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Reinforcing carbon nanotubes and photonics research cooperation between the Belarusian State University of Informatics and Radioelectronics and the European Research Area

Final Report Summary - BELERA (Reinforcing carbon nanotubes and photonics research cooperation between the Belarusian State University of Informatics and Radioelectronics and the European Research Area)

Executive Summary:
The overall aim of the BELERA project was to strengthen carbon nanotube (CNT) and photonics research cooperation between Belarusian State University of Informatics and Radioelectronics (BSUIR) and the European Research Area (ERA). In particular, the project focused on the following research topics highly relevant to the FP7 ICT and NMP work programmes: A) Magnetic properties of carbon nanotubes, B) Emission properties of carbon nanotube based cold cathodes, and C) Nanostructured materials for novel photonic devices.

The capacity building activities involved knowledge exchange, setting up joint experiments, and training development for BSUIR’s researchers focused on the 3 research topics and the FP7 programme. Also, it involved mapping and promotion of nanoelectronics and nanophotonics organisations across Belarus, and strategy development to support BSUIR and foundation of the Belarusian Nanoelectronics and Nanophotonics Technology Platform.

The main results of the project were the following:

i) Twinning activities between BSUIR and CNRS on Research Topic A: 4 scientists from CNRS-InESS travelled in Belarus and 8 scientists from BSUIR travelled in France; one publication in the renowned Journal of Applied Physics: “Microwave absorption by magnetic composite of disordered carbon nanotubes array”; and organisation of a summer school in Belarus (October 2012) on Research Topic A with the participation of three experts from CNRS.

ii) Twinning activities between BSUIR and BUW on Research Topic B: 4 scientists from BUW travelled in Belarus and 5 scientists from BSUIR travelled in Germany; joint contribution to a book chapter dealing with Cold Cathodes; and organisation of a summer school in Wuppertal (Germany) the 3-4 September 2012.

iii) Twinning activities between BSUIR and UPVLC on Research Topic C: 2 scientists from UPVLC travelled in Belarus and 4 scientists from BSUIR travelled in Spain and development of a biosensor.

iv) BSUIR signed a contract with the Chinese Institute of Electromagnenic Compatibility to perform joint activities. BSUIR will use BUW's equipment while sending students in Germany.

v) BSUIR and CNRS successfully submitted a joint application under the Belarusian Republican Foundation for Fundamental Research.

vi) BSUIR and UPVLC prepared the FP7 proposal SENSMIR and plan to re-submit it within Horizon 2020.

vii) Innoveo supported the participation of BSUIR in a FP7 proposal (NANOMAT-EPC, www.nanomat-epc.eu) which was successfully evaluated and have started in Period 2.

viii) BSUIR organised 3 workshops in Belarus and one international conference: Nanomeeting 2013.

ix) BELERA team worked on the Evaluation of BSUIR and the preparation of its Strategy Report as well as on the study for a Technology Platform in carbon nanotubes and photonics research in Belarus.

Project Context and Objectives:
The overall aim of the BELERA project was to strengthen carbon nanotube (CNT) and photonics research cooperation between Belarusian State University of Informatics and Radioelectronics (BSUIR) and the European Research Area (ERA). In particular, the project focused on the following research topics: A) Magnetic properties of carbon nanotubes, B) Emission properties of carbon nanotube based cold cathodes, and C) Nanostructured materials for novel photonic devices. These were also research topics highly relevant to the FP7 ICT and NMP work programmes.

BSUIR is the leading academic institution in Belarus for research in micro- and nanoelectronics; new perspective materials; beam-technologies and technics; and radio engineering devices and systems. It is a major university with over 70 professors, 300 PhD lecturers and researchers, and 12,500 students. Its researchers have published numerous research papers in international, peer-reviewed journals during the past 5 years (e.g. Journal of Applied Physics and International Journal of Nanotechnology). It has bilateral agreements with leading research organisations in over 20 countries around the world. BSUIR has a high potential for deeper integration into ERA as demonstrated by its participation in an impressive number of international CNT and photonics related projects during the past 10+ years.

The BELERA project was built upon BSUIR’s existing strengths as a high-quality research institution via twinning and capacity building activities with the following four excellent European research and innovation organisations: Institut d’Électronique du Solide et des Systèmes (CNRS-InESS), Bergische Universität Wuppertal (BUW), Universidad Politécnica de Valencia – Nanophotonics Technology Centre (UPVLC) and Innoveo Consulting (Innoveo). BELERA lasted 24 months and was implemented by a dedicated team of experienced BSUIR researchers.

Project Results:
Twinning between BSUIR and CNRS on Research Topic A

Several joint experiments have been conducted by both teams leading to significant results. The two major experiments consisted in the following:
i. Development of liquid-vaporized chemical vapour deposition for the preparation of hybrid transition metal/carbon nanotubes supported and oriented films, and
ii. Comprehensive studies in the preparation of transition metal/carbon nanotube films. Structural, textural (orientation), spectroscopic and magnetic properties of hybrid transition metal/carbon nanotubes

The experiments consisted in varying the temperature, the gas flow, the concentration of iron precursor as parameters to better defined a material where most of the iron metallic particles are inside the hollow core of the carbon nanotubes. Therefore they have performed the following testing on the samples: transmission electron microscopy (TEM), X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy and scanning electron microscopy.

Two new effects were obtained, i) a diamagnetic contribution is obtained when the magnetic field is perpendicular to the main axis of the nanotube and can be relied in a first interpretation that needs to be refined, to the contribution of the carbon paramagnetism, and ii) an effect on the hysteresis of the curve "size of wasp" due to the occurrence of two ferromagnetic phases, iron and iron carbide. Finally one experiment was done with iron irradiation at high energy on the samples.

During the Period 2 the twinning work consisted in a detailed study of the magnetic properties of iron based nanoparticles (NPs) intercalated into carbon nanotubes (CNT) aligned arrays synthesized by injection chemical vapor deposition (CVD). They have analyzed the temperature (T) and the ferrocene concentration (CF) dependences of the macroscopic magnetic parameters. They have observed the steady increase of both the squareness of magnetic hysteresis loops, M(H), and the coercive field, HC, with CF. Also zero field cooled (ZFC) and field cooled (FC) magnetizations were studied for different CF contents.

BSUIR together with CNRS wrote the following joint publications:
• Labunov V.A. Danilyuk A.L. Prischepa S.L. Prudnikava A.L. Komissarov I.V. Shulitski B.G. Speisser C., Antoni F. and Le Normand F., “Microwave absorption by magnetic composite of disordered carbon nanotubes array”, J. Applied Physics 112, (2012) 024302 (10p)
• A.L. Danilyuk, A.L. Prudnikava, I.V. Komissarov, K.I. Yanushkevich, A. Derory, F. Le Normand, V.A. Labunov, S.L. Prischepa. Interplay between exchange interaction and magnetic anisotropy for iron based nanoparticles in aligned carbon nanotube arrays. Carbon, published on line.
• I. Komissarov, Y. Shaman, J. Fedotova, B. Shulitski, S. Zavadsky, J. Kasiuk, A. Karoza , A. Pyatlitski, D. Zhigulin, P. Aleshkevych, P. Dluzewski, S. Prischepa, H. Szymczak and V. Labunov, “Structural and magnetic investigation of single wall carbon nanotube films with iron based nanoparticles inclusions synthesized by CVD technique from ferrocene/ethanol solution” P hys. Status Solidi C 10, No. 7–8, 1176–1179 (2013) / DOI 10.1002/pssc.201200938.
• A. Prudnikava, S. Prischepa, K. Yanushkevich, O. Demidenko, F. Le Normand, D. Muller, F. Antoni, A. Basaev, “Structural characterization of carbon nanotube arrays implanted with iron ions”, Proceedings of International Conference Nanomeeting. “Physics, Chemistry and Application of Nanostructures” Minsk, Belarus, 28-31 May 2013; Ed. by V.E.Borisenko S.V.Gaponenko V.S.Gurin C.H.Kam Word Scientific, (2013), 543-546 (4p)
• S.L. Prischepa, A.L. Danilyuk, A.L. Prudnikava, I.V. Komissarov, V.A. Labunov, F. Le Normand. Exchange coupling and magnetic anisotropy for different concentration of iron based nanoparticles in aligned carbon nanotube arrays. Physica Status Solidi c.
• S.L. Prischepa, A.L. Danilyuk, A.L. Prudnikava, I.V. Komissarov, K.I. Yanushkevich, V.A. Labunov, F. Le Normand, « Magnetic properties of nanocomposites based on magnetically functionalized carbon nanotubes », Invited contribution to the book “Nanomagnetism” (ed. Gonzalez, OCP, Manchester, UK).
• “Microwave absorption by magnetic nanocomposite of disordered carbon nanotubes arrays”, V.A. Labunov, A.L. Danilyuk, A.L. Prudnikova, I.V. Komissarov, B.G. Shulitski, F. Le Normand, S.L. Prischepa.
• Fundamental and Applied Nanoelectromagnetics. FANEM’12. Conference Proceedings, May 22-25, 2012, Belarusian State University, Minsk, Belarus, 57.
• “Магнитные свойства и параметры магнитной структуры нанокомпозита Fe C-УНТ » Е.Л. Прудникова, И.В. Комиссаров, А.Л. Данилюк, В.А. Лабунов, Ф. Ле Норманд, С.Л. Прищепа.
• Углеродные наночастицы в конденсированных средах. Сборник научных статей. – Минск: Институт тепло- и массообмена им. А. В. Лыкова НАН Беларуси, 2013. – С. 140-145.
• “Structural and magnetic properties of multiwall carbon nanotube arrays with incorporated iron-phase nanoparticles”. A.Prudnikava A.Danilyuk K.Yanushkevich J.Fedotova I.Komissarov S.Prischepa F. Le Normand, F. Antoni. Proceedings of 15th International Workshop “Nano-Design, Technology, Computers Simulations” (NDTCS'2013), 15, Edtrs V. Nelayev, V. Stempitsky, 11-15/06/2013, Minsk, Belarus. Published by Belarusian State University of Informatics and Radioelectronics, (2013), 26-28 (3p)


Twinning between BUW and BSUIR on Research Topic B

During the twinning visit at BUW, BSUIR researchers have gained knowledge in cathodes with horizontally aligned CNT networks and laser-structured cathodes with vertically aligned CNT columns. BUW has unique equipment for emission properties measurement and BSUIR's staff had the chance to use them to study some of their samples. Other knowledge consists in SEM measurements of CNT cathodes before and after FE measurements, FE scanning microscopy, local FE investigation of selected CNT cathodes and integral diode measurements of a selected CNT cathode with luminescent screen. Following this transfer of knowledge, discussions and publication of the field emission results on CNT cathodes with respect to the literature have been made

BSUIR and BUW set up joint experiments consisting in chemical vapour deposition and structuring of CNT-based cathodes and scanning electron microscope investigations of the resulting structures. In 2012 the metalorganic and catalytic CVD deposition processes were investigated and performed at BSUIR, as well as the laser-structuring of metallic catalyst layers for the fabrication of structured cathodes with CNT columns. At first some of these samples were investigated at BSUIR with high resolution SEM to select the most promising ones for the field emission measurements at BUW.

The majority of these samples were examined using a field emission scanning microscope (FESM) to judge about the emitter number density as well as the local FE properties of the CNT emitters. The integral current and the homogeneity of some CNT cathodes were also measured at BUW in diode configuration with luminescent screen (IMLS). Finally, SEM investigations of the processed cathodes were performed at BUW to judge about the stability of the emitters. The fabrication and measurements of a few samples took place during the mutual visits to understand the methodology and develop a common strategy for the optimization of the CNT cathodes. Most of the samples, however, were fabricated at BSUIR and measured systematically at BUW.

BUW and BSUIR joint experiments continued during the Period 2 and consisted in the systematic investigation of the structured CNT bundle cathodes fabricated at BSUIR by means of scanning electron microscope (SEM), field emission scanning microscope (FESM) and integral measurements system with luminescent or metallic screen (IMLS). The exchange of scientific knowledge focused on the requirements to structured cold cathodes for high power device applications and corresponding optimization of CVD fabrication technique of CNT-based cold cathodes.
The BELERA results were used by two young PhD students in their thesis prepared within the BELERA project, namely, A. Tymoshchyk (BSUIR) and P. Serbun (BUW).


BSUIR together with BUW wrote the following joint publications:
• V. Labunov, B. Shulitski, A. Tymoshchyk , I. Kashko, G. Müller, P. Serbun. Synthesis of field emission CNT-cathodes with Ni/Al/Mo localized catalyst. // Physics, Chemistry and Application of Nanostructures / World Scientific; editors: V.E. Borisenko [et al.]. Singapore, 2013, p. 539 - 542.
• P. Serbun, G. Müller, A. Tymoshchyk, I. Kashko, B. Shulitski, V. Labunov: ”High field emission current density from structured CNT bundle cathodes”, Techn. Digest of the 26th Int. Vacuum Nanoelectronics Conf., Roanoke, USA, July 9th (2013).
• P. Serbun, Dissertation, subm. to Univ. of Wuppertal, November 2013.
• Labunov V., Prudnikava A., Bushuk S., Filatov S., Shulitski B., Tay K. B., Shaman Y., Basaev A. Femtosecond laser modification of an array of vertically aligned carbon nanotubes intercalated with Fe phase nanoparticles. Nanoscale Res Lett. 2013; 8(1): 375.
• V. Labunov, A. Prudnikava, B. Shulitski, B. Tay, X. Wang, A. Basaev, V. Galperin, Y. Shaman. Self-organized hybrid nanostructures composed of the array of vertically aligned carbon nanotubes and planar graphite layer // IEEE Conference Publications. Nanoelectronics Conference (INEC), 2013 IEEE 5th International. Digital Object Identifier: 10.1109/INEC.2013.6466022. Publication Year: 2013, Page(s): 277 - 280.
• Vladimir A. Labunov, Alena L. Prudnikava, Beng Kang Tay, Maziar Shakersadeh, Wang Xingli, Alexander S. Basaev,Vyacheslac Galperin, Yuri Shaman/ Self-organised Hybrid Nanostructures Composed of the Array of Vertically allied Carbon Nanotubes and Planar Graphene Multi-Layer// Nanoscale Research Letters.
• Alla I. Vorobjova, Vladimir A. Labunov, Elena L. Prudnikova, Boris G. Shulitskii, Sergey A.Gavrilov Alexey N. Belov/ Aligned Carbon Nanotubes Synthesized Using Porous Aluminum Oxide // Physica Status Solidi c, submitted



Twinning between BSUIR and UPVLC on Research Topic C

During the first year BSUIR and UPVLC worked together and exchanged knowledge on integrated photonic structures and experimental procedures for the characterization of integrated photonic biosensors. Special knowledge on safety rules and protocols has been transferred in view of joint experiments. More specifically UPVLC taught BSUIR's researchers topics linked to electrochemical anodization of aluminium thin films and the characterization of porous silicon samples using I-V measures. Porous structures are the most commonly used materials in biosensors and an in-depth knowledge in this field has been transferred to BSUIR's staff.

In terms of joint experiments, BSUIR and UPVLC worked in the field of structural properties of Al nanomesh and coupling efficiency from Si-based LED source (C1, C2) using measurement facilities of BSUIR and UPVLC. The idea was to develop a metallization processes in UPVLC for porous silicon based emitters developed by BSUIR for their subsequent characterization.

UPVLC and BSUIR are involved in a long R&D work based on BSUIR's quality and innovative materials as well as UPVLC's experience and know-how on biosensor functionalisation. Therefore the Period 2 twinning activities consisted in further research investigation on Schottky junction solar cells, Porous silicon based LEDs with Al-nanomesh and development of an integrated biosensor.

Joint work on the Biosensor: The biomarker is detected by means of specific antibody attached to the surface of the sensing structure and their previous experiments were done in the opposite way: protein receptors for the identification of antibodies. In that sense the experimental protocol had to be changed. The new experimental protocol's requirements consisted in i) the functionalization providing well oriented antibodies, ii) possibility to regenerate the sensing structures for further experiments, and iii) keep functionalization process as simple as possible.

Joint work on the Schottky junction solar cells: The Schottky junction solar cell design contains silicon substrate, epitaxial layer, reverse-side metallization, and thin metal semitransparent electrode, and is distinguished by a metal semitransparent electrode that is made of aluminum nanocellular film with a layer of porous alumina to protect the structure from external action.

BSUIR together with UPVLC wrote the following joint publications:
• Effect of swirl-like resistivity striations in n+-type Sb doped Si wafers on the properties of Ag/porous silicon SERS substrates; Physica Status Solidi C, 1-4 (2013)/DOI 10.1002; A.Bandarenka K..Artsemyeva S.Pedko A.Panarin S.Terekhov V. Bondarenko
• Comparative study of initial stages of copper immersion deposition on bulk and porous silicon; Nanoscale Research Letters 2013, 8.85 8 pages; A.Bandarenka S.Pris-chepa R.Fittipaldi A.Vecchione P.Nenzi M. Balucani, V. Bondarenko
• Transparent Conductive Coatings Made by Electrochemical and Physicochemical Methods; Digest Int. Conf. “Display Week-2013”, Vancouver, Canada, May 2013; A. Smirnov, A.Stsiapanau Y. Mukha, V. Mazaeva, V.Belyaev
• New concept for the design, synthesis and application of nanostructured anisotropic materials and conductive and alignment coatings for high efficient displays and photonic devices; Int. Conf. “EuroDisplay-2013”, London, UK, September 2013; V. Bezborodov, S. Mikhalyonok, I. Zharski, O.Dormeshkin A.Smirnov A.Stsiapanau


The BELERA team worked hard on the scientific and technical part linked to the three (3) Research topics A) Magnetic properties of carbon nanotubes, B) Emission properties of carbon nanotube based cold cathodes, and C) Nanostructured materials for novel photonic devices. They took advantages of twinning visits in Belarus and Europe as well as training activities to led joint research and obtained this impressive number of S&T results/findings. The BELERA project aimed at stimulating exchange between BSUIR and its European counterparts but the BELERA consortium overtakes the project goals and obtained excellent results.

Potential Impact:
The BELERA project succeeded in reinforcing research cooperation and twinning activities between the Belarusian State University of Informatics and Radioelectronics (BSUIR) and the European partners (UPVLC, CNRS, BUW and Innoveo) in the field of carbon nanotubes and photonics research. BSUIR and the European partners implemented a whole lot of joint experiments and exchange of knowledge while promoting the BELERA project and disseminate its results.

The project’s final results demonstrated that a durable research cooperation had been established between the partners, as well as between BSUIR and further EU research organisations. The project contributed to the RTD capacity building of BSUIR, the enhancement of Belarusian participation in European Framework Programme and the increase of BSUIR’s visibility in Europe leading to linkages and networking with successful European research organisations.

Within the framework of the BELERA project the consortium partners contributed to the preparation of promotional materials to target the carbon nanotubes and photonics research communities, as well as the public. The following materials have been prepared in order to raise the impact of the project:
i) Project leaflet and poster
ii) PowerPoint presentation of the project
iii) Project website frequently updated and fed with news articles and downloadable documents (e.g. belera.org)
iv) Four newsletters have been prepared and disseminated through different channels (e.g. project website, mailshot campaign, distribution of hard copies during events, etc.)
v) 'Promotion brochure about BSUIR' presenting the different department of BSUIR dealing with carbon nanotubes and photonics research
vi) 'Promotion Guide featuring 20+ Belarusian nanoelectronics and photonics R&T groups' promoting other Belarusian research groups involved in carbon nanotubes and photonics research. This Promotion Guide is helping the Belarusian research institutions to increase their visibility in Europe.
vii) Preparation of the ' Feasibility Study for a Nanoelectronics and Nanophotonics Technology Platform' in Belarus. The aim of this study was to analyse existing nanoelectronics technology platforms in Europe and across the World, as well as assessing the current context in Belarus in order to adapt the best practices identified. This study impacts the entire carbon nanotubes and photonics research community in Belarus.

Within the BELERA project, BSUIR organised several workshops and one international conference involving BSUIR's staff but also other Belarusian research institutions involved in carbon nanotubes and photonics research. This project events favour the dissemination of project results as well as the overall impact of the BELERA project; they consisted in the following:
• 1st Workshop on Research Topic A: “Ion, laser beams and magnetization measurements as probes for solid state nanostructures characterization and modification”; 16-18 October 2012
• 2nd Workshop on Research Topic B: "Emission properties of carbon nanotube based cold cathodes"; 30 May 2013
• 3rd Workshop on Research Topic C: "Nanostructured materials for novel photonic devices"; 30 May 2013

During the BELERA project, the consortium partners participated in many international events where they promoted BSUIR and disseminated the BELERA project results. More than 200 leaflets and 50 brochures were distributed among participants.

In addition to this promotion and dissemination activities, the consortium supported the participation of BSUIR in new RTD projects in order to get more funding and develop new cooperation in Europe. The following proposals have been supported:
BSUIR and BUW supported the application of A. Tymoschik to the grant FP7 Marie Curie 'International Incoming Fellowship' with a deadline the 14th of August 2013. Unfortunately the proposal was not enough advanced to submit it to the current call but efforts will be valorised under the Horizon 2020 programme.
BSUIR signed a contract with the Chinese Institute of Electromagnenic Compatibility to perform joint activities. In the framework of this contract BSUIR will have grant to send scientists at BUW for few months in order to test samples.
BSUIR and CNRS successfully submitted a successful application under the Belarusian Republican Foundation for Fundamental Research. The project started in July 2013 and will last for 2 years. Also BSUIR and CNRS are discussing possibilities to offer a Postdoctoral position to I. Komissarov at CNRS.
BSUIR and UPVLC already collaborated on the joint proposal SENSMIR submitted to the FP7 Programme. They will re-submit the proposal idea to the forthcoming programme Horizon 2020.
Innoveo supported BSUIR to complete contract negotiations and consortium agreement negotiations for the FP7 NANOMAT-EPC (608906) project. The project started the 1st November 2013 and will last for 2 years. Within the project, BSUIR undertakes a pilot project with the Luxembourgish SME CleanCarb entitled “Deployment of hybrid CNT/graphene electrodes for supercapacitors”.

List of Websites:
http://belera.org/