The uniqueness of X-ray Microscopy

It is the complexity of analytical techniques that makes modern X-ray microscopy unique due to the specific interaction of X-rays with atoms in any kind of solid, liquid or gaseous matter. Shorter wavelengths allow higher optical resolution compared to visible light microscopy. High X-ray penetration power gives 'deeper' insight into the specimen and avoids in many cases slicing as required for electron microscopies. The electronic structure of atoms provides each element a specific finger print that allows X-ray microscopy to identify the elemental distribution. X-ray analytical techniques are even sensitive to slight modification in the electronic structure of an atom by its neighboring atoms, which can provide in addition a wealth of information on the chemical speciation of your specimen.

Research highlights

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Asbestos in lung tissue

Asbestos is a potent carcinogen associated with malignant mesothelioma and lung cancer but its carcinogenic mechanisms are still poorly understood. Asbestos toxicity is ascribed to its particular physico-chemical characteristics, and one of them is the presence of and ability to adsorb iron, which may cause an alteration of iron homeostasis in the tissue. 

L. Pascolo et al., Scientific Reports 3, 1123, (2013)

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Sealed Electrochemical Microcell


Dynamic studies in the realm of electrochemical materials science, able to follow morphochemical couplings under growth and operation conditions, are crucial to several technologies, among which are the following: electrochemical energetics (fuel cells, batteries, and supercapacitors), energy harvesting, catalysis, biosensing, and nanofabrication.
B. Bozzini et al., Anal. Chem. 2014, 86, 664−670.

In this paper we report on the fabrication and testing of a novel concept of sealed electrochemical microcell for in situ soft X-ray microspectroscopy in transmission, dedicated for nonvacuum compatible electrolytes. The microcell, fabricated using ultraviolet lithography, at variance with previous versions of electrochemical wet cells, that featured an optical window glued on top of the electrode system and a very limited electrolyte volume, the device presented here is a single solid block based around a microfabricated channel with fixed optical windows and apt for microfluidic work.
The first electrochemical experiments with this new cell explore the electrochemical growth of a Co-polypyrrole, a composite electrocatalyst material with promising performance to replace the expensive Pt catalyst in fuel-cell oxygen electrodes. 
  Morphological and chemical-state distributions of Co codeposited with polypyrrole has been followed as a function of time and position, yielding unprecedented information on the processes relevant to the synthesis of this catalyst.

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Fabrication of  a Sealed Electrochemical Microcell for in Situ X-ray Miscospectroscopy and Testing with in Situ Co-Polypyrrole Composite Electrodeposition for Pt-Free Oxygen Electrocatalysis; B. Bozzini, A. Gianoncelli, P. Bocchetta, S. Dal Zilio, G. Kourousias;
Analitycal Chemistry 2014 , 86, 664-670;  

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Spectromicroscopy using Ptychography

Ptychography is a form of scanning diffractive imaging that can successfully retrieve the modulus and phase of both the sample transmission function and the illuminating probe. An experimental difficulty commonly encountered in diffractive imaging is the large dynamic range of the diffraction data.

A. M. Maiden et al.Nature Communications 4, 1669 (2013).

In our work we report a novel ptychographic experiment using a randomly phased X-ray probe to considerably reduce the dynamic range of the recorded diffraction patterns. Images can be reconstructed reliably and robustly from this setup, even when scatter from the specimen is weak. A series of ptychographic reconstructions at X-ray energies around the L absorption edge of iron demonstrates the advantages of this method for soft X-ray 
spectromicroscopy, which can readily provide chemical sensitivity without the need for optical refocusing. In particular, the phase signal is in perfect registration with  the modulus signal and provides complementary information that can be more sensitive to changes in the local chemical environment.

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Soft X-ray spectromicroscopy using ptychography with randomly phased illumination
A. M. Maiden, G. R. Morrison, B. Kaulich, A. Gianoncelli, J. Rodenburg, Nature Communications 4, 1669 (2013)

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Phase-diverse Fresnel CDI

Phase-diverse Fresnel CDI has been shown to reveal the structure and composition of biological specimens with high sensitivity at nanoscale resolution. However, the method has yet to be applied in the ‘water-window’ that lies between the carbon and oxygen K edges. This is a proof-of-principle application of FCDI in the water-window to dehydrated red blood cells infected with the trophozoite stage of the malaria parasite. 

M. Jones et al., Optics Express 2013 21, 32151-32159.

This study demonstrates the application of phase-diverse FCDI on both a fabricated test sample and cellular specimens in the water-window. The general shape of the host red blood cells and parasite can easily be recognised from the X-ray images and correlate well with the information provided by the other imaging modalities. Because of the ability to acquire the X-ray images with relatively low dose, the method can be used as a correlative microscopy tool to inform the interpretation of images obtained using electron and optical methods. In particular, internal features of the whole cell such as the exomembrane system of the parasite, which cannot be resolved at high resolution using light microscopy and which are inaccessible to scanning electron microscopy, can be distinguished in the X-ray images.

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Phase-diverse Fresnel coherent diffractive imaging of malaria parasite-infected red blood cells in the water window
M. W.M. Jones, B. Abbey, A. Gianoncelli, E. Balaur, C. Millet, M. B Luu, H. D. Couglan, A. J. Carroll, A. G. Peele, L. Tilley, G. A. van Riessen, Optics Express 2132151-32159, (2013)  


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Al toxicity in soybean roots

Aluminum is one of the major causes for soil degradation, in particular in acidic soils, where soil minerals release soluble Al that limits the growth of plants. Unfortunately, acidic soils comprise ca. 40% of the world’s arable land and are typically present in the areas that are more favorable for intensive agriculture. Our LEXRF show that the AL accumulation is rather rapid process and Al remains concentrated in cell walls with exposure time.

P. Kopittke et al., Plant Physiology (2015)

The results obtained in this study have revealed that toxic effects of aluminum are already exerted within the first 5-30 min of exposure in specific cells located in a region approximately 5-10 mm behind the root tip. Since traditional techniques are not sensitive to access accumulation of aluminum in these initial stages we used a combination of synchrotron-based low-energy X-ray fluorescence spectromicroscopy (LEXRF) at the TwinMic beamline (Elettra Sincrotrone Trieste) and high-resolution secondary ion mass spectroscopy (NanoSIMS) to examine the spatial distribution of Al on a cellular and subcellular level. This integrated approach allowed us to identify the sequence of processes whereby Al reduces the growth of roots in rather short term. The obtained results demonstrate that the majority of Al starts to accumulate within the walls of cells in the outer root tissues (as shown in Figure 1) and this preferential storage in the walls of the outer tissues continues even after exposures of 24 h (Figure 2). This observation is particularly important since the cells located in the region 5-10 mm behind the root tip are the ones responsible for the root growth via walls loosening.
Our findings clearly show that the accumulation of Al is rather rapid process and Al remains concentrated in the cell walls with exposure time. The binding of Al to the cell walls exerts toxic effects, leading to inhibition of cell elongation and growth. The results clearly indicate that for overcoming the deleterious effects of Al it is important to focus on traits related to cell wall composition as well as traits involved in wall loosening. 

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Identification of the primary lesion of toxic aluminum (Al) in plant roots
Peter M. Kopittke, Katie L. Moore, Enzo Lombi, Alessandra Gianoncelli, Brett J. Ferguson, F. Pax C. Blamey, Neal W. Menzies, Timothy M. Nicholson, Brigid A. McKenna, Peng Wang, Peter M. Gresshoff, George Kourousias, Richard I. Webb, Kathryn Green, Alina Tollenaere , Plant Physiology  (2015) doi: 10.1104/pp.114.253229.

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Electrochemistry: Oxigen Reduction Reaction Electrocatalyst

Electrodeposition of manganese/polypyrrole (Mn/PPy) nanocomposites has been recently shown to be a technologically relevant synthesis method for the fabrication of Oxygen Reduction Reaction (ORR) electrocatalysts.

Bozzini et al., J. Mater. Chem. A (2015).

Novel non-noble metal/polypyrole composites have properties promising to be considered as substitutes of expensive platinum catalysts for the Oxygen Reduction Reaction (ORR) in energy devices, in particular in alkaline fuel cells. Following revelation the catalytic activity of cobalt phthalocyanine and the beneficial effect of pyrolysis at 400–800 °C on its stability and catalytic properties, considerable efforts have been made to explore the chemo-morphological transformations of non-precious metal-nitrogen–carbon composites (M/N/C, M¼Co, Fe, Mn, etc.) during pyrolysis in order to shed light on the modifications leading to the increased electrocatalytic activity. Up to date the majority of the results indicate the formation of MeNx-type moieties as active catalytic sites. Among the different strategies to include nitrogen in the catalyst, electrochemistry offers the possibility of using polypyrrole (PPy) with its dual function as a N-source and an electronically conducting catalyst support for the electrodeposition of metal-containing composite materials.
We used a new approach for the fabrication of MnO2/carbon and metal/PPy electrocatalysts that has allowed creation of more Mn/N/C catalytic active sites during the electrodeposition process. The work, coordinated by Prof. Benedetto Bozzini, is collaboration between the Department of Engineering and Innovation of Salento University, The Institute for Microelectronics and Microsystems, IMM-CNR and Elettra Iaboratory. The investigation combined material fabrication and characterization using clasical electrochemistry methods complemented with imaging and microspectroscopy methods available at the scanning microscopes operated at the TwinMic and ESCAMicroscopy beamlines at Elettra laboratory. In particular, at Elettra by using chemical mapping and X-ray absorption (XAS), fluorescence (XRF) and photoelectron XPS) microspectroscopy we were able to shed light on the evolution of both morphology and chemical composition of synthesized materials following in-situ their evolution under different fabrication conditions.
The representative calibrated Mn XRF images in Fig.1 clearly show the laterally inhomogeneous distribution at mesoscopic and submicrometric scales, achieved under low current densities, while the rationed Mn/O pinpoints the variations in the Mn oxidation state. Comparing the contrast levels of the two maps it is clear that the local concentration and chemical state of Mn are not fully correlated.

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Soft X-ray Radiation Damage

Soft X-ray radiation damaged has been studed by combining 3 different and independent miscoscopy techniques: X-ray Microsocpy, AFM microscopy and FTIR spectromicroscopy. XRM has been used to cause the damage while AFM and FTIR, both non destructive methods, have been emplyed for investigating the effect of soft X-rays on fixed cells.

Gianoncelli et al. Scientific Reports (2015)

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TwinMic: the European Soft X-ray Transmission and Emission Microscope

European scientists with highest expertise in X-ray microscopy, diffractive X-ray optics, X-ray contrast technologies and detection, started in 2001 to integrate the advantages of complementary scanning and full-field imaging modes into a single instrument, which they named 'TwinMic'. The microscope station has been designed as highly modular in its optical configuration and specimen environment, and scientists, engineers and technicians continuously improve the instruments performance and versatility to suit your experimenter's requirements.

One of the recent milestone implementations is the low-energy X-ray Fluorescence system.

User Area

Proposal Submission

We invite users and collaborators to discuss thier proposals with the beamline local contacts well in advance before the submission deadline. This is a crucial step for a careful assesment of the experiment feasibility and may lead to improvements in the proposed experimental plan. In a restricted number of cases, when doubts arise about the suitability of your samples or the planned measurements are too close to the microscope resolution limit, it may be possible for you to arrange a feasibility test. Our website provides a wealth of information on experiment feasibility and proposal submission. For more info, please vist the Info for Users.

Call for proposals

The deadline for proposal submission for beamtime allocation is to be announced


ICXOM24 conference (24-29 September 2017)

The 24th International Congress on X-ray Optics and Microanalysis, organized by Elettra Sincrotrone Trieste was successfully held at the congress hall at the Stazione Marittima. of Trieste. The ICXOM conference series is a prestigious international symposium for the discussion of new developments and advances in instrumentation, methods and applications in the fields of x-ray micro- and nano-analysis. This conference series started in 1956 in Cambridge, UK, in response to the need for physical scientists, instrument developers and those using x-ray microscopes and electron probe analysers to come together every three (and now two) years to exchange experiences, learn about new developments in the field and gain new ideas for further research.

This edition of ICXOM hosted for the very first time, during the first day of the event, the satellite workshop MA-XRF on “Macro X-ray Fluorescence Scanning in Conservation, Art and Archaeology”, preceded by a tutorial session at ICTP office on Sunday 24th September. The MA-XRF workshop scientific program was structured with 24 talks followed by a poster session, for a total of 145 participants.
The whole event, where state-of-the-art research was presented, was attended by 270 participants from all over the world. For more details about the event please visit here.



New members at TwinMic

Dr Milan Žižić recently (July 2022) joined the Twinmic team as PostDoc researcher.
Last Updated on Monday, 12 September 2022 15:38