Ordering Kinetics
in Nanoscale Systems
Present Experiments
and Future Applicationsat an ERL Light Source

Detlef-M. Smilgies

Smilgies - IMSS Symposium 08

cell membranes

BIOLOGY

MEDICINE

Organic
ThinFilms

medicalimplants

ENGINEERING
molecular
electronics

supramolecularassemblies

CHEMISTRY
self-organizednanostructures

PHYSICS
Smilgies - IMSS Symposium 08

Grazing-Incidence SAXS
qz

Nanoscale
Applications:• surfaces• thin films

q||FeaturedExperiments:• in-situ• real time
Smilgies et al., Synchrotron Radiation News 15(5), pp. 35-41 (2002).
http://staff.chess.cornell.edu/~smilgies/gisaxs/GISAXS.php
Smilgies - IMSS Symposium 08

Stability of a lamellar BCP film
sample cell
X-ray beam

Kapton window

polymer film

solvent injection
Smilgies - IMSS Symposium 08

In-situ & real time:
PS-PB film exposed to solvent vapor
Smilgies, Busch, Posselt & Papadakis, SRN 15(5), pp. 35-41 (2002).
1 min
swelling

17 minswelling

PS-b-PB
183 kg/mol,
Dlam= 836 Å,
Dfilm = 2340 Å→ 1 image
per 40 sec

4 min
swelling

dried film

Bragg rods shorten and bend:• increase of lamellar thickness• change of lamellar orientation during vapor treatment
Smilgies - IMSS Symposium 08

Block copolymer architectures
Aspheres

Bcylinders

block copolymers (BCP):
two inmiscible polymer
chains connectedby a chemical bondlamellaecylindersbicontinuousvolume fraction of block A¾ tunable morpholgies as templates for nanostructured films
Smilgies - IMSS Symposium 08

Selective Solvents:
Solvent induced phase transition

Katy Bosworth, Marvin Paik et al. ACS Nano 2, 1396 (2008)
Smilgies - IMSS Symposium 08

Selective solvents:
Solvent induced phase transition
BCP phase diagram

HEX cylinders

Sph CylLamCyl SphχN10.5

disorderedφΑ = vA/ (vA+vB)

BCC spheres

uptake of selective solvent• swelling of solvable block > vA
• rescaling of A-B interaction > χN
Smilgies - IMSS Symposium 08

Energy Recovery Linac Light Source>> extending current 3rd generation sources <<Smilgies - IMSS Symposium 08

Cornell ERL: Phase 1A
klystrongallery
dump

diagnostics
gun

cryomodule

Smilgies - IMSS Symposium 08

ERL Phase 1A Photographs
gun

dump

cryomodule
klystronsSmilgies - IMSS Symposium 08

Cornell ERL Project

ERL Experiments HallCornell
ElectronStorage
Ring Tunnel

CESR

north arc: high flux

LINAC

south arc: high coherence¾ funding for phase 1A: development of photo injector¾ proposal for phase 1B: further development¾ science proposal for phase 2: full facility
Smilgies - IMSS Symposium 08

ERL Beamline Projects- Joel Brock • Don Bilderback: nanofocus (1nm)• Joel Brock: ultrafast scattering (100 fs)• Darren Dale: coherent scattering (CDI, XPCS)• Ken Finkelstein: inelastic scattering (meV, eV)• Detlef Smilgies: microbeam scattering– Christian Riekel, ESRF
– Lois Pollack, Cornell– Ron Pindak, NSLS, Brookhaven Nat’l LabSmilgies - IMSS Symposium 08

A Microbeam Scattering Beamline
for the ERL
ERL key features: small source size small divergence round beam high coherence high brilliance

>>>
>>>
>>>
>>>
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focus size – r-resolution
flux & q-resolution
r & q resolution in 2Dhigh performance optics – flux
time-resolved studies (μsec, msec)>> An ERL is the ideal source for microbeam scattering. <<Smilgies - IMSS Symposium 08

Microbeam Scattering Beamline Suite
Microbeam Scattering – Applications¾ Hard Materials – grain structure, local structure, interfaces¾ High Pressure – ultrahigh pressure, laser heating¾ Protein Crystallography – protein microcrystals¾ Soft & Biologic Materials – complex materials¾ hierarchic materials (bone, muscle, wood, tissue)¾ biomimetic materials¾ microfluidics: fast mixing & combinatorics¾ devices: organic electronics & biosensors

Smilgies - IMSS Symposium 08

A Microbeam Scattering Beamline
for Soft Materials at the ERL
80m

75m

nanoWAXS

70m50mmicroUSAXS

ControlCabins

30m

Optics• Mirrors• MonoLab Space

Smilgies - IMSS Symposium 08

Front-end• 5m undulator• 1:1 Be lenses

A microGIWAXS setup at CHESS D1

focusing
optics
X-ray beam

samplemicroscope
scatteredphotons

X-ray
area
detectorsample on
x,y,z,θ micropositioner>> gaining experience for a future ERL beamline

Smilgies - IMSS Symposium 08

Example: Polythiophene Microstrips

How to put a 20 μm sample into a20 μm beam: sample microscope!

grazing-incidence μWAXS

Detlef-M. Smilgies, Ruipeng Li, Tomasc Young, and Tomasc Kowalewski(unpublished)

Smilgies - IMSS Symposium 08

Acknowledgements
Hiroshi Kawata, KEK ERL group
Sol Gruner & CHESS Senior Staff
Cornell ERL group
Don Bilderback & X-ray Capillary Group
MacCHESS: sample microscope

Students & Postdocs:
Ruipeng Li, CHESS & USTC
Sterling Cornaby, Cornell A&EP + CHESS
T. Miyajima, KEK & Cornell ERL groups

Samples: CMU Chemistry, Cornell MS&E
Smilgies - IMSS Symposium 08