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Synthesis of Cadmium Sulfide Nanoparticles Adapted by Kayleen Moore and Thomas C. Keane, Ph.D April 20, 2008 I. Abstract This experiment is an introductory study of Cadmium sulfide nanoparticles. The Cadmium sulfide nanoparticles are inverse phase micelles. 2 Micelles are an aggregate of surfactant molecules dispersed in a liquid colloid 1 , and are used in a wide variety of different biochemical and industrial applications. Specifically, this lab studies the shift in the absorption spectrum from the bulk sample of CdS to the micelle CdS absorption spectrum. This shift in absorption can aid in calculating the micelle radius. The experimentally obtained average shift is 71nm. Using this average the micelle radius was found to be 2.15nm. II. Learning Objectives 1) Interpret UVVis absorption spectra 2) Apply the concept of polarity to Micelle formation III. Introduction A micelle is an aggregate of surfactant molecules dispersed in a liquid colloid. Surfactant molecules are organic compounds that are amphiphilic. Amphiphilic means that they have both a polar (hydrophilic) end and a nonpolar (hydrophobic) end. Through this understanding a micelle can be defined as a nanoparticle of an organized organic molecule in a particular solvent. In the synthesis of cadmium sulfide (CdS) nanoparticles we will be using hexadecyltrimethylammonium bromide as the surfactant molecule. This molecule does not dissolve well in aqueous or organic solvents, but it is essential in making the micelle. The hexadecyltrimethylammonium bromide structure is shown below: There are different types of micelle phases. The two phases that will be focused on are the normal and inverse cylindrical phases. The normal phase micelle is produced when it is in a polar solution and the polar end of the surfactant is attracted to the polar solvent. The hydrophobic nonpolar hydrocarbons form the core of the micelle, and the polar end of the surfactant forms the outer layer of the micelle. This is also known as the oilinwater micelle. The inverse cylindrical phase is formed in just the opposite environment. The solvent is nonpolar. In this way the hydrocarbons make the outer layer and the polar end makes the core of the micelle. This is known as the waterinoil micelle. Hydrophilic Hydrophobic Hydrophobic Hydrophilic Organic Solvent Aqueous Solvent

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  • SynthesisofCadmiumSulfideNanoparticlesAdaptedbyKayleenMooreandThomasC.Keane,Ph.D

    April20,2008

    I.AbstractThisexperimentisanintroductorystudyofCadmiumsulfidenanoparticles.The

    Cadmiumsulfidenanoparticlesareinversephasemicelles.2Micellesareanaggregateofsurfactantmoleculesdispersedinaliquidcolloid1,andareusedinawidevarietyofdifferentbiochemicalandindustrialapplications.Specifically,thislabstudiestheshiftintheabsorptionspectrumfromthebulksampleofCdStothemicelleCdSabsorptionspectrum.Thisshiftinabsorptioncan aidincalculatingthemicelleradius.Theexperimentallyobtainedaverageshiftis71nm.Usingthisaveragethemicelleradiuswasfoundtobe2.15nm.

    II.LearningObjectives1) InterpretUVVisabsorptionspectra2) ApplytheconceptofpolaritytoMicelleformation

    III.IntroductionAmicelleisanaggregateofsurfactantmoleculesdispersedinaliquidcolloid.

    Surfactantmoleculesareorganiccompoundsthatareamphiphilic.Amphiphilicmeansthattheyhavebothapolar(hydrophilic)endandanonpolar(hydrophobic)end.Throughthisunderstandingamicellecanbedefinedasananoparticleofanorganizedorganicmoleculeinaparticularsolvent.

    Inthesynthesisofcadmium sulfide(CdS)nanoparticleswewillbeusinghexadecyltrimethylammoniumbromideasthesurfactantmolecule.Thismoleculedoesnotdissolvewellinaqueousororganicsolvents,butitisessentialinmakingthemicelle.Thehexadecyltrimethylammoniumbromidestructureisshownbelow:

    Therearedifferenttypesofmicellephases.Thetwophasesthatwillbefocusedonarethenormalandinversecylindricalphases.Thenormalphasemicelleisproducedwhenitisinapolarsolutionandthepolarendofthesurfactantisattractedtothepolarsolvent.Thehydrophobicnonpolarhydrocarbonsformthecoreofthemicelle,andthepolarendofthesurfactantformstheouterlayerofthemicelle.Thisisalsoknownastheoilinwatermicelle.Theinversecylindricalphaseisformedinjusttheoppositeenvironment.Thesolventisnonpolar.Inthiswaythehydrocarbonsmaketheouterlayerandthepolarendmakesthecoreofthemicelle.Thisisknownasthewaterinoilmicelle.

    Hydrophilic

    Hydrophobic Hydrophobic

    Hydrophilic

    OrganicSolventAqueousSolvent

  • Inordertoformthecadmiumsulfidemicelles,hexadecyltrimethylammoniumbromidewillbemixedwithpentanolinahexanesolution.Pentanolisacosurfactantthathastwomainfunctions.Thefirstfunctionofpentanolisthatinrelativeamountsitcontrolsthesizeof themicelles.PentanolisalsousedasacappingagenttostabilizetheCdSparticles.

    Cd+micellesaremadeandmixedwithSmicelleswhichproduceCdSparticles.CdSisfoundinthecoreofthemicelle.Theaqueoussolutionservesasananoreactorandtheparticlescannotgrowbiggerthanthemicelle.Thisphenomenonhasaneffectonthequantumsizeofthemicelle.SincethereisadifferenceinsizefromthebulkCdSandthemicelletheabsorptionspectrumcanbetakenforeachandthancompared.Therewillbeashiftofwavelengthbasedonsize.ThischangeinwavelengthcanbecalculatedandusedtofindtheradiusoftheCdSmicelle.Anexampleoftheshiftphenomenonandequationisshownbelow.

    bulk=512nmEg=hc/

    Thexinterceptofthelinearportionoftheabsorbanceasafunctionofwavelengthgraphisameasureof Eg.

  • ExampleCalculation

    r=2.34nm

    IV.Materials*0.012MCdCl2(0.110gin50mLdistilledwater)*0.012MNa2S(0.144gin50mLdistilledwater)0.20ghexadecyltrimethylammoniumbromide4mLHeptane1mLPentanolMortarandpestle2testtubes

    e=1.60x1019C0=8.85x10

    12

    C2/N/m2

    =5.7h=6.63x1034Jsc=2.998x108m/sme*=1.73x10

    31kgmh*=7.29x10

    31kg

    nano=495nmEgnano=hc/Egnano=(6.63E34)(3.0E8)/495E9m

    Egnano=4.018E19J

    bulk=550nmEgbulk=hc/Egbulk=(6.63E34)(3.0E8)/550E9m

    Egbulk=3.616E19J

  • 2smallmagneticstirbarsMagneticStirrerPlasticCuvettsVolumetircpipets,11mL,25mL

    *premade

    V.Procedure

    1) TurnontheUVVis,andconnectittothecomputer.Itwilltakealittletime.Goontotheothersteps.

    2) Obtainedabout5mleachoftheCdCl2solutionandtheNa2Ssolutioninseparate,smallvials.

    3) TestthereagentsCdCl2andNa2Sbyaddingadropofeachtogether.IfayellowcolorappearsthisshowsthattheNa2Ssolutionisgood.Ifthemixturestaysclear,remaketheNa2Ssolution.

    4) ReturningbacktotheUVVis,itshouldbeconnected.Takeabaseline.5) Placeequalamountsof CdCl2andNa2Sintoacuvet,mixgentlywithpipet(do

    notmakebubbles).Immediatelyobtain avisibleabsorptionspectrum,usinganemptycuvetastheblank.Visuallynote thechangeincolorbeforeandafteraddingtheNa2S totheCdCl2.

    6) Setuptwocleantesttubesover twoseparate magneticstirrers.7) Place0.20gofhexadecyltrimethylammoniumbromidetotesttube one.Adda

    smallstirbartoeachtesttube.8) Add4.0mLofHeptaneand1.0mLof1Pentanolintotesttubeone.Note:

    Rememberthattheamountofpentanolisthecappingagentandchangesthesizeofthemicelle.Makesurethat thepentanoldoesntgetstuckonthesideofthetesttube.Stirtogiveasuspension.

    9) Withvolumetricpipettransferalittleover2.5mLofthesuspensionintothesecondtesttube.

    10) Totesttubeone,add0.1mL(3drops)of0.012Mof CdCl2.Addthesolutiondropwiseuntilthesuspensioninthetesttubeclears,dontaddmorethan3drops.

    11) Add0.1mL(3drops)of0.012MNa2S totesttube2.Addthesolutiondropwiseuntilthesuspensioninthetesttubeclears.IFTHESOLUTIONCLEARSBEFOREADDINGALLTHREEDROPSDONTADDMORE.

    12) Placethesolutionfromtesttubetwointotesttubeone.Solutioncouldeitherhavealightyellowhueorbeclear.

    13) Recordthevisibleabsorptionspectrumin eitheraglassorplasticcuvet.

    VI.Questions

    1) Whatisamicelle?Stateitinyourownwords.Drawadiagramandlabelitsparts.

  • 2) Whatisthedifferencebetweenanormalandreversephasemicelle?WhatmicellephasedoestheCadmiumSulfidenanoparticleforminto?

    3) Whatpartdoespentanolplayinformingthemicelle?

    4) Whattwochangesoccurbetweenin theabsorptionspectraof theCdSsolutionandtheCdSmicelles?Talkaboutthedifferenceinabsorbanceandshiftinwavelength.

    5) Whentheformationofthemicellehasoccurred, whereisthelocationoftheCdSsalt? Whatistheothersaltbyproductthatisformed?

    6) Iftherewasashiftintheabsorptionspectrafrom575cm1to480cm1,wouldthemicellebesmallerorbiggerthantheoriginalsample?

    7) Whataretwopracticalusesformicelles?

    8) Whatwastheradiusofyourmicelle

    VII. References

    ImagesofNormalandInversePhaseMicelles.(2007).RetrievedApril19,2008.Website:http://en.wikipedia.org/wiki/Micelle

    Linsensky,GeorgeandHansen,Paul.(2005).SynthesisofCadmiumSulfideNanoparticle.RetrievedonMarch24,2008.Website:http://mrsec.wisc.edu/Edetc/nanolab/CdS/text.htm

  • PremadeMaterials

    0.012MNa2Ssolution1. Weighout0.144gofthepowderNa2S,placeinamortorandgrindintoafind

    powder.2. PlacethepowderedNa2Sina50mLgraduatedflaskandfillitwiththedeionized

    watertothemark.

    0.012MCdCl2solution

  • 1. Weighout0.110gofCdCl2 intoa50mlgraduatedflask,andfilltheflaskuptotheline.Swirlmixtureuntilallthedissolves.

    VIII. Answers

    1) Amicelleisclustersof organizedsurfactant, organiccompoundsthathaveapolarandnonpolarhead,thatform inaheterogeneousmixture.Maindefinition:Amicelleisanaggregate ofsurfactantmoleculesdispersedinaliquidcolloid.

    2) A)Normalphase:Thepolarregionisincontactwiththesolvent.(Polarhead,Polarsolvent)B)Reversephase:Thenonpolarchainregionisincontactwiththesolvent.(Nonpolarchain,Nonpolarsolvent)CdSmicellesarereversephase.

    3) Thepentanolcontrolsthesizeofthemicelle,italsoactsasacappingagenttostabilizetheCdSparticles.

    4) Absorbance:InthesolutiontheCdSisdiluteinthemicellesolution.Shift:Thesizeoftheparticlesdeterminestheshiftinwavelength.

    5) A)CdSislocatedinthecoreofthemicelle.B)NaCl.6) Smaller7) AnswerDependant8) Basedoffofdata.

    IX.ConclusionsandPlacement

    Thislabisveryinteresting,butnotforgeneralchemistrystudents.Thereissomedifficultyincreatingthemicellesandthecalculationmightbealittledifficulttounderstand.Thesuspensionsinthetesttubeswillnotalwaysclear,butwillstillformmicellesthathavetheappropriateabsorptionshift.Thislabmightbegoodforanalyticalchemistrybecauseitisdealingwithabsorption,concentrationandpH,butdoesntfocusontitration.Thiswillgivethestudentsabreakfromtitration,butleadstothesametypesofconcepts.Furthercalculationscanbedoneontheconcentrationofmicellesbasedoffofabsorption(BeersLaw).Applicationsofmicellescanalsobediscussed(forexampleinbiochemistryandindustry)duringanalyticalchemistrytomakethetopicinterdisciplinary.Theabsorptionspectraareinthelaboratorynotebook.

    Chemicals

    CdO

    OleicAcid

    Selenium

    Trioctylphosphine

  • TechnicalGradeOctadecene(ODE)

    SupplyListfor10Students

    100Smalltesttubes

    10Testtuberacks

    10tubesforice(bigenoughtofitthetesttuberackinto)

    Ice

    10Heatingmantles

    10Variacs

    10Thermometerscapableofmeasuring225oC

    10Roundbottomflasks(each)

    10ml 25ml

    10Syringes(capableofdelivering0.4ml)andmediumsizeneedle(10cmlong).

    10GlassPipettes

    10Volumetricpipettes(each)

    1ml graduated1mltodeliver0.6ml 10ml 5ml


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