Electronprobemicroanalysis

Variable
Pressure/
Environmental
SEMOperation
Revised22112

Whatsthepoint?
TraditionalSEMsandmicroprobesoperateathighvacuum.
Today,howevermany/mostSEMsbeingsoldareversatilein
beingabletooperatebothathighvacuum,andalower
vacuum,whereanygasincludingwatervapormaybepresent.
Thispresentsnewopportunitiesforexaminingspecimensthat
otherwisewouldbedifficulttoexamine.
HOWEVER,thereareseriousdifficultieswhenattempting
touseEDSinthevariablepressuremode.

Nottobelaborthepoint
But
Comparedtoelectronprobes,SEMsareveryeasytouse
.Whichmeansthatpeoplewillstickanythingand
everythingintothem!
.Andpeoplewithlittleornotrainingwillpushbuttons
togeneratedata(=EDS)whichtheyhavenobusiness
doing!
Andpossiblygeneratingdatathatisnotcorrect.

Vacuum
TraditionalSEMsandelectronprobeshaveoperatedwith
vacuumsintherangeof103Pa(105Torr).
Thiswasforseveralreasons:
protectingtheelectrongun(subjecttooxidationandruin)
keepingthebeamofelectronstighttoreachgoodspatial
resolution(thegasmoleculeswouldinteractandcause
scatteringbothelasticandinelastic)

Whyuseapoorervacuum?
Sometimesyouwanttolookatthingsthatarenaturally
moistorwetbiologicalspecimensorclaysandunder
thenormalhighvacuumSEMtheybecomedriedoutand
loseimportantfeaturesyouwanttoviewanddocument.
Therehasbeenanexperimentalundercurrentfrom1960,
attemptingtoimagewetmaterial,bymodifyinginan
SEM,and
sandwichingtheliquidbetween2thincarbonfilm,or
usingaspecialsubstage,aclosedboxenclosingthe
sampleandBSEdetector,withatinyapertureforthe
electronbeamtoenter,andavalvewherewatercouldbe
leakedin

Anotherbenefitofpoorervacuum
OnecriticalfeatureofhighvacuumSEMandEPMAwas
thatsampleseitherhadtobeconductiveorconductively
coated.
However,ifthereisapoorervacuum,thereareenoughgas
moleculesinthechamberthatinteractwithbothincident
electronsand(mainly)emergingbackscatteredand
secondaryelectrons,thatbecomeionized,andproducea
cloudofcationsthatneutralizeanycharging(bleedthe
electronstotheground).
Thus,havingapoorervacuumcanbecomeatoolto
examineinsulatingspecimensthoughtherearesome
seriousdrawbacksregardingEDS.

VPSEMandESEM
TodaytherearetwodistinctvarietiesofSEMoperatingin
thismanner:
theEnvironmentalSEM(trademarkofPhilips/FEI/
Electroscan),whichcanoperateupto2700Painchamber
andhasaproprietysecondaryelectrondetector.Formany
yearsitwastheonlyonethatcouldoperatewithliquidwater
stable.
thevariablepressureSEMsoldbytheotherSEM
companies,whicharelimitedtoamaximumpressureof
~266Paandmaynothaveaspecialsecondaryelectron
detector(insteadusingBSEdetector).
ButBOTHhavesamegeneralfeaturesforthemostpart.

Theskirtanditsimportance

Newbury,2002

InatraditionalSEM,100%oftheincidentelectronslandata
verytinyspot.ButwithVPSEM,theyscatterastheycome
downandcreateawidecircularregioncalledtheskirt

Theskirtanditsimportance

Newbury,2002

Forimaging,theskirtactsasasourceofnoiseanddegrades
slightlytheimagenotabigproblem
However,forXraymicroanalysis(EDS),thereare
significantproblemsbecausespuriousxrayscaneasilybe
generateduptotenstohundredsofmicronsaway,depending
onthegaspressureabigproblemasdiscussedbyDale
Newburyinhis2002article

Theskirt
Thisimageshows
graphicallytheskirtin
theformofluminescent
gasinsideaVPSEM.The
upperimageiscross
sectionalview,whereas
thebottomislooking
normaltothebeam.Note
thesmallverybright
centerspot,a~75um
brightdiameterhalo,and
a~250umdimmerhalo.

Goldsteinetal,2003

Theskirt
Analogy(bottomimage):
Youareonafoggyroad
andlookingatthebeam
ofanoncomingcar
headlight,diffused/
scatteredthruthefog.
Nowconsideryourself
thespecimenandthe
lightcomingatyouisthe
packageofelectrons
comingdownthecolumn
atyou
Goldsteinetal,2003

Theskirt
Theskirtisextremelyimportanttounderstand;itsradiusr s
canbeestimatedfromasimpleanalyticalmodel
(Danilatos,1988):

364Z
p
3/2
rs

GPL
E
T

whereGPListhegaspathlength(=workingdistance)in
meters;pispressureinPa;TisindegreesK,Zis
atomicnumberofgas,andEisE0involts.
rsisinmeters

Theskirt

Fig5.20.Plotofbeambroadening
(skirtradius)asfunctionofgas
speciesandpressure.Thegaspath
lengthis5mmandbeamenergyis
20keV

Fig5.21.Plotofbeambroadening
(skirtradius)asfunctionofgas
pathlength(GPL)andbeam
energyinhelium.
Goldsteinetal(2003)

EDSerrorsduetotheskirt1

ConsiderastandardblockwithFemetalinabrassholderandapieceof
Zrnearby(aboveleftimage).Undernormalhighvacuum,ifthe20kV
electronbeamisfocusedontheFeabout50micronsinfromtheedge,
theEDSpatternisasexpected(aboveright),showingessentiallyonlyFe
KaKbandFeLa
Goldsteinetal2003,Fig5.22

EDSerrorsduetotheskirt2

Nowbleedin20Paofair(aboveleft)andeventhoughwehavent
movedthebeam,wearenowseeingCuandZnfromthebrassholderin
theEDSspectrum.
Increasegas(air)pressureto50110PaandwenowseealsotheZrLa
fromtheZrmetal500micronsaway!
Goldsteinetal2003,Fig5.22

DetectorsforVPSEMESEM
Havinggaspresentinsidethevacuumchamberpresentsa
majorproblemforthetraditionalET(EverhartThornley)SE
detector.Thatdetectorhasahigh(e.g.+10kV)biasonit,and
wouldimmediatelyarcover,blowingoutafuse(ifyouare
lucky).
SoaVPSEMESEMcaninsteaduseitsBSEdetectorwithout
thatproblembuttheimageissomewhatwashedout.OK
butnotgreat,asthefinedetailofthesurfaceismuted.

DetectorsforVPSEMESEM
Goldsteinetal,2003

Abetterdetectorisabove,wherethecollisionsoftheemitted
secondary(andbackscattered)electronswiththegasmoleculesis
usedadvantageously,producinganavalancheeffect(=gas
amplification)withelectronsbeingattractedtoa+biaselectrode.
Thisyieldsasecondaryelectronimage.Thedetectoriscalleda
GSEDorESED.

ESEDDetectorforHitachiVPSEM1
BSE

In2007,weupgradedourSEM
toa2ndgenerationHitachi
EnvironmentSecondary
ElectronDetector(ESED)and
havedifferent/improvedimages
acquiredinVPSEMmode.

ESED

BSE:little/noshadowing,canlosetopo
ESED:directional(shadowing),topoenhanced

ESEDDetectorforHitachiVPSEM2

Toimprovetheimage,youcanmodifyyourconditions:
Lowervoltage(droppedfrom15to5keV)
Dropthestage(=increasetheworkingdistance)from
10mmto25mm,togiveagreaterdepthoffield
Increasethegaspressurefrom25to40Pa

WetSamples
InnormalhighvacSEM,
waterpresentatlow
pressureandroomT(*)is
stronglyoutofequilibrium
andwillevaporate(andbe
pumpedout)quickly.
However,foratrue
ESEM,youcansetthe
pressureto2600Pa(@)
andstabilizeliquidwater
inyoursample,sothereis
noevaporationandchange
inthematerialsproperties
orfeaturesyouare
imaging.

*
However,aVPSEM(likeourHitachi)
cannotreach2600Pa,sotheonly
alternativewouldbetoinstallacold
stagethatwouldkeepliquidwatermeta
stably,slowingtheevaporation(<)

Particles!
WhilewerediscussingHitachiSEMoperation,itis
importanttopointoutamajordifferencewiththe
electronprobe
Intheeprobeweexamineflatpolishedsamples
becausetheymustbe,sothereisconstantpathlengthfor
theabsorptioncorrection.
ButtheSEMissoflexibleyoucanputanythinginit,
e.g.lotsofparticlesofdifferentsizesandshapes
Q:Whatwouldbetheeffectonthepathlengthfora
jaggedhomogenousparticle?
A:Youwouldgetdifferentcompositionsdepending
uponwhereyouputthebeam.Lightelementswouldbe
particularlyabsorbedandincorrect.

LowVoltage
Whereimagingisconcerned,sometimesitpaysto
experimentwithE0WHY?
Theissueisspatialresolution.Recallthattheelectrons
scatter,andwithhigherE0,theyhavemoreenergyandwill
scatterfurtherfromthelandingpoint.
Itisthusabalancingactbetweenhavingadetectorthatis
sensitivetolowenergyelectrons(BSEdetector,right?)and
enoughE0togiveastrongenoughsignaltogiveagood
enoughimage
(Alongsimilarlines,loweringthebeamcurrentalsohelpsto
givelessbeamelectronscatteringbutthesignalwillbe
weaker.)
ButloweringE0ofcoursecreatescomplicationswithEDS

VPSEMApplicationsinWeeksHall
Imagingforams,somewhichmayhavecarbonisotope
measurements(ClayKellygroup)
ImagingZebramusselspriortocarbonisotopeanalysis
(DanaGearygroup)
Evaluatingsyntheticnanoparticles(sizemainly)(Nita
Sahaigroup)
locatingKfeldsparsinapopulationofgrainson
carbontape,forArArdating(BradSingergroup)
EBSD(needtheretobenocoatingonsurfacefor
optimalsignals)(LaurelGoodwinandBasilTikoff
groups)

VPSEMApplicationsinWeeksHall
Rapididentificationofmineralsinuncoatedmounts
(everyone!)
Imagingslightlywetsamples:faultgaugefromunderwater
zone,fromCalifornia(LaurelGoodwingroup)
Imagingshearedsedimentsamples(HaroldTobingroup)
Imagingverywetsamples:microbialcultures(EricRoden
group)wouldneedacoldstagetodothis

OperationalIssues
Usetheleastamountofairyoucangetawaywith;startwith
~2025Pabutincreaseifstillhavecharging;ifusingESED
detector,experimentwithhigherpressures
Haveexposedtheleastamountofnonconductivesurface,
especiallyglass;surroundareaofinterestwithconductivetape
ifatallpossible.Givetheelectronsaneasypath!
BeverywaryofEDSdataacquiredonparticles,and
particularlyinVPmode!Onlyconsidersuchdatatobevery
qualitative.Ifyouwishtobemorequantitative,youMUST
acquirestandardsofknowncompositionsimilartothe
unknownsandspendtimestudyingthemFIRST.

ThankstoKenSeverin,UAFprobe&SEMlabs