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.2010,110,111–131111
AtomicLayerDeposition:AnOverview
*
DepartmentofChemistryandBiochemistryandDepartmentofChemicalandBiologicalEngineering,UniversityofColorado,
Boulder,Colorado80309
ReceivedFebruary12,2009
Contents
uction
2
O
3
ALDasaModelALDSystem
landPlasmaorRadical-EnhancedALD
lALD
orRadical-EnhancedALD
rsforALD
LDUsingThermalChemistry
silaneEliminationChemistry
tionChemistry
enReductionChemistry
tionandGrowthduringALD
xideALDonH-Si(100)
LDonOxideSurfaces
2
O
3
ALDonCarbonNanotubesand
GrapheneSurfaces
peratureALD
2
O
3
ALDandOtherMetalOxideALD
ticSiO
2
ALD
olymers
ighAspectRatioStructures
articles
anolaminatesandAlloys
rMLD
cPolymers
Organic-InorganicPolymers
onalTopics
alALDBehaviorandtheALDWindow
-SelectiveALDforSpatialPatterning
hericPressureALD
iologicalTemplates
mergingAreas
sions
ledgments
nces
111
112
113
113
114
115
116
116
117
117
118
118
118
119
119
119
120
121
122
123
124
125
125
126
127
127
127
127
128
128
128
129
129
isProfessorintheDepartmentofChemistryand
BiochemistryandDepartmentofChemicalandBiologicalEngineeringat
ChemistryfromYaleUniversity(1977)istryfrom
theUniversityofCaliforniaatBerkeley(1983).Priortohisappointments
attheUniversityofColoradoatBoulder,wasaBantrell
PostdoctoralFellowatCaltech(1983-4)andanAssistantProfessorin
theDepartmentofChemistryatStanfordUniversity(1984-1991).Dr.
GeorgeisaFellowoftheAmericanVacuumSociety(2000)andaFellow
oftheAmericanPhysicalSociety(1997).Hehasalsoreceivedthe
AmericanChemicalSocietyColoradoSectionAward(2004),R&D100
AwardforParticle-ALD(2004),NSFPresidentialYoungInvestigatorAward
(1988-1993),oundationFellowship(1988).Dr.
George’sresearchinterestsareintheareasofsurfacechemistry,thin
filmgrowth,rrentlydirectinga
researcheffortfocusingonatomiclayerdeposition(ALD)andmolecular
layerdeposition(MLD).Thisresearchisexaminingnewsurfacechemistries
forALDandMLDgrowth,measuringthinfilmgrowthrates,and
characterizingthepropertiesofthinfiservedasChairof
thefirstAmericanVacuumSociety(AVS)TopicalConferenceonAtomic
LayerDeposition(ALD2001)heldinMonterey,teaches
isacofounder
ofALDNanoSolutions,Inc.,astartupcompanythatisworkingto
commercializeALDtechnology.
uction
Atomiclayerdeposition(ALD)hasemergedasan
importanttechniquefordepositingthinfilmsforavariety
nductorprocessinghasbeenoneof
themainmotivationsfortherecentdevelopmentofALD.
TheInternationalTechnologyRoadmapforSemiconductors
(ITRS)hasincludedALDforhighdielectricconstantgate
oxidesintheMOSFETstructureandforcopperdiffusion
barriersinbackendinterconnects.
1
Inaddition,ALDhasmet
*E-mailaddress:@.
challengingrequirementsinotherareasincludingthedeposi-
tionofhighqualitydielectricstofabricatetrenchcapacitors
forDRAM.
2
Miniaturizationinthesemiconductorindustryhasledto
therequirementforatomiclevelcontrolofthinfilm
urizationhasproducedveryhighaspect
rthin
filmtechniquecanapproachtheconformalityachievedby
essityforcontinuous
andpinhole-freefilmsinsemiconductordeviceshasdriven
pplicationswithsimilar
demandingrequirementsoutsideofthesemiconductorin-
dustryarelowelectronleakagedielectricsformagneticread/
writeheads
3
anddiffusionbarriercoatingswithlowgas
permeability.
4
10.1021/cr900056b2010AmericanChemicalSociety
PublishedonWeb11/30/2009
112ChemicalReviews,2010,Vol.110,No.1
ticrepresentationofALDusingself-limiting
surfacechemistryandanABbinaryreactionsequence.(Reprinted
ght1996AmericanChemical
Society.)
ALDisabletomeettheneedsforatomiclayercontrol
andconformaldepositionusingsequential,self-limiting
aticshowingthesequential,self-
limitingsurfacereactionsduringALDisdisplayedinFigure
1.
5
MostALDprocessesarebasedonbinaryreaction
sequenceswheretwosurfacereactionsoccuranddeposita
binarycompoundfiethereareonlyafinitenumber
ofsurfacesites,thereactionscanonlydepositafinitenumber
ofthetwosurfacereactionsis
self-limiting,thenthetworeactionsmayproceedina
sequentialfashiontodepositathinfilmwithatomiclevel
control.
TheadvantagesofALDareprecisethicknesscontrolat
theÅf-limitingaspect
ofALDleadstoexcellentstepcoverageandconformal
rfaceareas
willreactbeforeothersurfaceareasbecauseofdifferent
precursorgasflr,theprecursorswilladsorb
andsubsequentlydesorbfromthesurfaceareaswherethe
cursorswillthen
proceedtoreactwithotherunreactedsurfaceareasand
produceaveryconformaldeposition.
Theself-limitingnatureofthesurfacereactionsalso
producesanonstatisticaldepositionbecausetherandomness
oftheprecursorfl
aresult,ALDfilmsremainextremelysmoothandconformal
totheoriginalsubstratebecausethereactionsaredrivento
completionduringeveryreactioncycle.
6
Becausenosurface
sitesareleftbehindduringfilmgrowth,thefilmstendtobe
ctorisextremely
importantforthedepositionofexcellentdielectricfilms.
7
ALDprocessingisalsoextendibletoverylargesubstrates
precursorsaregasphasemolecules,andtheyfillallspace
independentofsubstrategeometryanddonotrequireline-
nlylimitedbythesizeof
processisalsodominated
ethesurfacereactionsare
performedsequentially,thetwogasphasereactantsarenot
parationofthetwo
reactionslimitspossiblegasphasereactionsthatcanform
particlesthatcoulddepositonthesurfacetoproducegranular
films.
Theuseoftheterm“ALD”datesbackapproximatelyto
o2000,thetermatomiclayerepitaxy(ALE)
wasincommonuse.
8-13
Othertermshavebeenusedto
describe
14
ALD,includingbinaryreactionsequencechemis-
tryandmolecularlayerepitaxy.
15
ThetransitionfromALE
George
toALDoccurredasaresultofthefactthatmostfilmsgrown
usingsequential,self-limitingsurfacereactionswerenot
er,amorphous
filmsweremostpreferredfordielectricanddiffusionbarrier
uently,theuseofALDgrewinprefer-
enceandnowdominateswiththepractitionersinthefield.
ThehistoryofALEandALDdatesbacktothe1970sin
ginalpioneerofALEwasTuomoSuntola,
whodemonstratedsomeofthefirstALEprocessesasearly
asAugust/September1974.
16
ThefirstALEsystemdevel-
opedwasZnS.
16
ThefirstALEpatentemergedin1977.
17
ThefirstliteraturepaperonALEappearedin1980inThin
SolidFilms.
18
ThefirstapplicationofALEwaselectrolu-
firstpublicdisplayofanALEdevice
wasanelectroluminescentdisplaythatoperatedinthe
firstcommercial
ALEreactorwastheF-120soldbyMicrochemistryin1988.
ThefirstofaseriesofALEmeetingswasheldin1990and
firstofaseriesofyearlyALD
meetingswasheldin2001andhascontinuedthroughthe
presentdate.
Manyearlierreviews
-21
haveaddressedthebasicsofALE
orALD.
5,8,11,12,19
Manypreviousreviewshaveconsidered
theapplicationofALE
27
orALDtomicroelectronicsand
nanotechnology.
19,22-
Theintentofthispresentreviewis
d,thisreview
isfocusedonanoverviewofkeyconceptsandnewdirections
iconductorroadmapiscomingtoanend
inafewyearsbecauseofthelimitsofthecurrentelectronic
tinuedprogress,thefutureforelectronic
materialswillembraceasyetundefil
almostcertainlybepartofthenewparadigmsbecauseofits
abilitytocontroldepositionontheatomicscaleandtodeposit
conformallyonveryhighaspectratiostructures.
2
O
3
ALDasaModelALDSystem
TheALDofAl
earlierextensive
2
O
3
hasdevelopedasamodelALDsystem.
AnreviewbyPuurunenhaspreviously
discussedthedetailsofAl
sectionwillonlymentionthe
2
O
highlights
3
ALD.
20
Consequently,this
ofAl
usuallyperformedusingtrimethylaluminum
2
O
ALDis
3
(TMA)
2
O
3
andH
2
firstreportsofAl
2
O
3
ALDusingTMAand
H
2
Odatebacktothelate1980sandearly1990s.
28,29
More
recentworkinthesemiconductorindustryisusingTMA
andozoneforAl
onAl
2
O
3
ALD.
30,31
Thisreviewwillconcentrate
2
O
3
ALDusingTMAandH
surfacechemistryduringAl
2
O.
The
2
O
3
ALDcanbedescribed
as
5,14,32
(A)AlOH*+Al(CH
3
)
3
fAlOAl(CH
3
)
2
*+CH
4
(1)
(B)AlCH
3
*+H
2
OfAlOH*+CH
4
(2)
growthoccursduringalternatingexposurestoTMA
2
O
ALD
3
andH
reactions
2
are
2
O
very
3
ALDisamodelsystembecausethesurface
effindriver
fortheefficientreactionsistheformationofaverystrong
rallreactionforAl
2
O
3
ALDis
2Al(CH
3
)
3
+3H
2
OfAl
2
O
3
+3CH
4
∆H)-376kcal(3)
AtomicLayerDeposition
onpathandpredictedenergeticsforreactionsof
Al(CH
3
)
3
ontheAl-OH*surfacesitecalculatedusingthe
Al(OAl(OH)
2
)
OH
2
-ucturesareshownusingthe
Al(OH
2
)-clusterforclarity.(Reprintedwithpermissionfrom
ght2002AmericanInstituteofPhysics.)
Thisreactionhasanextremelyhighreactionenthalpy.
33
This
isoneofthehighestreactionenthalpiesencounteredforany
ALDreaction.
ThepotentialenergysurfacesduringAl
2
O
densityfunctionaltheory(DFT).
3
ALD
34
have
beenmodeledusingThese
calculationsshowthatAl(CH
3
)
3
existsinadeepprecursor
wellcomplexedtoAlOH*speciespriortoitssurface
reaction,asshowninFigure2.
34
Likewise,thecalculations
showthatH
2
Oisalsoinadeepprecursorwellcomplexed
toAlCH
3
*
complexesresultfromstrongLewisacid-baseinteractions
ghtheseprecursorwellshavenotbeen
experimentallyobserved,theymaybefairlygeneralfor
variousclassesofALDreactions.
ThesurfacechemistryofAl
2
O
3
ALDhasbeenconfirmed
byinsituFTIRstudies.
32,35,36
TheFTIRdifferencespectra
clearlyshowthelossofAlOH*speciesandconcurrentgain
ofAlCH
3
*se,the
lossofAlCH
3
*speciesandtheconcurrentgainofAlOH*
speciesisobservedduringtheH
2
phase
reactionproductsduringAl
2
O
3
ALDhavealsobeen
37,38
identi-
fi
Al(CH
3
)
3
andD
2
Oasthereactants,CH
asexpected
3
Dwasobservedas
themainreactionproduct,fromthesurface
chemistryforAl
2
O
3
ALD.
37
Byrepeatingthesurfacereactions,Al
ABcycles.
2
O
3
14,39
growthis
extremelylinearwiththenumberofVarious
techniques,suchasspectroscopicellipsometryandquartz
crystalmicrobalance(QCM)measurements,havecharacter-
izedthegrowthpercycleduringAl
2
O
3
l
measured
14,39
Al
The
2
O
resulting
3
ALDgrowthratesare1.1-1.2ÅperAB
the
2
O
underlying
3
ALDfilmsaresmoothand
son
nanoparticlesshowexcellentconformalityofAl
films.
35,40,41
Investigationsonhighaspectratiotrench
2
O
3
ALD
sub-
stratesalsorevealsuperbconformality,asillustratedbythe
cross-sectionalscanningelectronmicroscopy(SEM)image
inFigure3.
42
OneofthehallmarksofALDisself-limitingsurface
f-limitingsurfacereactionsduringAl
2
O
ALDhavebeenobservedbyinsituFTIR
32,35
andQCM
39
3
investigations
14
aswellasbyspectroscopicellipsometry
ctantexposuresrequiredforthesurface
ChemicalReviews,2010,Vol.110,No.1113
-sectionalSEMimageofanAl
of300nmonaSiwaferwitha
2
O
trench
3
ALDfilmwith
athicknessstructure.
(ght1999JohnWiley
&Sons.)
reactionstoreachcompletionrevealthatthereactivesticking
coefficientsduringAl
2
O
3
ALDaremuchlessthanunity.
Basedonrequiredexposuretimes,thereactivesticking
coefficients
14
areintherangeof∼10
-3
-10
-4
duringAl
ALD.
2
O
3
ThegrowthperoneALDcycleisalsomuchsmallerthan
oneAl
2
O
3
“monolayer”.Thegrowthratesof1.1-1.2Åper
ABcyclecanbecomparedwiththethicknessofoneAl
“monolayer”.Thismonolayerthicknessisestimatedusing
2
O
3
thedensityof3.0g/cm
3
forAl
°
2
O
3
ALDfilmsgrownat177
units
C.
43
Basedonthisdensity,thenumberdensityof“Al
isF)1.77×10
22
Alnumber
2
O
3
”
2
O
3
units/cm
3
.The
6.8
of
Al
2
O
3
unitspersquarecentimeterisequaltoF
2/3
)×
10
14
F
-1/3
cm
-2
)3.8
.Likewise,
Å.Thegrowth
themonolayer
perABcycle
thickness
of1.1-
is
1.2
equal
Åper
to
ABcycleismuchlessthanthisestimateofthemonolayer
thickness.
ThedisagreementbetweengrowthperABcycleandthe
monolayerthicknessisnotsurprisingbecauseALDgrowth
surfacechemistryisnotrequiredtoalwaysyielda“mono-
layer”relation
betweenALDgrowthandsurfacechemistryisclearly
illustratedbythetemperature-dependenceofAl
wthperABcycle
2
O
decreases
3
ALD
progressivelywithtemperaturebetween177and300°
decreaseresultsfromtheprogressivelossofAlOH*and
AlCH
3
*surfacespeciesathighertemperatures.
14,32
Thecontinuousandpinhole-freenatureofAl
superbelectricalproperties.
2
O
isrevealedbytheir
3
ALD
films
Current-voltagecurvesforvariousAl
onn-Si(100)revealelectrical
2
O
3
ALDfilmthick-
nesses
7
behaviorthatisvery
similartothatofthermalSiO
2
fi
haveadielectricconstantof∼7anddisplayvery
2
O
3
ALDfilms
lowelectron
leakage.
7
Increasesinthecurrentdensityversusapplied
potentialoccurasaresultofFowler-Nordheimtunneling.
Thischaracteristicisconsistentwiththeabsenceofany
defectsorpinholesintheAl
Al
2
O
3
ALDfixcellent
propertieshaveenabled
2
O
3
ALDfilmstoserve
44-46
asgate
oxidesandtopassivatesemiconductorsurfaces.
landPlasmaorRadical-EnhancedALD
lALD
ALDiscloselyrelatedtochemicalvapordeposition
(CVD)basedonbinaryreactionssuchasA+BfProduct.
114ChemicalReviews,2010,Vol.110,No.1
ForCVDusingbinaryreactions,theAandBreactantsare
presentatthesametimeandformtheproductfilmcontinu-
,thesubstrateisexposedto
theAandBreactantsindividuallyandtheproductfilmis
ic
recipeforALDistofindaCVDprocessbasedonabinary
reactionandthentoapplytheAandBreactantsseparately
binaryreactionsequence.
TherearemanyexamplesofALDresultingfrombinary
esforTiO
binaryCVDreactions
2
andZnOare
basedonthefollowingandtheir
correspondingreactionenthalpies:
33
TiO
2
ALD:TiCl
4
+2H
2
OfTiO
2
+4HCl
∆H)-16kcal(4)
ZnOALD:Zn(CH
2
CH
3
)
2
+H
2
OfZnO+2C
2
H
6
∆H)-70kcal(5)
TheseALDsystemsyieldagrowthperABcycleof∼0.4Å
from150to600°CforTiO
2
ALD
47
and2.2-2.5Åfrom
100to160°CforZnOALD.
48,49
TheseALDchemistries
havenegativeheatsofreactionandarerobustALDreactions.
Thesereactionsoccurspontaneouslyatvarioustemperatures
andwillbereferredtoasthermalbecausetheycanbe
performedwithouttheaidofplasmaorradicalassistance.
AsurveyofdevelopedALDprocessesrevealsthatmost
thermalALDsystemsarebinarycompoundsbasedonbinary
reactantCVD.
20,21
ThemostcommonthermalALDsystems
arebinarymetaloxidessuchasAl
2
O
3
,TiO
commonthermalALD
2
,ZnO,ZrO
systemsare
2
,
HfO
binary
2
,andTa
metal
2
O
nitrides
5
.Other
suchasTiN,TaN,andW
systemsalsoexistforsulfidessuchasZnS
2
l
ALDandCdS
andphosphidessuchasGaPandInP.
orRadical-EnhancedALD
Thereisalsoaneedforsingle-elementALDmaterials,
suchasmetalsandsemiconductors,thatcanbedeposited
forsomenotable
exceptionsdiscussedinsection5,thesingle-elementfilms
ofmetalsandsemiconductorsareverydifficulttodeposit
ately,thesesingle-
elementscanbedepositedusingplasmaorradical-enhanced
ALD.
22
Theradicalsorotherenergeticspeciesintheplasma
helptoinducereactionsthatarenotpossibleusingjust
sourcescanbeusedtogenerate
hydrogenradicalsthatreducethemetalorsemiconductor
enradicalscanalsobeproducedusinga
hottungstenfieformetalALDusingmetal
reactantsandhydrogenradicalsisshowninFigure4.
Hydrogenradical-enhancedALDwasfirstdemonstrated
forTiALD
50
usingaH
2
sanotherALD
systemthathasbeenstudied
51
extensivelyusinghydrogen
radicalsfromH
2
ctantsforTaALDare
TaCl
ALD
5
andhydrogenradicals.
51
Thesurfacechemistryfor
Tacanbeexpressedas
(A)Ta*+TaCl
5
fTaTaCl
5
*(6)
(B)TaCl
5
*+5H·fTa*+5HCl(7)
TaCl
5
isfiuently,the
hydrogenradicalsreducetheTaatomsandremovethe
ghthegrowthpercycle
George
ticdiagramofhydrogenradical-enhancedALD
usingametalreactantandhydrogenradicals.
duringTaALDisonly0.08ÅperABcycle,theTaALD
filmshaveexcellentfilmresistivitiesandshowgoodCu
barrierproperties.
51
Thesmallgrowthpercycleisattributed
tosterichindrancecausedbythelargeTaCl
XRDalsoindicatesthattheTa
5
admolecule
filmis
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想要u盘重装系统的话,就需要先制作u盘启动盘.那么如何制作u盘启动盘呢?我们可以借助一些工具实现,比如说黑鲨装机大师工具.下面小编就教下大家. 1.插入U盘,然后打开黑鲨装机大师,在“U盘启动”的选项下,点击进入“U盘模
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