JEOL FX.docx

JEOL FX.docx

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JEOLFX

JEOL2000FX

WiththankstoProfessorJohnF.MansfieldfromtheUniversityofMichiganuponwhoprovidedthehandbookuponwhichtheseinstructionsarebased.

Preamble

1.Notethatthemicroscopeisastate-of-the-artresearchinstrumentandshouldbetreatedwithgreatcarebecausealargenumberofpeoplerelyonitfortheirday-to-daywork.

2.Withtheabovecommentinmind,beforeyoudoanythingtothemicroscope,i.e.insertorwithdrawaspecimenordetector,THINKanddeterminewhetheryouractionisliabletocompromiseanyofthefunctionsoraccessoriesofthemicroscope.

3.Intheinstructionsthatfollowyoushouldmonitorthevacuumstatusoftheinstrumentontheion-gaugemeterand/orthePenninggaugewhileyouareperforminganyactionthatmaychangethelevelofvacuuminsidethemicroscope.Ifthevacuumchangesradicallyandabnormallywhenyoustarttodosomething,STOPandreverseyouractions,waitforthevacuumtorecoveranddeterminewhythereisaproblem.ThiswillusuallyinvolveconsultingGabriellaChapman,JohnLynchorRonDoole.Donothesitatetocontactoneofthemifyouareunsureofwhattodoinanyparticularsituation.

StartingUp

∙CheckvacuumItshouldbelessthan10x10-5Paontheion-pumppowersupplybehindthemicroscope.

∙Ifyouwishtousetheanti–contaminationdevicepleaseseeGabriellaChapmanorJohnLynchforinstruction.Atpresentthemicroscoperequiresamodificationbeforeitcanbeused.

∙Loadyourspecimen,

-Putonsomegloves.

Tolimitunwantedcontaminantsinthespecimenenvironmentofthemicroscope,alwaysweargloveswhenhandlingthespecimenholders,donottouchanypartofthemetalrodoftheholderwithyourbarehands.Althoughonlypartoftherodactuallyentersthevacuumofthemicroscope,greaseandothercontaminantsfromyourhands（ifyoudonotweargloves）maybetransferredalongthespecimenrodtothesectionthatisinsertedintothevacuumsystem.

-ZerotheX,Ytilts.ZerotheX,Yspecimenposition.Lockgoniometer.Makesurethefilamentisoffandalldetectorsarefullyretracted.

-Removethespecimenholderfromthemicroscope.Pulltheholderoutuntilitstops,rotateanticlockwiseandeaseout.

-Turnthesampleholderupsidedownandtapgentlyonthebackend（awayfromthesample）tomakesureyoursamplewillnotfalloutinthemicroscope.

-Alwaysinspecttheo-ringbeforeinsertingtheholderintothemicroscope,astheytendtopickuphairs,dust,etc.Wipewithaglovedfinger.Donotgreasethespecimenholdero-ringswithoutfirstconsultingGabriellaChapmanorJohnLynch.

-Insertthespecimenholderstraightintothemicroscopewithoutturningit.（Ifyouturntheholderyouwillallowairintothecolumn）.Itshouldtriggeramicroswitchthatstartsthepumpdowncycle.Youmayhavetopushtheholderagainstthemicroswitchtotriggerit（don’tturntheholder!

!

）.

-Pumpforaminimumofthreecyclesandamaximumoffivebeforeinserting.YouMUSTwaitforthreecycles!

Donotinsertsampleholderiftheredlightison.Thesecyclesmaytakelongerifthefilmhasjustbeenchanged.Inserttherodbyrotatingclockwiseandallowthevacuumtopulltheholderin-donotreleaseituntilitisallthewayintothemicroscope.

-Ifthevacuumdoesnotrecoverwithinashorttime,checktoseeifthefilmwaschangedinthelasthour.Ifnot,theholdero-ringmaybedirty,removetheholderandcleantheo-ringwithalintfreewipe.

∙TurninguptheHT

BeforeswitchingontheHTcheckthevacuumislessthan10x10-5Pa.

StarttheHTat160kV.

TheHTmaybechangedwiththewhiterockerswitch,whichisabovetheHTon/offswitch.TheamountbywhichtheHTchangeseachtimeyouclicktherockerswitchmaybesetonthekeyboard.Type‘HT’andthentherequiredstepsize（e.g.05）onthekeyboard.Thesizeisdisplayedonthebottomlineofthedisplayasyoutype.AfterturningtheHTonat160kV,setthestepsizeto5kVandbringthevoltageupto190kV.Waitacoupleofsecondsaftereach5kVclicktoensurethevacuumreadingontheion-gaugedoesnotrise.At190kVchangethestepsizeto1kV,andcontinuetoraisethevoltageto200kV,checkingthatthevacuumlevelinthecolumndoesnotchangesignificantly.Ifthevacuumdoeschange,waitforittorecoverbeforeincreasingthevoltagefurther.Ifthereisaverylargechangeinthevacuumlevelorifthereisadischargeinthegunseekhelp.

Thedarkcurrentshouldread~103andnomorethan105at200kV.Ifitreads000,theHTisoff.

∙Filamentheating:

Starttoheatthefilamentwhenthevacuumislessthan10x10-5Pa.

IncreasethefilamentheatingtosaturationSLOWLYtakingabout2minutesinall.

Generallythereisstillsomedetailinthefilamentevenwhenitissaturated.Thestopissetattheusualsaturationpointforthecurrentfilament.Itisusuallybetween109-114µA.（emissioncurrentat~10µAabovedarkcurrentfromcoldandafter30minsto1hr5-8µAabovedarkcurrent）.

Ifyouhavereachedthestopandthereisnobeamonthescreen,seethenextsection（“AligningtheMicroscopeforGeneralUse”,step0.）tofindthebeam.

DONOTCHANGETHEBIAS–seekhelpifyouthinkitneedsresetting.

Ifthebrightnessofyourimageseemslow（lookataholeinyourspecimentobesurethebrightnessproblemisnotreallyjustaspecimenthicknessproblem）oriftheexposuretimesforyourpicturesaretoolong,pleaseaskforadviceonhowbesttoproceed.

-Alwaysturnthefilamentdowntozerobeforeremovingthespecimenfromthemicroscope.

-Turningdownthefilamentshouldbeaslowandcontinuousprocess,takingabout30-60seconds..Itisnotnecessarytotakeaslongaswheninitiallyheating.

Shuttingdown

∙Withdrawtheobjectiveandselectedareaapertures.

∙Leavelargestcondenserapertureinserted–levertotheleft

∙TEMimagemode.Spotsize2L.Mag15kx.Spreadbeamtojustfillthelargescreen.

∙X,Ytilttozero.Lockgoniometer.

∙X,Ypositiontozero.

∙Turnthefilamenttozerobeforeremovingthespecimenfromthemicroscope.

Turningdownthefilamentshouldbeaslowandcontinuousprocess,takingabout30-60seconds.Itisnotnecessarytotakeaslongaswheninitiallyheating.

∙TurntheHToff.

∙Turnthemagnificationbackupto100kx.

∙Removeyourspecimen–pullthesampleholdertothestop,rotatecounterclockwise,easeoutwiththumb.

∙Inserttheemptyspecimenrodintothemicroscope.

∙Changeexposedplatesifyouusedanyfilm.

Itisbettertodothisafterthespecimenrodisbackinthemicroscope,otherwisethevacuumwilltakemuchlongertopumpdown.

∙TurnoffthepanellightsandCRTscreen.

∙Signthelogbook.

∙Donotturnoffthemicroscope.

AligningtheMicroscopeforGeneralUse

0.Findthebeam

∙Thelastusershouldhaveleftthemicroscopewiththebeamjustfillingthescreenatamagnificationof5-20kX.Ifyoucan’tseeanybeam,themostlikelyreasonisthatyoursampleisintheway–trymovingitaround.DONOTmoveapertures,guntilt/shiftorbeamshifttofindthebeam!

∙Ifyoucan’tseethebeam,trythefollowing（approximatelyinorder）:

∙Checkthatthefilamentbrightcurrenthasreachedthenormalvalue（~109-114）.Thefilamentheatershouldbeatthestop.DONOTMOVEthestopposition.

∙Checkthespotsizeis2L.

∙Decreasethemagnificationandspreadthebeam.

∙Checkthattheobjectiveandselectedareaaperturesareout.DON’TMOVEtheXandYknobs!

∙Ifyouknowyoushouldhaveaholeapproximatelyinthecentreofyourspecimenoryouhaveagrid,movethespecimenalittleuntilyouseethehole.Watchthespecimenpositiononthemicroscopecomputerscreen.

∙Gotolowmag.modeandspreadthebeam.

∙Moveyoursampletofindthehole.

∙The2000FXhasatwo-sampleholder.Ifsomeonehasusedthisbeforeyou,itmaybesetatposition1or2.Forasinglespecimenholder,thepositionshouldbeinthemiddle.Theadjustmentisontheleftsideofthemicroscopecolumn.Itisaknurledwheelwithapositionmarker.

∙Ifyoustillcan’tseethebeam,goandgethelp.

1.FilamentAlignment

∙Beamonscreen,Magnificationat20Kx,SpotSizeat2L（Page1ofmicroscopedisplay）.

∙Chooseanappropriatecondenseraperture.Withthelevertotheleftthesizesare200,120and70μm.

∙AdjusttheGunAlignTiltformaximumbrightness.（rightdrawer）

∙BringBrightnesstocrossoverandcentrethebeamwithGunAlign.ShiftX,Y.（rightdrawer）

∙AdjustGunAlign.Tiltformaximumbrightness.

2.Gun/CondenserAlignment

∙ChangeSpotSizeto4L.（spotsizetoggleswitchonleftpanel）

∙BringBrightnesstocrossoverandcentrebeamwithBeamShiftsX,Y.

∙SwitchSpotSizebackto2L.

∙BringBrightnesstocrossoverandcentrethebeamwithGunAlignmentShiftsX,Y.

∙Repeatuntilbeamremainscentredforbothspotsizes.

∙RecentreGunTiltasin1above（tiltformax.brightness）.

CentrebeamfromnowonwithBeamShifts,NOTGunAlignmentShifts

3.CondenserApertureCentring

∙CentrebeamonscreenatcrossoverwithBeamShiftsX,Y.

∙Watchforbeam‘swing’whenspreadingthebeamwithBrightnesseithersideofcrossover.

∙Ifbeamswingsawayfromcentrewhenspread,correctbycentringthecondenseraperture.

4.Condenserstigmation

∙Correctcondenserlensastigmatismwithcondenserstigmator（buttonleftpanel;defX,Y）

5.OptimumObjectiveFocus./AdjustZAxis（EucentricCorrection）

CoarseAdjustment:

∙SetOBJLenscurrent（readonPage4）intheregionof7.00to7.05at200kV（5.21at120kV）usingObjectivefocusknob（rightpanel）.

∙LocatespecimenandcentreafeatureataMagnificationof15Kxorless.

∙FocustheimageusingtheZheightadjustknob.（upnearthespecimen