ILSF Progress Report

• Morteza Jafarzadeh (Iranain Light Source Facility)

Room: Allame Rafiee Conference Hall

ILSF Science Division Activities

• Ehsan Salimi (IPM)

Room: Allame Rafiee Conference Hall

Science Highlights and Perspectives Using the Light from the Elettra Storage Ring

• Maya Kiskinova (Elettra Synchrotron Light Source)

Room: Allame Rafiee Conference Hall Elettra laboratory operates a synchrotron storage ring since 1993 and offers most of the existing spectroscopic and scattering techniques based on interactions of light (IR to X-rays) with matter. Investigations performed using the Elettra storage ring span over all classes of materials: metals, semiconductors, superconductors, catalysts, ceramics, glasses, polymers, magnetic materials, materials for energy, electronic and bio-medical appliances, biomaterials, etc [1]. Elettra synchrotron has one of the most extensive programs worldwide in the development and applications of all types of photoelectron spectroscopies (PES), which include high resolution or time-resolved PES, nano-ARPES, spin-resolved ARPES, scanning and full-field imaging photoelectron microscopy (SPEM and PEEM). Experiments using photon-in/electron-out and photon-in/photon-out techniques span over 2D materials, strongly correlated electron systems, magnetism, surface and interface phenomena relevant to catalysis and electrochemistry. In particular, the response to operating conditions and external stimuli – temperature, radiation, electric and magnetic fields are the main targets. In the field of life sciences, along with protein crystallography experiments, rather extended programs have been focused on assessing potential health hazards of nano-materials and pollutants by means of photon-in/photon-out spectroscopies (XRF, XAS), IR and Soft X-ray Microscopy. Using selected exemplary systems the most recent achievements in basic and applied research will be illustrated with emphasis on in-situ characterization of various systems, where issues of complexity at microscopic length scales should be faced and understood.

How to Write Good Synchrotron Beamtime Proposals

• Miguel A. G. Aranda (ALBA-CELLS Synchrotron Light Source)

Room: Allame Rafiee Conference Hall ALBA synchrotron light source (www.cells.es) and IPM signed an agreement in September-2016 for boosting synchrotron usage by Iranian scientists. This agreement included the booking of 20 beamline days for the Iranian users to be allocated after the launching of a call for proposals and the appropriate evaluation based on scientific excellence (by an Iranian committee) and on technical and safety feasibility (by ALBA staff). As part of this effort, an IPM-ALBA workshop devoted to report and deeply discuss the available ALBA beamlines and techniques to the future Iranian users took place in Tehran in November-2016. This workshop was not general but tailored to the usage of the available ALBA techniques. Later, the call for proposals was launched with a deadline of March-10th 2017. The selected experiments, as today the evaluations are in progress, will be carried out at ALBA in the period September to December-2017. A core task within any user-oriented facility in the writing (by the users) and the evaluation (by expert committee(s)) of the proposals submitted for requesting to carry out an specific research. This talk, after introducing the IPM(ILSF)-ALBA agreement will be devoted to show how to write a good synchrotron beamtime proposal. Several guidelines (and tips) about the structure and content of a proposal will be given. A good proposal must be complete but not very large, and focused to address a clear scientific challenge. In addition to clearly establish the goal and scope of the proposal, several sections must be addressed in order to allow a thorough evaluation with a successful output: I) a brief and sound introduction to frame the research; ii) any relevant previous laboratory-based characterisation and results obtained by the research group; iii) the scientific methodology and synchrotron radiation technique to be employed; iv) the results to be expected; v) the justification of the requested beamtime; vi) the relevant bibliography. In case of non-expert users, it is strongly encouraged to contact the relevant beamline scientist in order to ask for the technical feasibility of the proposed work and to look for advised of an optimum match between the expected scientific outputs and the beamlines performances and capabilities.

Structures of Acuo-Ions and Coordination Complexes with EXAFS and XANES

• Adela Muñoz Páez (University of Seville)

Room: Allame Rafiee Conference Hall X-ray absorption spectroscopies (XAS) provide accurate information of local order around atoms in solid or liquid states. In the EXAFS region of a XAS spectrum, the high kinetic energy of the electron renders the analysis rather simple, since single scattering contributions are dominant. The adjustable parameters are coordination distances, R, coordination numbers, N, and Debye-Waller (DW) factors, which take into account static and dynamic disorder. The structure around the absorbing atom within a radius of 4 A˚, can be determined with uncertainties of 0.01 °A in coordination distances, while that for coordination numbers is much higher (10–15%), because they are highly correlated with DW factors. To overcome this correlation, DW factors can be eliminated by summing over a set of Molecular dynamics MD structural arrangements (snapshots) large enough to be representative of the whole system. The information provided by the analysis of the XANES region is complementary to that supplied by EXAFS because, due to the low kinetic energy of the electron, it is sensible to coordination polyhedron, although this renders data analysis more complex.1 The first example selected to show the capabilities of the technique are the highly stable and symmetric aqua ions with octahedral configuration [Cr(H2O)6]3+, [Rh(H2O)6]3+ and [Ir(H2O)6]3+, for which we determined the first and second hydration sphere by analyzing the EXAFS region taking into account single and multiple scattering contributions.2-4 The second example, the analysis of the asymmetric and lest stable aqua ions [Y(H2O)8]3+ and [Cf(H2O)6]3+, required the quantitative analysis of the XANES region and the use of MD simulations. It was found that the first hydration shell of Y(III) and Cf(III) cations was formed by eight water molecules. The value for Cf(III)–O coordination distance, 2.43 A˚ together with those of other three valent lighter actinides, pointed to the existence of an actinide contraction similar to that found for the lanthanide cations.5 Additional examples will be those of Cu(II) complexes containing N-coordinating ligands of relevance to understand the interactions of this cation with biomolecules.

I08-SXM: Recent Achievements and Future Scope

• Majid Kazemian Abyaneh (Diamond Light Source)

Room: Allame Rafiee Conference Hall Scanning X-ray microscope is now established and one of the key techniques found at the third generation synchrotron radiation facilities to tackle wide variety of studies in many fields such as microbiology, environmental sciences, medical and pharmaceutical sciences, and materials science. I08 Scanning X-ray Microscopy beamline (I08-SXM) is one of those facilities available worldwide, which covers the broadest soft x-ray photon energy range in the world to access all major K- and L-edges absorption for elemental and chemical analysis, combined with complementary imaging and spectroscopic techniques. Such multimodal detection is the strong point for the scanning regime contrast to the full-field. I will show-case our capability and some examples from our user experiments including NEXAFS spectromicroscopy in different photon energy range, X-ray micro-fluorescence (XRF) elemental mapping, Ptychographic image reconstruction, (measurement under cryogenic specimen condition) and so forth. Recent upgrades at I08 will be discussed

Macromolecular Crystallography Projects in Iran; the First Two Structures Deposited in the Protein Data Bank

• Arefeh Seyedarabi (Institute of Biochemistry and Biophysics, University of Tehran)

Room: Allame Rafiee Conference Hall In an attempt to initiate macromolecular crystallography projects in Iran, the study of hemoglobin structure belonging to two sturgeon fish (from the Caspian Sea) was undertaken with minimal facility. As the first dedicated macromolecular crystallography research laboratory in Iran, the research started from crystallization screening and optimization of the two hemoglobins, followed by transport of frozen crystals to the Beijing Synchrotron Radiation Facility for data collection and subsequent in house analysis of the data and determination of X-ray sequence and structure leading to the deposition of the two structures in the protein data bank. The structures have not only been important as the first two structures determined in Iran but have also been most novel and exciting as they unravel the cause of hemoglobin autoxidation and hemin loss which has been the focus of many international research studies for over two decades due to its great importance to cardiovascular medicine (in the field of plaque development in arteries and atherosclerosis) and the food industry (in the field of muscle prevention affecting the quality, odor and flavor of meat and ultimately affecting sales). Having said all this, structural study is lacking greatly in Iran both in research and industry since many interesting and important research studies are carried out in top Universities and research institutes in Iran, but because of the limited expertise and facilities so far, they have been put aside and other routes taken (particularly bioinformatics and non-experimental based structural research). However, it is the time for Iranian researchers to take the ultimate experimental approach, make use of the available facilities (although limited), and appreciate ILSF’s efforts in enabling researchers to be users of synchrotrons such as ALBA and Elettra in order to realize macromolecular crystallography projects in Iran.

State of the Art Research at Diamond Light Source and Recent Developments Room: Allame Rafiee Conference Hall

Research Highlights Using Coherent Radiation of FERMI Free Electron Laser

• Maya Kiskinova (Elettra Synchrotron Light Source)

Room: Allame Rafiee Conference Hall The most attractive features of laser-seeded FERMI operated at Elettra since 2012 are its high degree of coherence, tunability, multiple polarization and jitter-free pump-probe schemes, enabling multicolor IR or FEL pump/IR or FEL probe experiments with full control of the intensity and pulse durations. After short overview of the present experimental set-ups the unprecedented opportunity for exploiting ultrafast dynamics with chemical sensitivity will be illustrated using selected recent results. The emphasis will be on time-resolved experiments for tracking the response triggered by optical lasers or FEL pulses with lateral and temporal resolution determined only by the wavelength and duration of the probe.

ALBA Synchrotron Highlights

• Miguel A. G. Aranda (ALBA-CELLS Synchrotron Light Source)

Room: Allame Rafiee Conference Hall ALBA synchrotron light source (www.cells.es) is the largest Spanish research infrastructure that started full operation of its first seven beamlines on February 2013. Nowadays, there are eight beamlines in operation and three under construction. I will divide the talk in three parts: i) a very brief general description of ALBA synchrotron and the Experiments Division that it runs the user program; ii) an overview of the eight operating beamlines and some recent scientific highlights arising from their usage; and iii) a summary of the three beamlines under construction and those approved but still not funded. Firstly, I will start with a very brief description ALBA synchrotron including our structure to fulfil our mission as user-oriented Large Facility. Then, the structure of the Experiments Division which is optimised for running our external user program: both academic and industrial usage, will be discussed. This structure, with six sections, includes the user office (our interface with the users). Secondly, I will introduce our eight operating beamlines. I will give some technical details as well as recent scientific highlights. The beamlines within the Chemistry & Material Science Section are: 1) high-resolution and microdiffraction powder diffraction (BL04-MSPD) which has two endstations, one devoted to very high resolution and very fast powder diffraction and another to microdiffraction running a high-pressure program; and 2) X-ray absorption (XAS) and emission (XES) spectroscopies (BL22-CLAESS) which has also two endstations, one for XAS (both transmission and fluorescence) and a second for XES. The beamlines within the Electronic & Magnetic Structure of Matter Section are: 3) photoemission spectroscopy (BL24-CIRCE) which has two endstations, one devoted to near ambient pressure photoemission (NAPP) and another to photoelectron emission microscopy (PEEM); and 4) soft X-ray Magnetic Circular/Linear Dichroism Absorption and Scattering (BL29-BOREAS) which has two endstations, one devoted to absorption spectroscopy and another to scattering. The beamlines within the Life Science & Soft Condensed Matter Section are: 5) macromolecular crystallography (BL13-XALOC), 6) soft X-ray full-field cryo-tomography (BL09-MISTRAL); 7) small angle and wide angel X-ray scattering (BL11-NCD) with two endstations for SAXS and WAXS; and 8) infrared microspectroscopy (BL01-MIRAS). Thirdly, I will describe the three additional beamlines which are being currently built: 9) angle resolved photoemission spectroscopy BL (BL20-LOREA) that it will become operational in March 2019; the absorption / powder diffraction / metrology and development BL (NOTOS) which it comes to operation in April-2020, and 10) microfocus for macromolecular crystallography BL (BL06-XAIRA) which it is expected to become operational in late 2020. Some details about the additional ALBA phase-III beamlines will be provided.

Real Time Probing of 3D Ordering in Hydrated High-Density Poly (2-Hydroxyethyl Methacrylate) Brushes Using Synchrotron GISAXS and Neutron Reflectivity Room: Allame Rafiee Conference Hall Polymer brushes offer patternable, robust, three-dimensional coatings that can be used for, among other applications, the capture and release of medicine and nanoparticles. High-density poly(2-hydroxyethyl methacrylate) (PHEMA) brushes are complex because interlaced combination between chain conformation, n-clustering-induced interactions near surface proximal layers, and proton donor-acceptor and proton acceptor side chain functional groups are regulated by the local aqueous environment temperature. In this contribution, we demonstrate robust PHEMA brush with a high grafting density that exhibits differential dewetting transitions in the broad temperature range 18-40 C which can be tentatively ascribed to the n-cluster-induced collapse of the polymer segments in the innermost region and so-called “pseudo reverse-solubility” behavior in the outermost region of archetypal high-density PHEMA brush. The polymer segment density profiles of the PHEMA brush in the directional normal to the silicon-D2O interface during a heating-cooling cycle were determined by using in situ neutron reflectivity (NR) measurement technique along with the corresponding degree of hydration. The time-resolved high temporal resolution NR profiles of the swollen brush in D2O had figured out a layered segregated structure with three identical hydrated states inside of the PHEMA brush, consisting of dense surface and underneath regions with ~100Å and ~10Å thick, respectively, in combination with a highly hydrated diffuse brush regime extended between upper and lower collapsed segments. This sandwiched structure is attributed to the skinning of the dense outer region during segment collapse that retards solvent egress. µ-focused grazing incidence small-angle synchrotron X-ray scattering (µ-GISASXS) measurements show that the well-equilibrated initial film exhibits highly ordered structure with isotropic vertical orientation; the film initially swell at the ambient temperature and maintain strongly stretched conformation. However, for temperatures above ~ 30 C, lateral segregation and mesostructural ordering in the dense skin was evidenced from GISASXS patterns, in which the collapsed segments microdomains were distributed over the highly packed diffusive regime.

X-ray Single Crystal Crystallography of Two Amide-functionalized Interpenetrated Metal-Organic Frameworks

• Vahid Safarifard (Iran University of Science and Technology)

Room: Allame Rafiee Conference Hall Here we report the use of a pillaring strategy for the design and synthesis of two novel amide-functionalized isoreticular metal-organic frameworks (MOFs), [Zn2(oba)2(bpta)]·(DMF)3 (TMU-22) and [Zn2(oba)2(bpfb)]·(DMF)5 (TMU-23), where H2oba = 4,4´-oxybisbenzoic acid, bpta = N,N´-bis(4-pyridinyl)terephthalamide, bpfb = N,N´-bis-(4-pyridylformamide)-1,4-benzenediamine and DMF is N,Ndimethylformamide. Solvothermal reactions between Zn(NO3)2·6H2O, H2oba, and the corresponding pillar ligand in DMF at 120 °C for 3 days produced prismatic crystals of TMUs-22/-23 suitable for single-crystal X-ray diffraction analyses. Crystallographic data for TMU-22 and TMU-23 were collected at 100 K at XALOC beamline at ALBA synchrotron (λ = 0.79474 and 0.82653 Å, respectively). TMU-22 and TMU-23 crystallize in the monoclinic P21/n and P21/c space groups, respectively. They are neutral threefold interpenetrated MOFs formed by {Zn(oba)} layers connected through the N,N´-pillar ligands. Their basic unit is a dinuclear zinc cluster, in which both Zn(II) centers are penta-coordinated to four carboxylate O atoms from three fully deprotonated oba ligands and to one N atom from the N,N´-donor ligand.

Magnetic Nanoscopic Correlations in the Crossover between a Superspin Glass and a Superferromagnet

• Atieh Zamani (Institute for Research in Fundamental Sciences (IPM))

Room: Allame Rafiee Conference Hall In recent years Fe1-xZrx (FeZr) Fe-rich metallic glasses (7 < x < 14), have been attracted considerable attention because of their striking magnetic properties. In this composition range, the addition of 1 at.% of Zr increases the Curie temperature in 20 K. However, the changes in behavior that could occur on the magnetic properties due to the structural evolution during the doping process is actually subject of discussion. The Curie temperature (Tc) of amorphous FeZr alloys can be greatly enhanced by doping with light elements. In this investigation, ion implantation is used to dope FeZr thin films with H, He, B, C, and N. We present a preliminary study of the structural evolution of the FeZr sample during the first steps of adding impurities. The magnetic and local structural characterization from two experimental probes, SQUID magnetometry and X-ray absorption fine structure (EXAFS), are ideal experimental techniques to perfom this study. The conservation of the amorphous nature of the (FeZr) as-grown and implanted samples and the effect of incorporating dopant atoms in this structure is confirmed by EXAFS measurements on the Fe K-edge. EXAFS results indicate an almost negligible thermal expansion at temperatures below while normal thermal expansion takes place at higher temperatures. Such expansion seems to promote a reinforcement of the ferromagnetic interactions among Fe-Fe atoms that would account for the observed spontaneous increase in the magnetization as well as for the evolution of the coercive field. Finding the correlation between the structure and the magnetic properties could, with the use of simple sphere-stacking models, allow us to create structures with desired magnetic properties. We found a shortening of the Fe-Fe bond when the Zr content was increased, which can explain the experimentally observed decrease in the magnetic moment and Curie temperature.

X-Ray Reflectivity of Thin Layer and Multilayers

• Saeid Asgharizadeh (research institue of applied physics and astronomy)

Room: Allame Rafiee Conference Hall The X-rays interaction with matter can be described by an index of refraction which is less than one and characterizes the change of direction of the X-ray beam when passing from air to material. The value of the parameters in the index of refraction depend on the electron density and linear absorption coefficient. An index of refraction less than one causes a total reflection when X-ray interact with surfaces. Evaluating the critical angle due to the total reflection will provide average density of the layer. Dynamical and kinematical scattering theories will play role to discover thickness and roughness parameters of the surfaces (in layers) and interfaces (in multilayer systems).

Applications of Synchrotron Radiation in Infrared Spectroscopy Room: Allame Rafiee Conference Hall Users of synchrotron facilities mainly employ the relatively high-energy parts of the electromagnetic radiation i.e. the UV and X-ray regions. However, the infrared portion of the beam is also an exceptional tool for scientists who use infrared spectroscopy for their research. In this talk, a brief introduction to Fourier Transform Infrared (FTIR) spectroscopy technique (with a focus on microscopy) and its application to different areas of science will be given. Various examples of employing synchrotron radiation in this technique will be presented. The talk is aimed at a large population of scientists with interests in cancer-science, neuro-science, medical science, condensed matter physics, material science, agriculture and even archeology!

Study the Speciation of Technetium under Gamma and Alpha Irradiation in Concentrated Carbonate Media

• Mohammad Ghalei (French National Institute of Nuclear and Particle Physics (IN2P3))
• Mohammad Ghalei (ILSF)

Room: Allame Rafiee Conference Hall

Discussion & Concluding Remarks

• Ehsan Salimi (IPM)
• Javad Rahighi (Iranian Light Source Facility)

Room: Allame Rafiee Conference Hall