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 takknemlig Stephen Steiner ved Aerogel teknologier for hans inspirasjon og tekniske innsikt og Dr. Deryn Chu Army Research Laboratory-sensorer og elektron enheter Direktoratet, Dr. Christopher Haines på Armament forskning, Utvikling og Engineering Center, US Army RDECOM-ARDEC og Dr. Stephen Bartolucci på den amerikanske hæren Benet laboratorier for deres hjelp. Dette arbeidet ble støttet av fakultetet utvikling Research Fund stipend fra United States Military Academy, West Point.

FORSIKTIG: Se alle relevante Produktdatablad (SDS) før bruk. Bruke riktige sikkerhets praksis når kjemiske reaksjoner, med bruk av en avtrekksvifte og personlig verneutstyr. Rask hydrogen gass utvikling kan forårsake høyt trykk i reaksjon rør forårsaker caps pop og løsninger til sprøytes ut. Sikre at reaksjonen tube caps forblir åpen som angitt i protokollen.
1. metall Gel forberedelse
<ol><li>
Utarbeidelse av metall ion løsninger.
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<li>Forberede 2 mL 0.1 M l?...

<ol>
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Metoden noble metal aerogel syntese presenteres her resultater i rask dannelsen av porøs, høy areal monolitter som sammenlignes med tregere syntese teknikker. 1:1 (v/v) metall ion løsning reduksjonsmiddel løsning forhold er kritisk tilrettelegge foreslåtte gel formasjon modellen. Rask hydrogen gass utviklingen som et biprodukt av elektrokjemiske reduksjon av metall ioner fungerer som en sekundær reduksjonsmiddel og forenkler densification, og blanding av voksende nanopartikler under gel formasjon. Utvalg av optimal...

En rekke energilagring og konvertering, katalyse og sensor programmer nytte tredimensjonale metallisk nanostrukturer som gir deg kontroll over kjemiske reaktivitet og masse transport egenskaper1,2, 3,4,5. Slike 3-dimensjonale metallisk nanostrukturer ytterligere forbedre ledningsevne, ductility, malleability og styrke8,9. Integrering i enheter nødvendiggjør at materialer være frittstående eller kombinert med støttemateriell. Innlemmelse av nanomaterialer på støttestrukturer gir en måte å minimere aktive, men kan lide av svak adsorpsjon og eventuell agglomeration under enhet operasjon10,11.
Det finnes en rekke syntese metoder for å kontrollere individuelle hydrogenion størrelse og form, aktivere noen tilnærminger kontroll over sammenhengende 3-dimensjonale nanomaterialer12,13,14. Noble metal 3-dimensjonale nanostrukturer har blitt dannet gjennom dithiol kombinasjon av monodisperse nanopartikler, sol-gel formasjon, hydrogenion Koalesens, komposittmaterialer, nanosphere kjeder og biotemplating15,16 , 17 , 18. mange av disse metodene krever syntese tider på dager til uker å gi ønsket materiale. Noble metal nanofoams fra direkte reduksjon av forløperen salt løsninger er utarbeidet med en raskere syntese tidsskala og med kort rekkevidde for hundrevis av mikrometer i lengde, men krever mekanisk trykke for enheten integrering 19 , 20.
Først rapportert av Kistler, gir aerogels en syntese rute for å oppnå porøse strukturer med høy bestemt overflate områder som er flere størrelsesordener mindre tett enn sine bulk materiale kolleger21,22,23 . Utvide 3-dimensjonale strukturer makroskopisk lengde omfanget av bulkvarer tilbyr en fordel over hydrogenion tilslag eller nanofoams som krever støttemateriell eller mekaniske. Aerogels gir en syntese rute for å styre porøsitet og funksjonen partikkelstørrelse, men utvidet syntese ganger, og i noen tilfeller bruk capping agenter eller koblingsfunksjonalitet molekyler, øker total behandling tid.
Her er en metode for å syntetisere gull, palladium og platinum aerogels via en rask, direkte solution-baserte reduksjon presentert24. Kombinere ulike forløper noble metall ioner med reduksjonsmidler i en 1:1 (v/v) forholdet resultater i dannelsen av metall gels innen sekunder til minutter i forhold til mye lengre syntese tider for andre teknikker som sol-gel. Bruk av et microcentrifuge rør eller små konisk tube utnytter energisk hydrogen gass utvikling som et biprodukt av reduksjon trinnet tilrettelegge en foreslått nucleation, vekst, densification, fusion, balanse modell for gel-formasjonen. En nær sammenheng i aerogel nanostructure funksjonen størrelser bestemmes skanning elektronmikroskop bildeanalyser, røntgen diffractometry, nitrogen gass adsorpsjon, elektrokjemiske impedans spektroskopi og syklisk voltammetry. Løsemiddel tilgjengelig bestemt arealet avhenger både elektrokjemiske impedans spektroskopi og syklisk voltammetry. Denne syntese metoden for noble metal aerogels viser at høy bestemt areal monolitter kan oppnås med en rask og direkte tilnærming.

<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 vises en metode for å syntetisere gull, palladium og platinum aerogels via en rask, direkte solution-baserte reduksjon. Kombinasjonen av ulike forløper noble metall ioner med reduksjonsmidler i en 1:1 (v/v) forholdet fører til dannelsen av metall gels innen sekunder til minutter i forhold til mye lengre syntese tider for andre teknikker som sol-gel. Gjennomføre reduksjon trinnet i et microcentrifuge forenkler rør eller små konisk tube en foreslått nucleation, vekst, densification, fusion, balanse modell for gel formasjon, med siste gel geometri mindre enn første reaksjon. Denne metoden tar nytte av energisk hydrogen gass utviklingen som et biprodukt av reduksjon trinnet, og at reagens konsentrasjoner. Løsemiddel tilgjengelig bestemt arealet avhenger både elektrokjemiske impedans spektroskopi og syklisk voltammetry. Etter skylling og fryser tørking, er den resulterende aerogel strukturen undersøkt med skanning elektronmikroskop X-ray diffractometry og nitrogen gass adsorpsjon. Syntese metoden og identifikasjon teknikker føre en nær korrespondanse aerogel ligament størrelser. Denne syntese metoden for noble metal aerogels viser at høy bestemt areal monolitter kan oppnås med en rask og direkte tilnærming.

Tillegg av metall ion og reduksjonsmiddel løsninger sammen resulterer i løsninger umiddelbart slår en mørk svart farge med energisk gass utvikling. Observasjon av reaksjon fremdriften antyder den foreslåtte gel formasjonen mekanismen som vist i figur 1. Gel formasjon går gjennom fem trinn 1) hydrogenion nucleation, 2) vekst, 3) densification, 4) fusion og 5) balanse. De første fire trinnene er observert for å skje i løpet av de første minuttene av 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 rask syntese metode for Au og Pd Pt Aerogels Via direkte Solution-baserte reduksjon

Rask, direkte solution-baserte reduksjon syntese enmetoden å få Au og Pd Pt aerogels presenteres.

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

Forbereder Silica Aerogel Monoliths via en Rapid superkritisk Extraction Method

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

Syntese, karakterisering og funksjon av Hybrid Au / CDer og Au / ZnS Kjerne / 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 av Protein Bioconjugates<em&gt; via</em&gt; Cystein-maleimide kjemi

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 Solution-baserte teknikker: Syntese og reaktivitet av 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 av støttet Pt-Cu fast løsning Nanopartikkelkatalysatorer for 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 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 ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Fabrikasjon og Testing av katalytiske Aerogels forberedes Via raske superkritisk ekstraksjon

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

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