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2017  Nov 1 - Dec 21

2018  Feb 7 - Apr 3
2018  Proposal/BTR deadline: 12/1/17

2018  Apr 11 - Jun 4
2018  Proposal/BTR deadline: 2/1/18

CHESS users

 

Poster Abstracts

 

 
"Germanium Collimating Channel Arrays for x-ray fluorescence Microscopy"

David Agyeman-Budu
CHESS, Cornell University

 

 
"High Resolution Camera for Resonant Inelastic Soft X-Ray Scattering Spectroscopy"

N.C. Andersen1, P. Denes1, J. Farrington2, A. Goldschmidt*1, J. Joseph1, A. Karcher1 and C.S. Tindall1
1Lawrence Berkeley National Laboratory (LBNL), 1 Cyclotron Road, Berkeley, CA 94720, USA
2Sydor Instruments LLC, 291 Millstead Way, Rochester, NY 14624, USA

Abstract: Resonant inelastic scattering spectroscopy (RIXS) in the soft x-ray regime is a powerful technique to probe the electronic structure of matter. The technique utilizes energy dispersive spectrometers to disperse a scattered x-ray beam from a sample in such a way as to translate each x-ray energy into a corresponding position on a detector active area. Thus, in these spectrometers energy resolution is dependent on the position resolution of the detectors used. To increase the energy resolution of a detector, either the distance between the dispersive element and the detector is increased or the detector pixel pitch in the energy dispersive axis is reduced.

Researchers at the Lawrence Berkley National laboratory have demonstrated the technical feasibility of the Spectro CCD, a novel direct-detection, soft x-ray imaging camera with up to 3 times better position resolution than the current commercial offering. The Spectro CCD has been optimized for soft x-ray RIXS spectrometry by employing a 5 µm x 45 µm pixel geometry to increase resolution in the energy dispersive axis (5 µm direction) and by utilizing a 10 nm back entrance window to achieve high quantum efficiencies in the soft x-ray regime. The camera performance has been characterized at the Advance Light Source (ALS) 8.0.1 RIXS beamline, with a ~280 eV (CK) X-ray beam on a graphite sample. The Spectro CCD point spread function for soft X-rays in the energy dispersive axis was measured to be 4.5 µm, with a readout noise of 3-6 electrons. The tests demonstrated that individual oxygen ~520 eV (OK) x-rays can be identified and located with a 3.5 µm precision. In addition, the quantum efficiency of the CCD was measured to be greater than 75% in the range from 200 eV to 1 keV. A general overview of the system and the test results will be presented.

Acknowledgements
Support provided by the U.S. DOE Office of Science, Office of Basic Energy Sciences under the SBIR/STTR award DE-SC0011269. This material is based upon work supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, Accelerator and Detector Research.

 

 
"Detecting high energy photons: First results from an MM-PAD detector with GaAs sensor"

Julian Becker1,2, Katherine S. Shanks1, Hugh T. Philipp1, Mark W. Tate1, Joel T. Weiss1,2, Prafull Purohit1, Darol Chamberlain2, & Sol M. Gruner1,2
1Laboratory of Atomic and Solid State Physics, Physics Department, Cornell University, Ithaca, NY
2Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY

Abstract: Pixel Array Detectors (PADs) consist of an x-ray sensor layer bonded pixel-by-pixel to an underlying readout chip. This approach allows both the sensor and the custom pixel electronics to be tailored independently to best match the x-ray imaging requirements. Silicon sensors have limited stopping power for x-rays above about 20 keV, suggesting need for sensors with higher atomic number, like gallium arsenide. Chromium compensated gallium arsenide (GaAs:Cr) sensors offer superior quantum efficiency (i.e., the probability to detect a photon) in the energy range of 15-50 keV, and have been successfully used in photon counting detectors like the Medipix in the past decade. We mated GaAs:Cr sensors to one of our charge-integrating readout chips, the Mixed-Mode PAD (MM-PAD), which was developed previously in our laboratory.

Here we present results from first characterization measurements showing the drawbacks and advantages of using GaAs sensors with charge integrating detectors. The results also provide motivation for further studies of GaAs with photon counting detectors.

 

 
"High Throughput Mapping of Time and Temperature Dependence of Metastable Phase Nucleation"

Robert Bell
Cornell University

Abstract: The equilibrium phase of a material is only one of many structures that can potentially form. As structure plays the critical role in determining many material properties, accessing these non-equilibrium metastable phases can dramatically expand the design space of materials. While, metastable materials have a higher free energy than the stable phase, the differences are often small compared to the free energy of crystallization from either a liquid or amorphous precursor. Consequently, during thermal annealing metastable phases can readily nucleate and grow. At slow thermal quench rates, subsequent transformations often relax the materials to the equilibrium structure. However, if thermal quench rates are sufficiently high, these interesting metastable phases can be retained to low temperatures.

In this work, we report a high throughput process to characterize this metastable phase formation utilizing millisecond time scale thermal anneals with spatial temperature gradients. This technique, lateral gradient laser spike annealing (lgLSA), provides a robust and rapid platform to develop time and temperature maps of phase formation in a broad range of material systems ranging from metals to complex oxides. The formation and trapping to room temperature of numerous metastable metal oxide phases are reported.

 

 
"Briseno Group at CHESS"

Benjamin Cherniawski, Edmund Burnett, David Darutto, Detlef Smilgies and Alejandro L. Briseno*†
Department of Polymer Science and Engineering, Conte Research Center, University of Massachusetts, 120 Governors Drive, Amherst, MA, 01002, USA
Cornell High Energy Synchrotron Source, Cornell University, Ithaca, New York 14850, United States

Abstract: We give an overview of a variety of research projects in the field of organic electronics and photovoltaics that we are pursuing at CHESS.

 

 
"Detection of Residual Stress in Engineering Scale Components Using White Beam Transmission and Monochromatic reflection"

Christopher Budrow
Cornell University

 

 
"Developing and Applying New X-Ray Spectroscopic Scattering Techniques for Quantum Matter Studies"

Arthur Campello, Chase Goddard, Johnathan Kuan, Yuchao Chen and Carl Franck
Laboratory of Atomic and Solid State Physics, Cornell University

Abstract: In order to select particular initial electron states to excite in inelastic scattering experiments, we have been developing techniques that rely on coincidence detection of deexciattion radiation. These designs also serve to suppress otherwise limiting backgrounds due to extraneous scattering. Recently, we have used this approach to explore the low energy X-radiation, intraatomic bremsstrahlung, predicted but not hitherto observed to accompany the photoejection of K shell electrons. To achieve this observation we employed freestanding ultra-thin (80 nm) cooper films exposed to an intense 80keV incident beam. Meanwhile we are developing a scintillator on sample soft X-ray detection technique without the requirement of high vacuum. This will enable the flexible use of the coincidence methodology for inelastic X-ray scattering studies of condensed matter systems. While these approaches have immediate application, they are especially promising for CHESS-U and sister hard X-ray sources.

 

 
"Experimental Determination of Non-woven Bond Strength Distributions"

Naigeng Chen1,2 and Meredith N. Silberstein*1
1Sibley School of Mechanical and Aerospace Engineering, Cornell University, Ithaca, NY, USA 2Cornell High Energy Synchrotron Source, Cornell University, Ithaca, NY, USA

Abstract: Bond fracture greatly affects the strength and damage progression of many non-wovens. Here we present a novel combined experimental and simulation approach to extract the bond strength of a particular non-woven. The approach was implemented for a commercial polyprolylene non-woven. A small non-woven specimen was imaged by micro computed tomography (μCT) and then subjected to uniaxial tensile loading through complete failure. The geometry of the non-woven was imported from the μCT data into a discrete finite element model. Using known fiber properties, the bond properties were then determined by comparing the simulated load-displacement curve with the experimental load-displacement curve. The sensitivity of the load-displacement curve to bond strength distribution will also be presented.

 

 
"Synchrotron X-ray Fluorescence Imaging as a High-Precision Phenotyping Tool for Studies of the Relationship between Mineral Nutrient Homeostasis, Fertility and Crop Yield"

Ju-Chen Chia1, Huajin Sheng1, Jiapei Yan1, Rong Huang2, Louisa Smieska2, Arthur Woll2, Olena K. Vatamaniuk1
1Section of Crop and Soil Sciences, School of Integrative plant Sciences, Cornell University, Ithaca, NY, USA
2Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY, USA

Abstract: Transition metals such as iron (Fe), zinc (Zn) and copper (Cu) are required for the growth and development of plants. These elements are also essential components of the human diet. In fact, Fe-deficiency anemia affects over 30% of the world’s population, especially in poor populations across the globe. While Cu is not as limiting in human diets as Fe, Cu interacts with Fe and is required for plant fertility and seed/grain set. While the global demand for high-yield crops with a high density of Fe, Zn and Cu in edible tissues is increasing, limited Fe, Zn and Cu bioavailability in many agricultural soils worldwide significantly impedes crop production, their mineral quality and thus, the future of food security. Sustainable approaches for improving crop yield and mineral nutrient density relies on the knowledge of Fe, Cu and Zn transport systems and their regulators that ensure adequate mineral uptake into roots and root-to-shoot partitioning. In this regard, high-precision synchrotron x-ray fluorescent microscopy (XRM)- based mapping of the spatial distribution of mineral elements at the tissue, cellular and subcellular resolution in different plant genotypes emerges as a powerful tool connecting the genotype-to-phenotype gap as pertains to improving mineral nutrient uptake, delivery to reproductive organs and loading into grains. We will present our recent data showing the power of the integration of XRM imaging with functional genomics tools for uncovering the function of transporters and transcription factors in shoot-to-root signaling of Fe status and the role of Cu in male fertility in a model plant Arabidopsis thaliana. We will also discuss the advantages of including this phenotypic strategy as a gene mining and QTL-identification tool in molecular breeding efforts for crops with improved growth and yield/spike characteristics in marginal soils and soils now in cultivation.

 

 
"Innovative Application of Pressure Cryo-cooling"

Teck Khiang Chua and Doletha M. Szebenyi
MacCHESS, Cornell University

Abstract: The development of pressure cryo-cooling opened up new possibilities in structural biology research. One application is to trap reactants, products or reaction intermediates in protein crystals using biologically active gases in pressurized form. Here, we show that applying pressurized carbon dioxide gas (CO2) on bacterial β-class carbonic anhydrase (bCA) protein crystals can successfully trap its substrate CO2. Using the same technique, we also managed to trap the product, CO2 of orotidine 5’ –phosphate decarboxylase (ODCase) in the ODCase-UMP complexed protein crystals, again providing interesting insights on the reaction mechanism.

 

 
"Solution phase dynamics of DNA-capped gold nanoparticle assembly"

Thomas Derrien
Cornell University

Abstract: We have been working to expand the solution phase environment in which DNA-capped gold nanoparticles can form superlattices. By eliminating the complex base-pairing interactions, essentially treating DNA as a generic polymer we have greatly simplified the process, yet have not sacrificed the utility of DNA. In fact, our approach expands the ionic environments in which such superlattices form. Here we present ongoing work characterizing these assemblies, using QCM-D, SAXS, and SEM.

 

 
"High Resolution Camera for Resonant Inelastic Soft X-Ray Scattering Spectroscopy"

Jamie Farrington
Sydor Technologies Company

 

 
"Amazing new results at CHESS station C1"

Kenneth Finkelstein
CHESS, Cornell University

 

 
"Molecular Weight Distribution Shape as a Means to Control Polymer Properties"

Dillon Gentekos
Cornell University

Abstract: The breadth of polymer molecular weight distributions (MWDs) radically alters their physical properties, from viscoelasticity and fracture toughness to morphological phase behavior. Gaining control of the shape of these MWDs may offer a convenient avenue for precision tuning of the properties of homo- and block copolymers; however, studies of this type have been scarce due to the lack of experimental methods providing absolute control over MWD shape. To this end, we have recently developed a mod...

 

 
"Solution SAXS and in situ GISAXS Study of the Fabrication of Asymmetric Block Copolymer Membranes"

Yibei Gu, Rachel M. Dorin, Yuk Mun Li,¥ Qi Zhang, Kwan W. Tan, Debóra Salomon Marques, Hiroaki Sai, Ulla Vainio,§ William A. Phillip, Detlef-M. Smilgies, Klaus-Viktor Peinemann, Suzana P. Nunes and Ulrich Wiesner*†
Department of Materials Science and Engineering and ¥Robert Frederick Smith School of Chemical and Biomolecular Engineering, Cornell University, Ithaca, NY14850, US
Water Desalination and Reuse Center and Advanced Membrane and Porous Materials Center, King Abdullah University of Science and Technology (KAUST), Thuwal, 23955-6900, Saudi Arabia
§HASYLAB at DESY, Notkestr. 85, 22607 Hamburg, Germany
Department of Chemical and Biomolecular Engineering, University of Notre Dame, Notre Dame, Indiana 46556, United States
Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14850, US

Abstract: Evaporation-induced asymmetric block copolymer membrane formation from diblock copolymer polystyrene-block-poly(4-vinylpyridine) (SV) and triblock terpolymer polyisoprene-block-polystyrene-block-poly(4-vinylpyridine) (ISV) was studied using solution Small-angle X-ray scattering (SAXS) analysis and in situ grazing incidence small-angle X-ray scattering (GISAXS). Solution SAXS analysis of SV in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and ISV in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure.

Furthermore, an in-depth analysis during the self-assembly of doctor bladed solutions by in situ GISAXS shows transient ordered structures for two ISV terpolymers at intermediate evaporation times in the top surface layers of the films as a function of molar mass and solution concentration. Analysis of the GISAXS patterns revealed the evolution from disordered to ordered structures including a transition from body-centered cubic (BCC) to simple cubic (SC) lattices, and finally to an amorphous mesoscale structure. The BCC to SC transition solves an apparent structural puzzle resulting from comparisons of, on one side, earlier quiescent solution SAXS studies suggesting BCC terpolymer micelle structures at higher concentrations and, on the other side, electron microscopy studies consistent with SC lattices originating from polymer micelles in the top separation layer of asymmetric ISV membranes.

These studies suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure while in situ GISAXS offers insights into the structural evolution of asymmetric triblock terpolymer film formation, which may enable further optimization of self-assembly plus non-solvent induced phase separation (SNIPS) based high performance isoporous asymmetric block copolymer ultrafiltration membranes.

 

 
"Organic Molecule Crystallization Control for Pharmaceutical, Electronic, and Sensor Applications"

Stephanie Guthrie
University of Virginia

 

 
"What can otolith 87Sr/86Sr transects and Se/Ca, Sr/Ca mappings tell us about the migratory patterns of goliath catfish in the Amazon basin?"

Hauser, M.1,2,3, T.W. Hermann4, K. E. Limburg4, C. R.C. Doria1, M. Pouilly2,3, C. Pecheyran5, E. Ponzevera6, Á. García Vásquez7, D. J. Stewart4, J.-F. Renno2,3, G. Torrente-Vilara8, L. Castello9, and F. Duponchelle2,3
1Laboratório de Ictiologia e Pesca, Departamento de Biologia, Universidade Federal de Rondônia, Porto Velho, RO, Brasil. 2UMR BOREA (IRD-207, MNHN, CNRS-7208, UPMC, UCBN) Montpellier, France. 3Laboratoire Mixte International – Evolution et Domestication de l’Ichtyofaune Amazonienne (LMI – EDIA). 4Department of Environmental and Forest Biology, State University of New York, College of Environmental Science and Forestry, Syracuse, NY 13210, USA. 5Laboratoire de Chimie Analytique Bio-inorganique et Environnement, IPREM, CNRS UMR 5254, Université de Pau et des Pays de l’Adour, France. 6Laboratoire Cycles Géochimiques et ressources, IFREMER Brest, France. 7Instituto de Investigaciones de la Amazonía Peruana (IIAP), Programa para el Uso y Conservación del Agua y sus Recursos (AQUAREC), Iquitos, Peru. 8Universidade Federal de São Paulo, Brasil. 9Department of Fish and Wildlife Conservation, Virginia Tech, Blacksburg, VA 24061

Abstract: Abstract: Recently, otolith 87Sr/86Sr analyses revealed a > 8000 km long migration with natal homing in the Amazonian predatory catfish Brachyplatystoma rousseauxii. This exceptional life cycle between the breeding area in the Andean piedmont and the nursery area in the lower Amazon-estuary area was demonstrated for fish caught and hatched in the upper Madeira basin. Although suspected as well for fish caught and hatched in the upper Amazon, this migratory pattern could not be demonstrated owing to lower environmental waters 87Sr/86Sr gradients along the Amazon main stem. Here otoliths with known Sr isotope profiles (LA-MC-ICPMS) were analyzed using scanning x-ray fluorescence microscopy (SXFM) in order to test whether Sr:Ca and Se:Ca could shed some light on migratory patterns of fish caught in the upper Amazon: 2 natal homers from the upper Madeira, 2 forced-residents (born after the dams) from the upper Madeira and 3 fish from the upper Amazon (Marañon and Ucayali rivers). The results confirmed the existence of a homing behavior also in fish born in the upper Amazon and demonstrated the usefulness of both methods to unravel the migratory patterns of Amazonian catfish species. They also emphasized that the life cycle of B. rousseauxii is probably more complex than previously thought, with the observation of a resident life cycle in a fish from the upper Amazon (BR 008), without barrier to its downriver migration.

 

 
"Losing track of time: Use of otolith chemistry to solve the problem of age determination in Baltic Sea cod"

Heimbrand, Y.1, K.E. Limburg1,2, R.Huang3, and T. Naeraa4
1Department of Aquatic Resources, Coastal Laboratory, Swedish University of Agricultural Sciences, Öregrund, Sweden; 2Dept. of Environmental and Forest Biology, SUNY College of Environmental Science and Forestry, Syracuse, NY 13210 USA; 3Cornell High Energy Synchrotron Source, Wilson Laboratory, Cornell University, Ithaca, NY 14851; 4Department of Geosciences, Lund University, Lund, Sweden

Abstract: Cod, a primary fishery species in the Baltic Sea since prehistoric times, has recently experienced marked declines in size and condition. This is due to a combination of worsening water quality conditions from hypoxia intensification, reduction in prey availability even as cod densities have risen, and increased occurrence of parasites and disease. One of the net results of this has been a decrease in formation of clear annual growth rings in otoliths of Eastern Baltic Cod. Otoliths (ear-stones) are part of the hearing and balance system in fishes, and grow incrementally as a fish grows. In seasonal environments, growth bands are laid down, much like tree rings. But in Eastern Baltic cod it has become increasingly difficult to "read" otoliths and determine ages. We have been testing new methods to age cod, using otolith microchemistry in conjunction with optical imagery of otoliths. A suite of elements that represent both exogenous (environmental) and endogenous (physiological; growth related) processes can be mapped at micron scales. We present here 2-D trace elemental maps collected by scanning X-ray fluorescence microscopy or by laser-ablation inductively coupled mass spectrometry. The latter can quantify lower-Z elements that are beyond the scope of our setup at CHESS.

 

 
"Elucidating life history variability in Amazonian goliath catfishes using otolith microchemistry"

Hermann, T., K. E. Limburg, and D. J. Stewart
Dept. of Environmental and Forest Biology, SUNY College of Environmental Science and Forestry, Syracuse, NY 13210 USA

Abstract: Otoliths are bone-like structures in the inner ear of fishes composed of calcium carbonate and protein that leave visible annual or biannual rings as they grow outward from their nucleus. These rings can be counted to estimate the age of fish, similar to the aging of trees. Additionally, otoliths can entrain micro and trace elements in quantities that reflect ambient water conditions. These two characteristics of otoliths allow fisheries scientists to elucidate the environments inhabited by fish at particular ages, thereby revealing critical information such as nursery areas, migratory behavior, and spawning habitats. Not only do otoliths provide a “black box” of a fish’s entire life, they also facilitate the study of species that otherwise would be too difficult or expensive to track by traditional means (e.g., those living in remote locations and/or those that migrate exceptionally long distances). Poorly studied species in vulnerable habitats are beginning to benefit from these efficient techniques. The Amazon river basin in particular hosts thousands of such fishes, such as the goliath catfishes in the family Pimelodidae, which are among the Amazon’s most important species due to their key roles as predators and their valuable fisheries. Several recent studies, including those using otolith microchemistry, have demonstrated that some members of this family undertake spawning migrations that are thousands of kilometers roundtrip, representing the longest known freshwater migrations in the world1–4. Such studies have been limited to only a few members of the family, however, and the behaviors of other important pimelodids remain largely unknown. Here, we used scanning x-ray fluorescence microscopy (SXFM) to investigate the abundances of trace and microelements relative to Ca among several unstudied pimelodids. This study provides a first-look at the migratory behaviors of several important species.

 

 
"Disagreement of EXAFS data for aqueous Rb+ solutions with literature"

Markus M. Hoffmann
The College at Brockport, State University of New York

Abstract: A feasibility study on Rubidium Bromide and Nickel Bromide solutions was undertaken to see if EXAFS could shed light on how these mineral salts are dissolved in neat surfactant media. The obtained EXAFS data are indicative for ion pairing, but EXAFS amplitudes seemed unreasonable high. This issue was confirmed later for aqueous rubidium bromide solution where larger EXAFS amplitudes were observed compared to literature data. Feedback for experimentally rectifying this issue is welcomed.

 

 
"Time Resolved BioSAXS at MacCHESS"

Jesse Hopkins
MacCHESS, Cornell University

Abstract: Time Resolved SAXS measures time dependent structural changes of macromolecules in solution. It is often used to study conformational changes or unfolding/refolding. Reaction initiation is typically done by fluidic mixing, which can change the pH, salt concentration, or introduce ligands for the system to react with. This poster describes the design, fabrication, and initial testing of custom microfluidic mixers for use at the MacCHESS beamline.

 

 
"Pressurizing protein crystals using diamond anvil cell"

Qingqiu Huang and Doletha M. E. Szebenyi
MacCHESS, Cornell University, Ithaca, NY 14853

Abstract: Currently there are mainly two methods being used to high-pressurize macromolecular crystals: diamond anvil cell (DAC) and high-pressure cryocooling (HPC). Using the DAC method, higher pressure (up to 1 GPa, or even higher) can be reached and the crystal can be diffracted under high pressure. Moreover, diffraction data (not a completed data set) at different pressures can be collected on a same crystal. However, due to the limit of the diamond window, currently only less than 70° of diffraction data can be collected. Moreover, diffraction data are collected at room temperature so that most crystals can survive for only a few diffraction images. Therefore, the DAC method is only suitable for crystals with high symmetry. In the HPC method, the maximum pressure is much lower (400MPa, but usually 200MPa); the crystal can be diffracted only after it has been frozen to liquid nitrogen temperature and the pressure has been released; diffraction data at different pressures can’t be collected on a same crystal. However, the high-pressure crycooled crystal can be diffracted as a normal frozen crystal and a completed data set can be collected no matter which symmetry the crystal has. Chaeun Kim and others have believed that ultralow temperature can keep the crystal in its status under high pressure even after the high pressure is released. However, we think even at room temperature the crystal can keep its status under high pressure after the high pressure is released.

 

 
"Operando X-ray Microscopy and X-ray Diffraction of Lithium Sulfur Batteries"

Xin Huang
CHESS, Cornell University

Abstract: Lithium Sulfur battery has been extensively studied due to its high theoretical specific capacity (1672 mAh/g) and abundance on earth. However, the reaction between sulfur and lithium produces a series of polysulfide intermediate species that can be easily dissolved into the electrolyte, and migrate into the Li anode side, which leads to many problems such as shuttle reaction and the loss of the capacity. Moreover, the detailed reaction mechanism of this key effect is not fully understood. Here...

 

 
"High-pressure Small Angle X-ray Scattering of Biological Molecules"

Gabrielle Illavaa, Kelly Jenkinsb, Harish Balasubramanianb, Doug Barrickc, Sean Kleinc, Roland Winterd, Catherine Royerb & Sol M. Grunera,e
aCHESS, Cornell University, Ithaca, NY 14853
bDepartment of Biological Sciences, Rensselaer Polytechnic Institute, Troy, NY 12180
cDepartment of Biophysics, Johns Hopkins University, Baltimore, MD 21218
dDepartment of Biophysical Chemistry, Technische Universität Dortmund, Dortmund, Germany,D-44227
eDepartment of Physics, Cornell University, Ithaca, NY 14853

Abstract: High-pressure SAXS as a technique in molecular biology is a difficult, but worthwhile endeavor since no other synchrotron facility in the United States has this technology available. Pressure is a particularly useful thermodynamic perturbation of proteins since its effects arise because of differences in molar volume between biomolecular conformational states. Pressure affects the tertiary structure of proteins in several ways, most notably by changes to the internal cavities of the protein. Under high pressure, water hydrates the internal, hydrophobic cavities of the protein, causing it to unfold. This allows additional transition states to be stabilized. Measurement of these differences through SAXS is ideal to obtain global shape information as the protein unfolds under pressure.

Here we present the design and implementation of the high-pressure SAXS cell that is now available to the CHESS and MacCHESS user community.

 

 
"Fabrication of a coaxial turbulent-jet mixer for studying rapid nanoparticle reactions at CHESS"

A. Itskovichab, D. Smilgiesab A. Bhargavac, A. Nelsonc, R. Robinsonc
aChemical & Biomolecular Engineering, bCLASSE, cMaterials Science & Engineering, Cornell University

Abstract: Nanoparticle chemistry is one of the most rapidly evolving fields in modern chemistry, promising significant advancements in a variety of fields. The ability to accurately characterize the structures of nanoparticles (NPs) and their reactions is fundamental to the development of nanotechnology. One of the challenges involved in studying in-situ NP reactions is that certain transformations occur too quickly for spectroscopic analysis. A coaxial turbulent-jet mixer is a simple-to-build, inexpensive device that allows for the time-resolution of fast NP reactions by conducting a rapidly-combined reaction mixture down a transparent capillary where it can be probed with X-rays.

 

 
"Simultaneous, Synchrotron Based, Real-time X-ray Reflectivity Using Monochromatic Radiation"

Howie Joress
Cornell University

Abstract: We describe the development of a synchrotron based, monochromatic, real-time x-ray reflectivity (XRR) measurement technique. We utilize a polycapillary x-ray optic to produce a converging fan of radiation which provides the range of simultaneous incident angles necessary for monochromatic XRR. For sufficiently smooth surfaces, the specular reflection dominates the diffracted signal, and using a 2D detector allows us to collect a portion of the reflectivity curve simultaneously. Our capillary all...

 

 
"Annealing of Diblock Copolymer Thin Films using Solvent Vapor Mixtures"

Florian Jung1, Anatoly V. Berezkin1, Detlef-M. Smilgies2, Dorthe Posselt3, and Christine M. Papadakis1
1Technical University of Munich, Physics Department, Garching, Germany
2Cornell University, CHESS Wilson Lab, Ithaca, NY, U.S.A.
3Roskilde University, Department of Science and Environment, Denmark

Abstract: Block copolymers self-assemble into nanostructures. Solvent vapor an-nealing (SVA) is an efficient method to improve the long-range order or to alter the morphology in block copolymer thin films.

In the present work, SVA is carried out on thin films from a polystyrene-b-poly(dimethyl siloxane) (PS-b-PDMS) diblock copoly-mer. For annealing, vapor mixtures of toluene and n-heptane were used, which are weakly selective for PS and highly selective for PDMS, respectively. The morphological changes were investigated by in-situ, real-time grazing-incidence small-angle X-ray scattering (GISAXS). Varying the vapor composition during the annealing cycle results in a lamellar morphology and cylinders with different orientations. Us-ing the scattering contrast, the distribution of the two solvents in the microphase separated thin film can be determined. This information can be transferred to a phase diagram and be related to the observed morphologies during annealing.

The results show that solvent exchange during SVA gives control over the morphology, and that GISAXS can be used to track the tra-jectory through the phase diagram experimentally.

 

 
"Observation of freezing in grapevine bud tissues using X-ray phase contrast"

Alisson Pacheco Kovaleski, Jason Londo, and Kenneth Finkelstein
Cornell University

Abstract: Dormant grapevine buds cope with below freezing temperatures during the winter by freezing the extracellular portion of their tissues while supercooling the intracellular water. With this process, their maximum hardiness can reach close to –40 °C depending on the species and genotype, but the low limit is based on the ability of water to supercool (~ –42 °C). The state transition from liquid to solid in water greatly decreases density. Plant tissues where water freezes will tend to expand, although the exact direction of the movement is also influenced specially by the cell walls’ resistance. The objective of this study was to use time-lapse imaging to visualize the movement of bud structures and correlate that with the freezing behavior of buds. Although using 2D images of buds is not optimal due to the convoluted nature of this structure, some angles allow observation of bud scales and differentiation of primary and secondary buds.

Buds were held in a tube of Kapton in the path of the beam. The monochromatic beam was expanded to 7 × 7 mm with an intensity of 15 KeV. The phase contrast is obtained from wavefront angular deviations due to density variations in the sample. These deviations interact with the unperturbed beam and become intensity variations, recorded on 2D images with spatial resolution of ~ 1 μm. To observe the movement of structures due to ice formation, we recorded a time series with 1.5 s exposures (0.667 Hz) as the buds were exposed to a cryostream at 200 K. The time-lapse was then divided by the initial scan, and therefore any movement in the sample would result in a signature of the area that moved. Because we expect the outer parts of the bud to freeze before the inner parts, the movement from the outer parts should not result in movement of the inner portion.

We observed that freezing began in our samples in the outer scales, followed by the lower portion of bud where it was attached to a piece of cane and subtending tissues of the bud cushion. The inner tissues were frozen last as expected. The difference in timing of freezing between the different portions of the bud demonstrates that there was no influence of the movement of one part on the others. We were not able to detect when the intracellular water froze. It is possible that the rapid freezing did not allow for the natural process to occur, with no differentiation between intra and extracellular water freezing. In future experiments, a slower freezing protocol should be used, without direct contact between the bud and the cold stream. Additionally, using thermocouples to record temperatures in the surface of the bud and inside the bud would allow for identification of the timing and temperature of extra- and intracellular water freezing.

 

 
"Solution SAXS and in situ GISAXS Study of the Fabrication of Asymmetric Block Copolymer Membranes"

Yuk Mun Li
Cornell University

 

 
"Using Single Grain High Energy X-ray Diffraction Experiments to Study the Role of Plasticity in Hydrogen Embrittlement"

Timothy Long
Cornell University

 

 
"Unmixing enzyme allostery"

Steve P. Meisburger, Alexander B. Taylor, Crystal A. Khan, Shengnan Zhang, Paul F. Fitzpatrick, and Nozomi Ando

Abstract: Protein allostery is a key mechanism of metabolic control in all forms of life. Enzymes that change their activity in response to an effector are particularly important for regulating metabolite fluxes. I will discuss the application of small-angle X-ray scattering (SAXS) to study allosteric enzymes, which exist as complex mixtures in solution, using new strategies to “computationally purify” complex mixtures. In particular, I describe the powerful combination of chromatography-coupled SAXS and evolving factor analysis (EFA), an extension of singular value decomposition (SVD), which can separate scattering profiles of species that are not completely resolved by the column. We have used this technique to visualize the domain motions of phenylalanine hydroxylase (PheH), an enzyme that converts phenylalanine to tyrosine in the liver. The data support a model where tetrameric PheH is activated by dimerization of the regulatory domains, which bind phenylalanine in the active conformation. Surprisingly, the allosteric mechanism of this mammalian enzyme appears to be conserved from bacterial enzymes that synthesize aromatic amino acids.

 

 
"An In-situ investigation of solvent engineering of hybrid perovskite and its implication on morphological control"

Rahim Munir1, Yufei Zhong1, Arif D.Sheikh1, Maged Abdelsamie1, Liyang Yu1, Kui Zhao1, Hanlin Hu1, Taesoo Kim1, Ruipeng Li2, Detlef-M. Smilgies2, Aram Amassian1*
1King Abdullah University of Science and Technology (KAUST), Solar & Photovoltaics Engineering Research Center (SPERC), and, Physical Science and Engineering Division (PSE), Thuwal, 23955-6900, Saudi Arabia
2Cornell High Energy Synchrotron Source (CHESS), Cornell University, Wilson Laboratory, Ithaca, NY 14853, USA

Abstract: Although perovskite-based solar cells have achieved high power conversion efficience in short time span, still the basic understanding of the formation of perovskite active layer lacks behind1-4. To cater the need of deeper understanding of the processing parameters to form the active layer we have studied in-situ spin coating of perovskite material at a high energy x-ray source. Our results indicate that this solution processing resembles sol-gel processing to form thin films. Here we report the role of antisolvent dripping during the spin coating process.

[1] Nam-Gyu Park et al., J. Phys. Chem. Lett. 4, 2423−2429 (2013).
[2] Michael M. Lee, Henry J. Snaith et al., Science 338, 643 (2012).
[3] Giles E. Eperon, Henry J. Snaith et al., DOI: 10.1002/adfm.201302090 (2013).
[4] Huanping Zhou, Yang Yang et al., Science 345, 542 (2014).

 

 
"Beamline Front Ends for CHESS-U"

Alan Pauling1, Eric VanEvery2, Tim Shea2, Alan Baur2, Gary Navrotski3
1Cornell High Energy Synchrotron Source, Cornell University, Ithaca, NY
2ADC USA, Inc. Lansing, NY www.adc9001.com
3Advanced Photon Source (APS), Argonne National Laboratory, Lemont, IL

Abstract: The Cornell High Energy Synchrotron Source (CHESS) is a National Science Foundation funded International User Facility located on the Cornell University campus in Ithaca, New York, hosting over 1,300 user visits from a broad spectrum of scientific communities every year. In summer of 2017, CHESS will embark on a massive upgrade to the particle storage ring (CHESS-U), an evolution to a 3rd generation synchrotron source in late 2018. CHESS-U will increase the energy of the electron beam from 5.3 to 6.0 GeV, double the current from 100 to 200 mA, and reduce the horizontal emittance of the particle beam from 100 nm-rad to 30 nm-rad by eliminating the positron source. These upgrades to the storage ring will require new undulator-sourced beamlines to be built.

The beamline upgrade portion of the CHESS-U project is moving ahead at full steam. Scientific needs have been identified. A suitable layout for the experimental floor has been devised. The work breakdown structure (WBS) has been created and System Managers have been assigned. Two large contracts have been awarded and designs are being vetted. We are almost ready to cut metal.

 

 
"Time-Resolved Hard X-ray 3-D Imaging of Reciprocal Space for Material Science using the CdTe Mixed-Mode Pixel Array Detector (MM-PAD)"

Hugh T. Philipp1, Mark W. Tate1, Kamalika Chatterjee2, Armand J. Beaudoin2 & Sol M. Gruner1,3
1Laboratory of Atomic and Solid State Physics, Cornell University, Ithaca, NY 14853, USA
2Department of Mechanical Science and Engineering, University of Illinois at Urbana-Champaign, Champaign, IL, USA
3Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853, USA

Abstract: Several integrating pixel array detectors (PADs) developed by the Gruner Group have recently been coupled to CdTe sensors. This greatly improves the quantum efficiency of these high-speed, high-dynamic-range imagers in the hard x-ray regime [1]. A detector constructed using the mixed-mode PAD (MM-PAD) chips[2] bonded to CdTe sensors was used recently in an x-ray diffraction study of the fatigue and failure of metal alloys at 80 keV. The MM-PAD was used to image the diffraction from a polycrystalline sample under tensile stress at rates of 200-500 Hz in synchrony with a +/- 2.5 degree oscillation of the sample at 2-5 Hz. The method allows Bragg reflections to be tracked and studied in detail as evolving volumetric entities in reciprocal space. This contrasts with previous time-resolved studies using PADs and non-rocking samples in which reflections were subject to drifting out of the diffraction condition as grains reoriented and deformed.

[1] Julian Becker, Mark W. Tate, Katherine S. Shanks, Hugh T. Philipp, Joel T. Weiss, Prafull Purohit, Darol Chamberlain, Jacob P. C. Ruff and Sol M. Gruner (2016). Characterization of CdTe Sensors with Schottky Contacts Coupled to Charge-Integrating Pixel Array Detectors for X-Ray Science. JINST 11: P12013. Preprint: https://arxiv.org/abs/1609.03513. doi:10.1088/1748-0221/11/12/P12013

[2] M.W. Tate, D. Chamberlain, K.S. Green, H.T. Philipp, P. Purohit, C. Strohman, S.M. Gruner. A medium-format, mixed-mode pixel array detector for kilohertz x-ray imaging. Journal of Physics: Conference Series. 425 (2013) 062004 (pdf).

 

 
"X-Ray Shielding Lead Encapsulated Enclosures (“Hutches”)"

Dana Richter1, Eric VanEvery2, Alan Baur2, Alex Deyhim2, Gary Navrotski3
1Cornell High Energy Synchrotron Source, Cornell University, Ithaca, NY
2ADC USA, Inc. Lansing, NY www.adc9001.com
3Advanced Photon Source (APS), Argonne National Laboratory, Lemont, IL

Abstract: The Cornell High Energy Synchrotron Source (CHESS) is a National Science Foundation funded International User Facility located on the Cornell University campus in Ithaca, New York, hosting over 1,300 user visits from a broad spectrum of scientific communities every year. In summer of 2017, CHESS will embark on a massive upgrade to the particle storage ring (CHESS-U), an evolution to a 3rd generation synchrotron source in late 2018. CHESS-U will increase the energy of the electron beam from 5.3 to 6.0 GeV, double the current from 100 to 200 mA, and reduce the horizontal emittance of the X-ray beam from 100nm to 30nm by eliminating the positron source. These upgrades to the storage ring will require new undulator-sourced beamlines to be built.

ADC is producing the design and fabrication of two hutches for the first phase and five for second phase of upgrades. To reduce downtime, ADC is committed to the quickest on-site installation as possible. To reach our installation goals, ADC has implemented a highly modular design consisting of 15 wall segments and 13 ceiling segments, Figure 4. The hutches will be shipped as modular pieces after being fully assembled and tested at ADC.

 

 
"BAM-2 Automounter development at MacCHESS"

David J. Schuller, Michael Cook, Bill Miller, Scott Smith, D. Marian Szebenyi
MacCHESS, Cornell University, Ithaca, NY

Abstract: The Berkeley AutoMounter model 2 (BAM-2), developed at LBNL and implemented at MacCHESS and APS GMCA-CAT beamlines has undergone further development at MacCHESS, with an emphasis on improving reliability and speed. The BAM-2 at MacCHESS is now in regular service at CHESS beamline F1. The BAM-2 accepts the same samples as the earlier BAM model: "ALS" pins with ALS, Uni- or Rigaku ACTOR pucks; while the purpose-built pneumatic actuators have been replaced with a commercially available three-axis Cartesian robot. Examples will be presented to highlight the flexibility of a primarily software-based machine, and to show hardware and software changes designed to improve speed and reliability. Particular attention will be paid to more extensive utilization of the built-in force/torque sensor.

 

 
"Combined high-energy synchrotron scanning XRF and XRD for analysis of illuminated manuscript leaves"

Louisa Smieska
The Metropolitan Museum of Art

Abstract: We have recently had the opportunity to examine a group of 13th-15th century illuminated manuscript fragments from the Cornell Library Rare and Manuscript Collection using simultaneous synchrotron based MA-XRF and XRD measurements. Here, we (1) describe our study of trace elements in azurite blue pigments and (2) present examples where the addition of XRD to MA-XRF allowed us to identify unexpected materials in these illuminated manuscript fragments.

 

 
"Hybrid Organic-Inorganic Materials: from Small Angle to Wide Angle"

Ethan Susca, Kate Barteau, Peter Beaucage, Tom Gardinier, Ferdinand Kohle, Kai Ma, and Uli Wiesner
Department of Materials Science and Engineering, Cornell University

Abstract: Hybrid organic-inorganic systems have applications ranging from new metamaterials to high efficiency solar cells and ultra small particles for nano-medicine . Here we discuss our recent results on mapping the orientation and grain growth of gyroidal block copolymer-inorganic composites with high spatial resolution, using in-situ thermal annealing to study the early crystallization and degradation pathways in organic-inorganic perovskites, and characterizing C'-dots used for cancer treatment.

 

 
"Artificial Membranes for Protein Transport"

B. Sutisna,a G. Polymeropoulos,b E. Mygiakis,b V. Musteata,c K.-V. Peinemann,d D.-M. Smilgies,e N. Hadjichristidisb* and S. P. Nunesc*
King Abdullah University of Science and Technology (KAUST), Thuwal, 23955-6900, Saudi Arabia, a. Physical Science and Engineering Division (PSE), b. KAUST Catalysis Center (KCC), Physical Science and Engineering Division (PSE), c. Biological and Environmental Science and Engineering Division (BESE), d. Advanced Membranes and Porous Materials Center (AMPMC), Physical Science and Engineering Division (PSE), e. Cornell High Energy Synchrotron Source, Wilson Laboratory, Cornell University, Ithaca, New York 14853, USA

Abstract: Preparation of artificial membranes with bioinspired channels for protein separation and water transport is still troublesome when it comes to large scale production. In this work, a scalable and simplified method based on block copolymers is introduced. Our objective is to explore the possibility of using self-assembly and non-solvent induced phase separation (SNIPS) method to synthesize artificial preferential channels.

 

 
"What's New at MacCHESS"

D. Szebenyi, R. Cerione, T.K. Chua, M. Cook, R. Gillilan, J. Hopkins, Q. Huang, I. Kriksunov, W. Miller, D. Schuller, S. Smith and J. Wierman
MacCHESS, Cornell University, Ithaca, New York 14853

Abstract: MacCHESS conducts both core and collaborative research projects, and supports users doing "Macromolecular diffraction at CHESS". In 2016-2017, users employed CHESS facilities to collect crystallographic and small-angle solution scattering (BioSAXS) data on numerous molecules and complexes of biological interest. A sampling of users' important structural results, reported here, provides insight into how reactions can occur inside a cell membrane, how the rotary proton pump V-ATPase is regulated, and how changes in an enzyme's shape control its activity.

Developments in the major focus areas of MacCHESS include:

BioSAXS — in-line SEC-SAXS is routinely available and increasingly popular; continuing improvements in the RAW processing software improvements have been made; initial experiments in time-resolved studies using microfluidic mixing chips are in progress.

Pressure Cryocooling (HPC) — refinements to the sample mounting procedure are continuing; HPC has been applied to trap biologically active gases, e.g. CO2 in carbonic anhydrase and O2 in nitric oxide synthetase; several cases of pressure-induced reduction of disorder have been observed.

Microcrystallography — significant advances have been made in serial microcrystallography, using the intense focused beam at G3 and multicrystal holders from the Miller group (Toronto); development of on-line confocal microscopy is continuing.

New directions in high pressure — high-pressure BioSAXS is under development: a sample cell capable of pressurization to 4 kbar is available, and studies of protein folding are proceeding, in collaboration with Cathy Royer (RPI). Study of protein crystals in diamond anvil cells is also beginning.

 

 
"Improved s-XRF Mapping for a Painting Attributed to Honoré Daumier"

John Twilley, Louisa Smieska, Arthur Woll, Mary Schafer, Aimee Marcereau DeGalan

Abstract: Exit from the Theater has long been attributed to French satirical artist Honoré Daumier (1808-79) on the basis of style, materials, and details of technique but no historical link of the painting to the artist has been found. Identification of a landscape, long known to be present on the wood panel beneath the theater scene but irresolvable by conventional means of diagnostic imaging, holds the potential to bolster, or refute, the attribution to Daumier. SEM-based elemental analyses of microsamples have been used to optimize the excitation conditions for s-XRF elemental mapping with the MAIA detector. The tunability of the monochromatic primary excitation of the synchrotron source has been essential to reducing the interference of a layer of lead paint covering the landscape, resulting in greatly improved legibility relative to its mapping by a continuum (tube) source. Reprocessing of subsets of XRF data in Geopixe, based upon anti-correlations among elements present at trace levels, has lead to maps for an expanded set of elements in the landscape and the potential for archival research to finally resolve its origin.

 

 
"Cutting edge SMX at MacCHESS: Room temperature serial crystallography with oscillating fixed-targets and fast-framing detectors on a micro-focused x-ray beam"

Jennifer Wierman
MacCHESS, Cornell University

Abstract: There is growing interest in pursuing serial microcrystallography (SMX) experiments at existing storage ring (SR) sources. For very small crystals, radiation damage occurs before sufficient diffraction is recorded to determine the orientation of the crystal. The challenge is to merge data from a large enough number of crystals in order to determine the protein structure. At MacCHESS, we focus on providing a clean, bright micro-focused beam for serial microcrystallography together with advances in low-background sample delivery. In collaboration with the Dwayne Miller Group from the University of Toronto, we've developed a sample delivery system which allows for one degree of oscillation per crystal over thousands of positions within a micro-fabricated chip. In conjunction with a fast framing detector, this establishes the feasibility of rapid oscillation data collection in serial protein microcrystallography at CHESS.

 

 
"Solution SAXS and in situ GISAXS Study of the Fabrication of Asymmetric Block Copolymer Membranes"

Qi Zhang
Cornell University