NIST Synchrotron Measurement Science Vision at NSLS

Establish structure function relationships for rational materials design

to promote innovation and industrial competitiveness

Developing and exploiting new experimental methods, detectors

and physics approaches in synchrotron materials science

H HeK K

Li Be B C N O F NeK K K K K K K K

Na Mg Al Si P S Cl ArK K K K K K K K

L L L L L L L L

K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br KrK K K K K K K K K K K K K K K K K K

L L L L L L L L L L L L L L L L L L

Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I XeK K K K K K K K K K K K K K K K K K

L L L L L L L L L L L L L L L L L L

Cs Ba Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At RnK K K K K K K K K K K K K K K K K

L L L L L L L L L L L L L L L L L

Fr RaK K

L L

La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb LuK K K K K K K K K K K K K K K

L L L L L L L L L L L L L L L

Ac Th Pa UK K K K

L L L L

175-1300 eV 1.0-5.0 keV 4.7-30 keV

U7A X24A X23A2

A suite of three beamlines spanning the entire periodic table!

U7A, going strongX23A2 online 4/05X24A, make over

U7A: NEXAFS, XPSX23A2: XASX24A: XPS, NEXAFS

Soft Matter Science at NSLS IINeeds and Opportunities

Soft Matter: Treat me nicely!

“Physician do no harm” - Hippocrates“Love me tender, Love me true” - Elvis

Dan FischerMaterial Science & Engineering Laboratory

National Institute of Standards and TechnologyGaithersburg, Maryland 20899

NSLS II Workshop July 18, 2007Soft Matter Breakout Session

NSLS II Soft Matter Science NeedsSome NEXAFS Collaboration Examples from U7A

• Dean DeLongchamp (NIST): Organic electronics (some details next)• Vivek Prabhu (NIST): Photolithography PAG chemical depth profiling• Steve Hsu (NIST): MEMS lubrication; Organosilanes / silicon; chemistry / tribology

• Joe Lenhart (Sandia): Molecular orientation, solvent and stress induced polymer films

• Lin Loo (U.of Texas, Austin): molecular electronics, “Solvent-Dependent Assembly of Terphenyl- and Quaterphenyldithiol on Gold and Gallium Arsenide”\

• Gary Mitchell (Dow Chemical): PLED and Catalysts

• Jan Genzer (NCSU, Raleigh): Gradient SAMs

• Ed Kramer (UC Santa Barbara) and Chris Ober (Cornell):UV active SAMs, nonstick coatings, and organic electronics

• Dave Castner (U. of Wash, NESAC/Bio): Biomaterials; proteins, DNA

Printed organic components for ubiquitous electronics(NIST internal initiative, Dean DeLongchamp)

NOT a replacement for silicon: new products from new materials and new methods of production

• Large area / flexible

• Designed functionality (bio)

• Rapid prototyping

self-destructsorders refills rollable

photovoltaics

© Iowa Thin Film

sensor pack

power supply

processor &RFID communication

display

carbonylalkene

incidentsoft

X-rays = 90°

= 20°

E 90°

E 20°

NEXAFS for chemical conversion NEXAFS for molecular orientation

T6 heated

to 200 °C

• Soluble and printable• Convert at 150-250°C• Carrier mobility up to ~0.05 cm2/V·s• Film thickness from 20 nm to 3 nm (~1 monolayer)

Soluble oligothiophene precursorsIn collaboration with J.M.J. Fréchet, D. DeLongchamp (NIST)

Primary Chemical Structure ↓

Processing ↓

Film Structure and Chemistry ↓

Performance (Mobility)

• Clear correlations of field effect mobility to chemistry & microstructure

• Demonstration of NEXAFS as a microstructure evaluation tool for organic semiconductors

• Reveals consequences of molecular design on both microstructure & performance

Mobility:from saturation regime analysis(OFETs)

Chemistry:from carbonyl and alkene peaks

Orientation:from peak area vs. electric field vector

Coverage:from Oxygen Auger analysis

T6 correlation• Adv. Mater. 17, p2340 (2005)

Series conversion & coverage• Chem. Mater. 17, p6033 (2005)

Series orientation vs. molecular design • J. Phys. Chem. B 110 p10645 (2006)

sub-monolayer

Soft Matter Science Needs / Opportunities: NSLS II Soft Bends - NEXAFS and XPS

• Create in one beamline a broad energy range for spectroscopy; ~50 to ~3000eV

• High energy resolution; very bright source

• Small beams sometimes; nano-tribology

Big beams (1 cm x 1 cm); gradients and arrays; U7A

Continue U7A focus on detector development (EY/FY)(Imaging XPS, NIST high resolution X-ray detector)

Continue U7A focus on high throughput measurements

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10 eV 100 eV 1keV 10keV 100keV

Photon Energy [eV]

VUVhcrit

EPU100 VUV undulator100 mm, L=4 m, Kmax=14.0

EPU45 SXU45 mm, L=4.0 m, Kmax=4.33

U14 SCU14 mm, L=2.0 m, Kmax=2.2

W60 SCW,B=6.0 T, 60 mm,L=1.0 m, K=33.6

DW100 damping wiggler,B=1.8 T, 100 mm,L=7 m, K=16.8

U19 CPMU19 mm, L=3.0 m, Kmax=2.03

Ring parameters: 3.0 GeV, 0.5 A, h=0.55 nm, v=0.01 nm, energy spread=0.001

Straight section parameters: low-: h=2.7 m, v=0.945 m; high-: h=18.2 m, v=3.09 m; h=v=h=v=h=v=0

Bend magnet parameters: h=0.65 m, v=25.1 m, h=0.032, v=-0.044, h=0.04 m, h=0.056, v=v=0

25 m radius bend,B=0.4 T, Ec=2.39 keV

3-pole wiggler,B=1.0 T, Ec=5.98 keV

NSLS X21, 120mmB=1.1 T, K = 12.33L= 1.62 m

NSLS X25, 18mmKmax=1.5, L=1.0 m

NSLS X1, 80mmKmax=2.3, L=2.8 m

NSLS 6.88m radius bend,B=1.36 T, Ec=7.09 keV

NSLS 1.91m radius bend,B=1.41 T, Ec=0.61 keV

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Photon Energy

VUVhcrit

EPU100 VUV undulator100 mm, L=4 m, Kmax=14.0

EPU45 SXU45 mm, L=4.0 m, Kmax=4.33

U14 SCU14 mm, L=2.0 m, Kmax=2.2

W60 SCW,B=6.0 T, 60 mm,L=1.0 m, K=33.6

Damping Wiggler DW100B=1.8 T, 100 mm,L=7 m, K=16.8

U19 CPMU19 mm, L=3.0 m, Kmax=2.03

Ring parameters: 3.0 GeV, 0.5 A, h=0.55 nm, v=0.01 nm, energy spread=0.001

Straight section parameters: low-: h=2.7 m, v=0.945 m; high-: h=18.2 m, v=3.09 m; h=v=h=v=h=v=0

Bend magnet parameters: h=0.65 m, v=25.1 m, h=0.032, v=-0.044, h=0.04 m, h=0.056, v=v=0

25m-radius bend,B=0.4 T, Ec=2.39 keV

3-pole wiggler,B=1.0 T, Ec=5.98 keV

NSLS X1, 80mmKmax = 2.3, L = 2.8m NSLS X25, 18mm

Kmax = 1.5, L = 1.0m

NSLS X21, 120mm, B=1.1TK = 12.33, L = 1.62m

NSLS 1.91m-radius bend,B=1.41 T, Ec=0.61 keV NSLS 6.88m-radius bend,

B=1.36 T, Ec=7.09 keV

NSLS II soft bends 3-pole wigglers / NSLSBrightness and Flux Comparison

NSLS II Soft Bends - NEXAFS and XPSCreate in one beamline a broad energy range

for spectroscopy; ~50 to ~3000eV

U7AU8

U8

U7A

NIST and NSLS team to develop first NSLSII Soft Bend Beamline (at NSLS U8) FY08/09

80% GU time

~50eV to ~2500eV

NIST funded now

ASAP Transfer to NSLS II

U7A : High Throughput NEXAFS (EY/FY) and XPSSoft Matter Structure and Chemistry (in situ also)

  Creating and utilizing the best detectors for electrons and soft x-rays to increase sensitivity and throughput

Leveraging using a total 14 NIST SBIR grants to date = $2100 K

Applying automated data acquisition

Ultimately parallel processing of entire sample libraries

Large area partial electron yield detector

Windowless SiLi fluorescence detector

Sample bar(back)

Soft X-rays In

U7A : High Throughput NEXAFS (EY/FY) and XPSSoft Matter Structure and Chemistry (in situ also)

U7A: Creating / utilizing the best detectors for electrons and soft x-rays; increase sensitivity and throughput

Now fully working!

14 element Si(Li) detector with ultra-thin surface dead-layers

Physical Sciences Inc. Phase I and II SBIR Impact -> soft x-ray sensitivity and resolution

“Improvement in the Low Energy Collection Efficiency of Si(Li) X-ray Detectors”

Conference on the Application of Accelerators in Research and Industry, Ft Worth, TX (2005).

High Efficiency Circular Array Secondary Electron Yield Detectors: Final plan proceeding quickly

Detector Technology Inc. Phase I and II SBIR

Impact-> high throughput near surface chemical depth profile

How accomplished-> parallel detection of all electron takeoff angles

U7A: Parallel process NEXAFS imaging of Soft Matter (10mm2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces

Magnetic Lens(NIST SBIR)

(NIST SBIR)

Tunable soft x-ray beam 10 x 10 mm

-SAM gradients- DNA protein chips- Catalyst libraries- Patterned overlayers

Channel plate imaging detector

75 micron spatial resolution

(NIST SBIR)

Channel plate imaging detector

75 micron spatial resolution

U7A: Parallel process NEXAFS imaging of Soft Matter (10mm2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces

8/07 NIST SBIR Phase II Awarded to E. L. Principe Inc. (Combi-NEXAFS detector) Large Area Imaging Two-Dimensional Electron Energy Analyzer

B=2kG B=5kG

B=100G

samplemagnet

Image plane

Figure 3

soft x-ray beam 10 x 10 mm

soft x-ray beam 10 x 10 mm

High pass grid

Wobble Mirror optics for creating tunable Soft X-ray sample illumination

beam (1cm2)

Gradients or Sample Array (~100 samples) Sample introduction / manipulator system

“Large Area Magnetic Imaging Electron Energy Analyzer” Parallel process NEXAFS imaging, Phase II SBIR, delivery in FY07

U7A Existing Soft X-ray Experimental Chamber

U7A: Parallel process NEXAFS imaging of Soft Matter (10mm2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces

Summary: Soft Matter Science at NSLS IINeeds and Opportunities

Soft Matter: Treat me nicely!Beam sample damage possibleMany soft matter NEXAFS and XPS

experiments need to be accommodated

NSLS II Soft Bend for NEXAFS and XPSEndstation similar to U7A

In one beamline a broad energy range for spectroscopy; ~50 to ~3000eV

NIST and NSLS team to develop first NSLS II Soft Bend Beamline (at NSLS U8) FY08/09

NSLS II Workshop July 18, 2007Soft Matter Breakout Session