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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

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
YBa
2
Cu
3
O
7
-
x
,
Nature
,

327
, 310
-
312 (1987)


Superconductivity near 30
-
K without copper
-

the
Ba
0.6
K
0.4
BiO
3

Perovskite,
Nature
,

332
, 814
-
816 (1988)


Synthesis and superconducting properties of the strontium
copper oxy
-
fluoride Sr
2
CuO
2
F
2+
d
,
Nature
,

369
, 382
-
384 (1994)


Cation effects in doped La
2
CuO
4

superconductors,
Nature
,

394
, 157
-
159 (1998)


Systematic cation disorder effects in L
1.85
M
0.15
CuO
4

superconductors,
Phys. Rev. Lett
.
,

83
, 3289
-
3292 (1999)

Presentation for the DIAMOND SAC May 2002

5

Science


MgB
2

and Borocarbide Superconductors:


Structure of the 13
-
K superconductor La
3
Ni
2
B
2
N
3

and the
related phase LaNiBN",
Nature
,

372
, 759
-
761 (1994)


MgB
2

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


C
60

and its Superconducting Derivatives:


Superconductivity at 28 K in Rb
x
C
60
,
Phys. Rev. Lett.
,

66
,
2830
-
2832 (1991)


Intercalation of ammonia into K
3
C
60
,
Nature
,

364
, 425
-
427
(1993)


Crystal
-
structure, bonding, and phase
-
transition of the
superconducting Na
2
CsC
60

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
ZrW
2
O
8
,
Science
,

272
, 90
-
92 (1996)


Compressibility, phase transitions, and oxygen migration in
zirconium tungstate, ZrW
2
O
8
,
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
:LiCF
3
SO
3
,
Science
,

262
, 883
-
885 (1993)



Synthesis of layered LiMnO
2

as an electrode for
rechargeable lithium batteries,
Nature
,

381
, 499
-
500 (1996)


Structure of the polymer electrolyte poly(ethylene
oxide)
6
:LiAsF
6
,
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 [SnSe
4
] (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: LaSrCoO
3
H
0.7
,
Science
,

295
, 1882 (2002)


New Dielectric Materials:


Enhancement of the dielectric
-
constant of Ta
2
O
5

through
substitution with TiO
2
,
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 La
1
-
x
Ca
x
MnO
3

with x=0.25 and 0.50,
Phys.
Rev. Lett.
,

75
, 4488
-
4491 (1995)


Colossal magnetoresistance without Mn
3+
/Mn
4+

double
exchange in the stoichiometric pyrochlore Tl
2
Mn
2
O
7
,
Science
,

273
, 81
-
84 (1996)


Lattice effects and magnetic order in the canted
ferromagnetic insulator La
0.875
Sr
0.125
MnO
3+
d
",
Phys. Rev.
Lett.
,

76
, 3826
-
3829 (1996)


Direct observation of lattice polaron formation in the local
structure of La
1
-
x
Ca
x
MnO
3
",
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 Fe
2
OBO
3
,
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 Ir
3+

and Ir
4+

octamer and spin
dimerisation in the spinel CuIr
2
S
4
,
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 T
3
R
3

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

0
20
40
60
80
100
120
140
160
Number of Publications
1990
1991
1992
1993
1994
1995
1996
1997
1998
1999
2000
2001
UK Publications
Total Publications

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


Positive 2
q

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
q

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

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 END


Questions & Discussion