Beamline H - img.chem.ucl.ac.uk

Beamline H - img.chem.ucl.ac.uk

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 Presentation for the DIAMOND SAC May 2002 2 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 3 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)

Presentation for the DIAMOND SAC May 2002 4 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 5 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 6 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 7 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 8 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 9 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 10 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, 152155 (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 11 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 12 Science Giant Magneto-Resistive Materials (1): Simultaneous Structural, Magnetic, and ElectronicTransitions 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) Presentation for the DIAMOND SAC May 2002

13 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 14 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

15 Science Structures of Small Proteins: The first protein structure determined from high-resolution Xray 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 16 Science Pharmaceuticals: Structural transformations in zoplicone, Chem. Comm. 22042205 (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 17

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 UK Publications Total Publications 160 120 100 80 60 40 Presentation for the DIAMOND SAC May 2002 2001 2000 1999 1998 1997

1996 1995 1994 1993 1992 0 1991 20 1990 Number of Publications 140 18 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 19 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 20 Initial Proposal Three Page Initial Proposal for a HighResolution 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 21

Working Party Dr Jeremy Karl Cockcroft Dr John S. O. Evans Dr Joe Hriljac Prof. Matt Rosseinsky Dr Paul Attfield Dr Chiu Tang Prof. Bill David Dr Paulo G. Radaelli Prof. Andy Fitch Crystallography Chemistry Chemistry Chemistry Chemistry SRS ISIS ISIS ESRF Birkbeck Durham Birmingham Liverpool Cambridge DL

RAL RAL Grenoble + Prof. Colin Norris Dr Mike Smith "DIAMOND" "DIAMOND" RAL RAL Presentation for the DIAMOND SAC May 2002 22 Working Party Conclusions User-friendly beamline for the non-expert Ultra high resolution, but

Rapid high-resolution powder diffraction data required in minutes and not in hours!!! Energy range from 5 to 30+ keV As easy to use as the laboratory diffractometer 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 Presentation for the DIAMOND SAC May 2002 23 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 24

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.)

Presentation for the DIAMOND SAC May 2002 25 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 26 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 27 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 28 Instrument Layout Presentation for the DIAMOND SAC May 2002 29 User Community (1) Dr Dr Dr Dr Dr Prof Dr Dr Prof Dr Dr

Prof Dr Dr Dr Dr Dr Prof Mr Dr Dr Prof. Prof I Abrahams D R Allan PA Anderson M P Attfield JP Attfield P Barnes PD Battle A M T Bell P G Bruce

S G Carling M A Carpenter RJ Cernik J Charmant SJ Clarke S Clarke JK Cockcroft JM Cole H M Colquhoun L M D Cranswick SE Dann C N W Darlington W I F David P Day Department of Chemistry, Queen Mary and Westfield College Department of Physics and Astronomy, University of Edinburgh School of Chemistry, University of Birmingham School of Crystallography, Birkbeck College, University of London

Department of Chemistry, University of Cambridge School of Crystallography, Birkbeck College Inorganic Chemistry Laboratory, University of Oxford Department of Earth Sciences, University of Manchester School of Chemistry, University of St Andrews Royal Institution of Great Britain Department of Earth Sciences, University of Cambridge Daresbury Laboratory School of Chemistry, University of Bristol Department of Chemistry, University of Oxford Department of Chemistry, University of Cambridge School of Crystallography, Birkbeck College Department of Chemistry, University of Cambridge Department of Chemistry, University of Reading School of Crystallography, Birkbeck College, University of London Department of Chemistry, Loughborough University School of Physics and Astronomy, University of Birmingham ISIS, Rutherford Appleton Laboratory Royal Institution of Great Britain Presentation for the DIAMOND SAC May 2002 30 User Community (2) Dr Dr Dr

Prof Dr Dr Dr Prof Dr Dr Dr Prof Prof Dr Dr Dr Dr Dr Dr Dr Dr Dr Dr MT JSO AJ R CJ AE

DH KDM WTA A PD CMB JAK JA MJ S RM JTS AP RH DA P AJ Dove Evans Florence Freer Gilmore Goeta Gregory Harris Harrison

Harrison Hatton Henderson Howard Hriljac Hudson Hull Ibberson Irvine Jephcoat Jones Keen Lightfoot Markvardson Department of Earth Sciences, University of Cambridge Department of Chemistry, University of Durham Department of Pharmaceutical Sciences, University of Strathclyde Materials Science Centre, University of Manchester/UMIST Department of Chemistry, University of Glasgow Department of Chemistry, University of Durham School of Chemistry, University of Nottingham School of Chemistry, University of Birmingham Department of Chemistry, University of Aberdeen Department of Chemistry, University of Edinburgh Department of Physics, University of Durham Department of Earth Sciences, University of Manchester

Department of Chemistry, University of Durham School of Chemical Sciences, University of Birmingham Department of Chemistry, University of Reading ISIS, Rutherford Appleton Laboratory ISIS, Rutherford Appleton Laboratory School of Chemistry, University of St Andrews Department of Earth Sciences, University of Oxford Department of Chemistry, Keele University ISIS, Rutherford Appleton Laboratory School of Chemistry, University of St Andrews ISIS Facility, Rutherford Appleton Laboratory Presentation for the DIAMOND SAC May 2002 31 User Community (3) Prof Dr Dr Prof Dr Dr Dr Dr Dr Prof Dr

Prof Prof Dr Dr Dr Dr Dr Dr Prof Prof Dr Dr RE KU DM AG S RF CR K PR P SAT LVC MJ N

K SJ PR M CC BK DP AD M Morris Neumann O'Hare Orpen Parsons Pettifer Pulham Prassides Radaelli Raithby Redfern Rees Rosseinsky Shankland Shankland Skinner Slater

Sahibzada Tang Tanner Thompson Taylor Tremayne School of Chemistry, University of St Andrews Department of Physics, Loughborough University Inorganic Chemistry Laboratory, University of Oxford School of Chemistry, University of Bristol Department of Chemistry, University of Edinburgh Department of Physics, University of Warwick Department of Chemistry, University of Edinburgh School of Chemistry, University of Sussex ISIS Facility, Rutherford Appleton Laboratory School of Chemistry, University of Bath Department of Earth Sciences, University of Cambridge Department of Chemistry, University of Edinburgh Department of Chemistry, University of Liverpool Department of Pharmaceutical Sciences, University of Strathclyde ISIS Facility, Rutherford Appleton Laboratory Department of Materials, Imperial College, London Department of Chemistry, University of Surrey Department of Materials, Imperial College, London SRS Facility, Daresbury Laboratory Science Laboratories, University of Durham

Dept. MMME, Materials Division, University of Newcastle Upon Tyne Director of Isis, Rutherford Appleton Laboratory School of Chemical Sciences, University of Birmingham Presentation for the DIAMOND SAC May 2002 32 User Community (4) Dr Dr Prof Prof Dr Dr Prof R DJ MT BTM CC PA KRA Walton Watkin Weller

Willis Wilson Wright Ziebeck School of Chemistry, University of Exeter Chemical Crystallography Laboratory, University of Oxford Department of Chemistry, University of Southampton Chemical Crystallography Laboratory, University of Oxford ISIS, Rutherford Appleton Laboratory School of Chemistry, University of St Andrews 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 33 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-StatePhysicists, Earth & Material Scientists,.... Presentation for the DIAMOND SAC May 2002 34 THE END Questions & Discussion Presentation for the DIAMOND SAC May 2002 35

Recently Viewed Presentations

  • Subject Variable in Sentences - Ottawa TMG-UG

    Subject Variable in Sentences - Ottawa TMG-UG

    A typical sentence reads: "He was a Farmer with real estate valued at $2,100 (worth $52,888 in 2012 dollars)." I would suggest: …real estate valued at $2,100 ($53,000 in 2012)... Including more digits, especially the cents, suggests a lot more...
  • Investments - California State University, Northridge

    Investments - California State University, Northridge

    You have a ticket to a Dodgers game, ticket worth $60. On the day of the game there is a big rain. Although you can still go to the game and the game is playing, the rain will reduce the...
  • The Big Momma

    The Big Momma

    Use the Quotation Sandwich method. TOP SLICE Introduce the claim (You may quote a source here, too.) MEAT Embed the quote in your own sentence that supports the claim. Do not begin any sentence with quotation marks!! BOTTOM SLICE Provide...
  •  Macroevolution  The result of repeated speciation events  Evidences

    Macroevolution The result of repeated speciation events Evidences

    Von Baer's Law features common to all members of major phylogenetic group of animals develop earlier in ontogeny than do features that distinguish subdivisions of the group Evidences for macroevolution from the field of paleontology Confirmation of fossil age Strata...
  • The Metalworking Lathe - McLean County Unit District No. 5

    The Metalworking Lathe - McLean County Unit District No. 5

    The Metalworking Lathe. Unit 58. Metalwork Technology and Practice. ... Removing a bent ring is painful!!! Safety Precautions. Know your lathe parts. ... Move the carriage out of the way or down the bed while polishing, filing, cleaning, and when...
  • Physics - LAWRENCE MCNEIL, PH.D.

    Physics - LAWRENCE MCNEIL, PH.D.

    When the LRAC curve has a clear minimum point, then any firm producing a different quantity will have higher costs. In this case, a firm producing at a quantity of 10,000 will produce at a lower average cost than a...
  • SMP on SMBH Are these two empirical laws

    SMP on SMBH Are these two empirical laws

    Conclusions for the magnitude of dynamical friction in dark halos: the reason for efficient mergers Rotation and flattening of elliptical galaxies: only a weak connection Even the fantastic resolution of the VLBI radio interferometry cannot resolve the central engine. The...
  • Insurance accounting change FASB Exposure Draft

    Insurance accounting change FASB Exposure Draft

    Increase the decision usefulness of the information about the nature, amount, timing, and uncertainty of cash flows related to long-duration insurance contract assets and liabilities, and the effect on the financial statements. Improve the financial statement comparability of insurance entities...