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SynthesisofCadmiumSulfideNanoparticles

AdaptedbyKayleenMooreandThomasC.Keane,Ph.D
April20,2008
I.Abstract
ThisexperimentisanintroductorystudyofCadmiumsulfidenanoparticles.The
Cadmiumsulfidenanoparticlesareinversephasemicelles.2 Micellesareanaggregateof
surfactantmoleculesdispersedinaliquidcolloid1,andareusedinawidevarietyof
differentbiochemicalandindustrialapplications.Specifically,thislabstudiestheshiftin
theabsorptionspectrumfromthebulksampleofCdStothemicelleCdSabsorption
spectrum.Thisshiftinabsorptioncan aidincalculatingthemicelleradius.The
experimentallyobtainedaverageshiftis71nm.Usingthisaveragethemicelleradiuswas
foundtobe2.15nm.
II.LearningObjectives
1) InterpretUVVisabsorptionspectra
2) ApplytheconceptofpolaritytoMicelleformation
III.Introduction
Amicelleisanaggregateofsurfactantmoleculesdispersedinaliquidcolloid.
Surfactantmoleculesareorganiccompoundsthatareamphiphilic.Amphiphilicmeans
thattheyhavebothapolar(hydrophilic)endandanonpolar(hydrophobic)end.Through
thisunderstandingamicellecanbedefinedasananoparticleofanorganizedorganic
moleculeinaparticularsolvent.
Inthesynthesisofcadmium sulfide(CdS)nanoparticleswewillbeusing
hexadecyltrimethylammoniumbromideasthesurfactantmolecule.Thismoleculedoes
notdissolvewellinaqueousororganicsolvents,butitisessentialinmakingthemicelle.
Thehexadecyltrimethylammoniumbromidestructureisshownbelow:

Therearedifferenttypesofmicellephases.Thetwophasesthatwillbefocused
onarethenormalandinversecylindricalphases.Thenormalphasemicelleisproduced
whenitisinapolarsolutionandthepolarendofthesurfactantisattractedtothepolar
solvent.Thehydrophobicnonpolarhydrocarbonsformthecoreofthemicelle,andthe
polarendofthesurfactantformstheouterlayerofthemicelle.Thisisalsoknownasthe
oilinwatermicelle.Theinversecylindricalphaseisformedinjusttheopposite
environment.Thesolventisnonpolar.Inthiswaythehydrocarbonsmaketheouterlayer
andthepolarendmakesthecoreofthemicelle.Thisisknownasthewaterinoil
micelle.
Hydrophilic

Hydrophilic

Hydrophobic

Hydrophobic

Inordertoformthecadmiumsulfidemicelles,hexadecyltrimethylammoniumbromide
willbemixedwithpentanolinahexanesolution.Pentanolisacosurfactantthathastwo
mainfunctions.Thefirstfunctionofpentanolisthatinrelativeamountsitcontrolsthe
sizeof themicelles.PentanolisalsousedasacappingagenttostabilizetheCdS
particles.
Cd+micellesaremadeandmixedwithSmicelleswhichproduceCdSparticles.
CdSisfoundinthecoreofthemicelle.Theaqueoussolutionservesasananoreactorand
theparticlescannotgrowbiggerthanthemicelle.Thisphenomenonhasaneffectonthe
quantumsizeofthemicelle.SincethereisadifferenceinsizefromthebulkCdSandthe
micelletheabsorptionspectrumcanbetakenforeachandthancompared.Therewillbe
ashiftofwavelengthbasedonsize.Thischangeinwavelengthcanbecalculatedand
usedtofindtheradiusoftheCdSmicelle.Anexampleoftheshiftphenomenonand
equationisshownbelow.

bulk =512nm
Eg =hc/
Thexinterceptofthe
linearportionofthe
absorbanceasafunction
ofwavelengthgraphisa
measureof Eg.

e=1.60x1019 C
0 =8.85x1012
C2/N/m2
=5.7
h=6.63x1034 Js
c=2.998x108 m/s
me*=1.73x1031 kg
mh*=7.29x1031 kg
ExampleCalculation
nano=495nm
Egnano=hc/
Egnano=
(6.63E34)(3.0E8)/495E9m
Egnano=4.018E19J

bulk=550nm
Egbulk=hc/
Egbulk=
(6.63E34)(3.0E8)/550E9m
Egbulk=3.616E19J

r=2.34nm
IV.Materials
*0.012MCdCl2 (0.110gin50mLdistilledwater)
*0.012MNa2S(0.144gin50mLdistilledwater)
0.20ghexadecyltrimethylammoniumbromide
4mLHeptane
1mLPentanol
Mortarandpestle
2testtubes

2smallmagneticstirbars
MagneticStirrer
PlasticCuvetts
Volumetircpipets,11mL,25mL
*premade

V.Procedure
1) TurnontheUVVis,andconnectittothecomputer.Itwilltakealittletime.Go
ontotheothersteps.
2) Obtainedabout5mleachoftheCdCl2 solutionandtheNa2Ssolutioninseparate,
smallvials.
3) TestthereagentsCdCl2 andNa2Sbyaddingadropofeachtogether.Ifayellow
colorappearsthisshowsthattheNa2Ssolutionisgood.Ifthemixturestaysclear,
remaketheNa2Ssolution.
4) ReturningbacktotheUVVis,itshouldbeconnected.Takeabaseline.
5) Placeequalamountsof CdCl2 andNa2Sintoacuvet,mixgentlywithpipet(do
notmakebubbles).Immediatelyobtain avisibleabsorptionspectrum,usingan
emptycuvetastheblank.Visuallynote thechangeincolorbeforeandafter
addingtheNa2S totheCdCl2.
6) Setuptwocleantesttubesover twoseparate magneticstirrers.
7) Place0.20gofhexadecyltrimethylammoniumbromidetotesttube one.Adda
smallstirbartoeachtesttube.
8) Add4.0mLofHeptaneand1.0mLof1Pentanolintotesttubeone.Note:
Rememberthattheamountofpentanolisthecappingagentandchangesthesize
ofthemicelle.Makesurethat thepentanoldoesntgetstuckonthesideofthetest
tube.Stirtogiveasuspension.
9) Withvolumetricpipettransferalittleover2.5mLofthesuspensionintothe
secondtesttube.
10) Totesttubeone,add0.1mL(3drops)of0.012Mof CdCl2.Addthesolution
dropwiseuntilthesuspensioninthetesttubeclears,dontaddmorethan3drops.
11) Add0.1mL(3drops)of0.012MNa2S totesttube2.Addthesolutiondropwise
untilthesuspensioninthetesttubeclears.IFTHESOLUTIONCLEARS
BEFOREADDINGALLTHREEDROPSDONTADDMORE.
12) Placethesolutionfromtesttubetwointotesttubeone.Solutioncouldeitherhave
alightyellowhueorbeclear.
13) Recordthevisibleabsorptionspectrumin eitheraglassorplasticcuvet.

VI.Questions
1) Whatisamicelle?Stateitinyourownwords.Drawadiagramandlabelitsparts.

2) Whatisthedifferencebetweenanormalandreversephasemicelle?Whatmicelle
phasedoestheCadmiumSulfidenanoparticleforminto?

3) Whatpartdoespentanolplayinformingthemicelle?

4) Whattwochangesoccurbetweenin theabsorptionspectraof theCdSsolutionand


theCdSmicelles?Talkaboutthedifferenceinabsorbanceandshiftinwavelength.

5) Whentheformationofthemicellehasoccurred, whereisthelocationoftheCdS
salt? Whatistheothersaltbyproductthatisformed?

6) Iftherewasashiftintheabsorptionspectrafrom575cm1to480cm1,wouldthe
micellebesmallerorbiggerthantheoriginalsample?

7) Whataretwopracticalusesformicelles?

8) Whatwastheradiusofyourmicelle

VII. References
ImagesofNormalandInversePhaseMicelles.(2007).RetrievedApril19,2008.
Website:http://en.wikipedia.org/wiki/Micelle
Linsensky,GeorgeandHansen,Paul.(2005).SynthesisofCadmiumSulfide
Nanoparticle.RetrievedonMarch24,2008.
Website:http://mrsec.wisc.edu/Edetc/nanolab/CdS/text.htm

PremadeMaterials
0.012MNa2Ssolution
1. Weighout0.144gofthepowderNa2S,placeinamortorandgrindintoafind
powder.
2. PlacethepowderedNa2Sina50mLgraduatedflaskandfillitwiththedeionized
watertothemark.
0.012MCdCl2 solution

1. Weighout0.110gofCdCl2 intoa50mlgraduatedflask,andfilltheflaskupto
theline.Swirlmixtureuntilallthedissolves.

VIII. Answers
1) Amicelleisclustersof organizedsurfactant, organiccompoundsthathaveapolar
andnonpolarhead,thatform inaheterogeneousmixture.Maindefinition:A
micelleisanaggregate ofsurfactantmoleculesdispersedinaliquidcolloid.
2) A)Normalphase:Thepolarregionisincontactwiththesolvent.(Polarhead,Polar
solvent)B)Reversephase:Thenonpolarchainregionisincontactwiththesolvent.
(Nonpolarchain,Nonpolarsolvent)CdSmicellesarereversephase.
3) Thepentanolcontrolsthesizeofthemicelle,italsoactsasacappingagentto
stabilizetheCdSparticles.
4) Absorbance:InthesolutiontheCdSisdiluteinthemicellesolution.Shift:Thesize
oftheparticlesdeterminestheshiftinwavelength.
5) A)CdSislocatedinthecoreofthemicelle.B)NaCl.
6) Smaller
7) AnswerDependant
8) Basedoffofdata.
IX.ConclusionsandPlacement
Thislabisveryinteresting,butnotforgeneralchemistrystudents.Thereissome
difficultyincreatingthemicellesandthecalculationmightbealittledifficultto
understand.Thesuspensionsinthetesttubeswillnotalwaysclear,butwillstillform
micellesthathavetheappropriateabsorptionshift.Thislabmightbegoodfor
analyticalchemistrybecauseitisdealingwithabsorption,concentrationandpH,but
doesntfocusontitration.Thiswillgivethestudentsabreakfromtitration,butleadsto
thesametypesofconcepts.Furthercalculationscanbedoneontheconcentrationof
micellesbasedoffofabsorption(BeersLaw).Applicationsofmicellescanalsobe
discussed(forexampleinbiochemistryandindustry)duringanalyticalchemistryto
makethetopicinterdisciplinary.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