scholarly journals Dynamics of soft nanoparticle suspensions at hard X-ray FEL sources below the radiation-damage threshold

IUCrJ ◽  
2018 ◽  
Vol 5 (6) ◽  
pp. 801-807 ◽  
Author(s):  
Felix Lehmkühler ◽  
Joana Valerio ◽  
Dina Sheyfer ◽  
Wojciech Roseker ◽  
Martin A. Schroer ◽  
...  

The application of X-ray photon correlation spectroscopy (XPCS) at free-electron laser (FEL) facilities enables, for the first time, the study of dynamics on a (sub-)nanometre scale in an unreached time range between femtoseconds and seconds. For soft-matter materials, radiation damage is a major limitation when going beyond single-shot applications. Here, an XPCS study is presented at a hard X-ray FEL on radiation-sensitive polymeric poly(N-isopropylacrylamide) (PNIPAM) nanoparticles. The dynamics of aqueous suspensions of densely packed silica-PNIPAM core-shell particles and a PNIPAM nanogel below the radiation-damage threshold are determined. The XPCS data indicate non-diffusive behaviour, suggesting ballistic and stress-dominated heterogeneous particle motions. These results demonstrate the feasibility of XPCS experiments on radiation-sensitive soft-matter materials at FEL sources and pave the way for future applications at MHz repetition rates as well as ultrafast modes using split-pulse devices.

2009 ◽  
Vol 105 (9) ◽  
pp. 093117 ◽  
Author(s):  
L. Juha ◽  
V. Hájková ◽  
J. Chalupský ◽  
V. Vorlíček ◽  
A. Ritucci ◽  
...  

2014 ◽  
Vol 21 (5) ◽  
pp. 1153-1159 ◽  
Author(s):  
Andreas Späth ◽  
Benjamin Watts ◽  
Lutz Thilo Wasserthal ◽  
Rainer H. Fink

Quantitative studies of soft X-ray induced radiation damage in zone-plate-based X-ray microspectroscopy have so far concentrated on investigations of homogeneous specimens. However, more complex materials can show unexpected radiation-induced behaviour. Here a quantitative radiochemical analysis of biological tissue fromXantophan morganii praedictaeyes is presented. Contrast enhancement due to tissue selective mass loss leading to a significant improvement of imaging quality is reported. Since conventional quantitative analysis of the absorbed dose cannot conclusively explain the experimental observations on photon-energy-dependent radiation damage, a significant contribution of photo- and secondary electrons to soft matter damage for photon energies above the investigated absorption edge is proposed.


2015 ◽  
Vol 22 (2) ◽  
pp. 267-272 ◽  
Author(s):  
Selina Storm ◽  
Malte Ogurreck ◽  
Daniel Laipple ◽  
Christina Krywka ◽  
Manfred Burghammer ◽  
...  

The high flux density encountered in scanning X-ray nanodiffraction experiments can lead to severe radiation damage to biological samples. However, this technique is a suitable tool for investigating samples to high spatial resolution. The layered cell wall structure of softwood tracheids is an interesting system which has been extensively studied using this method. The tracheid cell has a complex geometry, which requires the sample to be prepared by cutting it perpendicularly to the cell wall axis. Focused ion beam (FIB) milling in combination with scanning electron microscopy allows precise alignment and cutting without splintering. Here, results of a scanning X-ray diffraction experiment performed on a biological sample prepared with a focused ion beam of gallium atoms are reported for the first time. It is shown that samples prepared and measured in this way suffer from the incorporation of gallium atoms up to a surprisingly large depth of 1 µm.


2021 ◽  
Vol 11 (11) ◽  
pp. 5082
Author(s):  
Daeho Sung ◽  
Daewoong Nam ◽  
Myong-jin Kim ◽  
Seonghan Kim ◽  
Kyung Sook Kim ◽  
...  

We developed a single-shot coherent X-ray imaging instrument at the hard X-ray beamline of the Pohang Accelerator Laboratory X-ray Free Electron Laser (PAL-XFEL). This experimental platform was established to conduct a variety of XFEL experiments, including coherent diffraction imaging (CDI), X-ray photon correlation spectroscopy (XPCS), and coherent X-ray scattering (CXS). Based on the forward-scattering geometry, this instrument utilizes a fixed-target method for sample delivery. It is well optimized for single-shot-based experiments in which one expects to observe the ultrafast phenomena of nanoparticles at picosecond temporal and nanometer spatial resolutions. In this paper, we introduce a single-shot coherent X-ray imaging instrument and report pump–probe coherent diffraction imaging (PPCDI) of Ag nanoparticles as an example of its applications.


IUCrJ ◽  
2021 ◽  
Vol 8 (5) ◽  
Author(s):  
Francesco Dallari ◽  
Avni Jain ◽  
Marcin Sikorski ◽  
Johannes Möller ◽  
Richard Bean ◽  
...  

Many soft-matter systems are composed of macromolecules or nanoparticles suspended in water. The characteristic times at intrinsic length scales of a few nanometres fall therefore in the microsecond and sub-microsecond time regimes. With the development of free-electron lasers (FELs) and fourth-generation synchrotron light-sources, time-resolved experiments in such time and length ranges will become routinely accessible in the near future. In the present work we report our findings on prototypical soft-matter systems, composed of charge-stabilized silica nanoparticles dispersed in water, with radii between 12 and 15 nm and volume fractions between 0.005 and 0.2. The sample dynamics were probed by means of X-ray photon correlation spectroscopy, employing the megahertz pulse repetition rate of the European XFEL and the Adaptive Gain Integrating Pixel Detector. We show that it is possible to correctly identify the dynamical properties that determine the diffusion constant, both for stationary samples and for systems driven by XFEL pulses. Remarkably, despite the high photon density the only observable induced effect is the heating of the scattering volume, meaning that all other X-ray induced effects do not influence the structure and the dynamics on the probed timescales. This work also illustrates the potential to control such induced heating and it can be predicted with thermodynamic models.


2020 ◽  
Vol 27 (5) ◽  
pp. 1218-1226
Author(s):  
Artur D. Surowka ◽  
A. Gianoncelli ◽  
G. Birarda ◽  
S. Sala ◽  
N. Cefarin ◽  
...  

In order to push the spatial resolution limits to the nanoscale, synchrotron-based soft X-ray microscopy (XRM) experiments require higher radiation doses to be delivered to materials. Nevertheless, the associated radiation damage impacts on the integrity of delicate biological samples. Herein, the extent of soft X-ray radiation damage in popular thin freeze-dried brain tissue samples mounted onto Si3N4 membranes, as highlighted by Fourier transform infrared microscopy (FTIR), is reported. The freeze-dried tissue samples were found to be affected by general degradation of the vibrational architecture, though these effects were weaker than those observed in paraffin-embedded and hydrated systems reported in the literature. In addition, weak, reversible and specific features of the tissue–Si3N4 interaction could be identified for the first time upon routine soft X-ray exposures, further highlighting the complex interplay between the biological sample, its preparation protocol and X-ray probe.


2020 ◽  
Author(s):  
Li Zeng ◽  
Duan Gu ◽  
Chao Feng ◽  
Bo Liu ◽  
Zhentang Zhao

Abstract X-ray free-electron lasers (FELs) hold promising prospects for opening up opportunities for ultra-fast sciences at the atomic and molecular system. A precise knowledge of temporal information of FEL pulses is the central issue for experiments. Here we demonstrated an online diagnostic method to determine the FEL temporal profiles at the Shanghai Soft X-ray FEL facility. This robust method, designed for seeded FELs, allows researchers to acquire real-time longitudinal profiles of FEL pulses with a resolution better than 3fs. Based on this method, for the first time, we can directly observe the generation and evolution of a seeded FEL online. This helps us to further understand the physics and realize the lasing of a stable, nearly fully coherent soft X-ray FEL through a two-stage harmonic up-shift configuration. This method also provides an intuitive way for precise detection and control of the relative timing between electron beams and external optical lasers.


2011 ◽  
Vol 2 ◽  
pp. 638-644 ◽  
Author(s):  
Lars Borchardt ◽  
Martin Oschatz ◽  
Robert Frind ◽  
Emanuel Kockrick ◽  
Martin R Lohe ◽  
...  

For the first time we present the synthesis of CeO2/Si(O)C core–shell particles prepared by the miniemulsion technique. The Si(O)C core was obtained by means of a polycarbosilane precursor (SMP10), which was subsequently functionalized with ceria and pyrolyzed to the ceramic. The size of these particles could easily be adjusted by varying the surfactants and the surfactant concentration, or by the addition of comonomers. Hence particle sizes ranged from 100 to 1000 nm, tunable by the preparation conditions. All materials were characterized by photon cross correlation spectroscopy, scanning electron microscopy and elemental mapping investigations. Furthermore, first catalytic tests were carried out by temperature programmed oxidation (TPO) of methane, and the activity of this material in lowering the onset temperature of methane combustion by 262 K was documented.


2007 ◽  
Vol 1027 ◽  
Author(s):  
Xinhui Lu ◽  
Simon G. J. Mochrie ◽  
S. Narayanan ◽  
Alec R. Sandy ◽  
Michael Sprung

AbstractMultispeckle x-ray photon correlation spectroscopy measurements, carried out at beamline 8-ID at the Advanced Photon Source at Argonne National Laboratory, of opaque suspensions of silica nanoparticles in water and lutidine-water binary mixtures are presented.


2015 ◽  
Vol 22 (3) ◽  
pp. 592-598 ◽  
Author(s):  
Kazuto Yamauchi ◽  
Makina Yabashi ◽  
Haruhiko Ohashi ◽  
Takahisa Koyama ◽  
Tetsuya Ishikawa

Total-reflection mirror devices for X-ray free-electron laser focusing are discussed in terms of optical design, mirror-fabrication technology, a wavefront diagnosis method and radiation-damage testing, as a review of the present status of the focusing optics at the SPring-8 angstrom compact free-electron laser (SACLA). Designed beam sizes of 1 µm and 50 nm, and spot sizes almost matching prediction have been achieved and used to explore topics at the forefront of natural science. The feasibility of these devices is determined to be sufficient for long-term and stable operation at SACLA by investigating the radiation-damage threshold and achievable accuracies in the mirror figure and alignment.


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