“Big Science and Materials -

Opportunities, Breakthroughs and the

Future”

The 53rd Hatfield Memorial Lecture

Professor John Wood FREng

6 December 2005

University of Sheffield

‘CCLRC’ – Council for the Central Laboratory of the

Research Councils

The CCLRC:

• operates world-class large-scale research facilities;

• provides strategic advice to the government on their development;

• manages international research projects in support of a broad

cross-section of the UK research community.

CCLRC is one of Europe's largest multidisciplinary research

organisations supporting scientists and engineers world-

wide and is one of eight Research Councils in the UK.

The Research Council Family

CCLRC

UK Government

DTI

Office of Science &

Technology

EPSRCPPARC NERC BBSRC MRCESRC

Daresbury

Laboratory

Rutherford Appleton

Laboratory

Chilbolton

Observatory

AHRC

The CCLRC Facilities offer a diversity of experimental

techniques which are not only complementary to each other, but

also to more traditional techniques used by materials scientists.

The physical characteristics of large research facilities offer new

opportunities for researchers, such as time resolved studies in a

broad range of areas:

• Super conductivity

• Joining techniques

• Radiation hard materials

• Electronic and photonic materials

• Surface properties

A variety of ‘case studies’ will be presented

The CCLRC sites

Three world class

research laboratories…

2

CCLRC Daresbury

Laboratory

Cheshire

1

CCLRC Rutherford

Appleton

Laboratory

Oxfordshire

3

CCLRC Chilbolton

Observatory

Hampshire

1

2

3

Portfolio of Current Facilities

Neutrons ISIS Pulsed Neutron Source, RAL

ILL Grenoble

Photons SRS, Daresbury

ESRF, Grenoble

Central Laser Facility, RAL

Supercomputing HPCx, Daresbury

….. a unique toolkit for materials scientists

ISIS Experimental

Facility

Central Laser

Facilities Astra &

Vulcan

SRS Experimental

Facility

Institut Laue Langevin

European Synchrotron

Radiation Facility

The HPCx Project

Operated by University of

Edinburgh and Daresbury

First Tera-scale research

computing facility in the UK

Largest academic HEC facility in

Europe; 2nd largest in the world

Funded by EPSRC, NERC,

BBSRC for capability large-scale

simulations

Portfolio of Current Programmes

Particle Physics

Computational Science

and Engineering

Space Science

and Technology

Engineering and

Instrumentation

Hard

Soft multidisciplinary condensed matter science

1960

1970

1990

1980

The impact of neutrons…

Length and Timescales

Complementary techniques, both conventional and state-of-the-art, offer a

broad range of options for the materials scientist.

Structural materials

CASE STUDY 1

A prototype wingbox typical of that

used on Very Large Aircraft being

manipulated on the ISIS ENGIN-X

instrument

Airbus wing spar being examined

on the ENGIN-X instrument at ISIS

Accommodation of Large Scale Engineering Structures

Intergranular stresses in engineering alloys

0 2000 40000

100

200

300

400

500

Elastic strain magnitude ?106Applied stress ma

0 2000 4000

000210-11

Compression Tension

In situ mechanical testing on

ENGIN-X diffractometer

Internal stress and selective transformation in TRIP steels

Microstructural evolution

Interphase stress generation Selective austenite transformation

austenite

back stress

Optimising residual stresses in inertia friction welds

Rolls-Royce plc. Compressor rotor factory (CRF)

400

600

600

800

800

100

0

1000

1200

2

1

0

-1

-2

R/mm

0 1 2 3 4 5

z/mm

As welded

200300

300

300

400

400 4

00

2

1

0

-1

-2

R/mm

0 1 2 3 4 5

z/mm

5h 810°C

Modified PWHT

1500 MPa

400

500

600

600

600

700

700

800

800

2

1

0

-1

-2

R/mm

0 1 2 3 4 5

z/mm

5h 760°C

Conventional PWHT

1000 MPa

unacceptable

Prototype welded ring

In-situ Non Destructive Testing of Jet Engines

FaME38 provides support to enable European materials engineers to

make the best use of the advanced neutron and synchrotron X-ray

scientific facilities at ILL-ESRF.

FaME38 services include:

• Microstructure characterisation

• Sample metrology

• Sample positioning

• Test rigs

• Furnaces

• Virtual beamline

FAME38 at the ILL and ESRF Grenoble

Aerodynamics of Helicopter Blades

Air flow around rotating

helicopter blades simulated by

solving the continuum

equations of fluid dynamics – a

demanding application, even for

HPCx.

Vortices thrown off by one blade

encounter the next blade as it

rotates.

Collaboration with Chris Allan (Bristol) UK Applied Aeronautics Consortium

Variant selection in shape memory materials

0 50 100 150 200 250 300

0.4

0.6

0.8

1

1.2

1.4

A li d S [MP ]

intensity / (init

111

200 311

220

202

113

002

1.0 1.5 2.0 2.5 3.00.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

Inte

nsity

d-spacing [10-10m]

Austenite

1.0 1.5 2.0 2.5 3.0

0.05

0.10

0.15

0.20

0.25

Inte

nsity

d-spacing [10-10m]

Martensite

ParentMartensiteMartensiteCoolStress loadHeatStress

NiTi

Fe-30.5at%Pd

Materials processing

CASE STUDY 2

646260585654525048464442403836343230282624222018161412

70

65

60

55

50

45

40

35

30

25

20

15

10

5

0

-5

-10

-15

-20

-25

-30

-35

Structure 100.00 %

XRD of alumina in 0.1s cooling at 105 deg min-1

Ceramic Formation from Molten Alumina

N. Greaves, Aberystwyth

2.4 2.6 2.8 3.00.00

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

0.09

0.10

2s

1s1900 C

1600 C

30 C

2600 C

Norm

aliz

ed W

AX

S inte

nsity

Q(A-1)

0.02 0.03 0.04 0.050.00

0.01

0.02

0.03

0.04

0.05

0.06

0.07

1900 C

1600 C

30 C

2600 C

Norm

aliz

ed S

AX

S inte

nsity

Q(A-1)

Ceramic formation from molten alumina

SAXS WAXS

liquid

crystallisation

100,0

00 d

egre

es

per m

inute

liquid

recalescenc

e

The Structure of Liquids in Real Time

Zeolites: The Oil Industry and Consumer Products

Camblor et al, Angew. Chem., Intl. Ed. Eng., 37,

2122-2126, (1998)

X-ray diffraction and X-ray absorption

spectroscopy have been used extensively to

support research into catalysts by industrial

scientists. Applications include catalysts

used in the oil refining process and those

used in washing powder.

Combined SAXS/WAXS study of Zeolite A

formation from clear solution

Q(1/nm)

SAXS

2 Theta

WAXS

Precursor particles Zeolite LTANano-sized particles

Tim

e (m

ins)

Tim

e (m

ins)

"Powder Materials Processing"

• Direct observation of powder filling of dies

• Simulation of powder agglomeration

• Localised density distribution in sintered materials

• Real time observations of crack growth during testing

TiO2 probe Withdrawal

How does Rock Salt Dissolve in Water?

Set up a small crystal of

NaCl surrounded by water

molecules, at a certain

temperature, and let the

system evolve classically

according to Newton’s

Laws of motion.

It’s quite rare for an ion to

move out of the crystal into

the solution – a challenge

for simulation methods.

Collaboration with Art Voter (Los Alamos)

Surface properties

CASE STUDY 3

Real time reduction/oxidation experiments

reduction/oxidation cycles of iron-molybdenum-

based catalyst at ~500ºC

H2 O2H2 O2

slower collection:

1 reduction + 1 oxidationcycle

Collection: 120 30 s = 60 min.

showing near-instantaneous

structural change during oxidation

and more gradual change during

reduction

fast collection:

just 1 oxidation cycle

Collection; 120 2 s = 4 minutes

showing, even on this time

framing, an extremely rapid

change.

Hydrogen sorption of Nb-catalysed, nanostructured Mg

Materials for Energy

Research

CASE STUDY 4

From renewables to nuclear there are significant

challenges for materials research ……

Materials

e.g. battery cathodes: LiMn2O4

fuel cells ZrO2: CsHSO4

hydrogen storage: CHxH, Li, O mobility

CsZrMnSOCLiH

X-rays

neutrons

Materials with mobile light atoms in the presence of heavy atoms

Clean power – neutron and X-ray probes

Structural Chemistry and Physics

Energy for the future

Mg2FeH6 Clathrate hydrates

Chemical Activity and Molecular Motions

0.2 0.40.8 0.6 0.4 0.20.2 0.40

200

400

600

800

1000

LX

( , , )( , ,0)

LiD, a Very Simple Model System

K

Fre

qu

en

cy/c

m-1

( ,0,0)LiH … CsH : Model systems

0 400 800 1200 1600 2000 2400 2800 3200

0 200

S(Q

,)/

Arb

. U

nits

Neutron Energy Loss/cm-1

Ti/NaAlH4 as measured Calculated Spectrum

NaAlH4 with Ti catalystAlnH3n clusters formed on the Ti

Catalysis, fuel cells

Powder neutron diffraction

of lithium nitridometallates Li3-x-yMxN, M=Co, Ni, Cu

The structural studies have enabled

control to be established over the precise

stoichiometry, ordering effects and Li

vacancy concentrations. These factors

are crucial in determining transport

properties

853 K

853 K

963 K

Powder neutron diffraction has been

used to determine the crystal structures,

thus revealing the defect chemistry.

• NERC e-ENV e-science

project

• Study of candidate

materials for long-term

storage of radioactive

elements

• Radiation damage to bulk

and surface

• Formation and stability of

defects, amorphisation and

percolation

• DL_POLY 3 - molecular

dynamics - domain

decomposition

• Zirconia - 5 million atoms

• Double damage event

Radiation Damage – Storage

Natural and Biomimetic

Materials

CASE STUDY 5

Natural laminate structures

Using SR to see the wood from the trees

glucoseglucose

cellulosecellulose

Structural Biology Programmes

Prof. J. Walker - 1997 Nobel PrizeProf. J. Walker - 1997 Nobel Prize

F1 F1 ATPaseATPase structure structure

Biomedical Applications

Muscle

Breast Brain

Sperm

The study of a diverse range

of biological systems,

particularly in real time, has

presented many challenges.

Advances in instrument and

detector development for

these systems have

benefited the physical and

materials research

communities

Synthetic Polymers as Artificial Muscles?

• Reversible phase

change due to external

stimuli response.

• pH, solvent composition

and temperature

pH = 3.5pH = 7.6

Swelling of a triblock gel

1 mm

Ryan, Howse, Sheffield University

Steve Scott, Leeds University

Non-invasive probing of bones through tissue

Two novel approaches for thenon-invasive probing ofdiffusely scattering mediabased on laser spectroscopyhave been pioneered at theCentral Laser Facility

– potential applicationsinclude disease diagnosis(e.g. osteoporosis, cancer)and quality control inpharmaceutical industry.

Cultural Heritage

CASE STUDY 6

Cultural Heritage

Engineering, Materials Science and other applications

Axes, coins, statues, helmets, spoons, marbles, pots …

Making techniques of prehistoric (4000 BC)

copper axes from the Alpine region

Neutron Archaeometry

• Metallurgists and ceramicists are engaged intexture research to develop materials withfavourable properties.

• In contrast, geologists and archaeologistsare using textures to interpret the past.

• Neutron texture data are representative ofbulk material properties

• Neutron diffraction is increasingly used tomeasure texture and strain, withinstrumentation dedicated to theses tasks.

1600 1200 800

Absorbance /Wavenumber (cm -1)

1650

1542

1450

1400

13221240

1172

10781044

carminic acid

protein material

CaC2O4·nH2O

15th century Catalan gothic altarpiece by Jaume Huguet.

FTIR of the red pigment shows the presence

of carminic acid. The presence of alum was

determined by SR X-ray diffraction and SEM-

EDX, this compound is used to precipitate

the lake pigments. This pigment is related to

ancient textile activity.

The Nature of Medieval Synthetic Pigments

• King Henry VIII’s flagship which sank in

1545 and was raised in 1982

Sulphur damage to the timbers of the

Mary Rose

• Water-logged woodcontains sulphur whichcan turn acidic onexposure to air

• SRS facilities have beenused to unravel theunderlying sulphurchemistry

The next generation

facilities….

3rd Gen. SR

2nd Gen. SR

Laser Slicing

SPPS

Initial

H.-D. Nuhn, H. Winick

Pe

ak

Bri

gh

tne

ss

[P

ho

t./(

s ·

mra

d2 ·

mm

2 ·

0.1

%b

an

dw

.)]

FWHM X-Ray Pulse Duration [ps]

Future

Future

ERLs

X-Ray FELs

InitialUltrafast x-ray sources willprobe space and time withatomic resolution.

Peak brightness of pulsed X-ray sources

what do we do today

and

what tomorrow?

ISIS 2nd Target Station

Diamond Light Source

SNS Oak Ridge USA

Schematic layout of a single pass XFEL

A new X-ray source is needed for

studies of new, of non-equilibrium states of matter

at atomic resolution in space and time

The Future – Inertial Fusion

ITER (International Thermonuclear

Experimental Reactor) is the

experimental step between today’s

studies of plasma physics and

tomorrow's electricity-producing

fusion power plants.

It is based around a hydrogen plasma

torus operating at over 100 million °C,

and will produce 500 MW of fusion

power.

International project involving China,

the EU and Switzerland, Japan, Korea,

the Russian Federation, and the USA..

Ready to start construction and the

first plasma operation expected in

2016.

International Fusion

Materials Irradiation

Facility (IFMIF)

Challenges for the future

• Improvements in detectors

• New sample handling methods

• Vast volumes of data to handle

• Different ways of accessing the facilities

CCLRC Detector capability

• gas filled detectors

– wires, microstrips

• solid state detectors

– strips, hybrid pixels, active pixels

• microelectronics and data acquisition

– signal extraction, processing, acquisition

Gamma rays to infra red, charged particles and

neutrons

BASIC

PIXELS

ADVANCED

PIXELS

ADVANCED

PIXELS

4m

m

10mm

Time-of-flight 20us

Photon Trace on Sensor

Binary image of

pixels hit along

the way

Sparse (Binary) Image Sparse (Timed) Image

Timing information

from hit pixels gives

80ns resolution

Single Frame

Moving Image Timed Capture

Basic Technology MI3 Development Sensor (J Crooks)

• Analogue-to-digital

conversion

• DRAM storage

• Logic to explore

"intelligent" functionality,

such as sparse readout

• fast frame imaging: ~5000

frame/sec

• timing capture: 80ns

timing resolution of bright

laser / particle events

‘Intelligent’ Digital Pixel sensors

Collaboration with Prof. Nigel

Allinson, Sheffield

Several long-baseline (~km long) interferometric gravitational wave

detectors are in operation around the world

– Aim is to detect the effects, on test masses on the Earth,

of gravitational waves generated by astrophysical sources

– Gravitational waves are fluctuations (‘ripples’) in spacetime caused

by the acceleration of mass (differential strain in space)

– These signals should provide unique information about astrophysical

objects like supernovae, neutron stars-pulsars, black holes and

interactions in the early Universe

– Signals are very weak – detection requires construction of very

sensitive optical instrumentation

– Considerable research ongoing on – high quality optics and

coatings

Gravitational Wave Detectors

Detect their effects on the motion

of mirrors in Fabry-Perot/Michelson

Interferometers

Gravitational waves have very weak

effect: Expect mirror movements of

less than 10-18 m over arm lengths of

4km

Detection of Gravitational Waves -

challenges

4km

Need substrates and coatings which:

(a) withstand ~108W/m2 of continuous laser

power at 1064nm on coated mirror

(~700kW/m2 through the mirror).

Need:• low optical absorption

• high substrate thermal conductivity

(b) low levels of Brownian motion

Different substrate materials under study: eg

fused silica, sapphire, silicon + othersLIGO fused silica mirror (10kg)

in suspension cradle

Sample handling – Stem Cells

Gelatin micro scaffolds are manufactured

by the Central Microstructure Facility.

The scaffolds are used as support

structures to align growing human stem

cells which will be used to form

connections between the spinal column

and the brain in paralysis patients.

Thermal Bimorph Actuators

Piezoresistive Sensor

TrackActivation Track

Signal lines

distributed to contact

pads

Sample handling - Laser Tweezers

A mist of decane aerosol

droplets (1-7 microns) was

produced using ultrasonic

nebulisation techniques

These were optically trapped

using the Raman Tweezers

apparatus

– Stable for 30 minutes

– Raman Spectra collected

from a single droplet

– Controlled droplet collisions

Applications– Atmospheric and

Environmental Chemistry– Fast stopped-flow reactions

0

2000

4000

6000

8000

10000

12000

14000

16000

750 1000 1250 1500 1750 2000 2250 2500 2750 3000

Raman shift (relative wavenumber)

Inte

ns

ity

(a

rbit

rary

un

its

)

Droplet

Bulk

The X-ray free-electron lasers

will provide coherent radiation

of the proper wavelength and

the proper time structure,

so that materials and the

changes of their properties

can be portrayed at atomic

resolution in four dimensions,

in space and time.

Diffraction pattern of 10 x 10 x 10 Au cluster

Fascination - FELs for hard X-rays

Firmenam e (Referentennam e)28

Coulomb explosion of lysozyme (50 fs)Coulomb explosion of Lysozyme LCLS

Radiation damage

interferes with atomic

scattering factors and

atomic positions

50 fs

3x1012 photons/100 nm spot

12 keV

R. Neutze, R. Wouts, D. van der Spoerl, E. Weckert, J. Hajdu: Nature 406 (2000) 752-757

t=0

t=50 fsec

t=100 fsec

Coulomb Explosion of Lyzosyme

Future directions and new

opportunities for materials

research

Where next for the materials

scientist?

Next generation facilities

more intense

brighter

wavelength optimised

increased compute power

New capabilities

smaller samples

more dilute samples

increased time resolution

‘Dirty’ & complex real systems

• In-situ online materials processing

• Real time materials imaging

• Reaction monitoring under extreme conditions

• Follow processes as ‘molecular movies’

Energy for the futureDrug design and pharmaceuticals

BiotechnologyMaterials and processing

Priority scientific areas for the next decade

Communications

Opportunities for Industry as a Supplier

Facilities such as ITER, IFMIF, the Linear Collider, XFEL and 4GLS

will require partnership with industry to develop for example:

• Superconducting cavities/solenoids

• Next generation materials for target materials and vessel

construction

The next generation facilities will present new technological

challenges which will enable UK industry to engage as

suppliers in their construction and commissioning.

…. but also equally importantly there will be key advantages

for industry by exploitation of these facilities

What opportunities will this bring for industry?

• To think beyond the traditional laboratory work bench

• To consider solving previously intractable problems

• To have ease of access to a powerful analytical toolkit

Competitive advantage for

companies taking advantage

of this extended portfolio of

instruments

Opportunities for Industry as a User

The work described has involved several

international and national collaborations between

academic colleagues and CCLRC staff.

Special thanks to Dr. Liz Towns-Andrews for

putting together the presentations and interfacing

with the many internal staff involved.

Acknowledgements

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