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Synchrotron Powder Diffraction Simplified: Introducing the Advanced Photon Source’s dedicated high-resolution beamline 11-BM
Ma#hewSuchomel,BrianToby,LynnRibaud,andRobertVonDreele
AdvancedPhotonSource,ArgonneNa3onalLaboratory
Presentation Outline
BackgroundtotheAPS&11‐BM
High‐ResoluBonPowderDiffracBon– Whyisituseful?
– Whatdoweoffer?
11‐BMBeamline“Tour”– withlive‐acBonrobotmovie!
Performance&Examples
RapidAccessMail‐inProgram:– Howdoesitwork?
– Howcanyougetaccess?
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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11‐BM=SynchrotronPowderDiffrac<onSimplified!!
Argonne’s Advanced Photon Source (APS)
APSopened1996
OnANLcampus– 30minfromChicago
7GeVringcurrent– ringcircumference>1km
33beamlineports– ~60acBvestaBons
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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High-Resolution beamline 11-BM
startedconstruc3on:spring2005 firstbeaminhutch:fall2007
mail‐inuserprogram:summer2008
firstuserpublica3on:fall2008
on‐siteexperiments:spring2010
Instrument Overview
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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Energyrange(BM):10‐35keV(1.0‐0.35Å)– mail‐inserviceopBmized@30keV(~0.4Å)
ResoluBon:Δd/d(ΔQ/Q)≈2×10‐4
– Equivalenttobest‐in‐world(ESRF,Diamond,PSIetc.)
– HighestresoluBonpowderdiffracBoninAmericas
Qrange:Qmax≈25Å‐1
– 1hrmail‐inscan:2Qrange0.5°50°(d≥0.5Å)
BeamSize:0.5mm(vert.)x1mm(horz.)– samplecapillary<1mmmin.axialdivergence
2θ
SiO2 (α - Quartz) “fingers”
Hot Gas Blower in Action
MulBpleSampleEnvironments– Cryostream(90K‐450K),HotGasBlower(<1000°C)
– acquiring:5KHeliumCryostat,In‐situPressure&GasCells
RoboBcArmAutomatedsamplechanges– Robot+DatabaseHighThroughput!
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Beamline Layout
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
~ 50 meters
collimating mirror
vert. focus mirror
x2 Si(111) mono tank
Sagittally bent Si(111) crystal horizontal focusing: ~ 50 mm 1 mm
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X-ray beam
OpBcsHutchExperimentalHutch
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11-BM Diffractometer
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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X-ray beam Huber 480 rotation stage: high precision (~0.35 arcsec) high accuracy (~1 arcsec) slew or step scans
12 analyzer array Si(111) crystals LaCl3 detectors 2° apart in 2Θ
Mitsubishi robot custom “fingers”
Sample Stage spinner > 90 Hz
12crystals/detectors– Individuallyadjusted
– 2°separaBon
– Total2Θrange=22°
Si(111)crystals– excellentdiscriminaBon
– lowbackground(&yield!)
– LaCl3ScinBllators
11-BM Detector Assembly
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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Mul<pleObserva<ons ReduceCollec<onTime
ImproveAccuracy
Enabling High-Throughput
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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RoboBcSampleChanger– 100+Samples
– WorksNights&Weekends
– OpBcalBarcodeReader
Mail‐inSampleBases– MagneBcBase
– Kapton®CapillaryTube(0.8mm)
– UniqueBarcodeforeachSample
Soxware&Database– AutomatesRepeBBveTasks
– Python,PHP/MySQL
– TrackSampleHistory&Detailrequest‐>receipt‐>scan‐>disposal
Performance
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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Q ≈ 8 (Å-1) Cu Kα1 2Θ ≈ 160°
How can YOU Access 11-BM ?
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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6easystepsfor11‐BMrapidaccess
StandardUserProposal– MulB‐dayexperiment
– On‐site(ormail‐in)
– AddiBonalsampleenvironments(temp,atmosphere,pressureetc)
– 3deadlines/year,commiyeereviewed
RapidAccessMail‐inProposal– Same‐dayapproval
– 1shix(~ 8scans)limit
– SelecBonofdefinedscans/temps
– NoBficaBon&datareceiptbyemail
– Quickturn‐around:Proposal‐>Datain~3weeks– ComplementsNPDstudies(jointX‐ray/Neutronrefinements)
Mail-In Service Overview:
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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1. Submitrapid‐accessAPSproposalfor11‐BMbeamBme
2. Proposalaccepted11‐BMstaffsendsamplebases
3. Userregisterssamplesonline&requestsscantype/temp
4. UsermailspreparedsamplesbacktoAPS
5. DatacollectedemailnoBficaBon,userdownloadsdata
6. Periodicremindersforanalysisstatus&publicaBonupdates
free serviceforallnon‐proprietaryusers
More Information
APSBeamline11‐BM:SynchrotronPowderDiffracBonSimplified
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11‐BMwebpage:hXp://11bm.xor.aps.anl.gov/
emailcontact:[email protected]
11‐BMstaff:BrianToby,LynnRibaud,BobVonDreeleandformerstaff:JenniferDoebbler,JunWang&SytleAntao.
APSSupport:PeterLee,MohanRamanathan,ChuckKurtz,CurtPreissner,XuesongJiaoandmanymanyothers…
DOEgrantproposal(2003)byJ.F.Mitchell,J.D.Jorgensen,R.B.VonDreele,P.L.Lee,&M.A.Beno
11‐BMAcknowledgements