presented by Jeremy Karl Cockcroft School of Crystallography

Beamline H A New Beamline for Structural

Crystallography by High-Resolution Powder Diffraction on DIAMOND

presented by

Jeremy Karl Cockcroft

School of Crystallography

Presentation for the DIAMOND SAC May 2002 2

Overview

• Scientific Successes of High-Resolution Powder Diffraction

• Beamline Requirements & Design


ScienceThe impact of powder diffraction and the use of the Rietveld method for structural

crystallography is

MASSIVEMASSIVEIn the last decade, powder diffraction has been the technique of choice to provide vital structural insight in diverse areas:


Science• High Temperature Cuprate and other Oxide

Superconductors:– Structure and crystal-chemistry of the high-Tc superconductor

YBa2Cu3O7-x, Nature, 327, 310-312 (1987)

– Superconductivity near 30-K without copper - the Ba0.6K0.4BiO3 Perovskite, Nature, 332, 814-816 (1988)

– Synthesis and superconducting properties of the strontium copper oxy-fluoride Sr2CuO2F2+, Nature, 369, 382-384 (1994)

– Cation effects in doped La2CuO4 superconductors, Nature, 394, 157-159 (1998)

– Systematic cation disorder effects in L1.85M0.15CuO4 superconductors, Phys. Rev. Lett., 83, 3289-3292 (1999)


Science

• MgB2 and Borocarbide Superconductors:– Structure of the 13-K superconductor La3Ni2B2N3 and the

related phase LaNiBN", Nature, 372, 759-761 (1994)– MgB2 superconducting thin films with a transition temperature

of 39 Kelvin", Science, 292, 1521-1523 (2001)– Superconductivity at 39 K in magnesium diboride", Nature,

410, 63-64 (2001)


Science

• C60 and its Superconducting Derivatives:– Superconductivity at 28 K in RbxC60, Phys. Rev. Lett., 66, 2830-

2832 (1991)– Intercalation of ammonia into K3C60, Nature, 364, 425-427

(1993) – Crystal-structure, bonding, and phase-transition of the

superconducting Na2CsC60 Fulleride, Science, 263, 950-954 (1994)

– Structural and electronic properties of the noncubic superconducting fullerides A ' C-4(60) (A '= Ba, Sr), Phys. Rev. Lett., 83, 2258-2261 (1999)


Science

• Negative Thermal Expansion Oxides:– Negative thermal expansion from 0.3 to 1050 Kelvin in

ZrW2O8, Science, 272, 90-92 (1996)

– Compressibility, phase transitions, and oxygen migration in zirconium tungstate, ZrW2O8, Science, 275, 61-65 (1997)


Science• Full 3-Dimensional Structure of

Oligopeptides:– Structure determination of an oligopeptide directly from

powder diffraction data, Angew. Chem.-Int. Edit., 39, 4488- (2000)

– Ab initio structure determination of a peptide beta-turn from powder X-ray diffraction data", Chem. Comm., 1460-1461 (2001)


Science

• Cathode and Electrolytic Materials for Portable, Rechargable Batteries:– Crystal-structure of the polymer electrolyte poly(ethylene

Oxide)3:LiCF3SO3, Science, 262, 883-885 (1993)

– Synthesis of layered LiMnO2 as an electrode for rechargeable lithium batteries, Nature, 381, 499-500 (1996)

– Structure of the polymer electrolyte poly(ethylene oxide)6:LiAsF6, Nature, 398, 792-794 (1999)

– Ionic conductivity in crystalline polymer electrolytes, Nature, 412, 520-523 (2001)


Science

• Microporous Materials:– Structure of the microporous titanosilicate ets-10, Nature,

367, 347-351 (1994)– On the nature of water bound to a solid acid catalyst,

Science, 271, 799-802 (1996)


Science• New Mesoporous Materials:

– Ordered Mesoporous Molecular-Sieves Synthesized by a Liquid- Crystal Template Mechanism, Nature, 359, 710-712 (1992)

– Conducting Polyaniline Filaments in a Mesoporous Channel Host, Science, 264, 1757-1759 (1994)

– Generalized syntheses of large-pore mesoporous metal oxides with semicrystalline frameworks, Nature, 396, 152-155 (1998)

– Varied pore organization in mesostructured semiconductors based on the [SnSe4] (4-) anion, Nature, 410, 671-675 (2001)


Science

• First Metal Oxide Hydride:– The hydride anion in an extended transition metal oxide array:

LaSrCoO3H0.7, Science, 295, 1882 (2002)

• New Dielectric Materials:– Enhancement of the dielectric-constant of Ta2O5 through

substitution with TiO2, Nature, 377, 215-217 (1995)

• Highly-Reactive Molecular Species:– Crystal and molecular-structures of rhenium heptafluoride,

Science, 263, 1265-1267 (1994)


Science• Giant Magneto-Resistive Materials (1):

– Simultaneous Structural, Magnetic, and Electronic-Transitions in La1-xCaxMnO3 with x=0.25 and 0.50, Phys. Rev. Lett., 75, 4488-4491 (1995)

– Colossal magnetoresistance without Mn3+/Mn4+ double exchange in the stoichiometric pyrochlore Tl2Mn2O7, Science, 273, 81-84 (1996)

– Lattice effects and magnetic order in the canted ferromagnetic insulator La0.875Sr0.125MnO3+", Phys. Rev. Lett., 76, 3826-3829 (1996)

– Direct observation of lattice polaron formation in the local structure of La1-xCaxMnO3", Phys. Rev. Lett., 77, 715-718 (1996)


Science• Giant Magneto-Resistive Materials (2):

– Colossal magnetoresistance in Cr-based chalcogenide spinels", Nature, 386, 156-159 (1997)

– Electrostatically driven charge-ordering in Fe2OBO3, Nature, 396, 655-658 (1998)

– Optimal T-C in layered manganites: Different roles of coherent and incoherent lattice distortions, Phys. Rev. Lett., 83, 1223-1226 (1999)

– Formation of isomorphic Ir3+ and Ir4+ octamer and spin dimerisation in the spinel CuIr2S4, Nature, 416 155-158 (2002)


Science

• Magnetic Nanomaterials:– Monodisperse FePt nanoparticles and ferromagnetic FePt

nanocrystal superlattices, Science, 287, 1989-1992 (2000)– Size-dependent grain-growth kinetics observed in

nanocrystalline Fe", Phys. Rev. Lett., 86, 842-845 (2001)


Science

• Structures of Small Proteins:– The first protein structure determined from high-resolution X-

ray powder diffraction data: a Variant of the T3R3 Human Insulin-Zinc Complex Produced by Grinding", Acta Cryst., D56, 1549-1553 (2000)

– Binding of N-acetylglucosamine to chicken egg lysozyme: a powder diffraction study, Acta Cryst., D57, 1836-1842 (2001)


Science

• Pharmaceuticals:– Structural transformations in zoplicone, Chem. Comm. 2204-

2205 (2001)

• Whole Field of SDPD:– "Structure Determination from Powder Diffraction Data"

editors: W I F David, K Shankland, L B McCusker and C Baerlocher, Oxford University Press (2002)


UK Scientific ImpactWeb of Science search showing proportion of publications specifically mentioning "synchrotron powder diffraction" in their abstracts to which UK scientists have contributed

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Future Trends in Structural Crystallography by Powder Diffraction

• Laboratory X-ray Diffractometers– Limited scope for orders of magnitude improvements

• Faster and better detectors

• Neutron Powder Diffractometers– Count rate on modern machines vastly improved

• e.g. GEM at ISIS

• Synchrotron Powder Diffractometers– Move of BM16 to ID31 at ESRF– Beamline H on DIAMOND


Background to Beamline H• September 2001 SRS User Meeting

– List of Possible Beamlines Required on DIAMOND– E-mail Invitation for "Expressions of Interest"

• Organised by Graham Bushnell-Wye

• Open Meeting held at Birkbeck in October 2001– Approx. 30 Attendees– Topics

• Insertion Devices (Mike Poole) & BM16/ID31 (Andy Fitch)• Science• High-Resolution versus High-Flux Diffractometers• User Instrument


Initial Proposal• Three Page Initial Proposal for a High-

Resolution Powder Diffraction Beamline Submitted on Behalf of the UK Powder Diffraction Community in November 2001– With much help from from Chiu Tang, Paolo Radaelli,

Bill David, John Evans• Of the 16 Initial Proposals, 6 Shortlisted by the

SAC in January 2002– A High-Resolution Powder Diffraction Beamline for

Structural Crystallography Short-Listed as

"BEAMLINE H"


Working PartyDr Jeremy Karl Cockcroft Crystallography BirkbeckDr John S. O. Evans Chemistry DurhamDr Joe Hriljac Chemistry BirminghamProf. Matt Rosseinsky Chemistry LiverpoolDr Paul Attfield Chemistry CambridgeDr Chiu Tang SRS DLProf. Bill David ISIS RALDr Paulo G. Radaelli ISIS RALProf. Andy Fitch ESRF Grenoble

+Prof. Colin Norris "DIAMOND" RALDr Mike Smith "DIAMOND" RAL


Working Party Conclusions• User-friendly beamline for the non-expert

– As easy to use as the laboratory diffractometer

• Ultra high resolution, but– Rapid high-resolution powder diffraction data required in minutes

and not in hours!!!

• Energy range from 5 to 30+ keV– Limits imposed by the choice of a medium energy (3 GeV) source – Optimised in 10 to 20 keV range– ESRF available for those requiring very hard (>30 Kev) X-rays

• Wavelength range from 2.5 down to 0.4 Å


Working Party Conclusions• Optics: in vacuo narrow-gap undulator is

essential:– High brightness with narrow horizontal divergence

• No need for beam focussing (simple optics)• No requirement for mirrors (more user friendly)

– Provides a continuous range of wavelengths over the desired wavelength range

• Ability for the user to change wavelength at the "click of a mouse"

– EXAFS quality monochromator with double Si(111) crystals– Fixed beam entry/exit with detuning for harmonic rejection


Working Party Conclusions• Positive 2 direction, 64 analysers & detectors

• Ultra-high resolution mode• Double bounce analysers?• Analysers synchronised with

monochromator• Low-angle detectors to be pixellated

to remove effect of axial divergence

• Negative 2 direction, 60° PSD• Saturation rate 1MHz• Data collection in 100s ms to s• Real-time monitor for parametric

studies (VT, VTP, VH, etc.)


Working Party Conclusions• Typical modus operandi :

– collection of PSD diffraction data while the sample is undergoing some of change of state

– switch to high-resolution mode once sample equilibrium has been reached

• Obtain a complete experiment on the same sample on the same instrument

• One disadvantage: additional ££££


Working Party Conclusions• Separate optics & experimental hutches• Large amount of space in experimental hutch

– Avoid SRS situation of cramped working conditions!

• Sample automation of the utmost importance– High throughput as in PX– Use of robotic sample changers– Automatic alignment

• Easy to use sample heating/cooling stages, variable humidity, gas, electric and/or magnetic field, etc.

– Must be available on Day 1

• Integrated & user-friendly control software– Must be properly budgeted


Working Party Conclusions• User control hutch and user data

analyses rooms– Multiple PCs & plug-in laptop facilities– Appropriate analysis software– Colour printing "on tap"– Data archiving facilities

• User laboratories close to beamline– Well-equipped for various sample manipulations– Share laboratories with beamline 1 & a single

crystal beamline?


Instrument Layout


User Community (1)Dr I Abrahams Department of Chemistry, Queen Mary and Westfield CollegeDr D R Allan Department of Physics and Astronomy, University of EdinburghDr P A Anderson School of Chemistry, University of BirminghamDr M P Attfield School of Crystallography, Birkbeck College, University of LondonDr J P Attfield Department of Chemistry, University of CambridgeProf P Barnes School of Crystallography, Birkbeck CollegeDr P D Battle Inorganic Chemistry Laboratory, University of OxfordDr A M T Bell Department of Earth Sciences, University of ManchesterProf P G Bruce School of Chemistry, University of St AndrewsDr S G Carling Royal Institution of Great BritainDr M A Carpenter Department of Earth Sciences, University of CambridgeProf R J Cernik Daresbury LaboratoryDr J Charmant School of Chemistry, University of BristolDr S J Clarke Department of Chemistry, University of OxfordDr S Clarke Department of Chemistry, University of CambridgeDr J K Cockcroft School of Crystallography, Birkbeck CollegeDr J M Cole Department of Chemistry, University of CambridgeProf H M Colquhoun Department of Chemistry, University of ReadingMr L M D Cranswick School of Crystallography, Birkbeck College, University of LondonDr S E Dann Department of Chemistry, Loughborough UniversityDr C N W Darlington School of Physics and Astronomy, University of BirminghamProf. W I F David ISIS, Rutherford Appleton LaboratoryProf P Day Royal Institution of Great Britain


User Community (2)Dr M T Dove Department of Earth Sciences, University of CambridgeDr J S O Evans Department of Chemistry, University of DurhamDr A J Florence Department of Pharmaceutical Sciences, University of StrathclydeProf R Freer Materials Science Centre, University of Manchester/UMISTDr C J Gilmore Department of Chemistry, University of GlasgowDr A E Goeta Department of Chemistry, University of DurhamDr D H Gregory School of Chemistry, University of NottinghamProf K D M Harris School of Chemistry, University of BirminghamDr W T A Harrison Department of Chemistry, University of AberdeenDr A Harrison Department of Chemistry, University of EdinburghDr P D Hatton Department of Physics, University of DurhamProf C M B Henderson Department of Earth Sciences, University of ManchesterProf J A K Howard Department of Chemistry, University of DurhamDr J A Hriljac School of Chemical Sciences, University of BirminghamDr M J Hudson Department of Chemistry, University of ReadingDr S Hull ISIS, Rutherford Appleton LaboratoryDr R M Ibberson ISIS, Rutherford Appleton LaboratoryDr J T S Irvine School of Chemistry, University of St AndrewsDr A P Jephcoat Department of Earth Sciences, University of OxfordDr R H Jones Department of Chemistry, Keele UniversityDr D A Keen ISIS, Rutherford Appleton LaboratoryDr P Lightfoot School of Chemistry, University of St AndrewsDr A J Markvardson ISIS Facility, Rutherford Appleton Laboratory


User Community (3)Prof R E Morris School of Chemistry, University of St AndrewsDr K U Neumann Department of Physics, Loughborough UniversityDr D M O'Hare Inorganic Chemistry Laboratory, University of OxfordProf A G Orpen School of Chemistry, University of BristolDr S Parsons Department of Chemistry, University of EdinburghDr R F Pettifer Department of Physics, University of WarwickDr C R Pulham Department of Chemistry, University of EdinburghDr K Prassides School of Chemistry, University of SussexDr P R Radaelli ISIS Facility, Rutherford Appleton LaboratoryProf P Raithby School of Chemistry, University of BathDr S A T Redfern Department of Earth Sciences, University of CambridgeProf L V C Rees Department of Chemistry, University of EdinburghProf M J Rosseinsky Department of Chemistry, University of LiverpoolDr N Shankland Department of Pharmaceutical Sciences, University of StrathclydeDr K Shankland ISIS Facility, Rutherford Appleton LaboratoryDr S J Skinner Department of Materials, Imperial College, LondonDr P R Slater Department of Chemistry, University of SurreyDr M Sahibzada Department of Materials, Imperial College, LondonDr C C Tang SRS Facility, Daresbury LaboratoryProf B K Tanner Science Laboratories, University of DurhamProf D P Thompson Dept. MMME, Materials Division, University of Newcastle Upon TyneDr A D Taylor Director of Isis, Rutherford Appleton LaboratoryDr M Tremayne School of Chemical Sciences, University of Birmingham


User Community (4)Dr R Walton School of Chemistry, University of ExeterDr D J Watkin Chemical Crystallography Laboratory, University of OxfordProf M T Weller Department of Chemistry, University of SouthamptonProf B T M Willis Chemical Crystallography Laboratory, University of OxfordDr C C Wilson ISIS, Rutherford Appleton LaboratoryDr P A Wright School of Chemistry, University of St AndrewsProf K R A Ziebeck Department of Physics, Loughborough University of Technology

• Represents 75+ UK User Groups– Chemists– Physicists– Earth Scientists– Material Scientists


Future ProspectsWhen Beamline H is built, the future for Structural Crystallography by Powder

Diffraction in the UK will be Looking Very Bright for Chemists, Solid-State-

Physicists, Earth & Material Scientists,....


THE END

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presented by Jeremy Karl Cockcroft School of Crystallography