“Energy Materials at ISIS”

1. Energy materials at ISIS
CNR Roadshow
ASI, Sala Cassini
May 27th 2014
Martin Owen Jones
ISIS Facility, Rutherford Appleton Laboratory

2. MEXT visit
Hard
So(
mul,disciplinary
condensed
ma4er
science
1960
1970
1990
1980
2000
1960
1970
1990
1980
No
One
Experiment

3. Length Scales

4. Studies
of
fabrica,on
processes
Novel
fuel
sources
for
cars
CO2
sequestra,on
Hydrogen
storage
Photovoltaics
Electrolytes
Fission
Catalysis
Novel
fuel
cells
High
performance
ba4eries
Lowering
exhaust
emissions
Advances
in
energy
conversion
Lower
emission
levels
of
pollutants
Significant
improvements
in
energy
storage
New
environmentally
friendly
materials
by
ra,onal
design
CLEAN
POWER:
MATERIALS
ISSUES
10-­‐10m
Macromolecules
(hydrogenase)
10-­‐8m
Reheater
tubing
failure
1m
Nuclear
industry
Li
ba4eries
10-­‐2m
p-­‐n
junc,ons
10-­‐6m
photovoltaics
fuel
cells 10-­‐4m
X-­‐ray
&
neutron
diffrac,on
EXAFS
Inelas,c
neutron
&
X-­‐ray
sca4ering
Computa,onal
modelling
(DFT
/
MD)
Small-­‐angle
X-­‐ray
&
neutron
diffrac,on
X-­‐ray
&
neutron
reflectometry
Protein
crystallography
First
principles
device
modelling
X-­‐ray
&
neutron
reflectometry
X-­‐ray
tomography
Device
design
High
energy
X-­‐ray
diffrac,on
Neutron
&
X-­‐ray
residual
stress
analysis
atomic
understanding

5. CASE
STUDIES

6. View
of
CO2
(top)
and
SO2
(bo4om)
sited
in
the
pore
of
NOTT-­‐300(Al)
as
determined
by
PXRD
(I11
Diamond),
inelas,c
neutron
sca4ering
(TOSCA,
ISIS)
and
DFT
analysis
(aClimax,
ISIS).
Scien0fic
discovery
offers
‘green’
solu0on
in
fight
against
greenhouse
gases
• UK
researchers
have
created
a
low
cost,
new
material
that
can
capture
harmful
gases
• The
porous
material,
NOTT-­‐300,
has
the
potenOal
to
reduce
fossil
fuel
emissions
through
cheaper
and
more
efficient
capture
of
polluOng
gases
such
as
carbon
dioxide
(CO2)
and
sulfur
dioxide
(SO2)
• TOSCA
and
WISH
at
ISIS
used
to
determine
crystal
structure
and
locate
CO2
and
SO2
within
the
pores
The
crystal
structure
of
NOTT-­‐300
Selec0vity
and
direct
visualiza0on
of
carbon
dioxide
and
sulfur
dioxide
in
a
decorated
porous
host
Sihai
Yang,
Bill
David,
Timmy
Ramirez-­‐Cuesta
et
al
4
887-­‐894
(2012)

7. The
origin
in
capacity
reduc0on
in
transi0on
metal
hydrogen
storage
materials
In-­‐Operando
neutron
diffrac0on
studies
of
transi0on
metal
hydrogen
storage
materials
Kazuya
Kamazawa,
Bill
David,
MarOn
Owen
Jones,
Sam
Callear
et
al
3
39-­‐42
(2013)
• ISIS
and
Toyota
scienOsts
have
revealed
the
origin
in
the
capacity
reducOon
exhibited
by
Ti-­‐Cr-­‐Mn
hydrogen
storage
alloys
• In-­‐Operando
studies
were
performed
using
non-­‐isotopically
enriched
hydrogen
on
GEM
at
temperatures
and
pressures
mimicking
those
uOlised
in
real-­‐world
applicaOons
• The
sequestered
hydrogen
was
found
to
preferenOally
occupy
the
octahedral
and
tetrahedral
intersOOal
sites

8. Mystery
of
car
baGery
material
solved
• researchers
from
Oxford
University,
the
University
of
Bath
and
Trinity
College
Dublin,
ISIS
has
helped
to
reveal
what
makes
lead
oxide
such
a
powerful
electrical
conductor
• Using
theoreOcal
calculaOons,
the
group
were
able
to
show
that
oxygen
vacancies
can
form
very
easily
in
lead
oxide
and
that
oxygen
vacancies
give
metallic
behaviour
by
freeing
up
electrons
to
carry
electrical
current
• Neutron
diffracOon
experiments
on
Polaris
confirmed
that
commercial
lead
oxide
powder
is
oxygen-­‐
deficient
by
showing
that
oxygen
sites
were
1.6%
vacant
Nature
of
the
Band
Gap
and
Origin
of
the
Conduc0vity
of
PbO2
Revealed
by
Theory
and
Experiment
David
O.
Scanlon,
Bill
David,
MarOn
Owen
Jones
et
al.
107
246402
(2011)
A
lead-­‐acid
ba4ery
Forma,on
energies
for
intrinsic
defects
under
O-­‐rich
(le()
and
O-­‐poor
(right)
condi,ons

9. submi4ed
to
Science
Probing
the
Evolu0on
and
Morphology
of
Hard
Carbon
Spheres
Vilas
G.
Pol,
Bill
David,
Sam
Callear,
Daniel
T.
Bowron
et
al
• researchers
from
ISIS
and
Argonne
NaOonal
Laboratory
have
invesOgated
a
new
lithium
baeery
electrode
material
comprised
of
hard
carbon
spheres
formed
from
HDPE
plasOc
bags
• Electron
microscopy
and
neutron
total
scaeering
experiments
on
NIMROD
showed
that
the
internal
structure
of
the
carbon
spheres
can
be
tailored
to
opOmize
properOes
such
as
lithium
ion
diffusion
and
tribological
properOes
Iden0fying
new
baGery
electrode
materials
2400oC
1
hour
Ar
700oC
1
min
490
PSI
Forma,on
process
for
the
spheres
from
HDPE
plas,c
bags
Total
sca4ering
data
from
NIMROD
HREM
on
samples
heated
to
700oC
(a)
and
2800oC
(b)
(a)
(b)

10. Determining
catalyst
mechanisms
• The
Lindlar
catalyst
is
used
for
selecOve
hydrogenaOon
of
carbon-­‐carbon
triple
bonds
to
double
bonds,
without
the
unwanted
formaOon
of
carbon-­‐carbon
single
bonds,
which
is
a
key
step
in
vitamin
A
synthesis
• Researchers
from
ISIS,
Evonik
Industries
and
Aqura
AnalyOcal
SoluOons
uOlised
neutron
scaeering
on
the
MAPS
spectrometer
to
idenOfy
the
catalyOc
mechanism
Characteriza0on
of
β-­‐Palladium
Hydride
Forma0on
in
the
Lindlar
Catalyst
and
in
Carbon-­‐Supported
Palladium
P.W.
Albers,
K.
Möbus,
C.D.
Frost
and
S.F.
Parker
115
24485-­‐24493
(2011)

11. Dry
reforming
of
methane:
a
use
for
CO2?
• Industrially,
hydrogen
is
produced
by
steam
reforming
of
methane:
CH4
+
H2O
→
CO
+
3H2
An
alternaOve
route
is
to
use
CO2
as
the
oxidant:
CH4
+
CO2
→
2
CO
+
2H2
• The
process
requires
a
Ni(20%)/Al2O3
catalyst,
which
deacOvates
by
carbon
deposiOon
• ScienOsts
at
ISIS,
University
of
Keele
and
University
of
Glasgow
have
used
inelasOc
neutron
scaeering
to
characterise
and
quanOfy
adsorbed
hydrocarbon
and
hydroxyls
determining
that
most
of
the
CO2
is
converted
to
valuable
CO
and
that
the
catalyst
is
very
efficient
at
cycling
hydrogen
but
not
carbon.
Data
from
the
MAPS
neutron
spectrometer
at
ISIS
iden,fying
C-­‐H
and
O-­‐H
stretches
A
methane
reforming
plant
Quan0fica0on
of
surface
species
present
on
a
nickel/alumina
methane
reforming
catalyst
I.
P.
Silverwood,
C.
D.
Frost,
S.
F.
Parker,
D.
Lennon
et
al
12
3102–3107
(2010)

12.
The
propeller-­‐shaped
molecules
of
Alq3,which
are
used
as
an
ac,ve
cons,tuent
of
organic
light
emi`ng
diode
(OLED)
displays.
Muons
probe
charge
transport
in
organic
semiconductors
• Electronic
devices
based
on
organic
semiconductors
such
as
Alq3
(tris[8-­‐hydroxy-­‐quinoline]
aluminium)
are
revoluOonising
electroluminescent
displays
and
large-­‐area
electronics
• Even
though
charge
transport
in
such
organic
conductors
is
fundamental
to
their
operaOon,
many
of
its
mechanisms
are
sOll
only
poorly
understood
• ScienOsts
at
ISIS,
the
University
of
Fribourg,
the
University
of
Sheffield,
Queen
Mary,
University
of
London
and
the
Paul
Scherrer
InsOtute
have
used
muons
as
a
local
probe
for
mobile
spin
dynamics
and
charge
carrier
moOon
in
Alq3
as
a
funcOon
of
temperature
to
provide
an
upper
limit
for
the
mobility
that
might
be
achievable
in
high
quality
bulk
organic
semiconductors
Intrinsic
Mobility
Limit
for
Anisotropic
Electron
Transport
in
Alq3
AJ
Drew,
FL
Prae
et
al,
100
116601
(2008)

13. Polymers
for
Organic
Solar
Cells
• Neutron
diffracOon
and
quasielasOc
scaeering
experiments
performed
on
the
OSIRIS
backscaeering
spectrometer
are
used
to
invesOgate
the
structure
and
dynamics
of
conjugated
polymers.
• This
characterisaOon
of
the
structure
and
dynamics
at
the
nanoscale
is
crucial
to
achieve
the
producOon
of
producOon
of
higher
performance
organic
solar
cells.
Polymer
solar
cell
The
Nanoscale
Morphology
of
a
PCDTBT:PCBM
Photovoltaic
Blend
P.
A.
Staniec,
A.
J.
Parnell,
C.
Kinane,
R.
M.
Dalgliesh
et
al,
1(4)
499
(2011)
neutron
sca4ering
experiments
help
to
improve
understanding
of
device
structure

14. In-­‐situ
ionic
conduc0vity
analysis
d-spacing
• Simultaneous
neutron
diffracOon
and
ionic
conducOvity
measurements
have
been
carried
out
at
the
ISIS
facility
• Researchers
from
ISIS
and
Heriot
Wae
University
have
developed
sample
environment
that
allows
simultaneous
measurements
of
ionic
mobility
and
structure
• Using
the
POLARIS
neutron
diffractometer,
the
team
has
been
able
to
study
lithium
and
proton
conducOvity
in
potenOal
baeery
and
proton
conductor
materials
Ionic
mobility
and
structure
sample
environment
apparatus
Typical
ionic
conduc,vity
(lower)
and
neutron
diffrac,on
data
collected
simultaneously
on
the
POLARIS
diffractometer

15. In-­‐situ
gravimetric
and
structural
characterisa0on
• ScienOsts
from
the
University
of
Oxford
and
ISIS
have
developed
sample
environment
to
simultaneously
study
the
structure
and
thermogravimetric
properOes
of
hydrogen
storage
materials
–
the
intelligent
gravimetric
analysis
apparatus
for
neutrons,
IGAn
• The
apparatus
allows
controlled
gas,
temperature
(to
500oC)
and
pressure
(20bar)
environments
to
be
used
to
invesOgate
gas
uptake,
desorpOon
and
cycling
in
hydrogen
storage
materials
on
the
HRPD,
WISH
and
GEM
neutron
diffractometers
at
ISIS
d-spacing
The
IGAn
apparatus
Sample
thermogravimetric
(le()
and
diffrac,on
(right)
data
collected
on
the
GEM
neutron
diffractometer
using
the
IGAn

16. Simultaneous Neutron-Raman Scattering
Cisplatin, a platinum-containing
anticancer drug (JPC B, in press)

17. POLARIS
:
REACTION
CELLS
In
progress
Microwave
characterisaOon
cell
(Cardiff
+
ISIS).
ConcentraOon
cell
(St
Andrews
+
ISIS).

18. Fin

19. Detec0ng
radioisotopes
• ScienOsts
from
ISIS
and
Cardiff
University,
in
conjuncOon
with
Magnox,
are
developing
a
rapid,
selecOve
method
for
the
detecOon
and
speciaOon
of
transuranic
radioisotopes
such
as
Np,
Pu,
Am
and
Cm
in
soluOon
• A
range
of
water
soluble
complexing
agents
have
been
synthesised
that
display
selecOvity
towards
the
radionuclides
of
interest,
bind
to
a
specific
radionuclide
caOon
and
separate
them
from
the
soluOon
out
within
a
microemulsion.
• Small
angle
neutron
scaeering
(SANS)
is
used
to
probe
the
separaOon
within
the
microemulsion
system
and
to
discover
unique
complexing
agent
–
metal
caOon
combinaOons.
Hydrophobic
ligands
selec,vely
sequester
ions
and
transport
them
to
specific
places
within
microemulsion
systems
for
detec,on.
SANS
studies
of
the
effects
of
surfactant
head
group
on
aggrega0on
proper0es
in
water/glycol
and
pure
glycol
systems
C.
Seguin,
J.
Eastoe,
R.
K.
Heenan,
I.
Grillo,
315
714
(2007)

20. Porosity
in
ac0vated
carbons
• ScienOsts
at
ISIS,
the
University
of
Salford
and
Chemviron
Carbon
Ltd
are
invesOgated
acOvated
carbon
materials.
• AcOvated
carbons
are
of
interest
for
hydrogen
storage
because
hydrogen
molecules
can
be
trapped
on
the
carbon
surface
• The
use
of
small
angle
neutron
scaeering
(SANS)
and
contrast-­‐matching
liquids
allows
accurate
measures
of
carbon
density
and
thus
hydrogen
storage
capaciOes
• SANS
data
also
allow
us
to
compare
the
accessible
pore
volumes
at
each
parOal
pressure
with
those
obtained
gravimetrically.
SANS
data
as
a
func,on
of
toluene
par,al
pressure.
The
inset
shows
a
comparison
between
SANS
and
gravimetric
data
The
use
of
small
angle
neutron
scaGering
with
contrast
matching
and
variable
adsorbate
par0al
pressures
in
the
study
of
porosity
in
ac0vated
carbons
Z.
Mileeva,
D.
K.
Ross,
D.
Wilkinson,
S.
M.
King
et
al
50
5062
(2012)

21. Earth
Science
Studying
ferropericlase
helps
understanding
of
earthquakes
Chemistry
catalyst
for
conversion
of
carbon
dioxide
to
cyclic
carbonates
Cultural
Heritage
understanding
molecular
processes
of
preservaOon
of
polychrome
carved
wood
Engineering
3-­‐D
high
speed
tomography
Environmental
Science
Electric-­‐field-­‐induced
phase
transformaOons
in
lead-­‐free
piezoelectric
ceramics
Life
Sciences
Structure
and
history
of
viruses
Physics
and
Materials
Science
MagneOc
contrast
imaging
for
FeRh
films