carbon working electrode</td>
			<td>Pine Instrument Company</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">RDE glassware</td>
			<td>Precision Glassblowing</td>
			<td></td>
			<td>Customized in-house</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Platinum wire</td>
			<td>Alfa Aesar</td>
			<td></td>
			<td>Customized in-house</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Platinum mesh</td>
			<td>Alfa Aesar</td>
			<td></td>
			<td>Customized in-house</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">MSR Rotator</td>
			<td>Pine Instrument Company</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">Potentiostat</td>
			<td>Metrohm Autolab</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis of platinum-nickel nanowires and optimization for oxygen reduction performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

Spontaneous galvanic displacement of Ni nanowires with Pt, using the specified amount, produced Pt-Ni nanowires that were 7.3 wt. % Pt (Figure 1 and Figure 2A). Some modification to the amount of Pt precursor may be required to reach the optimum Pt loading. Pt displacement is sensitive to the thickness of the surface Ni oxide layer, which can vary based on template age (air exposure) and upstream variability<sup ...

Watch this Scientific Journal Video about Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance at JoVE.com

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

The overall goal of this procedure is to produce platinum based, extended surface electro-catalysts, that demonstrate a high level of performance and durability in the oxygen reduction reaction. This method could help address key issues in hydrogen fuel cells by reducing the amount of platinum required, and cutting the cost of the catalyst layer. The main advantage of this technique is that produces materials with high electrochemical surface areas, attritional limitation of surface catalysts.Begin the nanowire synthesis steps with the displacement process. In a 50 milliliter centrifuge tube, add 20 milliliters deionized water, and 40 milliliters nickel nanowires. Place the mixture in a sonicator and sonicate for five minutes.Meanwhile, prepare a mineral oil bath and an electric stirrer. Retrieve the suspended nanowires from the sonicator, and transfer them to a glass, 250 milliliter round-bottom flask. Add to the flask, 60 milliliters of deionized water.Then place it in the mineral bath to be heated to 90 degrees Celsius, and simultaneously stirred at 500 RPM. Equip the stirrer with a PTFE paddle on a glass shaft. Now form the platinum nickel nanowires.Have ready an automated syringe pump, and prepare a syringe. Use a 20 milliliter syringe with about 8 centimeters of tubing on its tip. Next, obtain 15 milliliters of deionized water, and add 8.1 milligrams of potassium tetrachloroplatinate.Transfer the solution to the syringe. Then place the syringe on the syringe pump. Arrange for the pump to add the solution to the flask containing nanowires.Set the rate to one milliliter per minute, and start the pump. Once the transfer is complete, continue stirring and heating the flask at 90 degrees Celsius for two hours. After two hours, put the solution in to a centrifuge tube, and centrifuge at 2500 G, for 15 minutes.Centrifugation gives rise to supernatant in the tube. Pour this off in to a waste container. With the supernatant gone, add fresh deionized water to the solids.Sonicate the mixture for about 10 seconds. Repeat the centrifuge, supernatant removal, and re-suspension steps, 3 times with the water, and a fourth with 2-Proponal. In the end, put the nanowires in a 20 milliliter, glass scintillation vial.Take the nanowires to a vacuum oven to dry at 40 degrees Celsius, overnight. First prepare, in a 20 milliliter scintillation vial, what is called the Ink. This is deionized water, a catalyst with 73 micrograms of platinum, and 2-propanol.Ice the vial for five minutes. After five minutes, add 10 microliters of ionomer to the ink. Return the vial to the container of ice, and move both to the sonicator.Sonicate the vial for 30 seconds by horn. Follow this with bath sonication for 20 minutes. End with another 30 seconds of horned sonication.During sonication, prepare a container of graphitized carbon nanofibers. Get the sonicated ink and use a pipette to draw out 7.5 milliliters. Add the drawn out ink to the nanofibers.Now, sonicate the ink in ice with a horn for 30 seconds. Then by bath for 20 minutes. And by horn again, for 30 seconds.Have ready, an inverted rotator with a working electrode mounted on it. Here, a glassy carbon electrode is ready for coating. Start the electrode spinning at 100 RPM, and pipette 10 microliters of the sonicated ink on to it.When done, increase the rotation to 700 RPM. As the electrode drys, repeat the three sonication steps with the ink. With the mixture speed at 100 RPM, pipette and additional 10 micrograms of ink on to the working electrode, before increasing the rotation speed to 700 RPM.Fill the half cell with one-tenth molar perchloric acid. Now assemble the rotating disk electrode test station. The test station has a working reference, and counter electrode connected to the main testing cell.Next, connect the working electrode to a modulated speed controller. Then, submerge the working electrode tip in the acid. Set up a potentiostat to take electrochemical measurements.Prior to electrochemical conditioning, purge the electrolyte with nitrogen for seven minutes. Now, prepare to measure oxygen reduction polarization curves. Start the working electrode, rotating at 2500 RPM.Purge the electrolyte with oxygen. After seven minutes, set the oxygen purge to blanket the electrolyte. Slow the electrode rotation to 1600 RPM.Set the parameters for an automated linear sweep photometry measurement and run the experiment. When the measurement is completed, stop the rotation and discard the electrolyte. After refilling the cell with perchloric acid, and immersing the electrode, purge it with oxygen for seven minutes.Perform the linear sweep photometry measurement again, using the same parameters. These data show the platinum nickel nanowire composition as a function of the amount of the platinum precursor. Potassium tetrachloroplatinate, added to 40 milligrams of nickel nanowires during galvanic displacement.An increase of platinum precursor during galvanic displacement, increases the platinum content and the resulting catalyst. This plot is the electrochemical surface area versus the platinum displacement. Increasing platinum content, generally results in catalyst with lower platinum based electrochemical surface areas.Optimal performance occurred at a composition of 7.3%platinum. Here's the mass activity for the oxygen reduction reaction as a function of a kneeling temperature. A temperature of 250 degrees Celsius, produced catalyst with optimal mass activity.Once mastered, this technique can be completed at approximately one week, if performed properly. While attempting this procedure, it is important to remember that contaminants on a part-per-trillion level are electrochemically relevant. Following this procedure, other methods, including microscopy and membrane electrode assembly testing can be completed to answer additional questions, including kettle structure and device performance.From these protocols, we have developed extended service catalysts for proton and nano exchanged membrane fuel cells, electrolyzers and alcohol based fuel cells. After watching this video, you should have a good idea how to synthesize and electrochemically test platinum based extended surface electro-catalyst that demonstrate a high level of performance and durability in the ontra production reaction. Don't forget that working with concentrated acid and pressurized gas, particularly, hydrogen and carbon monoxide can be extremely hazardous and precautions such as, using personal protective equipment and ventilation control should always be taken while performing this procedure.

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