NIST Synchrotron Measurement Science Vision at NSLS Establish
NIST Synchrotron Measurement Science Vision at NSLS üEstablish structure function relationships for rational materials design to promote innovation and industrial competitiveness üDeveloping and exploiting new experimental methods, detectors and physics approaches in synchrotron materials science A suite of three beamlines spanning the entire periodic table! üU 7 A: U 7 A, NEXAFS, going strong ü XPS üX 23 A 2: X 23 A 2 online ü XAS 4/05 üX 24 A: X 24 A, XPS, make NEXAFS over ü
Soft Matter Science at NSLS II Needs and Opportunities Soft Matter: Treat me nicely! “Physician do no harm” - Hippocrates “Love me tender, Love me true” - Elvis Dan Fischer Material Science & Engineering Laboratory National Institute of Standards and Technology Gaithersburg, Maryland 20899 NSLS II Workshop July 18, 2007 Soft Matter Breakout Session
NSLS II Soft Matter Science Needs Some NEXAFS Collaboration Examples from U 7 A • • • Dean De. Longchamp (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 De. Longchamp) sensor pack power supply display processor & RFID communication • Large area / flexible • Designed functionality (bio) • self-destructs orders refills Rapid prototyping © Iowa Thin Film rollable photovoltaics NOT a replacement for silicon: new products from new materials and new methods of production
Soluble oligothiophene precursors In collaboration with J. M. J. Fréchet, D. De. Longchamp (NIST) • Soluble and printable • Convert at 150 -250°C • Carrier mobility up to ~0. 05 cm 2/V·s • Film thickness from 20 nm to 3 nm (~1 monolayer) incident soft X-rays Q = 90° s* p* carbonyl E 90° alkene Q = 20° E 20° NEXAFS for chemical conversion NEXAFS for molecular orientation T 6 heated to 200 °C
Primary Chemical Structure ↓ Processing ↓ Film Structure and Chemistry ↓ Performance (Mobility) Mobility: from saturation regime analysis (OFETs) • Clear correlations of field effect mobility to chemistry & microstructure Chemistry: from carbonyl and alkene peaks • Demonstration of NEXAFS as a microstructure evaluation tool for organic semiconductors Orientation: from peak area vs. electric field vector • Reveals consequences of molecular design on both microstructure & performance T 6 correlation • Adv. Mater. 17, p 2340 (2005) Series conversion & coverage • Chem. Mater. 17, p 6033 (2005) Series orientation vs. molecular design • J. Phys. Chem. B 110 p 10645 (2006) sub-monolayer Coverage: from Oxygen Auger analysis
Soft Matter Science Needs / Opportunities: NSLS II Soft Bends - NEXAFS and XPS • Create in one beamline a broad energy range for spectroscopy; ~50 to ~3000 e. V • High energy resolution; very bright source • Small beams sometimes; nano-tribology ü Big beams (1 cm x 1 cm); gradients and arrays; U 7 A ü Continue U 7 A focus on detector development (EY/FY) (Imaging XPS, NIST high resolution X-ray detector) ü Continue U 7 A focus on high throughput measurements
NSLS II soft bends 3 -pole wigglers / NSLS Brightness and Flux Comparison
NSLS II Soft Bends - NEXAFS and XPS Create in one beamline a broad energy range for spectroscopy; ~50 to ~3000 e. V
NIST and NSLS team to develop first NSLSII Soft Bend Beamline (at NSLS U 8) FY 08/09 ü 80% GU time U 7 A ü ~50 e. V to ~2500 e. V ü NIST funded now U 8 ü ASAP Transfer to NSLS II U 8 U 7 A
U 7 A : High Throughput NEXAFS (EY/FY) and XPS Soft Matter Structure and Chemistry (in situ also)
U 7 A : High Throughput NEXAFS (EY/FY) and XPS Soft Matter Structure and Chemistry (in situ also) Ø Creating and utilizing the best detectors for electrons and soft x-rays to increase sensitivity and throughput üLeveraging using a total 14 NIST SBIR grants to date = $2100 K Ø Applying automated data acquisition Ø Ultimately parallel processing of entire sample libraries Sample bar (back) Soft X-rays In Windowless Si. Li fluorescence detector Large area partial electron yield detector
U 7 A: 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
U 7 A: Parallel process NEXAFS imaging of Soft Matter (10 mm 2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces Tunable soft x-ray beam 10 x 10 mm Channel plate imaging detector (NIST SBIR) 75 micron spatial resolution (NIST SBIR) -SAM gradients - DNA protein chips - Catalyst libraries - Patterned overlayers Magnetic Lens (NIST SBIR)
U 7 A: Parallel process NEXAFS imaging of Soft Matter (10 mm 2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces ü 8/07 NIST SBIR Phase II Awarded to E. L. Principe Inc. (Combi-NEXAFS detector) Large Area Imaging Two-Dimensional Electron Energy Analyzer soft x-ray beam 10 x 10 mm High pass grid soft x-ray beam 10 x 10 mm Channel plate imaging detector 75 micron spatial resolution
U 7 A: Parallel process NEXAFS imaging of Soft Matter (10 mm 2 areas) SAM gradients, DNA / protein chips, Catalyst libraries, Patterned surfaces Gradients or Sample Array (~100 samples) Sample introduction / manipulator system Wobble Mirror optics for creating tunable Soft Xray sample illumination beam (1 cm 2) “Large Area Magnetic Imaging Electron Energy Analyzer” Parallel process NEXAFS imaging, Phase II SBIR, delivery in FY 07 U 7 A Existing Soft X-ray Experimental Chamber
Summary: Soft Matter Science at NSLS II Needs and Opportunities Soft Matter: Treat me nicely! Beam sample damage possible Many soft matter NEXAFS and XPS experiments need to be accommodated NSLS II Soft Bend for NEXAFS and XPS Endstation similar to U 7 A In one beamline a broad energy range for spectroscopy; ~50 to ~3000 e. V NIST and NSLS team to develop first NSLS II Soft Bend Beamline (at NSLS U 8) FY 08/09 NSLS II Workshop July 18, 2007 Soft Matter Breakout Session
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