Name: a rapid synthesis method for au, pd, and pt aerogels via direct solution-based reduction
Uploaded: 2018-06-18T15:00:00
Description: Watch this Scientific Journal Video about A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction at JoVE.com

Forfatterne er Stephen Steiner på Aerogel teknologier for hans inspiration og tekniske indsigt, og Dr. Deryn Chu på Army Research Laboratory-sensorer og elektron enheder direktorat, Dr. Christopher Haines på våbenforskning, taknemmelig Udvikling og Engineering Center, US Army RDECOM-ARDEC og Dr. Stephen Bartolucci på amerikanske hær Benet laboratorier for deres bistand. Dette arbejde blev støttet af et fakultet udvikling forskningsfond tilskud fra de Forenede Stater Military Academy, West Point.

Forsigtig: Høre alle relevante sikkerhedsdatablade (SDS) før brug. Brug passende sikkerhedspraksis når du udfører kemiske reaktioner, til at omfatte brugen af et stinkskab og personlige værnemidler. Hurtig hydrogen gas udvikling kan forårsage højt tryk i reaktion rør forårsager caps til pop og løsninger til at sprøjte ud. Sikre at reaktion tube caps forblive åben som angivet i protokollen.
1. metal Gel forberedelse
<ol><li>
Forberedelse af metal ion løsninger.
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<ol>
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Ædelmetal aerogel syntese metode præsenteres her resultaterne i dannelsen af porøse, høj areal Monoliter, der er sammenlignelige med langsommere syntese teknikker. 1:1 (v/v) metal ion opklaring at reduktionsmiddel løsning ratio er kritisk i lette foreslåede gel dannelse model. Den hurtige hydrogen gas udvikling som et biprodukt af elektrokemisk reduktion af metal ioner fungerer som en sekundær reduktionsmiddel og letter fortætning og fusion af voksende nanopartikler under gel dannelse. Udvalg af de optimale kombi...

En bred vifte af energilagring og konvertering, katalyse og sensor programmer drage fordel af tre-dimensionelle metallisk nanostrukturer, der giver kontrol over kemisk reaktivitet og massetransporten egenskaber1,2, 3,4,5. Sådan 3-dimensionelle metallisk nanostrukturer yderligere forbedre ledningsevne, sejhed, formbarhed og styrke8,9. Integration i enheder nødvendiggør at materialer være fritstående eller kombineret med støttematerialer. Indarbejdelse af nanomaterialer på støttestrukturer giver et middel til minimere aktive materiale, men muligvis lider af svag adsorption og eventuel bymæssigt område under enhed operation10,11.
Mens der er en række forskellige syntese metoder til at styre individuel nanopartikel størrelse og form, aktiverer par tilgange kontrol over sammenhængende 3-dimensionelle nanomaterialer12,13,14. Ædelmetal 3-dimensionelle nanostrukturer er blevet dannet gennem dithiol sammenkobling af monodisperse nanopartikler, sol-gel dannelse, nanopartikel sammensmeltning, kompositmaterialer, nanosphere kæder og biotemplating15,16 , 17 , 18. mange af disse metoder kræver syntese gange om dage til uger at give ønskede materialer. Ædelmetal nanofoams syntetiseret fra den direkte reduktion af forløber saltopløsninger har udarbejdet med en hurtigere syntese tidsskalaen og med kortrækkende bestilling af hundredvis af mikrometer i længden, men kræver mekaniske presser på for enheden integration 19 , 20.
Første rapporteret af Kistler, give aerogeler en sammenfattende rute for at nå porøse strukturer med høj specifik overflade områder, der er størrelsesordener mindre tætte end deres bulk materielle modparter21,22,23 . Forlænge 3-dimensionelle strukturer til makroskopisk længde omfanget af bulkgods tilbyder en fordel over nanopartikel aggregater eller nanofoams, der kræver støttematerialer eller mekanisk bearbejdning. Mens aerogeler give en sammenfattende rute for at styre porøsitet og partikel funktion størrelse, men udvidet syntese gange, og i nogle tilfælde brug af udjævningen agenter eller linker molekyler, øger samlede behandling trin og tid.
Her præsenteres en metode til at syntetisere guld, palladium og platin aerogeler via en hurtig, direkte løsning-baseret reduktion24. Kombinere forskellige forløber ædle metal ioner med reduktionsmiddel i en 1:1 sammenlignet (v/v) ratio resultater i dannelsen af metal geler inden for sekunder til minutter med meget længere syntese gange for andre teknikker såsom sol-gel. Brugen af et microcentrifuge rør eller lille volumen koniske rør udnytter energisk hydrogen gas udvikling som et biprodukt af trinnet reduktion at lette en foreslåede Nukleering, vækst, fortætning, fusion, ækvilibrering model for gel dannelse. En tæt korrelation i aerogel nanostrukturer funktion størrelser bestemmes med scanning Elektron Mikroskopi billedanalyse, X-ray diffractometry, nitrogen gas adsorption, elektrokemiske impedans spektroskopi og cyklisk voltammetry. Opløsningsmiddel tilgængelige specifikke areal bestemmes med både elektrokemiske impedans spektroskopi og cyklisk voltammetry. Denne syntese metode for ædelmetal aerogeler viser, at høje specifikke overfladeareal Monoliter kan opnås med en hurtig og direkte reduktion tilgang.

<table border="0" cellpadding="0" cellspacing="0" width="691">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">HAuCl4&#376;&#8226;3H2O&#160;</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16961-25-4</td>
			<td style="width:229px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">Na2PdCl4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13820-40-1</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">K2PtCl6</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16921-30-5</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Pd(NH3)4Cl2</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13933-31-8</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">K2PtCl4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">10025-99-7</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Pt(NH3)4Cl2&#376;&#8226;H2O</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13933-31-8</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">dimethylamine borane (DMAB)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">74-94-2</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">NaBH4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16940-66-2</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">NaH2PO2&#376;&#8226;H2O</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">10039-56-2</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Ethanol</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td>792780</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Snap Cap Microcentrifuge Tubes, 2.0 mL</td>
			<td style="width:128px;">Cole Parmer</td>
			<td>UX-06333-70</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Snap Cap Microcentrifuge Tubes, 1.7 mL</td>
			<td style="width:128px;">Cole Parmer</td>
			<td>UX-06333-60</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Conical Centrifuge Tubes 15mL</td>
			<td style="width:128px;">Stellar Scientific</td>
			<td>T15-101&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Ag/AgCl Reference Electrode</td>
			<td style="width:128px;">BASi</td>
			<td style="width:119px;">MF-2052</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Pt wire electrode</td>
			<td style="width:128px;">BASi</td>
			<td style="width:119px;">MF-4130</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Miccrostop Lacquer</td>
			<td style="width:128px;">Tober Chemical Division</td>
			<td style="width:119px;">NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Potentiostat</td>
			<td style="width:128px;">Biologic-USA</td>
			<td style="width:119px;">VMP-3</td>
			<td>Electrochemical analysis-EIS, CV</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Freeze Dryer</td>
			<td style="width:128px;">Labconco</td>
			<td style="width:119px;">Freezone 2.5 Liter</td>
			<td>Aerogel freeze drying</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">XRD</td>
			<td style="width:128px;">PanAlytical</td>
			<td style="width:119px;">Empyrean</td>
			<td>X-ray diffractometry</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Surface and Pore Analyzer</td>
			<td style="width:128px;">Quantachrome</td>
			<td style="width:119px;">NOVA 4000e</td>
			<td>Nitrogen gas adsorption</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">ImageJ, Image analysis software</td>
			<td style="width:128px;">National Institute of Health</td>
			<td style="width:119px;">NA</td>
			<td>SEM image analysis</td>
		</tr>
	</tbody>
</table>

a rapid synthesis method for au, pd, and pt aerogels via direct solution-based reduction

Her præsenteres en metode til at syntetisere guld, palladium og platin aerogeler via en hurtig, direkte løsning-baseret reduktion. Kombinationen af forskellige forløber ædle metal ioner med reduktionsmiddel i en 1:1 (v/v) ratio resultater i dannelsen af metal geler inden for sekunder til minutter i forhold til meget længere syntese gange for andre teknikker såsom sol-gel. Gennemføre trinnet reduktion i en microcentrifuge letter tube eller lille volumen koniske rør en foreslåede Nukleering, vækst, fortætning, fusion, ækvilibrering model for dannelse af gel med endelige gel geometri mindre end første reaktion volumen. Denne metode udnytter energisk hydrogen gas udvikling som et biprodukt af trinnet reduktion, og som følge af reagens koncentrationer. Opløsningsmiddel tilgængelige specifikke areal bestemmes med både elektrokemiske impedans spektroskopi og cyklisk voltammetry. Efter skylning og fryse tørring, behandles den resulterende aerogel struktur med scanning elektronmikroskopi, X-ray diffractometry og nitrogen gas adsorption. Syntese-metoden og karakterisering teknikker resultere i en tæt korrespondance af aerogel ligament størrelser. Denne syntese metode for ædelmetal aerogeler viser, at høje specifikke overfladeareal Monoliter kan opnås med en hurtig og direkte reduktion tilgang.

Tilsætning af metal-ion og reduktionsmiddel løsninger sammen resulterer i løsninger straks vender en mørk sort farve med kraftig gas evolution. Observation af reaktion fremskridt antyder den foreslåede gel formation mekanisme vist i figur 1. Gel dannelsen skrider frem gennem fem trin 1) nanopartikel Nukleering, 2) vækst, 3) fortætning, 4) fusion og 5) ækvilibrering. De første fire trin er observeret for at forekomme under de første par minutter af r...

Watch this Scientific Journal Video about A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction at JoVE.com

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

En hurtig syntese metode til Au, Pd og Pt aerogeler Via direkte løsning-baseret reduktion

En hurtig, direkte løsning-baseret reduktion syntese metode til at opnå Au, Pd og Pt aerogeler præsenteres.

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

Research

JoVE Journal

Chemistry

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

Forberedelse Silica Aerogelpartikler Monoliths via en hurtig Supercritical ekstraktionsmetode

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Synthesis, karakterisering, og Funktionalisering af Hybrid Au / cd&#39;er og Au / ZnS Core / Shell Nanopartikler

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

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

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

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Syntese af Protein biokonjugater<em&gt; via</em&gt; Cystein-maleimid Kemi

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or IV)

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

Kombinere Solid-state og løsning-baserede teknikker: Syntese og reaktivitet af Chalcogenidoplumbates (II eller IV)

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica ...

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

Syntese og test af understøttet Pt-Cu fast opløsning Nanopartiklekatalysatorer til propan dehydrogenering

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

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

Syntese af Platinum-nikkel Nanowires og optimering for ilt reduktion ydeevne

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

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Fabrikation og afprøvning af katalytisk aerogeler fremstillet Via Rapid superkritisk ekstraktion

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

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

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

Syntese og ydeevne beskrivelser af overgangen Metal enkelt Atom katalysator for elektrokemisk CO2 reduktion

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