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 at JoVE.com

Dette arbeidet ble støttet av Rowland Fellows programmet ved Rowland Institute av Harvard University. Dette arbeidet ble utført delvis ved Center for nanoskala systemer (CNS), medlem av det nasjonale nanoteknologi infrastrukturnettverk, som støttes av National Science Foundation under prisen ikke. ECS-0335765. CNS er del av Harvard University.

1. forberedelse av Ni enkelt Atom katalysator (NiN-GS)
<ol><li>Utarbeidelse av electrospinning forløper løsning<ol>
<li>Ta 20 mL scintillation ampuller, oppløse 0,5 g polyakrylonitril (Mw= 150.000), 0,5 g polypyrrolidone (Mw= 1,300,000), 0,5 g av Ni (ingen3)2·6H2O og 0,1 g dicyandiamide (DCDA) i 10 mL av vannistedenfor (DMF).</li>
		<li>Varm DMF blandingen til 80 ° C og holde blandingen på 80 ° C med konstant under omrøring til alle polyme...

<ol>
	<li>Lewis, N. S., Nocera, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Powering+the+planet:+Chemical+challenges+in+solar+energy+utilization.">Powering the planet: Chemical challenges in solar energy utilization.</a> P. Natl. Acad. Sci. USA. 103, 15729-15735 (2006).</li><li>Appel, A. 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=Frontiers,+Opportunities,+and+Challenges+in+Biochemical+and+Chemical+Catalysis+of+CO2+Fixation.">Frontiers, Opportunities, and Challenges in Biochemical and Chemical Catalysis of CO2 Fixation.</a> Chem. Rev. 113, 6621-6658 (2013).</li><li>Jhong, H. R., Ma, S. C., Kenis, P. J. 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I de ovennevnte electrospinning prosessen, to viktige skritt bør bemerkes materiale syntese prosedyrer: 1) oppvarming DMF blandingen (trinn 1.1.2), og 2) på pumpen rate justering (trinn 1.2.2) å matche spinning hastigheten. SEM bildet i figur 1A viser innhentet karbon nanofibers forbundet med hverandre (~ 200 nm i diameter). De ble brutt i små biter av ball fresing for karakteristikkene som vist i figur 1B. Ni nanopartikler ble fordelt i karbon nanofibers. K...

Konvertere CO2 i kjemikalier eller drivstoff bruker ren elektrisitet blir stadig viktigere som en potensiell måte å hindre ytterligere CO2 -utslipp1,2,3,4, 5,6. Men er denne praktiske anvendelsen for tiden utfordres av lav aktivitet og selektivitet av CO2 reduksjon reaksjon (CO2RR) høy kinetic barrierer og konkurransen med hydrogen utvikling reaksjon (HER) i vandig Media. De fleste av tradisjonelle transisjonsmetall katalysator, som Fe, Co, og Ni, utstilling lav CO2RR selektivitet på grunn av sine ypperlige henne aktiviteter7,8. Effektivt tuning materielle egenskapene for å endre reaksjon veier på disse transisjonsmetall katalysatorer blir kritisk å forbedre sine CO2RR selektivitet. Blant forskjellige metoder for å endre elektroniske egenskaper av katalysatorer, tiltrekker spre metall atomer i en enkelt-atom morfologi intensiv oppmerksomhet nylig på grunn av dramatisk endret katalytisk virkemåtene sammenlignet med deres bulk motpart 9 , 10 , 11. imidlertid på grunn av høy mobilitet av ubegrenset atomer, er det ganske utfordrende å få enkelt metall atomer uten tilstedeværelse av støttende materialer. Derfor, en vert matrix materiale med defekter opprettet for å begrense og koordinere med overgang metall atomer er nødvendig. Dette kan åpne opp nye muligheter til å: 1) stille elektroniske egenskapene av overgangen metaller som CO2RR aktive nettsteder og 2) samtidig opprettholde relativt enkel atomic koordinering for fundamental mekanisme studier. Lett i tillegg de transisjonsmetall atomene fanget i et begrenset miljø kan ikke flyttes rundt under katalyse, som hindrer nucleation eller rekonstruksjoner av overflaten atomer observert i mange tilfeller12,13 ,14.
Todimensjonal lagdelte Grafén er av spesiell interesse som vert for metall enkelt atomer på grunn av deres høye elektron ledningsevne, kjemiske stabilitet og inertness til både CO2 reduksjon og hennes katalytisk reaksjoner. Enda viktigere, var Fe, Co, og Ni metaller kjent kunne katalysere karbon graphitization prosessen på deres overflate15. Kort sagt, ville de overgang metallene legering med karbon under høy temperatur termisk annealing prosessen. Når temperaturen synker, karbon begynner å føre ut av den sveiseavsettet fasen og er katalysert skjemaet Grafén lag på overflaten av transisjonsmetall. Under denne prosessen ville med Grafén defekter generert, metall enkelt atomer være fanget i de Grafén feilene som de aktive områdene for CO2RR16,17,18,19. Her rapporterer vi denne detaljerte protokollen å hjelpe nye utøvere innen enkelt atom katalyse, så vel som å gi en eksplisitt demonstrasjon av on-line CO2 reduksjon produkt analyse. Mer informasjon finnes i våre nylig publisert artikkel19 og en rekke relaterte verk20,21,22,23.

<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

Denne protokollen gir både metoden syntese av Ni enkelt atom katalysator, og elektrokjemiske testing katalytisk aktivitet og selektivitet i vandig CO2 reduksjon. Forskjellig fra tradisjonell metall nanokrystaller, syntese av metall enkelt atomer innebærer en matrise materiale som kan begrense de enkelt atomene og hindre samling. Vi rapporterer en electrospinning og termisk annealing metoden for å forberede Ni enkelt atomer spredt og koordinert i en Grafén skall, som aktive sentre for CO2 reduksjon å CO. Under syntese spille N dopants en avgjørende rolle i genererer Grafén stillinger å fange Ni atomer. Avvik-korrigert skanning elektronmikroskop for overføring og tredimensjonale atom sonde tomografi ble brukt til å identifisere de enkelt Ni atomic webområdene i Grafén stillinger. Detaljert oppsett av elektrokjemiske CO2 reduksjon apparater kombinert med en on-line gass kromatografi er også demonstrert. Sammenlignet med metallisk Ni, Ni enkelt atom katalysator exhibit dramatisk forbedret CO2 reduksjon og undertrykt H2 utviklingen siden reaksjon.

Skanning elektronmikroskop (SEM), skanning overføring elektronmikroskop (STEM) og energi-dispersiv X-ray spektroskopi (EDX) vises kartlegging bilder i figur 1 for morfologi karakterisering av NiN-GS. Tredimensjonale atom sonde tomografi (3D-APT) resultater er vist i figur 2 for direkte identifikasjonen av enkelt Ni områder distribusjon samt nærliggende kjemiske miljøet. On-line elektrokjemiske GC målinger oppsett og resultat...

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

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

Syntese og ytelse karakteristikkene av transisjonsmetall enkelt Atom katalysator elektrokjemiske CO2 reduksjon

Her presenterer vi en protokoll for syntese og elektrokjemiske testing av transisjonsmetall enkelt atomer koordinert i Grafén stillinger som aktive sentre for selektiv karbondioksid reduksjon karbonmonoksid i vandige løsninger.

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

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Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; ...

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Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

Omvendt Mikroemulsjon-mediert Syntese av mono og bimetall Tidlig Transition Metal Carbide og Nitride Nanopartikler

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

En metode for å manipulere overflatespenningen i en Liquid Metal via Surface Oksidasjon og reduksjon

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

HKUST-en som en heterogen katalysator for syntese av Vanillin

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Facile Synthesis of Worm-lignende Miceller av synlig lys mediert dispersjonspolymeriseringen Bruke Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Synthesis of a Water-soluble Metal&#8211;Organic Complex Array

Synthesis of a Water-soluble MetalÃƒÆ’Ã‚Â¢ÃƒÂ¢Ã¢â‚¬Å¡Ã‚Â¬ÃƒÂ¢Ã¢â€šÂ¬Ã…â€œOrganic Complex Array

Syntese av en vann-løselig metall-organisk kompleks rekke

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as ...

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

Syntese av Platinum-nikkel Nanowires og optimalisering for oksygen ytelse

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

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

En rask syntese metode for Au og Pd Pt Aerogels Via direkte Solution-baserte reduksjon

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

Electrophoretic krystallisering av Ultrathin høyytelses Metal-organisk Framework membraner

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...