Name: synthesis and performance characterizations of transition metal single atom catalyst for electrochemical co2 reduction
Uploaded: 2018-04-10T14:45:00
Description: Watch this Scientific Journal Video about Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction Video at JoVE.com

This work was supported by the Rowland Fellows Program at the Rowland Institute of Harvard University. This work was performed in part at the Center for Nanoscale Systems (CNS), a member of the National Nanotechnology Infrastructure Network, which is supported by the National Science Foundation under award no. ECS-0335765. The CNS is part of Harvard University.

1. Preparation of Ni Single Atom Catalyst (NiN-GS)
<ol>
	<li>Preparation of electrospinning precursor solution
	<ol>
		<li>Take a 20 mL scintillation vial, dissolve 0.5 g of polyacrylonitrile (Mw=150,000), 0.5 g of polypyrrolidone (Mw=1,300,000), 0.5 g of Ni(NO3)2&#183;6H2O, and 0.1 g of dicyandiamide (DCDA) in 10 mL of dimethylformamide (DMF).</li>
		<li>Heat the DMF mixture to 80 &#176;C and keep the mixture at 80 &#176;C with constant stirring ...

<ol>
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In the above electrospinning process, two important steps should be noted in material synthesis procedures: 1) heating the DMF mixture (step 1.1.2), and 2) the pump rate adjusting (step 1.2.2) to match the spinning rate. The SEM image in Figure 1A shows the obtained carbon nanofibers interconnected with each other (~200 nm in diameter). They were broken into small pieces by ball milling for characterizations as shown in Figure 1B. Ni nanoparticles were uniformly...

Converting CO2 into chemicals or fuels using clean electricity is becoming increasingly important as a potential route to prevent further CO2 emissions1,2,3,4,5,6. However, this practical application is currently challenged by the low activity and selectivity of CO2 reduction reaction (CO2RR) due to the high kinetic barriers and the competition with hydrogen evolution reaction (HER) in aqueous media. Most of the traditional transition metal catalyst, such as Fe, Co, and Ni, exhibit low CO2RR selectivity due to their superb HER activities7,8. Effectively tuning their material properties to change the reaction pathways on these transition metal catalysts becomes critical to improve their CO2RR selectivity. Among different methods to modify the electronic properties of catalysts, dispersing metal atoms into a single-atom morphology attracts intensive attentions recently due to their dramatically changed catalytic behaviors compared to their bulk counterpart9,10,11. However, due to the high mobility of unbounded atoms, it is quite challenging to obtain single metal atoms without the presence of supportive materials. Therefore, a host matrix material with defects created to confine and coordinate with transition metal atoms is necessary. This could open up new opportunities to: 1) tune the electronic properties of transition metals as CO2RR active sites, and 2) at the same time maintain relatively simple atomic coordination for fundamental mechanism studies. In addition, those transition metal atoms trapped in a confined environment cannot be easily moved around during catalysis, which prevents the nucleation or reconstructions of surface atoms observed in many cases12,13,14.
Two-dimensional layered graphene is of particular interest as host for metal single atoms due to their high electron conductivity, chemical stability, and inertness to both CO2 reduction and HER catalytic reactions. More importantly, Fe, Co, and Ni metals were known to be able to catalyze the carbon graphitization process on their surface15. In short, those transition metals would alloy with carbon during the high temperature thermal annealing process. When the temperature drops, carbon starts to precipitate out of the alloying phase and is catalyzed to form graphene layers on the surface of transition metal. During this process, with graphene defects generated, metal single atoms would be trapped in those graphene defects as the active sites for CO2RR16,17,18,19. Here, we report this detailed protocol intending to help new practitioners in the field of single atom catalysis, as well as to provide an explicit demonstration of on-line CO2 reduction product analysis. More information can be found in our recently published article19 and a series of related works20,21,22,23.

<table border="0" cellpadding="0" cellspacing="0" width="829">
	<tbody>
		<tr height="23">
			<td height="23" style="height:23px;width:216px;">syringe pump&#160;</td>
			<td style="width:164px;">KD Scientific</td>
			<td style="width:151px;">KDS-100</td>
			<td style="width:299px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:216px;">tube furnance</td>
			<td style="width:164px;">Lindberg/Blue M</td>
			<td style="width:151px;">TF55035A-1</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ball miller</td>
			<td style="width:164px;">SPEX SamplePrep</td>
			<td style="width:151px;">5100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">electrochemical work station</td>
			<td style="width:164px;">BioLogic</td>
			<td style="width:151px;">VMP3</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pH meter</td>
			<td style="width:164px;">Orion</td>
			<td style="width:151px;">320 PerpHecT&#160;</td>
			<td>2 points calibration before use</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">gas chromatograph</td>
			<td style="width:164px;">Shimadzu</td>
			<td style="width:151px;">GC-2014</td>
			<td>a combined seperation system consisting of molecular sieve 5A, Hayesep Q, Hayesep T, and Hayesep N</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">mass flow controller</td>
			<td>Alicat Scientific&#160;</td>
			<td style="width:151px;">MC-50SCCM-D/5M</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">ultrapure water system</td>
			<td>Millipore</td>
			<td>Synergy</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">vacuum desiccator&#160;</td>
			<td>PolyLab</td>
			<td>55205</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">polyacrylonitrile</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">181315</td>
			<td>Mw=150,000</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">polypyrrolidone</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">437190</td>
			<td>Mw=1,300,000</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Ni(NO3)26H2O</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">244074</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">dicyandiamide</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">D76609</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">dimethylformamide</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">227056</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">carbon fiber paper&#160;</td>
			<td style="width:164px;">AvCarb</td>
			<td style="width:151px;">MGL370</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Nafion 117 membrane</td>
			<td style="width:164px;">Fuel Cell Store</td>
			<td style="width:151px;">117</td>
			<td>used as proton exchange membrane in H-cell</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">KHCO3</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">431583</td>
			<td>further purified by electrolysis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">platinum foil&#160;</td>
			<td style="width:164px;">Beantown Chemical</td>
			<td style="width:151px;">126580</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">saturated calomel electrode</td>
			<td style="width:164px;">CH Instruments</td>
			<td style="width:151px;">CHI150</td>
			<td></td>
		</tr>
		<tr height="27">
			<td height="27" style="height:27px;width:216px;">glassy carbon electrode</td>
			<td style="width:164px;">HTW GmbH</td>
			<td style="width:151px;">SIGRADUR</td>
			<td>1 cm &#215; 2 cm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">wax</td>
			<td>Apiezon</td>
			<td style="width:151px;">W-W100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nafion 117 solution</td>
			<td>Sigma-Aldrich</td>
			<td>70160</td>
			<td>used as ionomer in catalyst ink preparation&#160;</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">forming gas</td>
			<td>Airgas</td>
			<td>UHP</td>
			<td>5% H2 balanced with Ar</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">carbon dioxide</td>
			<td>Airgas</td>
			<td>LaserPlus</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">sandard gas</td>
			<td>Airgas</td>
			<td>customized</td>
			<td>500 ppm CO, 500 ppm CH4, 1000 ppm H2 balanced with Ar</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">sandard gas</td>
			<td>Air Liquide</td>
			<td>customized</td>
			<td>100 ppm H2, 100 ppm CO and other alkanes balanced with Ar</td>
		</tr>
	</tbody>
</table>

synthesis and performance characterizations of transition metal single atom catalyst for electrochemical co2 reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) and energy-dispersive X-ray spectroscopy (EDX) mapping images are shown in Figure 1 for the morphology characterization of NiN-GS. Three-dimensional atom probe tomography (3D-APT) results are shown in Figure 2 for the direct identification of single Ni sites distribution as well as their neighboring chemical environment. On-line electrochemical G...

Watch this Scientific Journal Video about Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction Video at JoVE.com

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction Video (Video) | JoVE

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

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