Deliverables

WP1 - Management
D1.1 - Internal test of NFFA-Europe Website
This deliverable describes the results achieved within task 1.5 “Communication”, and is also connected to the dissemination purposes of the project (WP11). The work done aimed at setting up the main information and functionalities of the website as a Single Entry Point (SEP) to find out about the project and access the offer of tools made available through NFFA-Europe research infrastructure.
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WP1 - Management
D1.2 - Implementation of the online two-step proposal submission
This deliverable is part of the results achieved within task 1.4, “Set-up and usage of a transnational Access structure”. Specifically, it relates to the integration of an electronic presubmission advice and submission procedure into a Single Entry Portal, as well as the development of an electronic form for users’ proposal.
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WP1 - Management
D1.3 - Setup and implementation of the TA and evaluation procedures
NFFA-Europe offers to European and Third Country1 scientists from both academia and industry the possibility to carry out comprehensive projects for multidisciplinary research at the nanoscale. Activities are performed in six different types of Installations: - Lithography and nano-patterning (Litho) - Growth and synthesis (Growth) - Theory and Simulation (Theory) - Structural and Morphological nano-characterisation (SM Charact.) - Electronic and Chemical nano-characterisation (EC Charact.) - Magnetic, Optical and Electric nano-characterisation (ME Charact.) Each Installation includes laboratories located in different NFFA-EU sites; furthermore, when needed, limited2 access to co-located Large-Scale Facilities for Fine Analysis is offered as part of the access to Litho, or SM, EC or ME nano-characterisation. NFFA-Europe proposals necessarily include access to more than one type of Installation (e.g. Litho and Growth, Growth and Theory, SM Charact. and EC Charact., etc.) and cannot be limited to Fine Analysis only. Whenever possible access will be granted in a single NFFA-Europe site for all research steps. Access to more than one site for a given proposal will be considered only when technically or scientifically justified.
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WP6 - JRA1 – Research on In-Operando and high throughput methods
D6.1 - Prototype of Fast SPM module for STM experiments
Time-resolution is one of the main limitations for Scanning Probe Microscopy (SPM) investigations of surface processes under in-operando conditions. In the past, this problem was overcome by designing specific fast microscopes, where the resonance frequencies of the scanners were pushed above the desired scanning frequency. Starting from a concept and an early prototype previously developed by CNR and TUM, we designed, assembled and tested an add-on module that can be added to commercial Scanning Tunnelling Microscopes (STM) to increase their time resolution to video-rate and above.
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WP6 - JRA1 – Research on In-Operando and high throughput methods
D6.2 - Test of prototype of multifunctional environmental cells
Understanding the function of materials in reactive environments is a crucial issue to advancing several of the world’s most pressing energy needs, specifically in the areas of catalysis, energy conversion and energy storage. In most of the cases, much of the current knowledge has been obtained under conditions that largely deviate from those of practical. A relevant example is represented by heterogeneous catalysis, where the traditional surface science approach has provided fundamental knowledge on the behaviour of catalytic systems under (ultra)high vacuum conditions though changes in the reaction mechanisms and structures of their active phase relevant for industrial applications display at ambient pressure conditions.
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WP6 - JRA1 - Research on In-Operando and high throughput methods
D6.3 - Soft X-ray Fresnel zone plates with a resolution of 10 nm or better for users
Fabricating nanostructures with small lateral sizes and high aspect ratio is one of the key challenges, for instance, in developing highly resolving diffractive X-ray optics. While conventional lithography approaches break down below 20 nm feature size, growth processes can achieve extreme precision which reaches sometimes down to the atomic level. This approach has allowed for the production of diffractive X-ray lenses (Fresnel zone plates) with down to 12 nm line width in the past [1]. Targeting sub-10 nm resolution in X-ray microscopy, line widths have to be decreased to 8 nm or below. As direct fabrication of the required nanostructures is impossible with conventional lithography methods based on direct electron-beam writing, the line doubling method relaxes the demand of the lithography step to write every second line only. Utilizing atomic layer deposition (ALD) of iridium allows for doubling, or even multiplying the line density of the template structure. In this deliverable, we report on the fabrication of Fresnel zone plates (FZPs) which feature 10 nm spatial resolution in soft X-ray microscopy. We have successfully fabricated a set of zone plates with outermost zone widths of 8.8, 8.0, 7.2 and 6.4 nm at aspect ratios between 5 and 10 (see Deliverable 7.3 – Month 24). These FZPs have now been thoroughly tested and their microscopic resolution has been evaluated with dedicated test samples which exhibit 10, 9 and 8 nm metal lines and spaces. The work described above will be presented on the X-ray Microscopy conference in Saskatoon, Canada, in August 2018. The fabrication process has been presented at the MNE2017 conference in Braga, Portugal, in September 2017, and published in the journal Microelectronic Engineering. The results from resolution tests will be submitted for publication in a high-impact journal. FZPs with 10 nm resolution are available for users at the Hermes beamline at Soleil and at the Pollux beamline at the Swiss Light Source.
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WP6 - JRA1 – Research on In-Operando and high throughput methods
D6.4 - Prototype of Fast SPM module for AFM experiments
This document describes the implementation of the FAST module, initially conceived for Scanning Tunnelling Microscopes, in a commercial Atomic Force Microscope (AFM) system, namely a Keysight Technologies 5500 AFM located at ICN2, to operate in fast scan mode in both contact and tapping operational modes. The technical description of the whole experimental set-up is given, including the interfacing of the AFM control electronics with the FAST module, the spectral characterization of the scanner, calibration of lateral dimensions, a description of the used cantilevers and samples, the optimization of the functional parameters such as feedback control and the modification of the control software to adapt to the AFM requirements. Examples are given involving both contact and dynamic (amplitude modulation) operational modes and finally, a short analysis of future implementations is provided. The experimental results show that frame rates above 8 frames per second (fps) in static (contact) mode and 1 fps in dynamic mode have been consistently achieved using commercial microfabricated silicon cantilevers with resonance frequencies below 1 MHz and silicon and PS-PMMA block copolymer reference samples with a pitch of about 38 nm. Thus, we can conclude that the FAST module can be implemented in commercial AFMs. However, a more userfriendly operation would require additional improvements of the control software.
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WP6 - JRA1-Research on In-Operando and high throughput methods
D6.6 - Diffractive beamshapers, objective lens, and phase shifters for Zernike full-field X-ray microscopy users with 50 nm resolution or better
We designed a set of diffractive optics for high resolution full-field microscopy and tomography in the range between 6.6 and 18.4 keV photon energy. This high photon energy range will provide 2D and 3D imaging with extended penetration depth. The optics are optimized for taking advantage of Zernike phase contrast imaging. Combining high resolution imaging at the 50 nm level with reasonable diffraction efficiencies, we employed two methods: the line-doubling technique as reported on in report to Deliverable D6.3, and the fabrication of composite Fresnel zone plates in two lithography steps which are optimized for different structural sizes. We fabricated beam shapers (condeser lenses), Fresnel zone plates and phase rings for three different photon energies: 6.6 keV, 10.0 keV, and 18.4 keV. The set of optics for 10 keV was commissioned and tested at the Anatomics beamline. First results confirm a microscopic resolution of 50 nm, currently limited by the detector pixel. At the moment, thermal instabilities prevent achieving this resolution in 3D imaging. After commissioning of newly installed components at the Anatomix beamline at Soleil, the Zernike full-field microscopy setup with 50 nm resolution will be available to users.
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WP7 - JRA1 - Research on In-Operando and high throughput methods
D6.7 - Hard X-ray Fresnel zone plates with 20 nm or better for users
We designed a set of diffractive optics for high resolution scanning microscopy and ptychography in the range between 5 and 15 keV photon energy. This high photon energy range will provide 2D imaging capabilities with high penetration depth. The fabricated optics have outermost zone widths of 30, 25, and 20 nm. Combining high resolution imaging in X-ray microscopy and diffractive X-ray lenses with reasonable efficiencies, we employed the line-doubling technique as reported on in report to Deliverable D6.3. We fabricated Fresnel zone plates which can be used over an extended range of photon energies from 5 keV to 15 keV. The Fresnel zone plates were commissioned and tested at the ID01 beamline at the ESRF. First results confirm a spatial resolution of 18 nm in ptychography. The Fresnel zone plates delivered and tested so far are available to users.
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WP6 - JRA1 – Research on In-Operando and high throughput methods
D6.8 - Realization 3D focusing mixer for X-ray and nanoanalytic applications
Microfluidic mixers are useful instruments for the investigation of fast (bio)chemical reactions, as they allow time-resolved measurements using small sample volumes. Many reactions, especially those leading to nucleation and growth of nanoparticles, pose problems for microfluidic systems, as the reaction products have a tendency to aggregate and stick to the channel walls, known as the fouling of the reaction. Aggregates invalidate the gathered data and may clog the device by obstructing the channel. The goal of this project was to develop a mixer employing 3D-sheathing to prevent channel blockage, by inhibiting aggregation at the channel walls. We report here on the development of a micromixer geometry that would accomplish the 3Dsheathing behavior. Despite the ease in devising the necessary peripheral systems to perform experiments, the realization of the mixer itself proved to be more difficult. We found that both the correct design of the mixing part and the precision in the fabricated channels are crucial for this approach. We tested a number of materials and production methods to determine an optimal mixer geometry that should achieve the desired 3D-sheathing The precision of the channels we have produced thus far has inhibited the satisfactory function of the instrument. Measurements could be conducted with the prototype, but after some time the lacking precision still led to recirculation and agglomeration. We are currently working towards the improvement of the channels and the channel profile to resolve the remaining problems. Research performed as part of this project has been presented at the MNE2017 conference and the ÖPG Tagung 2018, and been published in Microelectronic Engineering. The development of the prototype itself has been presented on various occasions, e.g. SAXS Excites 2017, Nesy 2019.
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WP6 - JRA1 – Research on In-Operando and high throughput methods
D6.9 - Nanodrop cell for X-ray and nanoanalytic applications
In today's competitive world of science efficient analysis tools are indispensable. The tools should be instruments providing measurements of small sample amounts, being both cost and time effective. Measurements should be not only easy and fast to execute, but also reliable and precise. Here we report on a new instrument, which enables measurements in a routine and automated way for the high throughput screening of liquid samples. The instrument is an automatic sample changer feeding a novel sample holder for volumes in the range of 5-20 μL. The general operating principle of the sample holder not only allows for precise measurements of very small volumes, but also the reduction of sample quality. High surface-tovolume effects easily occur in more conventional systems based on pumping the sample through tubing into capillaries. While avoiding such high surface-to-volume effects the automatic sample changer enables the measurement of hundreds of samples without requiring of manual intervention. We extensively tested the instrument and showed that it satisfies the initial specifications. It quickly provides reliable, high-quality data using minimal volumes of sample. This new instrument greatly simplifies and accelerates experiments, constituting therefore a valuable contribution for accessing large scale infrastructures. The prototype is already available for testing during general user access at the Austrian SAXS beamline at the Elettra-Sincrotrone Trieste (first experiments are scheduled within March and April 2019) and later on in the NFFA workpackage TNA4. The development of the instrument has been reported at several conferences, including MNE2017, OEPG 2018, NESY Winterschool 2017 and 2019. A publication concerning the system and its testing is currently in preparation.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.1 - Investigation of optimum NIL stamp fabrication method to copy sub-10 nm BCP features
We studied different approaches in fabrication of nanoimprint stamps with ultra-high resolution in the 10 nm range and compared their performance. As the main method of nanoimprint replication we used a combined thermal and UV-imprint process with optimum conditions and materials to demonstrate ≈20 nm pattern transfer to silicon oxide substrate. Negative master stamps are preferred as they require a single replication step to make intermediate polymer stamp (IPS). Electron beam lithography and reactive ion etching have a decisive role to produce a master stamp with sufficiently sharp shapes required for sub-10 nm resolution during the replication of the IPS. A reliable pattern transfer into a hard substrate depends critically on thickness of the residual layer after nanoimprint.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.3 - Fabrication of sub-10 nm metal structures by line multiplication based on atomic layer deposition
Fabricating nanostructures with small lateral sizes and high aspect ratio is one of the key challenges, for instance, in developing highly resolving diffractive X-ray optics. While conventional lithography approaches break down below 20 nm feature size, growth processes can achieve extreme precision which reaches sometimes down to the atomic level. This approach enabled to produce diffractive Xray lenses (Fresnel zone plates) with down to 12 nm line width.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.7 - Test of 3D hierarchical scaffold with and without liposome membranes
Microfluidic systems for handling/sensing chemical and biological samples could improve their performance through the employment of materials with selected functionalities in specific regions of the device. Among these, mesoporous materials feature ordered tailored structures with uniform pore sizes, highly accessible surface areas and large pore volumes, making them an attractive support for functionalization and catalysis. The ordered mesopores are an ideal host for functional organic molecules or nanoparticles and patterning them would allow the design of devices for different types of advanced applications, like DNA nanoarrays. Patterning of such films to obtain circuits or dot arrays can be reached by coupling the bottom-up route with top-down processing such as lithography. In this way, hierarchically structured materials can be obtained in which organization resides on multiple length scales: porosity (typically 2–10 nm), film thickness (200–500 nm), and pattern size (1 - 500 μm).
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.8 - Resolution tests on inorganic resist materials with EBL and EUV lithography
Advanced UV and electron beam lithography (EBL) techniques have enabled semiconductor industry to successfully accomplish the device miniaturization over the last decades. However, to pursue developments further towards nanoscale high performance devices as well as to support the growth of quantum and MEMS/NEMS technologies, the resolution limits of these techniques need to be pushed into the sub-10 nm range. The highest patterning resolution achievable in state-of-the-art EBL systems is mainly limited by resist contrast and the point-spread function of the exposing beam. In the case commonly used high-resolution negative-tone resist hydrogen silsesquioxane (HSQ), much work was devoted to improve the contrast of the development process using hot development [1-4], KOH development [5,6], or salty development [7]. More recently, some authors have addressed the problem using focused helium-ion beam lithography (FHIBL) which features smaller proximity effects as compared to an electron beam at the same incident kinetic energy [8-10]. This deliverable aims at investigating and developing inorganic resists for high resolution patterning. To compliment EBL and FHIBL data of HSQ patterning, EUV interference lithography using this resist was investigated in the course of the joint research activity and results compared for these patterning techniques. Also, hybrid organic-inorganic resists were studied as possible materials for high resolution patterning as incorporation of inorganic network containing higher atomic mass elements (aluminum, vanadium, titanium, zirconium) into the composition of resists allows to reduce proximity effects and also enhances dry etching selectivity. In particular, we have been working along these directions: - Investigation of high resolution patterning and pattern transfer using recently developed alumina based resist. - Development of a new class of hybrid organic-inorganic resists based on vanadium oxide. - Investigation of chemical changes in hybrid organic-inorganic resists upon exposure using near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Using alumina based resist we demonstrate the patterning of isolated features as small as 6.5 nm using EBL and 5 nm using FHIBL. We also show the pattern transfer of 10 nm lines with an aspect ratio of 10 in silicon, using an optimized reactive ion etching process. In addition to the work described above, we tested a material that had never before been tried as a resist: a procedure for the spin-coating, exposure, and development for vanadium oxide based resist. The smallest feature sizes achieved using EBL exposures were 13.5 nm. These first demonstrator experiments show that this material can serve as a negative-tone resist for EBL. Further work is in progress to further improve the uniformity of spin-coated films and the development procedures. To better understand chemical changes in hybrid organic-inorganic resists during the exposure, a NEXAFS study was carried out. The experiments show that exposure to soft X-rays determines a (partial or total) removal of the organic ligand of the hybrid resists. The dissociation efficiency of the ligand was found to be dependent on its chemical configuration and several different dissociation pathways are possible. A persistence of strongly bonded C=C after the exposure was also identified, which is especially relevant for lithography applications and pattern transfer by etching. These findings provide insight into the mechanism according to which hybrid organic-inorganic resists work and can open new opportunities for their chemical synthesis for performance improvement.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.9 - Development of NIL replication using polymer and sol-gel resists
In the present deliverable, we report on sub-10 nm replication in both polymeric and sol-gel resists. Intermediate polymer stamp made of OrmoStamp material was used for the UV nanoimprint replication experiments in TU7 polymer and alumina-based sol-gel inorganic resist. The sol-gel resist viscosity has been optimised in order to demonstrate the 10 nm resolution. High etch stability of the AlOx mask is very promising for development of high-resolution pattern transfer using e.g. reactive ion etching, but a descum process to remove the alumina residual layer after imprint is to be developed.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.10 - Test of 3D hierarchical scaffolds with embedded protein nanoparticles and natural biomolecules
Biomimetics offer the possibility of biological systems simulation on artificial surfaces, with desired properties. In our case, our interest focuses on the application of such surfaces as cell culture platforms, and in particular fabrication of functionalized (and bioconjugated) substrates and their physicochemical (in terms of morphology, topography, structure) and biological (cell growth, proliferation and differentiation) characterization. The present project comprises three approaches. The first one is the fabrication of micropatterned silicon substrates via ultra-short pulsed laser irradiation under specific experimental parameters, including laser fluence and irradiation environment. The second approach is the fabrication of hierarchical micro-nano-patterned substrates. These substrates include i) micro-patterned silicon substrates which have been nano-decorated with spherical gold nanoparticles of various functionalities and ii) micro-patterned silicon substrates which have been coated with gold layer (50nm thickness) via sputtering method. Gold nanoparticles have been attached via silane chemistry. All types of substrates have been characterized for their morphological properties. The third approach is based on a new route for the preparation of porous matrices with appropriate physicchemical properties using compressed fluids as solvent media. In particular, we investigate PLA processed with Supercritical CO2 for the preparation of porous matrices and its decoration with protein nanoparticles (pNPs) as inductive factors. Regarding the micropatterned substrates, the morphological characterization showed that as the laser fluence increased the roughness of the surface increased as well. Micropatterned substrates comprised microcones of varying height and density. Specifically, the density and the height of the micro-features (i.e. microcones) decreased and increased respectively, with increasing laser fluence. Regarding the hierarchical micro-nano substrates, scanning electron microscope (SEM) analysis confirmed the successful deposition of both gold nanoparticles and gold layer, on the micropattenred silicon substrates. Deposition gave a homogenous distribution of single nanoparticles and some regions of small clusters. All types of the gold nanoparticles (AuNPs) being tested, which carried diverse functionalities (including the oligopeptide CALNN-RGD, RGD-CDI, the stabilizer citrate and mPEG, PEG-COOH groups) have been successfully attached on the surfaces of the micropatterned silicon substrates. Remarkably, the NPs covered the whole 3D surface of the micropatterned substrates giving a distribution that was comparable to that on the flat silicon substrates. Finally, both the micropatterned and the hierarchical micro-nano substrates have been characterized for their use as cell culture platfroms for the growth of PC12 cells. As a proof of concept, hierarchical substrates incorporating AuNPs carrying the RGD peptide cell-binding moiety, were used to study the PC12 cell growth and differentiation. Our results show an impressive growth and NGF-induced differentiation of the PC12 cells on the nano-micro-patterned substrates, especially at early timepoints, compared to NPs-free, bare, micropatterned substrates. Regarding the functionalization of 3D scaffolds with pNPs the study here presented reveals that the appropriate combination between compressed fluid technology and the pNP gives as a result a promising biomaterial for tissue regeneration. Specifically, using a filtration procedure, these 3D scaffolds can be efficiently loaded with pNPs formed by Green fluorescent protein, which promotes and accelerate cell proliferation. Results presented in this study confirm that nano-fabrication of pNPs enhance cell growth and converts 3D scaffolds like PLA processed with scCO2 and decorated with these protein aggregates in a potential cellular support for regenerating an injured tissue.
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WP7 - JRA2 Research on High Precision Manufacturing
D7.11 - Test of 2D engineered surfaces (patterns with spatial resolution and gradients) with protein nanoparticles
Cells responses, like positioning, morphological changes, proliferation and apoptosis are the result of complex chemical, topographical and biological stimuli. Here we show the macroscopic responses of cells when nanoscale profiles made with protein nanoparticles (pNPs) or soluble RGD peptides are used for the 2D engineering of biological interfaces at the microscale. A novel and deep statistical data treatment of fibroblasts cultivated on supports patterned with green fluorescent protein (GFP) and with human basic fibroblast growth factor (FGF) derived pNPs demonstrates that these cells preferentially adhere to the pNPs areas and align and elongate according to specific patterns. These findings prove the potential of surface nanopatterning with functional pNPs being this novel process of nanostructuration with protein-based nanomaterial promising for tissue engineering. A versatile evaporation-assisted methodology based on the coffee-drop effect is also described to deposit nanoparticles on surfaces, obtaining for the first time patterned gradients of protein nanoparticles (pNPs) by using a simple hand-made device. Fully customizable patterns with specific periodicities consisting of stripes with different widths, heights and with distinct nanoparticle concentration gradients can be obtained over large areas (~10 cm2) in a fast (up to 1 mm/min), reproducible, and cost-effective manner using an operational protocol optimized by an evolutionary algorithm. Grids consisting of pNPs derived from GFP were produced to study the mobility of fibroblasts. Indeed, such cells were confined between the walls of the grids with particle concentrations higher than 5·105 particles/mm2 limiting their movement. However, the cells freely move inside the areas containing lower particle concentrations, as in a corral. The developed method opens the possibility to decorate surfaces “a-la-carte” with pNPs or other kind of NPs enabling different kinds of cell motility studies. Encouraged by these methodologies and the findings demonstrating that pNPs can be a useful tool to govern cell´s positioning, orientation and morphology, we have explored its applicability in the research of cell motility. In vitro studies suggest that not only physical structures (topography) but a combination of topography and biological cues (growth factors) induce cell responses and signaling mechanisms that promote cell migration. In order to include biological activity to the topographic factors already brought by the use of fluorescent GFPderived pNPs, we have also used a fibroblast grow factor; FGF-based pNPs giving a real biological activity to the substrate. In this way, cells have been stimulated not only by the topographical alteration of the substrate, but also by the biological activity of proteic nanoparticles. Here we have compared cell responses to substrates decorated with various pNPs patterns. In particular, we compare: A) Constant vs. gradient concentrations of pNPs, B) Different steepness of pNP’s concentration gradients, C) Different absolute pNP´s concentrations, and D) Broad vs. narrow paths to study the influence of cell movement constraining. In summary, two different strategies have been stablished for 2D engineering of surfaces with spatial resolution and gradients using cell adhesive peptides and protein nanoparticles (pNPs). The developed device for gradient deposition of NPs and the PDMS stamps and protocols for the 2D microstructuration of the nanoparticles could be offered to users of TNA access.
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WP7 - JRA2 – High precision manufacturing
D7.12 - Investigation of development processes allowing for high ARs (>5) at the 10 nm line width level
Fabrication of nanostructures with high aspect ratios (AR) of 5 or more is a true challenge. Especially when approaching the 10 nm line width regime, aspect ratios can get comparably high by the demand of minimum resist thickness for pattern transfer by, e.g., plasma etching, lift-off or electrodeposition. Using conventional wet-chemical development processes, patterns with small line width and high aspect ratios easily collapse, especially during drying of the liquid agents the specimen are processed with. The main reasons for this are capillary forces and a decrease in mechanical stability as the lines get smaller. This deliverable aims at investigating the development of resists that can be used for high-resolution processing. Within this report we focus on the development of nanostructures with high AR using three negative-tone resist systems, which are described in their fundamental aspects in another deliverable report (D7.8): - Hydrogen silsesquioxane (HSQ), - the sol-gel alumina resist tested at C2N and PSI laboratories within JRA 2, - and the vanadate-based resist [5,6] newly developed in collaboration with the University of Ulm which was tested at PSI. Of several ideas and possibilities to develop and dry resists with an AR exceeding 5 and line widths in the 10 nm regime, critical point drying (CPD) was identified as the method of choice. We thus tested this method comprehensively and characterized the resist materials above as well as different nanostructures which exhibit a range of thicknesses between 60 and 550 nm and line widths from 6 to 20 nm.
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WP7 - JRA2 – High precision manufacturing
D7.13 - Fabrication and synchrotron characterization of 3D nanomagnets arrangement with sub-100 nm resolution
Advanced patterning techniques allowing the production of nanoscale structures have enabled breakthroughs in multiple fields of science. In particular, over the past decades, tailoring the shape of magnets on the nanoscale has enabled the study of a large number of novel quasi-static and dynamic phenomena in nanostructured magnetic materials. In recent years, a novel class of magnetic materials – artificial spin ices – has been the focus of intense research because it displays a rich spectrum of emergent phenomena. Artificial spin ices are composed of geometrically frustrated arrangements of interacting nanomagnets and have mainly been used to investigate fundamental aspects of the physics of frustration. They also have the potential to become a class of functional materials with technological applications. Indeed, it has been shown that spin ices support topological defects [1], can be tailored to act as metamaterials for spin waves [2], and even to realize thermal ratchets [3]. However, only 2D ‘flat’ structures have been studied so far. The study of magnetism in 3D nanostructures is a young field of research and has mainly been limited to simple three dimensional magnetic nanostructures such as cylinders and nanotubes. Those studies have for example demonstrated that curvature can give rise to novel magnetochiral effects in the presence of magnetic fields [4]. Such effects are promising for applications, in particular for data storage concepts, which rely on magnetic domain walls to store bits of information. In contrast, our goal was to extend artificial spin systems into three dimensions and to study aspects of their collective dynamics on the nanosecond time scale. Indeed, so far only the quasi-static behavior of free-form ferromagnetic 3D structures, such as magnetization reversal and hysteretic behavior, has been investigated [5]. Our study of the GHz dynamics in 3D structures opens the possibility of investigating the influence of finite-size effects on the dynamic response of the magnetization, in particular of spin waves, and of exploring the possibility of creating functional materials, such as reconfigurable magnonic crystals [6]. Investigating such systems requires specific fabrication and measurement techniques. The deliverable addresses these challenges and aims at: - DEVELOPING TECHNIQUES ALLOWING FOR FABRICATION OF FREE FORM 3D MAGNETIC STRUCTURES AT THE MICRO/NANO-SCALE; - USING STATE-OF-THE-ART METHODS TO INVESTIGATE COMPOSITION OF 3D MAGNETIC STRUCTURES AND THEIR MAGNETIC PROPERTIES. In our approach, the fabrication of 3D magnetic structures is based on high resolution laser scaffolding technique developed previously within NFFA and described in report of MS9 “Sub-100 nm 3D photopolymer structures fabricated by non-linear laser lithography”. The reported technique enables production of high quality sub-100 nm resolution free form resist scaffolds. These scaffolds are later uniformly coated by a few nanometer thick conductive layer and electroplated by nickel to obtain a magnetic structure. Synchrotron-based imaging techniques were used for the structural characterization of the fabricated 3D magnetic samples. In particular, high resolution ptychographic tomography was carried out at the cSAXS beamline (Swiss Light Source) revealing a mostly homogeneous nickel film coating around the polymerized scaffold. For studying the magnetization dynamics, the 3D structures were transferred into microresonators by using micromanipulators and the ferromagnetic response was measured as a function external magnetic field strength and angle with respect to the structure to achieve a full 3D characterization. The recoded complex periodic ferromagnetic resonance signal 5 indicates the effect of the three dimensional structure on the magnetic resonances. Further studies of these architectures should give insights into three dimensional nanomagnetism and provide a basis for tailoring collective behavior, which can be used to design novel functional magnetic microdevices.
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WP7 - JRA2 – Research on High Precision Manufacturing
D7.14 - Test of re-alignment of nanostructures in synchrotron experiment by in-situ marker deposition
This deliverable report D7.14 is part of the overall development of a protocol to enable the reliable re-alignment of nanostructures in synchrotron experiments by in-situ marker deposition. Here, we specifically report on the activities within the subtask of the Joint Research Action JRA2 “High Precision Manufacturing” with the aim to create and employ well defined markers in terms of the marker position on a sample, the marker size, and the optimal marker thickness. The re-alignment protocol developed within the Joint Research Action JRA5 “Advanced Nano-Object Transfer and Positioning” requires an in-situ deposition of markers in order to create the markers in close vicinity to the region of interest containing the nano-objects. In particular, we applied ion- (IBID) and electron- (EBID) beam induced deposition in a dual beam focused ion beam instrument (FIB-SEM) to create Pt based markers from a metal-organic precursor with systematically varied system parameters like, e.g., the spot- or beam-size of the electron or ion beam, as well as the electron or ion beam energy, and determined the resulting thickness by atomic force microscopy (AFM). Based on our results we conclude that with the here applied settings, it is possible to reliably create markers for re-localization with nanometre precision, provided a careful calibration is carried out. Moreover, it is not only possible to provide markers for wide range of thicknesses and applications, but also marker thicknesses outside the tested parameter range by extrapolating and adjusting the writing time. As such, we developed a protocol based on the IBID/EBID technique to produce in-situ fabrication of alignment markers. Along with the concepts, software protocols and hardware implementations for a hierarchical marker arrangement developed within the Joint Research Action JRA5, the outcome of this JRA2 deliverable report permits a well-defined nano-transfer between nanoscience instruments and focused X-ray beamlines that is already by now offered to NFFA user requests within the category “Lithography and Patterning”. The report also stresses the strength and the fruitful cross-JRA interactions between the technical developments pushed forwarded within JRA2 and JRA5.
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WP7 - JRA2 - Research on High Precision Manufacturing
D7.15 - Realization of coplanar electrode arrays with 10 nm gaps
There is growing interest in the study of the electrical properties of single nano-objects. This deliverable demonstrates the successful fabrication of arrays of nanogaps via exploiting the precision of growth processes for lateral patterning, as the nanogaps arrays could be used as a substrate to correlate the structural properties of nanomaterials immobilized between the gaps with their electrical properties. In particular, technologies for fabrication of metallic nanogaps down to 10 nm and nanogaps arrays, as well as arrays of individual nanogaps, have been developed. Also fabrication parameters have been optimized for minimising leakage currents and improving electrode characteristics. Current technology is now readilly available for the needs of NFFA users via the transnational access procedure.
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.1 - Design of Trusted authentication source for NFFA-EUROPE services
This document presents the guideline of the design of Authentication and Authorization Infrastructure (AAI) for NFFA-EUROPE community. This AAI will allow NFFA-EUROPE scientific users to access NFFA services through a simplified approach. Such services include the NFFA portal where proposal are submitted, access to all the physically distributed repositories at different facilities and finally global access to the Information and Data Repository Platform (IDRP) that is presented in the twin Deliverable 8.2: “Design of the finalized repository architecture”.
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.2 - Design of the finalized repository architecture
This deliverable presents the finalized architecture of the NFFA Information and Data Repository platform (IDRP). The goal of the IDRP is to allow the user to cover the full research data lifecycle. Therefore, the IDRP has to provide, on one hand, generic data services that allow to manage data and metadata, as well as to search, retrieve, share and publish measurements. On the other hand, the IDRP must provide access to specific European wide distributed data archives that hold the actual data and must support various scientific sub-domains using numerous data and metadata formats. This document presents the overall architecture consisting of multiple components accessible via a well-defined interface. It also presents several standard use cases covered by the architecture, the components involved and the expected side effects for the IDRP, for a facility and a data archive holding data assets. During the design phase of the architecture it was always ensured that its influence on external infrastructures and workflows, e.g. on facilities or data archives, was as low as possible. This will lower the barriers for integrating existing infrastructures, at least on a generic level, and will offer the potential to expand in future.
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.3 - Internal Test of the Information System
This deliverable presents all the procedures and actions tested to provide a shared authentication mechanism across NFFA facilities.
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.4 - First Testbed Available
This deliverable reports a short description of the first NFFA Information and Data Repository Platform (IDRP) prototype developed by KIT [1], in collaboration with CNR-IOM [2] and Promoscience srl [3], and deployed on CNR-IOM OpenStack cloud infrastructure [4]. The prototype implements what is described in detail in D8.2 deliverable “Design of the finalized architecture” [5].
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.5 - Testbed fully deployed, including DASS services
This deliverable reports a short description of the final NFFA Information and Data Repository Platform (IDRP) testbed developed by KIT [1], in collaboration with CNR-IOM [2] and Promoscience srl [3], and deployed on CNR-IOM OpenStack cloud infrastructure [4]. The testbed is the enhanced version of the original prototype version described in [5], which implements now also some first Data Analysis Software as Services (DASS). All the components of the prototype have been deployed as independent virtual machines. Each single element, and the interaction with the others, will be briefly described in Section 1. A user guide describing the basic procedures to interact with the IDRP can again be found at [6]. These web pages will be constantly updated and is intended to become the manual for the IDRP infrastructure usage and the associated DASS services.
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WP8 - JRA3 – Research on e-infrastructure for data and information management
D8.6 - Internal test of NFFA Distributed Repository
This deliverable briefly reports about the internal testing of the final NFFA Information and Data Repository Platform (IDRP) testbed. The infrastructure has been described in some details in deliverable D8.5 [1] and has been developed by KIT [2], in collaboration with CNR-IOM [3] and Promoscience srl [4]. Its deployment has been done on CNR-IOM OpenStack cloud infrastructure [5]. All the components of the prototype have been deployed as independent virtual machines. Each single element and the interaction with the others has been described in Deliverable 8.5 available on the NFFA-Europe web site. We report here the internal testing procedures adopted for each element and the results of such procedures. The overall result is positive and the testbed infrastructure was found stable and robust.
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WP9 - JRA4 - Research on Time-resolved ultrafast probes on nanosystems
D9.1 - Pump-probe setup with tunable pump beam
To understand the physics of nanomaterials and nanosystems is cornerstone for contemporary Science and Technology. To this end, the macroscopic properties of materials can be traced down to their structural and electronic properties at the nanoscopic level. Knowledge of the electronic and lattice dynamics sets the basis for efficient modelling of the material in time and highlights properties useful for promoting technological applications. The time-resolved differential pump probe technique, with use of ultrafast laser sources, is ideal for such studies. By monitoring the differential transmissivity / reflectivity of nanosystems we provide insight into their ultrafast optical, optoelectronic and structural-phononic response. Deliverable 9.1 refers to building a pump-probe workstations for VIS near-VIS, near-IR and THz spectroscopy of nanosystems that will be readily available to NFFA-Europe users.
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WP9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.2 - HHG Optical setup for XUV spectroscopy
Ultrashort pulsed laser techniques such as harmonic generation and multi-photon excitation, have recently found their application in nanomaterials research, as non-invasive tools for imaging and manipulation of nanosystems, and spectroscopy with unprecedented time resolution. The Attosecond Science and Technology (AST) activity at FORTH-IESL focuses on the generation, characterization and applications of intense Extreme Ultraviolet (EUV) radiation emitted in the form of pulses of duration less than 1fs (attosecond pulses). It targets the development, upgrades and running of a state of the art, table-top, attosecond beam lines dedicated to the investigation of ultrafast dynamics in all states of matter, as well as of non-linear and strong field phenomena induced solely by the XUV radiation. Deliverable 9.2 refers to the development of a high-harmonic generation (HHG) optical setup for XUV spectroscopy that will be readily available to NFFA-Europe users.
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WP9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.3 - Demonstration of a multiple beam delay line for X-ray streaking experiments
We designed and fabricated optical elements in order to streak the time delay of an incoming EUV beam along one dimension on a two-dimensional detector. This concept allows for conducting pumpprobe experiments with time windows of up to 3.5 ps in a single shot from an XFEL. We tested this concept in two XFEL beamtimes at the DiProI beamline at FERMI. With this approach, we are able to investigate magnetic dynamics in scientifically and technologically relevant magnetic materials. By tailoring the optical elements, we furthermore opened up a possibility to investigate compound materials at two different absorption edges without major changes in the experimental geometry. Two different off-axis zone plates are mounted in this case, and the energy can be easily switched forth and back from one absorption edge to the other. This is a major advantage in terms of speed and efficiency of an experiment. Taking this approach further, we have developed a dedicated optical element that can be illuminated with a beam containing two different energies in a fixed ratio. This novel off-axis zone plate additionally includes an integrated beam splitter, allowing us to separate two diffraction orders for normalization purposes.
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WP9 - JRA4 - Research on Time-resolved ultrafast probes on nanosystems
D9.4 - Setup for pump-probe small and wide angle scattering experiments
With the drastic need for renewable energy sources, materials with solar harvesting capabilities receive increasingly attention for technological and scientific purposes. In such energy-conversion materials, the principal interaction between light and matter occurs on the nanometer level – a regime in which most properties of bulk-matter do not hold. A comprehensive understanding of these phenomena, particularly the structural material response within the first pico- and nanoseconds after the absorption of light, is critical for the design of novel nanomaterials with enhanced energy conversion efficiency. Deliverable 9.4 aims at building a time-resolved opticalpump X-Ray-probe setup, capable of studying the picosecond lattice dynamics of nanomaterials. This is achieved by installing an ultrafast high-repetition-rate laser at the AustroSAXS beamline of the Elettra synchrotron, where X-Ray scattering / diffraction patterns are taken before, during and after optical excitation. Pilot-experiments were successful, paving the way for accessibility by future NFFA-Europe users.
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WP9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.5 - Protocol of time resolved X-rays absorption spectroscopy
The dynamical studies through Time-resolved x-ray absorption studies (TR-XAS) in the 1 ps- 100 ns time scales are crucial in solids and nanostructured systems to understand carrier dynamics, structural photo-induced phases, electron-phonon coupling, shock-waves and similar processes. This timescale is achievable at Synchrotron radiation and Free Electron Laser facilities. We present here our activity devoted to define a protocol which describes key steps in performing feasibility of pumpprobe measurements that combine a femtosecond optical laser with X-ray probes. The main guidelines of the protocol are: (1) the calculation of Flourescence yield counts as a function of geometrical requirements of the pump and probe beams and the sample-specific penetration depths of the Laser (ZL) and X-ray (ZX) beams (2) evaluation of the signal to noise ratio of the dynamical data (3) evaluation of the sample thermal damage induced by the incident beams. The procedure is based on our simulations meant to perform feasibility evaluations for Fluorescence XAS Pump and Probe experiments on solid samples. Test and feasibility of time resolved set-up for the pump-probe workstation with ps-ns resolution for soft and hard X-rays spectroscopy. Thanks to this work, we performed a preliminary design of a versatile experimental vacuum chamber for time resolved (pump – probe) X-ray spectroscopy experiments operating at Synchrotrons and Pulsed sources in the Soft and Hard-X regime. This activity benefited of one post doc contract (Luca Cozzarini) funded by the NFFA Europe.
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WP9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.6 - Protocols for temporal characterization of ultrashort FEL pulses
The pulse duration, and, more generally, the temporal intensity profile of free-electron laser (FEL) pulses, is of utmost importance for exploring the new perspectives offered by FELs; it is a nontrivial experimental parameter that needs to be characterized. We measured the pulse shape of an extreme ultraviolet externally seeded FEL operating in high-gain harmonic generation mode. Two different methods based on the cross-correlation of the FEL pulses with an external optical laser were used. The two methods, one capable of single-shot performance, may both be implemented as online diagnostics in FEL facilities. The measurements were carried out at the seeded FEL facility FERMI. The FEL temporal pulse characteristics were measured and studied in a range of FEL wavelengths and machine settings, and they were compared to the predictions of a theoretical model. The measurements allowed a direct observation of the pulse lengthening and splitting at saturation, in agreement with the proposed theory.
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Wp9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.7 - Computational protocol for material optical properties during pump-probe experiments and in nanostructures irradiated with ultrashort pulses
To design appropriate efficient pump-probe experiments and evaluate the response of nanostructured materials to ultrashort-pulsed laser irradiation, it is important to understand the underlying physical mechanisms that characterise laser-matter interaction. To this end, a computational protocol is developed to describe the multiscale analysis of all physical processes that are involved following irradiation with very short pulses. To efficiently quantify the optical response of the material in the first stages after the irradiation, a quantum mechanical approach is followed through the synergy of Quantum Espresso and Yambo Code that are coupled with revised versions of the Two Temperature Model (TTM) to eventually describe relaxation processes and/or morphological changes. To test the computational code, 6H-SiC is used as a test material for which the damage threshold fluence (i.e. minimum temperature at which the material melts) is being calculated. The reason for which this material is used is because there are existing experimental protocols designed by groups in the consortium.
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WP9 - JRA4 – Research on Time-resolved ultrafast probes on nanosystems
D9.8 - Numerical codes and software for real time simulation of pump-probe experiments
Computational materials science based on first principles atomistic methods plays a key role in the discovery, characterization, and engineering of novel and complex materials. While density functional theory (DFT) is the established workhorse for ground state properties of a wide range of systems ranging from atoms and molecules to solids and nanostructures containing thousands of atoms, there is an increasing demand for an accurate description of excited state properties in even the most challenging materials. Within the framework of solid state physics, the Green's function formulation of many-body perturbation theory (MBPT), specifically the GW approach to quasiparticle (QP) for charged excitations and the Bethe-Salpeter equation (BSE) for neutral excitations, offers a quantitatively accurate solution. The GW-BSE approach has been implemented in a number of free and commercially available codes and applied to a wide range of materials [1]. Nonetheless, the complexity and relatively poor scaling of the GW-BSE method, and often of its implementation, constitutes a barrier towards its application to realistic systems of large size or to physical phenomena that lie outside the scope of most state-of-the-art approaches. The situation in the out-of-equilibrium scenario changes dramatically and the role of NFFA turns to be essential. Despite the great scientific interest and the relevant technological applications, we have still a poor understanding of several key aspects of the ultra-fast dynamics following the primary excitation pulse, the reason being the enormous delay in the theoretical and numerical development. Indeed, the dynamics of the initial ensemble of electron-hole pairs excited by the laser pulse represents a theoretical and numerical challenge, whose description in realistic materials was well beyond the capabilities of state-of-the-art first principles approaches, and up to now is still mostly based on ad-hoc models and/or approximations. In addition, experiments can approach a new temporal regimes and physical phenomena where the gap with theory appear to be even more profound. With this deliverable, we have extended the state-of-the-art Ab-Initio tools (QE and Yambo) to predict out-of-equilibrium properties. With these implementations, it is now possible to perform realtime simulations of pump and probe experiments.
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WP10 - JRA5 – Research on Advanced Nano-Object Transfer and Positioning
D10.1 - Software routine for coordinate definition and relocation of single nano-objects
This deliverable report D10.1 describes the development of a software script for the “Advanced Nano-Object Transfer and Positioning” with two GUI implementations in Matlab and Python. This immediate outcome of the Joint Research Action JRA5 shows that one important task of its working package WP10 is achieved, ready to use, and has indeed come into routine usage and user operation. The software scripts permit to calculate the marker and nano-ROI positions after the sample was transferred from a nanoscience instrument like a scanning electron (SEM), optical light (OM) microscope to a focused X-ray beamline. Each script reads-in the coordinates of the markers and the nano-ROI provided by a standardized file export from the nanoscience instruments, like, SEM or OM. After moving the sample to the focused X-ray beamline, the sample edges or coarse zero-level hierarchy markers have to be manually re-located and focused. After entering the new beamline coordinates into the software scripts, the latter provides the calculated positions of the next higher level of hierarchy markers, or the nano-ROI. At beamline ID01 at ESRF, the Python script communicates with the beamline motor control system SPEC. It furthermore permits a direct, automated sample coordinate transfer that takes place in the background on request. In the near future, these software scripts assist NFFA nanoscience users in the framework of the transnational access in re-localizing their specific nano-objects. Since beginning of 2018, the outcome of the JRA5 development has become a new offer of the transnational access, providing i) hierarchical markers with electron- or ion beam induced deposition (EBID/IBID) at DESY NanoLab, ii) the software scripts, and iii) a tailored design of the marker size like thickness, lateral arrangement, etc. in order to optimize the search for the nano-ROI.
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WP10 - JRA5 – Research on Advanced Nano-Object Transfer and Positioning
D10.2 - Implementation of transfer and positioning system at nanolabs and ALSFs
We are describing the status and implementation of the transfer and positioning developed within the joint research action JRA5 “Advanced Nano-Object Transfer & Positioning” at dedicated X-ray beamlines at SOLEIL, ESRF and PETRA III/DESY and co-located nanolabs permitting novel one-toone nano-experiments on single pre-selected nano-objects. This includes i) the development of a software script that assists in relocating pre-selected nanoobjects based on a marker and coordinate system, ii) the development of a tailored design of the nano-transfer ii) the implementation at scanning electron (SEM) and optical light (LM) or scanning probe microscopes (AFM) at the nanolabs and at the dedicated beamlines including hard- and software hand-over from and to the nano-instrument and the beamline motor control system, iii) a test-experiment showing the steps and the function of the Advanced Nano-Object Transfer and Positioning package, and iv) the offer to NFFA users within the transnational access (TNA) and other regular users of the nanolabs and the ALSF synchrotron X-ray beamlines. In a separate deliverable report D10.1 of the joint research action JRA5 “Advanced Nano-Object Transfer and Positioning”, we are reporting on the establishment of a standardized software protocol for the coordinate definition and relocation of single nano-objects, which is an integral part of the implementation described in this deliverable report. In the framework of a research project in the field of nano-catalysis, we were able to show i) the need, ii) the opportunities for novel operando nanoscience experiments that directly benefit from the outcome of the JRA5 “Advanced Nano-Object Transfer and Positioning”, and iii) the feasibility to determine and track one to one structure-property-relationships of pre-selected single nano-objects or nano-assemblies. Both, the soft-and hardware integrations have been experimentally proofed to be successful and reliable, and as such received a degree of maturity that since the beginning of 2018 these technical developments within the JRA5 “Advanced Nano-Object Transfer and Positioning” are being offered to external users as part of the European NFFA transnational user access program in the category “Lithography & Patterning”. The remaining 6 months of the JRA5 period will be used to complete, test and optimize the implementation at all dedicated nano-instruments and X-ray beamlines.
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WP10 - JRA5 – Research on Advanced Nano-Object Transfer and Positioning
D10.3 - Methods for deposition of array markers for transfer and position system by laser-based lithography
We fabricated array markers by laser-based direct-write non-linear lithography [1], which shall permit a controlled deposition of nano-sized objects into ordered patterns and in turn serve to re-localize previously identified nano-objects. The pattern shall be sensitive for tracking by different nanoscience techniques like, e.g., atomic force microscopy (AFM), transmission electron microscopy (TEM), scanning electron microscopy (SEM) [2] or by the electron- or X-ray excited X-ray fluorescence in an SEM or a nano-focused X-ray beam, respectively. Here we report that laser-based direct-write non-linear lithography is capable to create line patterns with a lateral line resolution of ~100 nm, and that on these pattern lines can be deposited plasmonic nano-objects, such as gold nanoparticles, and more specifically gold nanorods with a longitudinal axis of 52 nm. Plasmonic nanostructures has emerged as a promising route to improve light absorption in various optoelectronic devices due to their ability to confine light in spaces of significantly shorter than one fourth of the wavelength of the incident light, thereby providing strong light absorption or scattering. Gold nanoparticles are widely used in many fields as preferred materials for their unique optical and physical properties, such as surface plasmon oscillations for labeling, imaging, and sensing [3]. The peak of the extinction spectra of the NPs occur at the resonant wavelength which highly depends on NPs size, shape, type of metal as well as the local dielectric environment [4,5] . The tunable optical properties along with their strong resonant characteristics make metal NPs attractive for a wide range of applications ranging from biosensing to photovoltaics (PV) [5-10]. Gold nanorods [11–14] have attracted significant attention, due to the ease of preparation, the large number of synthetic methods available, the high monodispersity possible, and the rational control over the aspect ratio, which is primarily responsible for the change in their optical properties. Nanorods have been shown to have two plasmon resonances [15], one due to the transverse oscillation of the electrons around 520 nm for gold and the other due to the longitudinal plasmon resonance at longer wavelengths. The transverse surface plasmon resonance does not depend on the aspect ratio and is at the same wavelength as the plasmon resonance of spheres. The longitudinal surface plasmon resonance increases with larger aspect ratios. This work is embedded into the task to develop and to provide user-friendly and easy-to-use platforms for re-localization of small objects like gold nanoparticles, and constitutes one of the two marker strategies that are followed within the framework of the NFFA Joint Research Action “Advanced Nano-Object Transfer and Positioning”. On one hand, the development of hierarchical marker strategies is focusing on several markers of different lateral sizes and thickness values, which shall guide the experimenter towards the pre-selected small object by refining the coordinate system and moving towards the next level of vicinity. On the other hand, we discuss here the successful deposition of single gold nanoparticles onto glass nano-patterned areas, via droplet evaporation of gold nanoparticles’ solution, following proper chemical functionalizaion of the nanopatterns. The overall goal is to use such substrates with array patterns for deposition of nano-objects like nanoparticles, for a pre-selection of the nanoparticles at the nanoscience centers, by, e.g., SEM, the relocalisation based on the array markers, and a subsequent characterization at the ALSF’s.
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WP10 - JRA5 – Nano-Object Transfer and Positioning
D10.4 - Methods for deposition of hierarchical markers
This deliverable report D10.4 of the Joint Research Action JRA5 “Advanced Nano-Object Transfer and Positioning” describes how hierarchical markers can be created on sample surfaces in a controlled way and optimized for several applications based on different processing and deposition methods. As selected examples, we are dealing here with the following approaches: i) E-beam lithography, ii) electron- (EBID) and ion- (IBID) beam induced deposition of a precursor material, and iii) parallel markers using the direct laser writing via multiphoton polymerization. For a given application, the appropriate method should be carefully chosen depending on the process steps involved in the sample preparation, the sample size, and the spatial resolution and scanning range of the nano-science and focused X-ray beam instruments planned to be used, and finally, the precision, size and total amount of the markers required. An optimal marker system to ensure an easy and quick nano-transfer comprises hierarchically arranged markers at dedicated marker positions with a designed lateral size and thickness. From the methods listed above, e-beam lithography and direct laser writing can be employed in case many markers at given positions on larger areas are needed. On the other hand, the strategy followed exploiting the EBID/ IBID process permits a pre-selection of regions of interest that contain the nano-objects, and a subsequent placement of the highest level hierarchical markers in their close vicinity. Here, we are describing all three techniques with experimental details on the methods, discuss advantages and limitations for each of the technique, and give examples on how and where these methods are ideally used for, and how they have been tested within the framework of NFFA - JRA5. Moreover, this report contains guidelines and suggestions that may be considered to optimize the hierarchical arrangement and shape of the markers in order to further simplify the search algorithm for the nano-objects of interest.
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WP10 - JRA5 – Nano-Object Transfer and Positioning
D10.5 - Demonstration of relocating nanoobjects based on in-situ deposited fluorescence
In this deliverable report we describe a multistep workflow for re-locating pre-selected nano-objects based on i) the design and arrangement of markers, ii) their creation on a sample surface and iii) the nano-transfer to an X-ray beamline based on the X-ray fluorescence signal of the deposited markers. The workflow relies on a “marker design on demand” principle developed within the Joint Research Action 5 “Advanced Nano-Object Transfer and Positioning” and also includes hierarchical marker arrangement concepts. A software protocol has been created and optimized in Matlab and Python that assists in the position coordinate transformation from a nano-instrument at a nanoscience centre to a focused X-ray beamline at an Analytic Large Scale Facility (ALSF). With the SEM or AFM stage coordinates for each marker and nano-object serving as input, the software tool calculates the new motor positions for the X-ray experiment. With this workflow comprising the marker design, the software protocol and the hardware implementation we provide a versatile solution for various nano-transfer demands not only for ex-situ but more importantly for in-situ or operando studies where the transfer and re-location of small objects is challenging. The workflow proposed here has been successfully tested during several experiments using different nano-science centres and ALSF infrastructures within the participating institutions of the NFFA consortium, and as such proofs the intra- and inter- institutional capabilities of the nano-transfer workflow developed within JRA5. At the same time it shows the benefit of the mutual interactions between the NFFA partners and the overall success in spreading the technical achievements across European institutions. As such, the JRA5 nano-transfer workflow may serve as a seed to establish standard procedures for re-locating of small objects facilitating a multi-analysis of the regions of interest permitting to bridge different techniques and providing a novel level of insight.
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WP10 - JRA5 – Nano-Object Transfer and Positioning
D10.6 - Test experiment of transfer and positioning system to a soft X-ray microscopy setup
This JRA5 deliverable report D10.6 “Test experiment of transfer and positioning system to a soft Xray microscopy setup” describes the status of the implementation of the transfer and positioning system to the soft X-ray microscopy setups at SOLEIL, France. All technical prerequisites have been developed, are readily available for use and are in particular as part already offered to NFFA transnational access users. In particular, both, the nano-transfer tool developed within JRA5, including the three columns i) the Matlab and Python implementation of the software script, ii) the “hierarchical marker design on demand” as well as iii) the electron- (EBID) and ion-(IBID) induced deposition, as well as the capabilities for a nano-transfer at the SOLEIL beamlines are all implemented and integrated. The goals of all three columns have been achieved, as separately documented in several JRA5 deliverable reports. The software-setup and the marker technology has been tested and approved, and are ready to use. At the soft X-ray beamlines at SOLEIL dedicated for the “Advanced Nano- Object Transfer and Positioning” the equipment and technical infrastructure ensures compatibility and easy implementation. In a test experiment to be scheduled at the time of the deadline, the full integration of the nanotransfer tool on one hand and the positioning devices at the SOLEIL beamline at the other hand will be shown. At the same time, the array markers created by direct-write non-linear lithography at FORTH will be utilised to permit a nano-transfer based on the re-location of selected nano-objects at a nano-science centre to a soft-X-ray beamline setup at an Analytical Large Scale Facility (ALSF). We in particular stress here that the compatibility between the modular transfer and positioning system and the hardware at the two dedicated SOLEIL parallel imaging X-ray photoemission electron microscope (XPEEM) and the scanning microscope (STXM) beamlines at SOLEIL has been achieved and the technical feasibility of D10.6 is assured.
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WP10 - JRA5 – Nano-Object Transfer and Positioning
D10.7 - UHV sample transport environment for MBE and neutron reflectometer
This deliverable report D10.7 presents the achievements on a small UHV transfer chamber, which was successfully designed and built. It serves as a means for transport of thin film samples and nano-objects and as well as measurement chamber for neutron reflectivity of samples which are sensitive to ambient condition. Especially, it connects the MBE setup and the MAgnetic Reflectometer with high Incident Angle (MARIA) at MLZ in Garching, Germany for sample preparation and polarized neutron reflectivity measurement in UHV. The functionality was published in A. Syed Mohd, S. Pütter, S. Mattauch, A. Koutsioubas, H. Schneider, A. Weber, and T. Brückel; A versatile UHV transport and measurement chamber for neutron reflectometry under UHV conditions; Rev. Sci. Instrum. 87, 123909 (2016). The design of the transfer chamber bases on standard UHV parts with some special tools like a wobble stick and a nonevapoarable getter and ion pump and takes the conditions for neutron reflectometry into account. It is easy to handle. For retaining compatibility with other experiments a customized Omicron flag style sample plate is used as standard sample holder. The chamber was successfully tested with thin film samples, which were prepared in the MBE setup in Garching. The polarized neutron reflectivity measurements of polycrystalline and epitaxial Co thin films at MARIA revealed that the transfer chamber works and that it is applicable as user instrument. Consequently, since 2018 it may be booked as an additional feature to the MBE setup (NFFA installation 2) and MARIA (NFFA installation 6), which are both part of the TNA package within the NFFA Europe. A next generation transfer chamber consisting mainly of Aluminum was built which will minimize the movement of the transfer chamber within the applied magnetic field of MARIA during measurement. A test will be performed within the next available beam time.
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WP10 - JRA5 – Nano-Object Transfer and Positioning
D10.8 - Industry-friendly sample holder providing interoperability and repositioning
The deliverable report for D10.8 shows the status and development of the unified sample holder for correlative microscopy, in collaboration with CEA-LETI, ZEISS, and ESRF. The development was initiated within the joint research action JRA5 “Advanced Nano-Object Transfer and Positioning” and aims at developing a sample holder with fiducial markers to enhance correlative microscopy for Nano-labs, -institutions, micro- and nano synchrotron beamlines and industrial research facilities. In the first instance, it was meant to enhance the defect and failure analysis investigations of the semiconductor industry. Therefore, an industry friendly sample holder, with a hierarchical marker system is developed and will be tested. The deliverable reports for D10.1 and D10.2 are showing the software scripts to calculate the positions of a nano-object and to transfer it from a FIB-SEM to a focused nano x-ray beamline. Here they used Pt-markers deposited “close” to the Nano-object. This software script will be used as the basis for the development of transferring software for the sample holder as well and will be tested on ID01, as well as other Nano- and micro beamlines at ESRF. This and the ZEISS software “Shuttle and Find” and “ZEN-Connect” will be used for validating the function of the sample holder. Further tests should proof the possibility to spot a region of interest (ROI) in one institution and bring the sample holder together with the sample to a different institution, calibrate the sample holder and transfer the coordinates of the ROI, to investigate with different techniques. At the end the data of the different instruments should be combined (with the “ZEN-Connect” software). With a defined procedure and workflow we want to be able to do correlative microscopy analysis beyond semiconductors, and use the sample holder for samples of other fields of science to correlate the images taken and to combine the information gained with different analysis techniques. On top, we want to enhance the aligning procedures on the beamlines, by having a standardised system, with which scientists and synchrotron users can save time by finding their ROI’s quicker. Without having to do a time-consuming, coarse pre-scan of the complete sample, but being able to spot the region of interest beforehand on a different microscope and transfer its coordinates to the beamlines. Since the beginning of June 2018 we assessed the needs with beamline scientist, industrial users and partners involved in NFFA. After defining the specifications for the sample holder, a technical design followed, which has been reviewed with the scientists and a prototype has been produced. The following steps be to test the prototype against the specifications and after the validation of the concept, we plan to go through a scientific proof within a real scientific intend. Once the sample holder is proven to be a successful tool for correlative microscopy it will be made available for all NFFA partner institutions and their industrial users.
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WP11 - NA – Innovation and networking activities
D11.1 - NFFA-Europe corporate slide & poster presentations
This deliverable describes the results achieved within task 11.2 ”Building NFFA-Europe branding”, and it includes, besides the outputs mentioned in the Deliverable title, also the logo, the project booklet, three versions of project posters, deliverable and the related communication guidelines, published on the following website available to project partners: https://app.frontify.com/d/GafVzXOij5wm/nffa-europe-style-guide
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WP11 - NA – Innovation and networking activities
D11.2 - Draft metadata standard for nanoscience data
This document contains the NFFA Deliverable D11.2 “Draft metadata standard for nanoscience data” due in M6. It describes the approach, the relevant information management practices, standards and recommendations taken into account, as well as empirical research done by NFFA JRA3 for the purpose of metadata design, and then suggests a draft recommendation for NFFA metadata model. Having a common and well-defined metadata model is essential for human-to-human, human-to-machine and machine-to-machine interoperability in NFFA. Such a model will support the development of Information and Data management Repository Platform (IDRP) and will contribute to structured business analysis across the project. In return, the model will get further inputs from the continuing IT architecture design and business analysis. In addition to the NA activities, the deliverable has been discussed and validated through a number of conference calls and electronic communication in JRA3, as well as in the course of a dedicated face-to-face meeting in Abingdon, UK, in February 2016. The metadata model here proposed will be further validated, updated and detailed through the NFFA project activities within and beyond JRA3. It will be then finalised in D11.14 “Final metadata standard for nanoscience data” in M30. Approach
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WP11 - NA – Innovation and networking activities
D11.3 - First Annual report on NFFA-EUROPE dissemination activities
The dissemination activities of the NFFA-Europe project are crucial in the early stage of any Infrastructure EU project, as it has the important task to explain the NFFA-Europe offer to the scientific community. This communication activity consists of many different actions and, with the exception of the dissemination programme, all others have to be considered very succesfull.
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WP11 - NA – Innovation and networking activities
D11.4 - First Report on the NFFA-EUROPE schools
This document reports on the 1st NFFA-Europe Summer School , and points out its main goal, the organisational structure, and the list of speakers and attendees of. It is also reported an assessment of the school made by the participants which can be specially useful in view of the organisation of the 2nd NFFA-Europe school programmed in the 3rd year of the NFFA-Europe project.
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WP11 - NA – Innovation and networking activities
D11.5 - First Report on the industry and business development networking meetings
A strong scientific knowledge base is one of Europe’s traditional key assets, and it has allowed the European Union to become world class in several research fields, such as nanosciences and nanotechnologies. In spite of these merits, the global position of European research is currently being challenged by a rapidly changing research landscape. Simultaneously, European research is faced with the implications of globalisation of markets and industries, digitalisation and new technologies, as well as a need to address societal issues such as an ageing population or climate change.
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WP11 - NA – Innovation and networking activities
D11.6 - Second Annual report on NFFA-EUROPE dissemination activities
The dissemination and awareness activities of NFFA-Europe in the first year had a very positive impact to the TransNational Access programme, as revealed by the large number of proposals submitted for the use of the NFFA-Europe infrastructure. During the second year, no major changes in these activities have been applied, and very good results on all the actions have been found. During the second year the NFFA-Europe project has been (or will be) presented at least at 8 conferences; the second issue of the NFFA-Europe Newsletter has been published and distributed to a number of scientists. The international collaborations to US and Australian similar projects are producing good results in terms of future collaborations. Two NFFA-Europe sessions at International Conferences have been applied, showing also a great interest for this activity. The NFFA-Europe dissemination programme is producing very important results for the project in terms of scientific proposals and collaborations, in line with the expectations.
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WP11 - NA – Innovation and networking activities
D11.7 - NFFA videos and marketing material
This deliverable refers to the activities concerning the preparation of videos and marketing materials within task 11.2 “Building NFFA-EUROPE branding”. The objective of this task is to create a unique brand for the project in order to give consistency to all communication and dissemination tools and activities, respectively. The key tools for a unique brand are an original logo, colour palette and font combined with templates for documents, presentations and posters (described in deliverable 11.1), as well as other marketing materials and videos.
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WP11 - NA – Innovation and networking activities
D11.8 - Operational marketing plan towards industry
Industrial innovation and knowledge transfer by exploiting the NFFA-Europe facilities are common objectives that the Technical and the Industrial Liaison Networks (TLNet/ILNet) set out jointly to achieve through six primary tasks in the 2017-2018 period. Two of these tasks answer back the actual needs of increasing both the industrial participation in the feasibility studies as well as the success rate in the number of granted access. The strategies enacted by NFFA-Europe in reaching out towards industry are described in the Operational Marketing Plan which is divided into two main sections.
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WP11 - NA – Innovation and networking activities
D11.9 - Publication of the online catalogue and one-stop-shop
NFFA-Europe can boast an offer of about 300 experimental apparata, representing over 80 different experimental techniques, grouped into 4 types of Installations (i.e. lithography, growth, theory and characterisation, the latter further subdivided into three 3 kind of installations). To showcase adequately this vast array of installations, an online catalogue was developed into three different informative levels each displaying increasing degrees of details but always presenting a clear layout and a high level of easiness in the navigation. The catalogue is now fully operative and implemented on the nffa.eu web portal.
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WP11 - NA – Innovation and networking activities
D11.10 - Educational videos
NFFA-Europe is a Research and Innovation Action committed to providing free access to state-of-the art tools for multidisciplinary, frontier research at the nanoscale: available techniques range from nano-characterisation to theory and numerical simulation. With the aim to enhance the knowledge in the nanoscale area for the European research community, this deliverable explains the action towards obtaining some educational materials freely available through the web-site. This material is based on the edition of a set of short-duration Educational Videos. The videos are being designed by expert scientists in the field and edited by Promoscience. Fifteen videos have been established to cover most of the NFFA-Europe techniques: 6 videos deal with lithography techniques, 2 videos deal with chemical and physical materials growth, 2 videos deal with theory and simulation techniques and finally 5 videos deal with characterization techniques at the nanoscale.
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WP11 - NA – Innovation and networking activities
D11.11 - Seminars provided through the web portal
In this report the work done to have a set of seminars available in relation with the research areas of the NFFA-Europe project is explained (task 11.4.2). These seminars, mainly developed during the 1st NFFA Summer School, were identified and adapted to be specialised courses, useful for PhD and Master students, and also for engineers and research staff from inside and outside the consortium. These seminars were made free available through the web portal.
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WP11 - NA – Innovation and networking activities
D11.12 - First Report on the incentivised knowledge transfer and feasibility work with industry
This first report on the incentivised knowledge transfer and feasibility work with industry aims at describing the work carried out by the Technical Liaison Network to raise more awareness on the feasibility studies and on the next steps to upgrade the portal to harvest industrial requests. A survey on feasibility studies in the NFFA-Europe offer has highlighted a temporary under-exploitation of this tool by potential industrial users.
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WP11 - NA – Innovation and networking activities
D11.13 - Second Report on the industry and business development networking meetings
Previous report on the incentivized knowledge transfer and feasibility work with industry resulted of the vow made by the Technical Liaison Network to take the feasibility studies to the next level, since conclusions surrounding feasibility studies in the NFFA-Europe offer were highlighting an apparent lack of interest from potential industrial users for it. The following operational marketing plan proposed in the second report was in many ways coming from NFFA-Europes’ will to fully realise and enhance its strategy toward industry. The last report issued was the Barcelona meeting report, this meeting has been the first time TLNet/ILNet met since the Milan kick-off meeting (except in live events) and it is launching a series of forthcoming meetings to keep the implication of the NFFA nodes at its best. Therefore this report will focus on the proactivity of NFFA-Europe toward industry Europewide, and will connect with the previous reports issued by the industry liaison team. It will also address NFFAEurope’ communication strategy through events, regarding NFFA-Europe industry policy and in the One-Stop-Shop aspects that will be embodied in the Single-Entry-Point, and considering NFFAEurope plans after the creation of its Single-Entry-Point dedicated to industry.
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WP11 - NA – Innovation and networking activities
D11.14 - Final metadata standard for nanoscience data
This document contains the NFFA Deliverable D11.14 “Final metadata standard for nanoscience data” due in M30. It contains references to the NFFA Deliverable D11.2 “Draft metadata standard for nanoscience data” (M6) for the earlier defined design approach, for relevant information management practices, standards and recommendations, as well as for empirical research done by NFFA JRA3. The deliverable contains a final recommendation for NFFA metadata model, describes effort on its implementation and indicates directions for its further implementation and development. The deliverable has been discussed and validated through a number of conference calls and electronic communication in JRA3, as well as through engagement with Research Data Alliance groups and external projects outlined in a dedicated section “NFFA metadata interoperability and NFFA engagement with other metadata initiatives”. Implementation effort is outlined in the “NFFA metadata implementation” section. Possible choices for potential NFFA metadata model implementation by third parties, as well as a few directions for further work on nano-facilities metadata are discussed in “Metadata operational recommendations and future developments” section. Particular details of the metadata model design and implementation have been moved into Appendices, in order to keep the main text more concise. The aforementioned sections “NFFA metadata interoperability and NFFA engagement with other metadata initiatives”, “NFFA metadata implementation” and “Metadata operational recommendations and future developments”, as well as Appendices C, D and E are new to this deliverable. The “Approach and methodology” section is a (much) shortened version of the same from Deliverable D11.2. The “An idealised workflow for NFFA experiments” section and Appendices A, B are inherited and updated from Deliverable D11.2.
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WP11 - NA – Innovation and networking activities
D11.15 - Third Annual report on NFFA-EUROPE dissemination activities
The dissemination and awareness activities of NFFA-Europe heavily contributed to the success of the NFFA-Europe project. Its very positive impact to the TransNational Access programme, this is shown by the large number of proposals submitted for the use of the NFFA-Europe infrastructure. During the third year, the activities were not only kept at the same level of the previous years but were broadened, because the end of the project is still far away and there is atill enough time to approach new users for let them use the infrastructure available within the NFFA-Europe project. During the third year the NFFA-Europe project has been presented at 22 conferences; two dedicated NFFA-Europe events have been organized; two issues of the NFFA-Europe Newsletter have been published and distributed to a number of scientists; an advertisment page has been published reaching a huge number of scientists. The international collaborations to US and Australian similar projects are producing good results in terms of future collaborations. The NFFA-Europe dissemination programme is definitely in line with the expectations.
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WP11 - NA – Innovation and networking activities
D11.16 - Second Report on the NFFA-EUROPE schools
NFFA-Europe is a Research and Innovation Action under the H2020 Work Programme committed to providing free access to state-of-the art tools for multidisciplinary, frontier research at the nanoscale: available techniques range from nano-characterisation to theory and numerical simulation. This document reports on the 2nd NFFA-Europe Summer School, one of the training activities organized by NFFA-Europe to promote the knowledge of the techniques and instruments available in the NFFA-Europe Consortium to the young scientific community. This second edition of the NFFAEurope Summer School follows the 1st NFFA-Europe Summer School (Barcelona, 2016), and was held in Trieste (Basovizza) from the 9th of July to the 13th of July, 2018 . The document points out the main goal of the school, the organisational structure, the list of speakers and specifies the list of visits made. An assessment of the school made by the attendees to the school is also included.
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