Basics2:TheCompleteDummy'sGuidetoOperationofaTypicalDiffusion

PumpedHighVacuumSystem
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1.Introduction
Thissectionisjustforallthosepeoplewhohaveneverhadanythingtodowithavacuumsystemofany
kindbutneedtouseone.Diffusionpumpedsystemsarestillquitecommon,andusedforallsortsof
applicationse.g.VacuumEvaporatorsformakingmetalcoatings.Thediagrambelowisofasmallbell
jarsystemthatweuseforavarietyofthingshereinthelab.
SincetheintroductionoftheSIunits,theunit"torr"isnolongertobeused.Preferredunitsarenowto
bePascal,it'sderivativemillibarr,andbar.HerearetheConversionTablesforPressureUnitsfrom
EdwardsHighVacuum'swebpageforthosewho,likeus,arestillusingolderequipmentcalibratedin
torr.
Ihavetakentongueincheek"artisticlicense"andchangedafewthingsinthedrawing.Thereallife
glassbelljarhasbeenreplacedbyametalvacuumchamberinthepictureandtheiongaugeisshownin
therecommendedinletdownpositiontopreventproblemswithdetritusdroppingintothegauge.The
diagrambelowispictorial,thereareastandardsetofschematicsymbolsforvacuumsystemswhich
willalsobeincludedhereeventually.

2.GettingStarted
Thesystemshownhereistypicallyusedforvacuumevaporation,etc.Thisguideassumesthat
everythingisoffinitiallyandthatthebelljarisatatmosphericpressuretostartwith.
1.Preliminary
BesureyouhaveliquidNitrogenavailablebeforestartingthistypeofsystem,andthatyouhave
somefamiliaritywithproperLN2handlingtechniques.Youshouldweareyeprotection,along
sleevedlabcoat,andprotectivegloves.Frostbiteispainful!
Switchpowerontothegaugecontrollersbutdon'ttrystartingtheiongaugeyet.
2.Watercooling
Turnonthewatercoolinglinestothediffusionpumpandthewatercooledbaffle.Verifywater
flowbeforeproceedingfurther.
Beforegoingtoomuchfurther,Iwouldliketoaddalittlesermononwatercoolinglines.
Therehavebeenseveralfloodsinthisareaduetoplasticwaterlinescomingoffofequipmentleft
runningovernight.Soakingsomeone'spreciouscollectionofbooksorhavingwatergetinto
electricalconduittendstocreatealotmorewavesthantherelativelysmallexpenseoftaking
someprecautions.
Awaterflowswitchcontrollingawaterinletsolenoidwillpreventproblemsandinsureyour
gettinginvitedtothenextbushpartyorwhatever.Allofourlabsystemsareplumbedinwithsoft
coppertubing,haveflowinterlocks,andhaven'thadfloodingproblemsinyears.
3.Valves
Allofthevacuumvalvesinthedrawingshouldbeclosedtostartwith.Thepumpventvalvemay
beasshown,orinsomecasesitispartoftherotaryvacuumpumpandclosesautomaticallywhen
thepumpisrunning.
4.TheRotaryPump
Switchthepowerontotherotarypump.Thepumpwillbequitenoisyandspewoilvapourout
it'sexhaustwhenstartingfromatmosphericpressure.Don'tbealarmed,that'snormaloperation
andthenoiseandvapourshouldsubsideasthevacuumimproves.
Iftheracketandoilvapourspewingpersistmorethanafewminutes(Orlongerforlarger
systems.)it'squitelikelythatyouhaveagrossleakormajorcontaminationandyouwillhaveto
shutthepumpdownandinvestigate.
5.TheDiffusionPump
Opentheforelinetothediffusionpumpandwaituntilthepressureonthermocouplegauge1is
below.15mbars.(200millitorr.)Switchthediffusionpumpheateronandwaitforaminimum1/2
hour.Largerpumpsoftentakelonger,infactjustaboutalldiffusionpumpstakeaboutanhourto
reallygetgoingbutmaybeusableinlesstimewithlessperformance.
FillthecoldtrapslowlywithliquidNitrogen.TheLN2willboillikemadinitiallyasithitsthe
warmsurfacesinsidethecoldtrap.Bepatientandjustpartiallyfillthetrapinitiallytoallowitto
coolslowly.

Theimportantthingtorememberatthispointistoneverletahotdiffusionpumpseehigh
oratmosphericpressure,asituationthatwillcrackmanydiffusionpumpoilsandcreatea
horriblemess.Ifyoubreakityougettofixitanditmaynotbepretty!
6.RoughPumpingtheVacuumChamber
Closetheforelinevalvetothediffusionpump.Makesuretheventvalvetothevacuumchamber
isclosed,thenopenthevacuumchamberroughingline.
Therotarypumpwillgetnoisyagain,thenoiseshouldsubsideinafewminutesandthepressure
onthermocouplegauge2shouldbegintodrop.Keepaneyealsoontheforelinepressure.If
pressurerisesaboveabout.15millibarrs(200millitorr)youwillhavetopausebyclosingthe
chamberroughingvalve,openingtheforelinevalve,andrepumpingtheforeline.Closethe
forelinevalveandreopenthechamberroughingvalvewheneverythinglooksok.Skipthenext
paragraphunlessthereisaproblem.
Ifyoucan'tgetthechamberdownto.15mbar(200millitorr)orlessinaboutfifteenminutes
thereismostlikelyaleakorgrossoutgassinginthevacuumchamber.Closetheroughingvalve,
reopentheforelinevalve,andarrangetoleaktestorcleanthevacuumchamber.Donotpass
GO,STOPHERE.
Roughpumpthevacuumchamberdowntoabout.15mbar(200millitorr),thenclosethe
roughingvalve.Notethatthereisnogreatadvantageingoingmuchbelowthispressureastheoil
backstreamingrateformostmechanicalpumpsgetsprogressivelyworsebelowtheviscousflow
regionandcancausesomesystemcontamination.OneschoolofthoughtalsoconsidersitaGood
Thingtoalwaysstartadiffusionpumpwiththechamberpressureslightlyhigherthantheforeline
pressuretoreducediffusionpumpbackstreamingatstartup.
7.PumpingtoHighVacuum
Opentheforelinevalvethenopenthehighvacuum(a.k.a.baffleorgate)valve.Waitforafew
minutesthenstarttheiongauge.Ifiongaugepressureisabove1.3X10e05mbar(1X10e05
torr)agoodpracticeistoswitchthegaugeoffandjustmakespotchecksuntilbelow1.3e05
mbartopreventoxidationofthehotgaugeelements.Gaugeoutgassingshouldalwaysbedoneat
1.3e05mbarorlesswithpausestolettheevolvedgasesbepumpedaway.
Congratulations,you'reinbusiness!Havepatience.Reachingultimatepressuremaytakeseveral
hours.
TopuptheliquidNitrogentrap,checkitoccasionally,andproceedwithwhateveritwasthatyou
wantedtodoinvacuum.
4.SystemOperation
1.Toremoveorreplaceitemsinthebelljar:
1.Switchtheiongaugeoff.
2.Closethehighvacuumvalve.
3.Openthechamberventvalve.Ideallythisvalveshouldbeconnectedtoalowpressure
sourceofdrynitrogenandthereshouldalsobesomesortofpressurereliefvalveonthe
system.
Warning:somesystemsmayuseargonasabackfillgas,yourthermalheatloss(e.g.
thermocouple,Pirani)gaugeswillindicatemuchlowerpressuresthanactualpressures,so
pleasereadandusethegaugemanufacturer'scorrectioncharts.

4.Waitforthevacuumchambertorisetoatmospheric.
5.Raisethebelljar.(Caution,itshouldhaveavacuuminterlockswitchsodon'ttrytoforceit
openprematurely.)
6.Remove/replaceitemsinvacuumchamber.
7.Checkthebelljarsealingsurfaceandthebaseplatefordirt,etc.andwipeifnecessary.
8.Lowerthebelljar.
9.Evacuatethevacuumchamber.
5.StandbyOperation
Runningsystemscontinuouslytopreventtheingestionofwatervapourandtopreventcorrosionofoil
sealedrotarypumpsisgoodvacuumpracticeandshouldbedoneifpossible.Somemeansofkeeping
coldtrapsfilledshouldbeusedonanuntendedsystem.
Backstreamingfromanuntrappeddiffusionpumpwillcontaminateyourvacuumchamberinmany
cases,soit'sbesttoclosethehighvacuumvalve,shutthepumpheateroff,andjustkeeptherough
pumponthediffusionpumpforeline.Alternativelyagoodwatercooledchevronbaffleandadiffusion
pumpfluidselectedforlowbackstreamingmayallowcontinuousoperationwithnoliquidnitrogen.
We'vehadgoodsuccesswithpolyphenyletherbutitisveryexpensive.
6.ShuttingtheSystemDown
1.EmergencyShutdownduetoPowerFailure
Closeallthevalvesonthevacuumsystemandshutoffheaterpowertothediffusionpump.
2.CompleteShutDown
1.Removeitemsfromthevacuumchamberandreevacuatethechambertohighvacuum.
2.Switchtheiongaugeoff.
3.Closethehighvacuumvalve.Leavethebelljarundervacuum.
4.Switchthediffusionpumpheateroff.
5.Waitforthediffusionpumptocooldown.Ifthediffusionpumpiscleanandusesafluid
thatwillwithstandashorttimeatpoorvacuum,youmaygetawaywithjustclosingthe
forelinevalveatthispointandlettingthepumpcoolina"sealedoff"mode.
6.Closetheforelinevalveleavingthediffusionpumpundervacuum.
7.Switchtherotarypumpoffifyou'reintoenergyconservationthenopentherotarypump
ventvalveifit'snotautomatic.
Whetherornottoswitchanunusedpumpoffwillbeyourdecision.Leavingthepump
runningcontinuouslyisthepreferredoptionsinceanywatervapour,etc.thathasbeen
pumpedwillremaininthepumpandcauseinstantcorrosion.Ifyourapplicationis
relativelyclean,asmostofoursare,thenswitchoff.Fordirtierapplications,anoilchange
isrecommendedbeforestorage.
7.Conclusion
Techniquesshownherearegenerallyusedfortheoperationofdiffusionpumpedsystemsatthissite.
Yourmileagemayvary.
RoySchmaus,October4,1995RevisedOctober18,2000
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