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Spatial resolution and spectroscopy: The ultimate “cross-over” tool
in real and reciprocal space? NSLS-II Workshop
February 11, 2008
H. Ade
Department of Physics
North Carolina State University
http://www.physics.ncsu.edu/stxm/
Thanks to J. Stoehr, G. Mitchell, for their viewgraphs/data
and many other colleagues, collaborators, and users
Thanks to organizers for invitation
and NSF, DOE, Dow Chemical for financial support over the years
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Goal: Frame afternoon discussion workshop is tasked with “what kind of beamlines”
and science case
Revolutionary of evolutionary?Extrapolation of techniques?
What will be new?
Totally new techniques?
Are we going to just move “stuff/beamlines”?We should prevent that!
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How much better? NSLS-II is not an FEL, ERL
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Soft matter
Consists mostly of C, N, and O250-600 eV covers C, N, and O edge
> 2 orders of magnitude improvement in brightness> 1 order of magnitude improvement in S/N♦
Low signal experiments> 2 order of magnitude in acquisition speed
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Opportunities: Parameter Space
Spatial resolutionSmall, with large dynamic range generally best
Spectral resolution, specific interactionsComposition, labeling
Time resolutionDynamic phenomena
Sample environmentX-ray cross sections?
Polarization control
Combination of the above!
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Opportunities: Science
MembranesWater purificationFuel cellBiology: rafts
“Shampoo” and other complex matter (Helmut Frey)
Organic devicesOLEDsPVs
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Length scales probed by some “conventional” tools
RSoXS - complement to SANS, conventional SAXS Real space info would be best, but
Contrast? Spatial resolution? Damage limits?♦
TEM needs staining♦
NEXAFS in STXM and PEEM limited to ~40 nm spatial resolution
♦
In-situ environments?
1992
H. Ade et al., Science 258, 972 (1992)
Example: Neutron-scattering at IPNS, ANL…peptides (cylinders) inserting themselves in holes they form in a cell membrane.
But:…, the best way to see part of a biomolecule
is by replacing hydrogens
with deuterium.http://www.sns.gov/aboutsns/importance.htm NEXAFS microscopy
10-11 m 10-7 m10-9 m 10-5 m 10-3 m
nano-structurecrystallography structure
atomic structure
protein
polymers
micelle
bacteria
porous media
precipitates
DIFFRACTIONX-rays, n, e- SAXS, SANS
USAXS, USANS
Light scattering
TEM
Optical microscopy
10-11 m 10-7 m10-9 m 10-5 m 10-3 m
nano-structurecrystallography structure
atomic structure
protein
polymers
micelle
bacteria
porous media
precipitates
DIFFRACTIONX-rays, n, e- SAXS, SANS
USAXS, USANS
Light scattering
TEM
Optical microscopy
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Microscopy: Morphology characterization in real space
- Contrast Mechanism- Effective “resolution”?- Quantitation?
Visible light microscopyElectron microscopyScanning probe micros.Infra RedRaman microscopyNMR microscopy
X-ray Microscopy???
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Small Angle ScatteringCoherence length larger than domains,but smaller than illuminated area
log (intensity)40
-20
-40
0
20
-40 -20 0 20 40-40
-20
0
20
40
scattering vector q (μm-1)
scat
terin
g ve
ctor
q(μ
m-1
)Structure function:
informationabout domain
statistics.
Scattering/diffraction: Structure/morphology
characterization in reciprocal space
X-rays alternative to
neutrons
Spallation Neutron Source: total cost of $1.4 billion, http://www.sns.gov/
Figure courtesy of J. Stohr
- Contrast Mechanism- Effective “resolution”?- Quantitation?
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X-ray Microscopy: X-rays have come a long way!
(Examples “biased” towards polymers/magnetic materials)
1895
1993
2003
1 μm
1992
1993 1996
NEXAFS microscopy XMCD microscopy
XLD microscopy XMLD microscopy Dynamics
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Soft X-rays
Unique interaction with matter yields unique contrast
and unique characterization capabilities
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e-
hν
C 1s edge ~ 290 eVN 1s edge ~ 405 eVO 1s edge ~ 540 eV
CH2 CH2
n[ ]
[ ]C C
n
CH2C
CH3
C
O
O
CH3
n[ ]
N
H
CC
C
C
CC N C
H
C
O
C
C
C
CC C
O
][n
Unoccupied Molecular Orbital
Near Edge X-ray Absorption Fine Structure (NEXAFS) SpectroscopyExample: “”Richness” of Polymer NEXAFS Spectra
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13Photon Energy / eV285 290
C OO
73O
C
O
27
vectra™
CH3
CH3
O CO
O n
PC
PAR
CH3
CH3
O CO C O
O
n
CCO O
NH
NH
n
Kevlar™
CCO
OO
O (CH2)4 n
PBT
PNIC
O
O
CH2 CH3
CH3
CH3
CH2 *CO
O*
n
CCO
OO
O (CH2)2 n
PET
Photon Energy / eV285 290
PS
PBrS
SAN
n
78
Br
22
n
*
C N
m
CH2 NH CO
NHNH ** n
MDI polyurea
CH2 NH CO
ONHCO
OCH2 4* *n
MDI polyurethane
CH3
N
HN
H
C
O
n
TDI polyurea
CH3
NH
NH
CO
OC
O*
O
(CH2)4 *n
TDI polyurethane
Photon Energy / eV285 290
CH2 CC
CH3
OO
CH3(CH2)3
n PBMA
CH2 CC
CH3
OO
CH3
n PMMA
* NH
C *
O
n
On PEO
Nylon-6
EPRCH3
* n
PP *CH3
n
PE * n
Fingerpt.ppt 8 May 1998
Spectroscopy = high resolution Dhez, Ade, and UrquhartJ. Electron Spectrosc. 128, 85 (2003)
Data: Stony Brook STXM at NSLS
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Types of X- ray
Microscopes
Sample
MagnifiedImage
X-ray Beam
Objective LensProjective Lens
Screen
MCP
Aperture
X-Photoemission Electron Microscope
PEEM
ALS 5.3.2 and 11.0.2 STXM
TXM
Also: Scanning Photoemission X-ray Microscope (SPEM) Ade et al. Appl. Phys. Lett. 56, 1841 (1990)
Best for NEXAFSRelatively slow
FastLimited NEXAFS
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15 C. R. McNeill et al. Macromolecues 40, 3263 (2007)
poly(9,9´-dioctylfluorene-co-bis-N,N´-
(4,butylphenyl)-bis-N,N´-phenyl-1,4-phenylene-
diamine) (PFB) and poly(9,9΄-dioctylfluorene-co-
benzothiadiazole) (F8BT)
solar cells
280 285 290 295 300 305 310 315 3200.0
2.0x104
4.0x104
6.0x104
8.0x104
1.0x105
1.2x105
F8BT PFB
Mas
s A
bsor
ptio
n C
o-ef
ficie
nt (
cm2/g
)
Energy (eV)
283 284 285 286 287
F8BT
NS
N
N N n
PFB
n
0 nm
15 nm
60
100
1:5 PFB:F8BTwt.%0
50
wt.%1 μm
0 nm
50 nm
0 wt.%
100
0 nm
50 nm
5:1 PFB:F8BT
0
50
wt.%50
90
wt.%1 μm
ihg
fed
1 μm
F8BT % composition PFB % composition Height
a cb
1:1 PFB:F8BT0
wt.%
100
Figure courtesy C. McNeill
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“Parameter space” for real space microscopy: Higher brightness, more intensity
SoXBIC would clearly benefitDamage threshold?
Surface (SPEM, PEEM) microscopy would benefitDamage threshold?
Traditional NEXAFS microscopyTransmission: Relatively little benefit from NSLS-II undulator♦
Unless some form of time resolution is achieved ♦
Would need better detectors and scanning stages♦
Great workhorse on bending magnet beamlineSecondary yield mode♦
Clear benefit, but technological hurdles♦
Damage threshold for soft matter?
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Resonant Scattering/Reflectivity
Contrast: Carbon edge examples
280 290 3000.000
0.001
0.002
0.003
0.004
0.005
β
E (eV)
PS PMMA P2VP
270 280 290 300 310
-0.003
-0.002
-0.001
0.000
0.001
0.002
δ
E (eV)
PS PMMA P2VP
Scattering factors f’
and f”
(optical const. δ
and β, respectively) show strong energy dependence
“Bond specific”
scattering!Substantial potential as complementary tool!
NP2VPPS PMMA
R or I ∝
(Δδ2+Δβ2)
Absorption (NEXAFS)
Dispersion
270 280 290 300 310 320
1x10-6
2x10-6
3x10-6
4x10-6
5x10-6
Energy (eV)
PS-PMMA Interface PS-Vacuum Interface
(c)
Ref
lect
ivity
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270 eV
Si
PMMA
Momentum transfer:
if kkqrrr
−=λαπ i
zq sin4=
Reflectivity: Tuturial-1
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21 Data: Araki, BL6.3.2. ALS, Berkeley
NC STATE
University Ade Research Group (Polymer Physics/XAde Research Group (Polymer Physics/X--ray Characterization Techniques)ray Characterization Techniques)
Complementary Tool to Neutrons and hard X-
rays
Soft X-ray Resonant Reflectivity PS/PMMA bilayer
Potential: Diffuse scattering from interfaces
Observed strong photon energy dependence
0.0 0.5 1.0 1.5 2.0
Fit Data
14.2 KeV
PS(15nm)/PMMA(42nm)
320 eV
288.5 eV
285.2 eV
283.4 eV280 eV270 eV
10-12
10-9
10-6
10-3
0
Ref
lect
ance
q (nm-1)
PS
Si
PMMA
air
270 280 290 300 310 320
1E-6
2E-6
3E-6
4E-6
5E-6 PS-PMMA Interface PS-Vacuum Interface
(c)
Ref
lect
ivity
(dδ2+dβ2)/4
C. Wang, T. Araki, H. AdeAppl. Phys. Lett. 87, 214109 (2005)
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PS 50nm/PMMA 200nmReflectivity: Tuturial-2
PS
Si
PMMA
air
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Interpretation of Reflectivity Data
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
1E-4
1E-3
0.01
0.1
1
Ref
lect
ance
q (nm -1)
PS/PM M A 50 nm /200 nm 270 eV
PS
Si
PMMA
Phenomenon Physics behind it
High frequency fringes Total film thickness, sensitivity to the surface
Damping of the amplitude Surface roughness
Low frequency beating Sensitivity to the interface
Damping of the beating Interfacial roughness
Momentum transfer:if kkqrrr
−=
λαπ i
zq sin4=
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MEH-PPV is a neutral conjugated polymer spun-cast from non-polar solvent
PFNBr is a charged conjugated polymer (conjugated polyelectrolyte) spun-cast from polar solvent
interface influence?little is known about the interfacial structure and how it affects properties of such devices
C.Wang, B. Watts, T. Araki, H. Ade (NCSU) A. Hexemer, A. Garcia, T.- Q. Nguyen, G. C. Bazan, K.E. Sohn, and E.J. Kramer (UCSB).
N+ N+
n
Br- Br-MEH-PPV PFNBr
Polymer LED interfaces poly[2-methoxy-5-(2'-ethylhexyloxy)-p-
phenylene vinylene] (MEH-PPV) and
poly[9,9-bis(6’-N,N,N,-
trimethylammoniumhexyl)fluorene-co-
alt-1,4 phenylene
bromide] (PFNBr)
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Multilayer Device
270 eV
~80 nm MEH-PPV
20 nm PFNBr
~ 30 nm PEDOT:PSS
~ 30 nm ITO
Glass
Sample A. Garcia, T.-Q. Nguyen, G. C. Bazan, K.E. Sohn, and E.J. Kramer (UCSB).
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Multilayer Device
~80 nm MEH-PPV
~20 nm PFNBr
~ 50 nm PEDOT:PSS
~ 30 nm ITO
Glass
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-500x10-6
-400
-300
-200
-100
0
100
Re
flect
ance
*q4
1.21.00.80.60.40.20.0q (nm
-1)
284.6 eV
285.2 eV
285.4 eV
284.8 eV
data fit
σVacuum/PFNBr=0.9 nmσPFNBr/MEHPPV=1.1 nmσMEHPPV/PEDOT:PSS=3.5 nm
d=23.8 nm
d=75.8 nm
Sample A. Garcia, T.-Q. Nguyen, G. C. Bazan, K.E. Sohn, and E.J. Kramer (UCSB).
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Other organic electronic materials
F8BT P3HT PCBM PFB
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Resonant Soft X-ray Scattering (hard x-rays terminology ASAXS)
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Resonant Scattering: Low Contrast Example -
Developmental Porous SiLK* Resins
G. Mitchell, Dow Chemical
Decreasing feature size in integrated circuits require lower dielectric constants for insulating layers to:
increase circuit speed, decrease power consumption, decrease crosstalk
Adding pores to SiLK dielectric resin is used to decrease dielectric constant from 2.65 to 2.1 and lessFuture materials require more and smaller pores
* SiLK
is a trademark of The Dow Chemical Company
G. E. Mitchell et al., Appl. Phys. Lett. 89, 044101 (2006)
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Systematic variation in porogen size
Smallest pores collapse
Still issues with background, need to improve instrumentationWouldn’t be able to do the experiment with STXM, TEM, or SAXS. - Deuteration and SANS would work.
G. E. Mitchell et al., Appl. Phys. Lett. 89, 044101 (2006)
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Scat
terin
g In
tens
ity [a
.u]
q (1/nm)
PMMA/P(BA-co-S)
Idealized, “consensus” particle
“PS”“PS”
“PS”-”shell”
J.M. Stubbs, D.C. Sundberg Polymer 46 (2005) 1125
P(MA-b-MMA) / PS
Fuzzy TEMmodified core/shell structure?Phase less separated?Where really is the PS?
“PS”
effective radius larger than PMMA “radius”
“PS”
about same size than PMMA/acrylate!Scattering indicates PS is slightly more in center of nanoparticle relative to PMMA/P(BA-co-S)
Different process and composition
T. Araki et al. Appl. Phys. Lett. 89, 124106 (2006
(Figure courtesy J. Stubbs UNH)
NC STATE
University Ade Research Group (Polymer Physics/XAde Research Group (Polymer Physics/X--ray Characterization Techniques)ray Characterization Techniques)
10-1
100
101
102
103
0.120.080.040.00
200 nm
150 nm
100 nm
280.0 eV285.2 eV288.4 eV320.0 eV
10-1
100
101
102
103
0.120.080.040.00
qR=4.5q=0.39
qR=7.73q=0.68
qR=10.9q=0.95
R=115 nm
q (1/nm)
Scat
terin
g In
tens
ity [a
.u] 280.0 eV
285.2 eV288.4 eV320.0 eV
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0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.71E-3
0.01
0.1
1
10
100
1000
10000
284.75 eV as cast 120oC for 10 min 180oC for 10 min 200oC for 10 min
I/Bea
mcu
rren
t
q(nm-1)
#0: As spun
200 deg C annealed
All polymer Solar Cell: PFB:F8BT cast from chloroform
Scale bar: 200nm
STXM
RSoXS
S. Swaratj, B. Watts, H. Ade, C. McNeill
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All polymer Solar Cell: PFB:F8BT cast from chloroform
RSoXS
278 280 282 284 286 288 290 292 294 296 298 300 302
0.0
8.0x10-3
1.6x10-2
284.8 eV #6
I/Io
Photon energy [eV]
Energy scans: 1deg off-axis
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.71E-3
0.01
0.1
1
10
100
1000
10000
284.75 eV as cast 120oC for 10 min 180oC for 10 min 200oC for 10 min
I/Bea
mcu
rren
t
q(nm-1)
S. Swaratj, B. Watts, H. Ade, C. McNeill
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GoalUse model systems (with two or three components) to establish utility and applicability of GIRSoXSCan sensitivity of each component can be tuned by tuning photon energy?
ExperimentDiblock and triblock copolymer thin films were prepared by S-J.Park, C. TangGIRSoXS experiment was carried at BL5-2 SSRL by C. Wang, B. Watts, T. Araki and B. Schlotter.9 degree incident angle, i..e above critical angle - Not true GIRSoXS.
Brief SummaryBasic quality of GIRSoXS data looks promising, but the instrument needs to be further optimizedContrast variations and scattering intensity changes as a function of photon energy have been observedFuture experiments with three-component-systems with a photon energy dependent structure factor should be explored
Resonant GISAXS on block copolymersC. Wang, T. Araki, B. Watts, H. Ade (NCSU), A. Hexemer (LBNL)
S-J. Park, T.P. Russell (UMass), B.Schlotter (SSRL) C.Tang, E.J.Kramer (UCSB)
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qy
qz
qx
Sample
CCD
CCD area 1300 x 1340, 20 μm/pixel
CCD -
Sample ~ 43 mm
Incident Angle ~ 9 deg (above critical angle)
Beam stop 15 um wire with a 200 um diameter epoxy bead. About 1 cm from the CCD
Aperture (75 x 125 μm)
Beam size: ~400 μm x ~100 μm (H x V)
X-ray
Experimental Setup•Chamber is not optimized for the reflection geometry
•The CCD angle is approx. perpendicular to the specular reflected beam.
• The Sample-CCD distance and incidence angle are estimates
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Use NSLS-II for improved energy resolution?
NEXAFS already limited by core-hole lifetimeResonant Inelastic X-ray Scattering for improved spectroscopy
But, damage!Need to back off on spatial resolution
Photon Energy (eV)
280 285 290 295 300 305 310 315 320
Opt
ical
Den
sity
0
1
2
3
4
5
6
7
Kevlar®
149
Kevlar®
49
N N C C
OO
HH][
n
Spectra with horizontal polarization in locations indicated
-30°
38°
8°
Determine degree of orientational
order
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Radiation DamageTypical critical dose ~ 1000 eV/nm3
Rose criterion for detection: S/N=5Transmission, S=-ln(I/I0)(10 nm)3 PS feature has S/N of 5 for 650 incident photons, and 115 absorbed photons in pi* peak at 285 eV
Dose= ~32 eV/nm3
Quantitation/spectra/tomography typically require 100x dose
Near critical at 10 nm for PSDose ∝ 1/(Δα)
Imaging using phase contrastScattering using phase and absorption contrast
T. Coffey et al. J. Electron Spectroscopy 122 (2002) 65 –78
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39 Data: Beamline 6.3.2 ALS
What about a “cross-over”?
I ∝ Δδ2 + Δβ2Works with low contrast
Q-range ~ 3 nm-1 (@300 eV)Dose is distributed!!Time resolution could be quite good“RSoXS” not intrinsically a brightness driven experiment
Combine low resolution STXM and RSoXS: Microbeam resonant scattering
Damage?
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Incoherent vs. Coherent X-Ray ScatteringSmall Angle ScatteringCoherence length larger than domains,but smaller than illuminated area
SpeckleCoherence lengthlarger than illuminated area
log (intensity)40
-20
-40
0
20
-40 -20 0 20 40-40
-20
0
20
40
scattering vector q (μm-1)
scat
terin
g ve
ctor
q(μ
m-1
)
log (intensity)40
-20
-40
0
20
-40 -20 0 20 40-40
-20
0
20
40
scattering vector q (μm-1)
scat
terin
g ve
ctor
q(μ
m-1
)
informatio n
about domainstatistics
trueinformatio
nabout
domainstructureFigure courtesy J. Stohr
Resonant scattering and resonant speckle should be excellent tools for organic materials !!!!
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Other possibilities
Resonant x-ray photon correlation spectroscopy?R-XPCS
Resonant coherent imaging?Coherent imaging proposed by other workshop!
Spatially resolved inelastic scattering?Damage?Sensible domain size?
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Conclusions
NEXAFS microscopy and resonant reciprocal space techniques are excellent “compositional” tools with 1D, 2D, and 3D (tomography) spatial resolution well below 1 micron.C,N, O edges have feature-rich spectroscopy for organic materials.
SpecificityMany organic, soft condensed matter application will continue to benefit from these toolsThin samples 100-2000 nm thick.
Science opportunitiesSee Helmut Frey
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If we were a rich man?
Bending magnet STXM workhorseBending magnet RSoXR/RSoXR workhorse
Microfocus RSoXS undulator beamlineIntensity at sample scales with brightness/coherenceSoft x-ray EPU beamline
R-XCPSNeeds coherenceSoft x-ray EPU beamline
……..
Beamline design(s) most likely relatively conventional (except heatload). Most advances are in the endstations
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Thank you for your attention!!!!
Thanks to members of my group: B. Watts, S. Swaratj, T. Araki, and C. Wang
and
Bill Slotter, Jan Luning
(Stanford). C. McNeill (Cambridge), A. Hexemer
(ALS), A. Garcia, T.-Q. Nguyen,
G. C. Bazan, K.E. Sohn, and E.J. Kramer (UCSB).