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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. Overview. Scientific Successes of High-Resolution Powder Diffraction Beamline Requirements & Design. Science.

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presented by Jeremy Karl Cockcroft School of Crystallography

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  1. Beamline HA New Beamline for Structural Crystallography by High-Resolution Powder Diffraction on DIAMOND presented by Jeremy Karl Cockcroft School of Crystallography

  2. Overview • Scientific Successes of High-Resolution Powder Diffraction • Beamline Requirements & Design Presentation for the DIAMOND SAC May 2002

  3. Science The impact of powder diffraction and the use of the Rietveld method for structural crystallography is MASSIVE In the last decade, powder diffraction has been the technique of choice to provide vital structural insight in diverse areas: Presentation for the DIAMOND SAC May 2002

  4. 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+d, 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) Presentation for the DIAMOND SAC May 2002

  5. 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) Presentation for the DIAMOND SAC May 2002

  6. 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) Presentation for the DIAMOND SAC May 2002

  7. 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) Presentation for the DIAMOND SAC May 2002

  8. 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) Presentation for the DIAMOND SAC May 2002

  9. 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) Presentation for the DIAMOND SAC May 2002

  10. 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) Presentation for the DIAMOND SAC May 2002

  11. 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) Presentation for the DIAMOND SAC May 2002

  12. 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) Presentation for the DIAMOND SAC May 2002

  13. 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+d", 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) Presentation for the DIAMOND SAC May 2002

  14. 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) Presentation for the DIAMOND SAC May 2002

  15. 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) Presentation for the DIAMOND SAC May 2002

  16. 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) Presentation for the DIAMOND SAC May 2002

  17. 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) Presentation for the DIAMOND SAC May 2002

  18. UK Scientific Impact Web of Science search showing proportion of publications specifically mentioning "synchrotron powder diffraction" in their abstracts to which UK scientists have contributed Presentation for the DIAMOND SAC May 2002

  19. 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 Presentation for the DIAMOND SAC May 2002

  20. 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 Presentation for the DIAMOND SAC May 2002

  21. 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" Presentation for the DIAMOND SAC May 2002

  22. Working Party Dr Jeremy Karl Cockcroft Crystallography Birkbeck Dr John S. O. Evans Chemistry Durham Dr Joe Hriljac Chemistry Birmingham Prof. Matt Rosseinsky Chemistry Liverpool Dr Paul Attfield Chemistry Cambridge Dr Chiu Tang SRS DL Prof. Bill David ISIS RAL Dr Paulo G. Radaelli ISIS RAL Prof. Andy Fitch ESRF Grenoble + Prof. Colin Norris "DIAMOND" RAL Dr Mike Smith "DIAMOND" RAL Presentation for the DIAMOND SAC May 2002

  23. 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 Presentation for the DIAMOND SAC May 2002

  24. 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 Presentation for the DIAMOND SAC May 2002

  25. Working Party Conclusions • Ultra-high resolution mode • Double bounce analysers? • Analysers synchronised with monochromator • Low-angle detectors to be pixellated to remove effect of axial divergence • Negative 2q direction, 60° PSD • Saturation rate 1MHz • Data collection in 100s ms to s • Real-time monitor for parametric studies (VT, VTP, VH, etc.) • Positive 2q direction, 64 analysers & detectors Presentation for the DIAMOND SAC May 2002

  26. 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 ££££ Presentation for the DIAMOND SAC May 2002

  27. 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 Presentation for the DIAMOND SAC May 2002

  28. 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? Presentation for the DIAMOND SAC May 2002

  29. Instrument Layout Presentation for the DIAMOND SAC May 2002

  30. User Community (1) Dr I Abrahams Department of Chemistry, Queen Mary and Westfield College Dr D R Allan Department of Physics and Astronomy, University of Edinburgh Dr P A Anderson School of Chemistry, University of Birmingham Dr M P Attfield School of Crystallography, Birkbeck College, University of London Dr J P Attfield Department of Chemistry, University of Cambridge Prof P Barnes School of Crystallography, Birkbeck College Dr P D Battle Inorganic Chemistry Laboratory, University of Oxford Dr A M T Bell Department of Earth Sciences, University of Manchester Prof P G Bruce School of Chemistry, University of St Andrews Dr S G Carling Royal Institution of Great Britain Dr M A Carpenter Department of Earth Sciences, University of Cambridge Prof R J Cernik Daresbury Laboratory Dr J Charmant School of Chemistry, University of Bristol Dr S J Clarke Department of Chemistry, University of Oxford Dr S Clarke Department of Chemistry, University of Cambridge Dr J K Cockcroft School of Crystallography, Birkbeck College Dr J M Cole Department of Chemistry, University of Cambridge Prof H M Colquhoun Department of Chemistry, University of Reading Mr L M D Cranswick School of Crystallography, Birkbeck College, University of London Dr S E Dann Department of Chemistry, Loughborough University Dr C N W Darlington School of Physics and Astronomy, University of Birmingham Prof. W I F David ISIS, Rutherford Appleton Laboratory Prof P Day Royal Institution of Great Britain Presentation for the DIAMOND SAC May 2002

  31. User Community (2) Dr M T Dove Department of Earth Sciences, University of Cambridge Dr J S O Evans Department of Chemistry, University of Durham Dr A J Florence Department of Pharmaceutical Sciences, University of Strathclyde Prof R Freer Materials Science Centre, University of Manchester/UMIST Dr C J Gilmore Department of Chemistry, University of Glasgow Dr A E Goeta Department of Chemistry, University of Durham Dr D H Gregory School of Chemistry, University of Nottingham Prof K D M Harris School of Chemistry, University of Birmingham Dr W T A Harrison Department of Chemistry, University of Aberdeen Dr A Harrison Department of Chemistry, University of Edinburgh Dr P D Hatton Department of Physics, University of Durham Prof C M B Henderson Department of Earth Sciences, University of Manchester Prof J A K Howard Department of Chemistry, University of Durham Dr J A Hriljac School of Chemical Sciences, University of Birmingham Dr M J Hudson Department of Chemistry, University of Reading Dr S Hull ISIS, Rutherford Appleton Laboratory Dr R M Ibberson ISIS, Rutherford Appleton Laboratory Dr J T S Irvine School of Chemistry, University of St Andrews Dr A P Jephcoat Department of Earth Sciences, University of Oxford Dr R H Jones Department of Chemistry, Keele University Dr D A Keen ISIS, Rutherford Appleton Laboratory Dr P Lightfoot School of Chemistry, University of St Andrews Dr A J Markvardson ISIS Facility, Rutherford Appleton Laboratory Presentation for the DIAMOND SAC May 2002

  32. User Community (3) Prof R E Morris School of Chemistry, University of St Andrews Dr K U Neumann Department of Physics, Loughborough University Dr D M O'Hare Inorganic Chemistry Laboratory, University of Oxford Prof A G Orpen School of Chemistry, University of Bristol Dr S Parsons Department of Chemistry, University of Edinburgh Dr R F Pettifer Department of Physics, University of Warwick Dr C R Pulham Department of Chemistry, University of Edinburgh Dr K Prassides School of Chemistry, University of Sussex Dr P R Radaelli ISIS Facility, Rutherford Appleton Laboratory Prof P Raithby School of Chemistry, University of Bath Dr S A T Redfern Department of Earth Sciences, University of Cambridge Prof L V C Rees Department of Chemistry, University of Edinburgh Prof M J Rosseinsky Department of Chemistry, University of Liverpool Dr N Shankland Department of Pharmaceutical Sciences, University of Strathclyde Dr K Shankland ISIS Facility, Rutherford Appleton Laboratory Dr S J Skinner Department of Materials, Imperial College, London Dr P R Slater Department of Chemistry, University of Surrey Dr M Sahibzada Department of Materials, Imperial College, London Dr C C Tang SRS Facility, Daresbury Laboratory Prof B K Tanner Science Laboratories, University of Durham Prof D P Thompson Dept. MMME, Materials Division, University of Newcastle Upon Tyne Dr A D Taylor Director of Isis, Rutherford Appleton Laboratory Dr M Tremayne School of Chemical Sciences, University of Birmingham Presentation for the DIAMOND SAC May 2002

  33. User Community (4) Dr R Walton School of Chemistry, University of Exeter Dr D J Watkin Chemical Crystallography Laboratory, University of Oxford Prof M T Weller Department of Chemistry, University of Southampton Prof B T M Willis Chemical Crystallography Laboratory, University of Oxford Dr C C Wilson ISIS, Rutherford Appleton Laboratory Dr P A Wright School of Chemistry, University of St Andrews Prof K R A Ziebeck Department of Physics, Loughborough University of Technology • Represents 75+ UK User Groups • Chemists • Physicists • Earth Scientists • Material Scientists Presentation for the DIAMOND SAC May 2002

  34. Future Prospects When 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,.... Presentation for the DIAMOND SAC May 2002

  35. THE ENDQuestions & Discussion Presentation for the DIAMOND SAC May 2002

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