Showing papers by "Stefano Marchesini published in 2008"

Single particle X-ray diffractive imaging.

Abstract: In nanotechnology, strategies for the creation and manipulation of nanoparticles in the gas phase are critically important for surface modification and substrate-free characterization. Recent coherent diffractive imaging with intense femtosecond X-ray pulses has verified the capability of single-shot imaging of nanoscale objects at suboptical resolutions beyond the radiation-induced damage threshold. By intercepting electrospray-generated particles with a single 15 femtosecond soft-X-ray pulse, we demonstrate diffractive imaging of a nanoscale specimen in free flight for the first time, an important step toward imaging uncrystallized biomolecules.

Ultrafast single-shot diffraction imaging of nanoscale dynamics

Abstract: The transient nanoscale dynamics of materials on femtosecond to picosecond timescales is of great interest in the study of condensed phase dynamics such as crack formation, phase separation and nucleation, and rapid fluctuations in the liquid state or in biologically relevant environments. The ability to take images in a single shot is the key to studying non-repetitive behaviour mechanisms, a capability that is of great importance in many of these problems. Using coherent diffraction imaging with femtosecond X-ray free-electron-laser pulses we capture time-series snapshots of a solid as it evolves on the ultrafast timescale. Artificial structures imprinted on a Si3N4 window are excited with an optical laser and undergo laser ablation, which is imaged with a spatial resolution of 50 nm and a temporal resolution of 10 ps. By using the shortest available free-electron-laser wavelengths1 and proven synchronization methods2 this technique could be extended to spatial resolutions of a few nanometres and temporal resolutions of a few tens of femtoseconds. This experiment opens the door to a new regime of time-resolved experiments in mesoscopic dynamics. High-speed imaging gives us a fascinating insight into ultrafast changes in materials. By combining the speed of optical pulses and the short wavelength of X-ray pulses, imaging with 50-nm spatial and 10-ps temporal resolution is possible, with scope to go much further.

Massively parallel X-ray holography

Abstract: Advances in the development of free-electron lasers offer the realistic prospect of nanoscale imaging on the timescale of atomic motions. We identify X-ray Fourier-transform holography1,2,3 as a promising but, so far, inefficient scheme to do this. We show that a uniformly redundant array4 placed next to the sample, multiplies the efficiency of X-ray Fourier transform holography by more than three orders of magnitude, approaching that of a perfect lens, and provides holographic images with both amplitude- and phase-contrast information. The experiments reported here demonstrate this concept by imaging a nano-fabricated object at a synchrotron source, and a bacterial cell with a soft-X-ray free-electron laser, where illumination by a single 15-fs pulse was successfully used in producing the holographic image. As X-ray lasers move to shorter wavelengths we expect to obtain higher spatial resolution ultrafast movies of transient states of matter. X-ray Fourier transform holography using free-electron lasers has the potential to enable nanoscale imaging on the timescale of atomic motion. A technique that dramatically increases the efficiency of this technique could move us a step towards such imaging.

Three-Dimensional Coherent X-Ray Diffraction Imaging of a Ceramic Nanofoam: Determination of Structural Deformation Mechanisms

Abstract: Ultralow density polymers, metals, and ceramic nanofoams are valued for their high strength-to-weight ratio, high surface area, and insulating properties ascribed to their structural geometry. We obtain the labrynthine internal structure of a tantalum oxide nanofoam by x-ray diffractive imaging. Finite-element analysis from the structure reveals mechanical properties consistent with bulk samples and with a diffusion-limited cluster aggregation model, while excess mass on the nodes discounts the dangling fragments hypothesis of percolation theory.

Powder diffraction from a continuous microjet of submicrometer protein crystals.

Abstract: Atomic-resolution structures from small proteins have recently been determined from high-quality powder diffraction patterns using a combination of stereochemical restraints and Rietveld refinement [Von Dreele (2007), J. Appl. Cryst. 40, 133–143; Margiolaki et al. (2007), J. Am. Chem. Soc. 129, 11865–11871]. While powder diffraction data have been obtained from batch samples of small crystal-suspensions, which are exposed to X-rays for long periods of time and undergo significant radiation damage, the proof-of-concept that protein powder diffraction data from nanocrystals of a membrane protein can be obtained using a continuous microjet is shown. This flow-focusing aerojet has been developed to deliver a solution of hydrated protein nanocrystals to an X-ray beam for diffraction analysis. This method requires neither the crushing of larger polycrystalline samples nor any techniques to avoid radiation damage such as cryocooling. Apparatus to record protein powder diffraction in this manner has been commissioned, and in this paper the first powder diffraction patterns from a membrane protein, photosystem I, with crystallite sizes of less than 500 nm are presented. These preliminary patterns show the lowest-order reflections, which agree quantitatively with theoretical calculations of the powder profile. The results also serve to test our aerojet injector system, with future application to femtosecond diffraction in free-electron X-ray laser schemes, and for serial crystallography using a single-file beam of aligned hydrated molecules.

Temperature dependent evolution of the electronic and local atomic structure in the cubic colossal magnetoresistive manganite La1-xSrxMnO3

Abstract: Temperature dependent evolution of the electronic and local atomic structure in the cubic colossal magnetoresistive manganite La 1-x Sr x MnO 3 N. Mannella 1,2,a,b , C. H. Booth 3 , A. Rosenhahn 2,c , B. C. Sell 1,2 , A. Nambu 2,4,d , S. Marchesini 2,b ,B. S. Mun 1,2,b , S.-H. Yang 2,e , M. Watanabe 2,5 , K. Ibrahim 2,6 , E. Arenholz 7 , A. Young 7 , J. Guo 7 , Y. Tomioka 8 and C.S. Fadley 1,2 Department of Physics, UC Davis, Davis, CA, 95616, USA Materials Sciences Division, LBNL, Berkeley, CA, 94720, USA Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, USA. Department of Chemistry,The University of Tokyo, Tokyo,113-0033, Japan RIKEN, HYOGO 679-5148, Japan Beijing Synchrotron Radiation Laboratory, Beijing, China. Advanced Light Source, LBNL, Berkeley CA, 94720, USA National Institute for Advanced Industrial Science and Technolog (AIST), Tsukuba Central 4, Tsukuba 305-8562, Japan Present address: Physics Department, Stanford University, Stanford, CA, USA b Present address: Advanced Light Source, LBNL, Berkeley CA, 94720, USA c Present address: Heidelberg University, Heidelberg, Germany d Chemistry Department, Brookhaven National Laboratory, Upton, NY 11973-5000, USA e Present address: IBM Almaden Research Center, San Jose, CA 95120, USA a ABSTRACT We have studied the temperature-dependent evolution of the electronic and local atomic structure in the cubic colossal magnetoresistive manganite La 1-x Sr x MnO 3 (x= 0.3 – 0.4) with core and valence level photoemission (PE), x-ray absorption specroscopy (XAS), x-ray emission spectroscopy (XES), resonant inelastic x-ray scattering (RIXS), extended x-ray absorption fine structure (EXAFS) spectroscopy and magnetometry. As the temperature is varied across the Curie temperature T C, our PE experiments reveal a dramatic change of the electronic structure involving an increase in the Mn spin moment from ≈ 3 μ B to ≈ 4 μ B , and a modification of the local chemical environment of the other constituent atoms indicative of electron localization on the Mn atom. These effects are reversible and exhibit a slow-timescale ≈ 200 K- wide hysteresis centered at T C . Based upon the probing depths accessed in our PE measurements, these effects seem to survive for at least 35-50 A inward from the surface, while other consistent signatures for this modification of the electronic structure are revealed by more bulk sensitive spectroscopies like XAS and XES/RIXS. We interpret these effects as spectroscopic fingerprints for polaron formation, consistent with the presence of local Jahn-Teller distortions of the MnO 6 octahedra around the Mn atom, as revealed by the EXAFS data. Magnetic susceptibility measurements in addition show typical signatures of ferro- magnetic clusters formation well above the Curie temperature.

Camera for coherent diffractive imaging and holography with a soft-x-ray free-electron laser.

Abstract: We describe a camera to record coherent scattering patterns with a soft-x-ray free-electron laser (FEL). The camera consists of a laterally graded multilayer mirror, which reflects the diffraction pattern onto a CCD detector. The mirror acts as a bandpass filter for both the wavelength and the angle, which isolates the desired scattering pattern from nonsample scattering or incoherent emission from the sample. The mirror also solves the particular problem of the extreme intensity of the FEL pulses, which are focused to greater than 10(14) W/cm2. The strong undiffracted pulse passes through a hole in the mirror and propagates onto a beam dump at a distance behind the instrument rather than interacting with a beam stop placed near the CCD. The camera concept is extendable for the full range of the fundamental wavelength of the free electron laser in Hamburg (FLASH) FEL (i.e., between 6 and 60 nm) and into the water window. We have fabricated and tested various multilayer mirrors for wavelengths of 32, 16, 13.5, and 4.5 nm. At the shorter wavelengths mirror roughness must be minimized to reduce scattering from the mirror. We have recorded over 30,000 diffraction patterns at the FLASH FEL with no observable mirror damage or degradation of performance.

Ab initio compressive phase retrieval

Abstract: Any object on earth has two fundamental properties: it is finite, and it is made of atoms. Structural information about an object can be obtained from diffraction amplitude measurements that account for either one of these traits. Nyquist-sampling of the Fourier amplitudes is sufficient to image single particles of finite size at any resolution. Atomic resolution data is routinely used to image molecules replicated in a crystal structure. Here we report an algorithm that requires neither information, but uses the fact that an image of a natural object is compressible. Intended applications include tomographic diffractive imaging, crystallography, powder diffraction, small angle x-ray scattering and random Fourier amplitude measurements.

Area X-ray or UV camera system for high-intensity beams

Abstract: A system in one embodiment includes a source for directing a beam of radiation at a sample; a multilayer mirror having a face oriented at an angle of less than 90 degrees from an axis of the beam from the source, the mirror reflecting at least a portion of the radiation after the beam encounters a sample; and a pixellated detector for detecting radiation reflected by the mirror. A method in a further embodiment includes directing a beam of radiation at a sample; reflecting at least some of the radiation diffracted by the sample; not reflecting at least a majority of the radiation that is not diffracted by the sample; and detecting at least some of the reflected radiation. A method in yet another embodiment includes directing a beam of radiation at a sample; reflecting at least some of the radiation diffracted by the sample using a multilayer mirror; and detecting at least some of the reflected radiation.

X-Ray Powder Diffraction from Sub-Micron Crystals of Photosystem-1 Membrane Protein

Abstract: We demonstrate that powder diffraction data can be collected from sub-micron crystals of a mbrane protein with nearly two orders of magnitude more atoms than the molecules commonly used for powder diffraction. The crystals of photosystem-1 protein were size-selected using a 500 nm pore- size filter and delivered to a soft x-ray beam with a photon energy of 1.5 keV using a dynamically focused micro-jet developed for the serial crystallography experiment at beamline 9.0.1. The 10-micron jet places many such randomly oriented crystals in the x-ray beam simultaneously resulting in a powder diffraction pattern which extends to 28 angstrom resolution with just 200 seconds of x-ray exposure. The use of the jet for particle delivery allows for a thin sample, appropriate for the soft x-rays used, and continuously refreshes the crystals so that radiation damage is not possible. The small size of the crystals requires the use of lower energy photons for increased scattering strength and increased spacing between powder rings. The powder patterns obtained in this way, from abundant nano-crystals, could be used to provide low resolution molecular envelopes if phased using techniques such as compressive sensing which do not require atomic resolution data. The results also serve to test our aerojet injector system, with future application to femtosecond diffraction in Free Electron X-ray Laser schemes, and for Serial Crystallography using a single-file beam of aligned hydrated molecules.