Ultra-high strain in epitaxial silicon carbide nanostructures utilizing residual stress amplification

0.49 MB·

by  Hoang-Phuong Phan

Ultra-highstrainin epitaxialsiliconcarbidenanostructuresutilizingresidualstress
amplification
Hoang-PhuongPhan,∗,† Tuan-KhoaNguyen,†ToanDinh,†InaGinnosuke,‡AtiehRanjbarKermany,†
AfzaalQamar,† JishengHan,†TakahiroNamazu,¶MaedaRyutaro,§DzungVietDao,†andNam-Trung
Nguyen†
7
1
QueenslandMicroandNanotechnologyCentre,GriffithUniversity,Queensland,Australia,DepartmentofMechanical
0
Engineering,UniversityofHyogo,Hyogo,Japan,DepartmentofMechanicalEngineering,AichiInstituteofTechnology,
2
Toyota,Japan,andNationalInstituteofAdvancedIndustrialScienceandTechnology(AIST),Tsukuba,Ibaraki,Japan

n ReceivedJanuary12,2017;E-mail:hoangphuong.phan@griffithuni.edu.au
a
J

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Abstract: Strainengineering hasattractedgreatattention,particularlyforepitaxialfilmsgrownonadifferentsubstrate. Residualstrainsof

] SiChavebeenwidelyemployed toformultra-high frequency and highQfactorresonators. However, todatethehighest residual strainof
i
c SiCwasreportedtobelimitedtoapproximately0.6%. LargestrainsinducedintoSiCcouldleadtoseveralinterestingphysicalphenomena,
s
aswellassignificantimprovement ofresonant frequencies. Wereportanunprecedented nanostrain-amplifierstructurewithanunltra-high
-
l residualstrainupto8%utilizingthenaturalresidualstressbetweenepitaxial3CSiCandSi. Inaddition,theappliedstraincanbetunedby
r
t changingthedimensionsoftheamplifierstructure.Thepossibilityofintroducingsuchacontrollableandultra-highstrainwillopenthedoorto
m
investigatingthephysicsofSiCinlargestrainregimes,andthedevelopmentofultrasensitivemechanicalsensors.
. Keyword:SiliconCarbide,ResidualStress,Ultra-highStrain,HighFrequency
t
a
m
- Strain engineering plays an important role in electronic de- strain, the higher resonant frequency can be achieved. In addi-
d
vices.1,2Forinstance,incomplementarymetaloxidesemiconduc- tion, largestrainsupto10%couldalsoleadtoseveral significant
n
tor (CMOS) technology, scaling down the device to sub 100 nm changesinelectrical/opticalproperties,whichhavebeenobserved
o
c regimeencountersseveralchallengesduetothedegradationofcar- inseveralmaterials.31,32Alargestresscouldalsocauseunintended
[ riermobility.3,4ToenhancetheperformanceofsiliconCMOSwith propertiessuchaswaferbowandcracks,makingtherealizationof

shrinkingsize,theintroductionofstrainintoSichannelhasbeena ultra-high strainin SiCan challenging issue. Therefore, tomake
1 keyconcept tocompensate thedecreaseincarriermobility.5–7 In extremelyhighstraininSiCpossible,itisimportanttolocallyam-
v
addition, micro/nano electromechanical systems (MEMS/NEMS) plifystraininaspecificarea,whilekeepingthestraininthewhole
1
have also benefited from strain engineering where the residual filminarelativelysmallregime.
9
7 strainwasapplied betweenepilayers toenhance the resonant fre- We propose here a novel approach to induce extremely high
2 quency(f)andthequality(Q)factorfollowingEuler-Bernoullithe- strainintoSiC by using a nano strain-amplifier. For the proof of
0 ory.8 concept, we demonstrate the feasibility of introducing a strain of
. Siliconcarbide, awideband gapmaterial, hasshowed itshigh approximately 8% into a SiC nano-spring structures, which is to
1
potential in MEMS/NEMS applications.9,10 The large band gap the best of our knowledge at least one order of magnitude larger
0
7 makesSiCanexcellentcandidateforhightemperatureelectronics thanthatreportedintheliterature.Thepossibilityofinducingsuch
1 applicationswhereSihaslimitation. ThelargeYoungâA˘Z´smod- a high strain will pave the path for experimental investigation of
: ulus of above 300 GPaoffersSiC resonators higher resonant fre- thephysicsofSiCinhighstrainregimesaswellasforthedevel-
v quenciesincomparisontoSibasedcounterparts.11,12Otherphysi- opmentofhighlysensitiveSiCsensors. Ourmethodology should
i
X calpropertiessuchasthepiezoresistiveeffectandthethermoresis- also be applicable for not only SiC but other materials including
tiveeffectinSiChavealsobeenemployedtodevelopmechanical grapheneandtransitionmetaldichalcogenides(TMD),wherehigh
r
a andthermal sensorsforstructural healthmonitoring(SHM).13–20 strainregimesareofsignificantinterest.
CubicSiC(3C-SiC)istheonlypolytype,amongover200SiCpoly- Figure 1(a) illustrates the basic concept to induce large strain
types,thatcanbegrown(epitaxially)onSisubstrateandthusisthe intoSiCdevices.Thenanostrain-amplifierconsistsofaSiCmicro
mostsuitablepolytypeforMEMS/NEMSapplications.9,21Thisal- bridgewhich isreleased fromaSisubstrate, andamodified area
lowsthereductionofSiC/Siwafercostaswellasmakesitcompat- whichislocatedatthecentreofthebridge. Inaddition,themod-
iblewiththeconventionalmicromachiningprocessthatdeveloped ifiedarea isdesigned to exhibit a smaller stiffness incomparison
forSi. TheepitaxialgrowthofSiConSifurtherresultsinalarge totheremainingareasof theSiCbridge. Tosoftenthismodified
residualstresswithintheSiCfilmduetothelatticeandthermalmis- area, thefollowingtechniques canbeutilized. First,thewidthof
matchesbetweentheSiCfilmandtheSisubstrate.22Thisresidual themiddleareacanbeshrunkdowntonanometerscalesothatthe
stresscan be potentially applied to enhance the f×Q of theres- ratioofthestiffnessbetweenthenanowireandmicro-frameissig-
onators. Resonatorswithhighfrequenciesuptoseveral GHzand nificantlydiminished. Second,themiddlesectioncanbesoftened
f×Qfactorsupto1011havebeendevelopedthroughtheapplica- by modifying itsstructure; as such a nano-spring can offer much
tionofresidualstress.22–24 larger elongation than that of a nano rod with the same dimen-
Inmostpreviousstudies,themaximumstraininducedintoSiC sion. Furthermore,bychangingmaterialfromsingle-crystallineto
rangedfrom0.1%to0.6%.27–30 Itshouldbenotedthatthelarger amorphous,itisalsopossibletotunethestiffnessofaspecificre-
1
(b) Stress relaxation
(a) Concept
(i) low dimension
Shrink
σ Stiff areas Soft area σ
r r
(i) structure modification
σr Area of interest Strain ε1
+
(iii) material modification (c) Stress gradient Bending moment
Strain
M M
σ Strain ε2
r
ε =ε +ε
1 2
Figure1. (a)Conceptofdevicestoinducelargestrainintointerestedarea;(b)(c)Principleofthenanostrain-amplifierbasedonplanarresidualstressand
stressgradient(side-viewsketch).
gion.25,26 Inthesubsequent experiment,weselectedthestructure a tensile stress in the epitaxial 3C-SiC film. The average tensile
modificationapproachtoformthesoftarea,asitcanprovidelarge strain (er) in the SiC film can be quantified using the coefficient
elongationwhicheasesthestrainobservationusingscanningelec- reportedbyRohmfeldetal.:27
tronmicroscopy(SEM). w
The key factor of our structure is that the low stiffness of the cmT−O1 =(795.9±0.1)−(1125±20)er (1)
modified nano-area allows it tofollow the deformation of the se-
Consequently,theaveragestraininducedintotheas-depositedSiC
riallyconnectedmicrostructures. As3C-SiChasasmallerlattice
filmisapproximately 0.16%to0.2%, whichisinthesamerange
sizethanSi,theSiCfilmtypicallyundergoesaconsiderabletensile
withotherepitaxial3C-SiCfilmreportedpreviously.Once,theSiC
stress when being epitaxially grown on the Si substrate. When a
bridgeissuspended,theresidualstressisreleasedandSiCtendsto
SiCbridgeisreleased,itslacticconstanttendstoreturntoitsorig-
returntoitsfree-stressstate.Furthermore,astheSiCmicroframes
inal size, which subsequently shrinks the size of the bridge. Be-
aremuchharderthanthenano-spring(orothernanostructures)lo-
causethisphenomenon ismoredominant intheSiCmicro-areas,
catedatthecentre,theshrinkoftheseframesaremuchmoredom-
thenano-arewillbestressedfollowingthemotionofthesemicro-
inant. Assumingthatthemicroframescompletelyshrinkdownto
area,Fig. 1(b). Furthermore,inaepitaxialfilm,largestressestyp- theirstrain-freestate,thestraininducedintothenano-spring(ens)
icallydistributenear theinterface between toplayer andthe sub-
canbeapproximatedusingthefollowingequation:
strate. Theresidualstressgraduallydecreaseswithincreasingfilm
L
thicknessorevenrelaxforsufficientlythickfilms.Thisvariationof ens= f er (2)
theresidualstresswillcauseastressgradientalongthethicknessdi- Lns
mension,resultinginabendingmomentoncethefilmissuspended whereLf andLns arethelengthoftheframeandthenano-spring,
fromthesubstrate. Therefore,undertheresidualbendingmoment, respectively.
themicro-frameswilldeflectvertically,leadingtoanelongationin Additionally,thequalityoftheSiCfilmwascharacterizedusing
the softened nano-area, Fig. 1(c). Combining the two phenom- transmissionelectronmicroscopy(TEM).TheTEMimageshown
enaofin-planeshrinkingandout-of-planedeflection,anultra-high inFig.2(c)indicatesahighdensityofdefectsnear theSiC/Siin-
strainisexpectedtoinduceintotheSiCnanostructures. terface. Mostdefectswerefoundtobethestackingfaultsin[111]
TheSiCfilmwaspreparedonaSi(100)waferusinglowpres- crystallographyorientationduetothelatticemismatchbetweenSiC
sure chemical vapor deposition (CVD) where silane (SiH4) and andSi. QualityoftheSiCfilmincreasesevidentlywithincreasing
propylene (C H ) were employed as the precursors.35 As afore- filmthickness,exhibitinglesscrystaldefectonthetoplayers.This
3 6
mentioned,SiCandSihassignificantlatticeandthermalexpansion observation also indicates a stress gradient through out the film.
mismatchof∼20%and∼8%respectively,thegrowntemperature Assuchinourpreviousreport,alargestresswasmeasuredatthe
◦
waskeptat1000 Cutilizingalternatingsupplyepitaxy(ASE)ap- bottomlayersof3C-SiC(100)films,whilethestressdecreasedor
proach. X-RayDiffraction(XRD)methodwasutilizedtoinvesti- relaxedatlayersnearthetopsurface.34 Thebendingmomentex-
gatethecrystallinityoftheSiCfilm. Figure2(a)showsdiffraction erted on SiC can be estimated from the Young’s modulus of SiC
◦ ◦
peaksat35.6 and90 ,correspondingto3C-SiC(200)and3C-SiC and the deflection of free standing SiC cantilevers. Accordingly,
(400)orientations.Inaddition,besidesthesetwopeaks,onlyapeak thedeflection(d )ofasuspendedSiCcantileverisgivenby:
◦
at69.1 wasobserved,correspondingtoSi(400). Thisresultindi-
Ml2
catedthatsinglecrystalline(100)3C-SiCwassuccessfullygrown d = (3)
2EI
onaSisubstrate. Thethicknessofthefilmswasfoundtobe294
where M is the bending moment; and l, E and I are the length,
nmusingNANOMETRICSNanospec/AFT210.
Young’smodulus,andmomentofinertiaoftheSiCcantilever. As
The Raman scattering measurement was performed using
TMRenishaw inVia Raman microscope 514 nm, Fig .2(b). The a result, the bending moment caused by stress gradient is M =
peak observed at 794 cm−1 corresponds to the transverse optical 2EId /l2. Figure3showsalargeout-of-planedeflectionofaSiC
cantileverduetoresidualstressgradientobservedinaFocusedIon
(TO)vibrationof3C-SiC.OurTOpeakwasrelativelysmallerthan
◦
that of free-stress 3C-SiC which was reported to be 795.9 cm−1. Beam(FIB)equipment withatiltangleof 60 . Fromthedeflec-
tionof24m m,thedimensionofthecantileverof200m m×5m m
Therefore, theleftshift of theTOpeakindicates theexistenceof
×0.3m m,andtheSiCYoung’smodulusof350GPa,thebending
2
(a) (b) (c)
1800
Si(400) LO SiC
1400
]
u. 3C-SiC(200)
y [a. ount1000 TO
Intensit 3(C4-0S0i)C C600 [1c1k1i] ng faults
a
st
Si
200
30 50 70 90 700 800 900 1000 1100
200 nm
2θ [degree] Raman shift [cm-1]
Figure2. PropertiesoftheSiCfilms.(a)X-RayDiffraction;(b)Ramanspectroscopy;(c)Transmissionelectronmicroscopy.
momentisestimatedtobe5m N.m m. Consequently,thisrelatively almostflatshape,indicatingauniformstraincontributingalongits
largebendingmomentexcretedonthemicroframesinnanostrain- longitudinaldirection. Figure5(b)presentstheSEMimageofthe
amplifierwillcausealargeverticaldisplacement,andthusresults nano-spring afterremovingthesupporting wires. Themicrocan-
inalargetensilestraininthebridgingnano-spring. tileversoneach sideof thebridgeweredeflectedvertically, lead-
Figure4showsthefabricationprocessoftheproposeddevices. ing to a large displacement in the nano-spring. Furthermore, the
Fortheproofofconceptweusedaspringstructuresinceitoffers cantileverswere bent downward, indicating that alargecompres-
alowerspringconstantincomparisontonanowireswiththesame sivestressdistributedatthebottomlayerwithrespecttothatofthe
width and thickness. The use of long SiC springs also allows a toplayers. ThisresultisingoodagreementwithTEMobservation
directmeasurementofstrainusingatypicalSEM. mentioned above. Interestingly, because thetwocantilevers were
Initially,siliconcarbidemicrostructureswerepatternedusingin- deflected at almost thesame degree, thenano-spring remained in
ductivecoupledplasmaetching(HCl+O )withanetchingrateof thelateral plane. Consequently thelengthof thenano-spring can
2
approximately100nm/min(step1).36 TheSiCbridgeswerethen beaccuratelymeasuredfromthetopviewSEMimage,asshownin
released from the substrate by under-etching Si using TMAH at Figure5(d).
◦
90 Cforapproximately1hour(step2). Thewidthofthebridges Figure6plotsthestraininSiCnano-springsagainsttheratiobe-
was fixed at 5 m m, while their length was varied from 100 m m tweenthelengthofthenano-springtothatofthesuspendedbridge
to500m m. Consequently, SiCnano-springsandsupportingwires (Lns/Lf). A strain of 7.6% in the SiC nano-spring was observed
were then formed at the middle of the bridge using focused ion when Lns/Lf) was 0.055, which is to the best of our knowledge
beam(Ga+)(step3).37Thelengthofthespringwasapproximately the largest strain reported in SiC so far. Additionally, increasing
27.71m m,andthecross-sectionalareawasapproximately294nm the Lns/Ls results in a decrease in the applied strain, which is in
×300nm.Finally,thesupportingwireswasremovedbyFIB(step solidagreementwithEq.??andEq.??.Moreimportantly,thede-
3),releasingthenano-spring. pendenceofthestrainofthenano-springonLns/Lf indicatesthat
Figure 5(a) shows the SEM image of suspended SiC bridges ultra-highstrainiscontrollablebychangingthedevicedimensions.
prior toreleasingthenano-spring. Evidently, thebridgeswerein Thiscouldbeappliedtotunetheresonant frequencyinSiCnano
resonators.
Anotherinterestingpropertyinournano-strainamplifieristhat
thestrainwasonlyconcentratedinthelocallyformednano-spring,
(1) (2)
(3) (4)
FIB Remove
Supporting-wires Supporting-wires
FIB
Figure3. Observationoftheout-of-planedeflectioninareleased3C-SiC
cantileverduetoresidualstressgradient(fallcolor). Figure4. Fabricationprocessofthenanostrainamplifier.
3
Figure5. ColorizedSEMimagesofSiCnano-springs.(a)SuspendedSiCbridgewithnano-springfabricatedatthecenter(priortoremovingthesupporting
wires);(b)SiCnano-springsaftercuttingthesupportingwires;(c)Deflectionofmicroframe(orcantilever)oneachside;(d)Theelongationofthenano-spring
observedfromthetopview.
whilethemicroframe(i.e. theSiCcantileveroneachsideofthe structure can be applied to locally induce extremely high strain
bridge)canbealmostfreelydeformedreleasingtheresidualstress. into 2D materials such as graphene or transition metal dichalco-
Itmeansthatthestraincanbeamplifiedatinterestedarea,whilea genide,wheretheVanderWallsadhesionforcebetweenthemand
small strain is maintained at other area. Therefore, the proposed thesubstrate(e.g. Si,PDMS,glass)typicallycannotwithstand1%
strain.38–41
Inconclusion,thisworkpresentsanovelmechanicalapproachto
8 applyextremelylargestraintoSiCutilizingananostrain-amplifier
Measured data andtheresidualstress.Wesuccessfullydemonstratedanextremely
high strain up to nearly 8% in a SiC nano-spring structure. The
7 Fit line
%] proposedplatformshowsitspotentialforfurtherinvestigationsinto
g [ the physics of SiC nano structures in high strain regimes, along
n 6 withthedevelopment ofhighfrequency, highQfactor, andultra-
ri
p sensitiveSiCmechanicalsensors.
s
o
n
na 5 L
Strain of 4 Lf =100 to 500 nμs = 27.7 μm Acknowledgment
m
This work was performed in part at the Queensland node of the
3 Australian National Fabrication Facility, a company established
0.05 0.1 0.15 0.2 0.25 0.3 under theNational Collaborative ResearchInfrastructureStrategy
Length of nanospring/Length of frame (L /L [-]) toprovidenanoandmicro-fabricationfacilitiesforAustralia’sre-
ns f
searchers.
Figure6. StraininSiCnano-springswithdifferentLns/Lf ratios. Forthe
sameLns,increasingthelengthoftheSiCbridgeLf leadstoanincreasein
thestrainofthenano-spring.
4
(22) Huang,X.M.H.,Zorman,C.A.,Mehregany,M.,Roukes,M.L.Nano-
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