Programul Operational Sectorial „Cresterea Competitivitatii Economice”
„Investitii pentru viitorul dumneavoastra”

Proiect de modernizare a infrastructurii de cercetare
"Centru Euro-Regional de Studii al Materialelor Avansate, a Suprafetelor si Interfetelor"
- acronim CEUREMAVSU;
„Proiect cofinantat prin Fondul European de Dezvoltare Regionala”
Pentru informatii detaliate despre celelalte programe cofinantate de Uniunea Europeana, va invitam sa vizitati www.fonduri-ue.ro

- proiect nr. 141 finantat de Programul Operational Sectorial "Cresterea Competitivitatii Economice";

- Axa II: Competitivitate prin cercetare, dezvoltare tehnologica si inovare

- Operatiunea 2.2.1: Dezvoltarea infrastructurii C-D existente si crearea de noi infrastructuri C-D (laboratoare, centre de cercetare).

- Valoare totala de 43.004.595 lei

- perioada 1 martie 2009 - 28 februarie 2011
Beneficiar: Institutul National de Cercetare-Dezvoltare pentru Fizica Materialelor (INCDFM) Magurele
General
Description

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The POS-CCE Project of the National Institute of Materials Physics: four months to its end. Status report

C.M. Teodorescu, POS-CCE Project Manager

The POS-CCE project of the National Institute of Materials Physics Bucharest-Magurele, entitled "Euro-Regional Centre for Studies of Advanced Materials, Surfaces and Interfaces" (CEUREMAVSU, SMIS code 2665) started on 1st March 2009 and will end on 28th February 2011. The Project was mainly dedicated to the purchase of new equipment. Up to now, all the foreseen acquisitions are subject to contracts already signed. The complete situation of the acquisitions is listed in Table 1.

Table 1. List of foreseen acquisitions (exceeding 100,000 EUR estimated price) purchased through the CEUREMAVSU Project. Note that the intended number of such acquisitions was 18, therefore the number of equipments exceeded the intended one.

1OT = Open tender, DN = Direct negotiation
2S = Signed contract, D = delivered, I = installed, R = scientific results already produced

There are actually seven PhD students in areas connected with the new equipments: Dragoi Cristina, George-Adrian Lungu, Marius Adrian Husanu, Ana-Maria Lepadatu, Nedelcu Liviu Nicoleta Georgiana Gheorghe and Roxana Radu (of a total of 15 intended*). Also, there are to dat 26 new jobs created of Research Assistants (24 intended*): A.M. Lepadatu, A. Velea, N.G. Gheorghe, T. Popescu, M. Scocioreanu, I. Simandan, I.S. Ghita, F.C. Dragoi, I. Dumitrescu, I. Gontia, M. Galatanu, J.N. Barascu, I. Smaranda, C. Jinga, A. Ibanescu, C. Florica, B. Ostahie, C. Palade, S. Sandu, I. Arghir, I.C. Radu, D. Popescu, I. Mihalache, R. Damian, E. Busuioc, S. Busuioc. Three young post-docs regained the Romanian scientific community at NIMP through RP Projects: Ruxandra Maria Costescu, Lucian Dragos Filip, Corneliu Florin Miclea. The infrastructure purchased through the Project allowed the successful participation to 8 international cooperative projects up to now, including a large-scale FP7 integrated project.

___________________________________________________________________________
* The reference period for these figures is the Project's duration (2009-2011) and the forthcoming five years (2011-2016 )

„Continutul acestui material nu reprezinta în mod obligatoriu pozitia oficiala a Uniunii Europene sau a Guvernului României”

Status report of the Surface and Interface Science facility in the National Institute of Materials Physics after one year of operation
C.M. Teodorescu, Head of the Nanoscale Condensed Matter Physics Department
The surface and interface science facility in the National Institute of Materials Physics (see the Figure below), commissioned in September 2009, has achieved one year of almost uninterrupted operation. During this very first year of operation, around 23 different themes were tackled, some of them resulting in papers already published or submitted. The following paragraphs offer more detailed information about the scientific output, the economic impact and the manpower issues related to this new facility.

Figure: The experimental setup of the first Romanian complex surface and interface science cluster
Scientific output:

Published papers to date:

1. Mesoporous Tin-Triflate Based Catalysts for Transesterification of Sunflower Oil, M. Verziu, J. El Haskouri, D. Beltran, P. Amoros, D. Macovei, N.G. Gheorghe, C.M. Teodorescu, S.M. Coman, V. I. Parvulescu, Top. Catal. 53, 763-772 (2010).
2. Chemical Imaging of Catalyst Deactivation during Biomass Conversion Processes: The Etherification of Biomass-based Alcohols with Alkenes over H-Beta Zeolites, A.N. Parvulescu, D. Mores, E. Stavitski, C.M. Teodorescu, P.C.A. Bruijnincx, R.J.M. Klein Gebbink and B.M. Weckhuysen, J. Amer. Chem. Soc. 132, 10429-10439 (2010).
3. Thermodynamic destabilization of Li-N-H system by Si addition, P. Palade, G.A. Lungu, A.M. Husanu, J. Alloys Compnds. 505, 343-347 (2010).
4. Structural investigations of Ge nanoparticles embedded in an amorphous SiO2 matrix, I. Stavarache, A.M. Lepadatu, N.G. Gheorghe, R.M. Costescu, G. Stan, D. Marcov, A. Slav, G. Iordache, T.F. Stoica, V. Iancu, V.S. Teodorescu, C.M. Teodorescu, M.L. Ciurea, J. Nanopart. Res., accepted (2010).
5. One-Pot Synthesis of Menthol Catalyzed by a Highly Diastereoselective Ionic Gold/MgF2 Catalyst,  A. Negoi, S. Wuttke, E. Kemnitz, D. Macovei, C. M. Teodorescu, V.I. Parvulescu, S.M. Coman, Angew. Chem. Intl. Ed., accepted DOI: 10.1002/anie.201002090(2010).
6. Novel Pd heterogeneous catalysts for cycloisomerisation of acetylenic carboxylic acids, F. Neatu, L. Protesescu, M. Florea, V.I. Parvulescu, C.M. Teodorescu, N. Apostol, P.Y. Toullec, V. Michelet, Green Chemistry, accepted (2010).
7. Reactivity, magnetism and local atomic structure in ferromagnetic Fe layers deposited on Si(001),
N.G. Gheorghe, M.A. Husanu, G.A. Lungu, R.M. Costescu, D. Macovei, C.M. Teodorescu, phys. stat. sol. (a), corrected version submitted (2010).
8. Epitaxial ferromagnetic SmSi synthesized on Si(001), R.M. Costescu, N.G. Gheorghe, M.A. Husanu, G.A. Lungu, D. Macovei, I. Pintilie, C.M. Teodorescu, Phys. Rev. B., submitted (2010).
9. Substrate-target distance dependence of structural and optical properties in case of Pb(Zr,Ti)O3
films obtained by Pulsed Laser Deposition, A.C. Galca, V. Stancu, M.A. Husanu, C. Dragoi, N.G. Gheorghe, L. Trupina, M. Enculescu, E. Vasile, Appl. Surf. Sci., submitted (2010).

Other 3-5 papers are now in advanced stage of preparation.

Economic impact: An economic contract with the National Institute of Lasers, Plasma and Radiation Physics (Dr. Cristian P. Lungu) was carried out in order to investigate by depth profiling XPS multilayers of Be/W, Be/C, Be/Al2O3/W of interest for the forthcoming nuclear fusion facilities in the framework of the Euratom project. Another economic contract was signed with the National Institute of Isotopic and Molecular Technologies Cluj-Napoca for synthesising and in situ characterizing of Au layers of interest for molecular and biomolecular adsorption.

Manpower issues:

A team of four young researchers crystallized around this new setup and of the in-charge scientist, Dr. Cristian-Mihail Teodorescu, 44, Senior Researcher 1, actually Head of the Nanoscale Condensed Matter Physics Department, and around Dr. Dan Macovei, 63, Senior Researcher 1, former head of the group of Structure and Thin Films:
1. Dr. Ruxandra Maria Costescu, 33, Senior Researcher 3, came into the group in March 2010 from the Leibniz Institute for Solid State and Materials Research Dresden. In July 2010 she succeded with an RP grant to further develop the MBE setup with an annex chamber for III-V semiconductor epitaxy.
1. Marius Adrian Husanu, 29, Researcher, came into the group in January 2009. He is supposed to defend his PhD thesis in December 2010.
2. George Adrian Lungu, 32, Research Assistant, completely reformulated his PhD work centred on the new setup, dealing with magnetism of low dimensional systems (surfaces and interfaces)
3. Nicoleta Georgiana Gheorghe, 25, Research Assistant, was temporary hired in the group from January 2009 and successful won a permanent position in April 2009. She started a PhD work on mesoporous materials investigated by X-ray absorption and X-ray photoelectron spectroscopies.
            There are also two technicians in the group. Two new positions of Research Assistants will be fulfilled in the group during the forthcoming 3-4 months. The group will therefore have 10 members and will become one of the most powerful research teams in Romania.

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Photoemission electron microscopy (PEEM) and Low-energy electron microscopy (LEEM) at the National Institute of Materials Physics Bucharest-Magurele

C.M. Teodorescu, POS-CCE Project Manager

In the framework of the POS-CCE project of the National Institute of Materials Physics Bucharest-Magurele, entitled "Euro-Regional Centre for Studies of Advanced Materials, Surfaces and Interfaces" (CEUREMAVSU, SMIS code 2665) a new setup for photoemission electron microscopy (PEEM) and low-energy electron microscopy (LEEM) was delivered and installed by the manufacturer Specs GmbH, Germany, at the National Institute of Materials Physics Bucharest-Magurele (Fig. 1). The original setup is described in Ref. [1].
            This setup is amongst the four existing actually in Europe, and one of the two operational ones, the other being installed at the synchrotron radiation facility Bessy II, Berlin-Adlershof (Germany). It consititutes a guarantee of high impact forthcoming results, see Refs. [2-4]. It allows the following techniques:
A. In the PEEM mode:
a) Photoelectron emission microscopy with a spatial resolution of about 10 nm (Fig. 2); this technique allows simultaneous imaging of structures at the nanoscale by using a non-destructive technique (the sample is illuminated with UV light instead of being bombarded by electrons).
b) Energy-dispersive PEEM with an energy resolution of 0.25 eV. This technique allows: (i) band mapping of separate nanocrystallites; (ii) element-specific nano-spectroscopy of shallow core levels. Photon energies as high as 21.2 eV (He I) or 40.8 eV (He II) may be used for primary excitation.

Figure 1. Images of the LEEM-PEEM setup during the training programme

B. In the LEEM mode:
a) Low-energy electron microscopy with a spatial resolution of 4.1 nm.
b) Low-energy electron difraction and microdiffraction (<< 1 mm).
c) Low-energy electron microscopy in the dark field mode (spatial resolution of 5 nm). An example of this technique is illustrated in Fig. 3. One of the c(2 x 1) spots of the surface reconstruction of Si(001) and backtransformed in real space; this technique allows the direct visualisation of domains presenting this specific reconstruction.

C. Other techniques:
a) Mirror electron microscopy (MEM);
b) Phase contrast imaging;
c) Reflectivity contrast imaging.
The setup was delivered with a load-lock chamber and with facilities for sample preparation (flashing at very high temperatures in UHV). There are possibilities of recording spectacular movies of the surface dynamics at the nanoscale with all the above mentioned techniques.

Figure 2. PEEM images using a Xe lamp of a nanostructure fabricated by e-beam nanolitography. From left to right, the field of view (FOV) was: 196 mm, 60.3 mm, 60.3 mm, 33.3 mm, and 16.8 mm.

Figure 3. Dark-field LEEM images on a Si(001) c(2 x 1) spot. The field of view (FOV) is 3 mm.

References:

[1] R.M.Tromp, M. Mankos, M.C. Reuter, A.W. Ellis, and M. Copel, A New and Improved Low Energy Electron Microscope, Surface Review and Letters 5, 1189 (1998).
[2] F. M. Ross, R. M. Tromp and M. C. Reuter, Transition states between pyramids and domes during Si/Ge island growth, Science 286, 1931 (1999).
[3] F.-J. Meyer zu Heringdorf, M.C. Reuter and R.M. Tromp, Growth Dynamics of Pentacene Thin Films, Nature 412, 517 (2001).
[4] W.L. Yang, J.D. Fabbri, T.M. Wilet, J.R.I. Lee, J.E. Dahl, R.M.K. Carlson, P.R. Schreiner, A.A. Fokin, B.A. Tkachenko, N.A. Fokina, W. Meevasana, N. Mannella, K. Tanaka, X.J. Zhou, T. van Buuren, M.A. Kelly, Z. Hussain, N.A. Melosh, and Z.X. Shen, Monochromatic electron photoemission from diamondoid monolayers, Science 316, 1460 (2007).

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Advanced measurement facilities in microwaves and millimeter waves

in National Institute of Materials Physics, Bucharest-Magurele, Romania

In the framework of the POS-CCE Axis II project entitled “Euro-Regional Centre for Studies of Advanced Materials, Surfaces and Interfaces” (CEUREMAVSU), beneficiary the National Institute of Materials Physics, new equipment was installed for characterization materials and devices in microwave and millimeter wave frequency range.

1. The main piece of the equipment is the Agilent PNA-X N5245A Vector Network Analyzer shown in Fig. 1, which is equipped with 4-ports, dual source, internal combiner and mechanical switches, extended power range and bias-tees, frequency offset and added IF inputs for antenna and millimeter wave characterization.

Fig. 1. The Agilent N5245A PNA-X Vector Network Analyzer
The Microsoft Windows operating system installed on the PNA-X allows a friendly management of applications and data.
The system allows several types of measurements:

1. S parameters (magnitude and phase) in frequency domain
2. Nonlinear component characterization
3. Nonlinear X-parameter
4. Time domain measurements

As standalone, the PNA-X operates in the 10 MHz to 50 GHz frequency range. However, the N5261A 2-Port Millimeter – wave Test Set Controller and the millimeter-wave head modules (220-325 GHz and 325-500 GHz) shown in Fig. 2, extend the measurement frequency range towards much higher frequencies. With the millimeter-wave transmitter – receiver head modules, already existing in the institute, the full frequency range for microwave and millimeter-wave characterization is
10 MHz – 500 GHz.
The accuracy of the measured data is assured by the adequate calibration with an coaxial electronic calibration module (10 MHz to 67 GHz) and waveguide calibration kit for each frequency band of the millimeter-wave heads.
The nonlinear measurement capabilities of the system allows characterization of nonlinear materials (such as ferroelectrics and multiferroics) and nonlinear devices.
Accurate dielectric material characterization can be carried out by using Agilent 85072A split cylinder resonator. This completes the continuous measurements methods (in coaxial line or rectangular waveguide) already existent in the institute. Such accessories as wide-band horn antennas and very high performance broadband pyramidal absorbers (ECCOSORB VHP-8-NRL from Emerson & Cuming) are used for antenna and material characterization by using free-space method in millimeter-waves.

Fig. 2. Millimeter wave Test heads for calibrated measurements
(magnitude and phase) up to 500 GHz.

Dr.M.G.Banciu, Dr.A.Ioachim
National Institute of Materials Physics, Atomistilor 105bis, 077125 Magurele ,Ilfov, Romania

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Surface Science Facility

in National Institute R&D of Materials Physics, Bucharest-Magurele, Romania

This presentation aims at promoting a new research area in Romania: surface science. Researches in this area have interdisciplinary character, "including all interfaces between solid bodies, polymers, biomaterials, nanostructures, soft matter, liquids, gases and/or vacuum" (definition taken from the site of the journal Surface Science [1]). Surface science is an actual very high interest area, as demonstrated by the following Table, representing searches performed on the Thomson ISI Web of Science on July 14th, 2008, concerning only 2008 publications.

One may observe that, with the exception of broad areas implying everything related to applications, to electricity, mechanics, and bio- systems, surface science lies in a top position, even above everything related to physics, chemistry, quantum phenomena, and theory.
The 2007 Nobel prizes for Physics and Chemistry were awarded to Albert Fert for the discovery of giant magnetoresistance, respectively to Gerhard Ertl, for his studies on chemical processes at surfaces of solid bodies. Fert's most popular article (over 3600 citations) reports the results of the investigation of Fe(001)/Cr(001) superlattices, prepared by surface science methods [2]. Ertl's career is tightly connected to surface science (~ 160 papers in Surface Science, including the most cited one [3]).
The Romanian scientific community could not lie outside this highly interesting area. Recently, a new setup (see the Photos attached) was comissioned in the National Institute of Materials Physics for preparation and complex characterization of surfaces and interfaces. It consists mainly in three units, the Molecular Beam Epitaxy (MBE) chamber, the Scanning Tunneling Microscopy (STM) chamber, and the spin- and angle-resolved photoelectron spectroscopy (SARPES) chamber. Additional chambers are the load-lock for sample introduction and a sample preparation and storage facility (SPS). All four chambers: MBE, SPS, STM and SARPES operate in ultrahigh vacuum (UHV), base pressure 1-2 x 10-10 mbar. The techniques employed are:

In the MBE chamber:
a) preparation facilities:
- sample heating up to 1200 °C; cooling down to 77 K;
- evaporation from a 4-target e-beam evaporator;
- evaporation from a high temperature (2000 °C);
- controlled gas adsorption and desorption;
- monitoring of thicknesses using a quartz microbalance.
b) in situ characterization:
- LEED (Low Energy Electron Diffraction)
- RHEED (Reflection High Energy Electron Spectroscopy)
- AES (Auger Electron Spectroscopy)
- Quadrupole Mass Spectroscopy (thermal induced desorption, photodesorption)

In the STM chamber:
- sample preparation stage (heating, ion sputtering);
- tip preparation (ion sputtering);
- variable temperature (77 - 453 K) scanning tunneling microscopy;
- scanning tunneling spectroscopy (STS).

In the SARPES chamber:
- conventional X-ray photoelectron spectroscopy using a dual (Al/Mg Ka) anode;
- high resolution XPS using a monochromatized dual (Al  Ka /Ag La) source;
- ultraviolet photoelectron spectroscopy (UPS);
- angle-resolved XPS: X-ray photoelectron diffraction (XPD);
- angle-resolved UPS (ARUPS): band structure, Fermi surface, etc.;
- spin-resolved UPS: spin-polarized density of states;
- angle- and spin-resolved UPS: spin-polarized band structure;
- programmable ion sputtering: depth profiling;
- flood gun for sample neutralization;
- electron gun for AES.

            Since the commissioning, requests from external users to beneficiate of this national multi-technique facility increases exponentially. In two months of operation of the MBE chamber alone, two papers were written and submitted to ISI journals. The first paper including XPS results was sent to Topics in Catalysis just the day after the comissioning of the SARPES.
The SARPES facility was integrally supported from the infrastructure POS-CCE Project of NIMP "Euro-Regional Centre for Advanced Materials, for Surfaces and Interfaces", Project-No. 141/2009, acronym CEUREMAVSU.

    Cristian-Mihail Teodorescu

 National Institute R&D of Materials Physics, Atomistilor 105b, 077125 Magurele-Ilfov, Romania

References
[1] http://www.elsevier.com/wps/find/journaldescription.cws_home/505676/description.
[2] M.N. Baibich et al., Phys. Rev. Lett. 61, 2472 (1988).
[3] K. Christmann et al., Surf. Science 54, 365 (1976).

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Advanced technique for advanced materials
in National Institute R&D of Materials Physics, Bucharest- Magurele, Romania

As a part of the project 141 POS CCE Axis II, project financed by the European Commission and aiming at creating an euro-regional center for studying advanced materials, surfaces and interfaces , beneficiary National Institute of Materials Physics, a near field microscope/microspectrometer was installed. The near-field scanning optical micro-photoluminescence spectrometer is a new kind of micro-spectrometer for observation of photoluminescence and fluorescence spectra at sub-wavelength high-spatial resolution. Spectra and spectrally resolved mapped images can be obtained from single semiconductor quantum dots and wires at better than 100 nm spatial resolution. Metals, semiconductors, plastics and biological materials can be examined and sample preparation is unnecessary.
Images can be generated by both topographically (optical contrast and probe feedback) and PL emission spectral mapping from the near-UV to NIR wavelength range. The microscope can actually  map a sample within the area of a single spot with high spectral resolution.
The computer-controlled optics integrates the scanning probe, laser and spectrometer / detector in a complete, stand-alone system. Peltier cooled CCD detector allows rapid instrument start-up and high sensitivity. The system allows also ultra-low temperature (~5 K) being the first commercial helium cryostat equipped NSOM system. The aperture fiber probe near-field system allows various optical arrangements for illuminating and collecting the light from the sample. High-throughput probes with a range of apertures are available as standard.
Specifications
Optical System
Aperture probe scanning near-field optical micro-spectrometer.  Integrated instrument includes probe system, illumination optics (including laser source), single or dual switchable-grating Raman spectrometer with Rayleigh rejection holographic notch-filter and cooled CCD detector.
Optical system allows computer (software) switchable illumination, collection, and illumination - collection modes.
Probes
Optical fibre probes produced by chemical etching, with a range of standard tip apertures available. Illumination apertures of 100, 200, 300, 400 and 500 nm
Excitation laser
A variety of laser sources, e.g. diode (785 nm), He-Ne (632.8 nm), Nd-YAG / SHG (532 nm) can be used with the system. At this moment a 100 mW, green light 532 nm laser is available.
Spectrometer / Detector
The detector employs a dual, software-switchable grating spectrometer  allowing dual-resolution modes or optimal matching of excitation laser to the grating dispersion. Standard holographic grating for 532 nm excitation has 1,800 gr / mm with 600 gr / mm available.
The microspectrometer represents a technique complementary to the existing ones ranging from optical spectroscopy to electron microscopy and X ray diffraction. Besides the traditional Academia partners of the institute, the infrastructure is available to high tech enterprises, which aim at high added value production. The infrastructure is backed up by personnel with high qualification and with the necessary scientific and technique expertise.
Dr. Ionut Enculescu
National Institute of Materials Physics, Atomistilor 105b, 077125 Magurele-Ilfov, Romania

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 Complex system for electrical characterization
in the National Institute of Materials Physics, Bucharest- Magurele, Romania

The experimental system developed in the last years serves to measure magneto-transport, electrical, electro-optical, photoelectric, ferroelectric and microwave properties, as well as to determine the main characteristics of the electrically active defects generated during the growth, implantation, processing or irradiation of the materials and test devices.

Two Janis cryostats, each with 4 optical windows: one for the temperature range from 20K to 475 K; the other for the temperature range between 77K and 800K. Both cryostats are connected to turbo-molecular vacuum pumps.

Gratting Monochromator Oriel, wavelengths 200-6000 nm, with chopper for modulating UV-Vis-NIR light up to 1 kHz, for photoelectric signal measurements.

Keithley electrometers (2) with incorporated sources for voltages up to 1000 V, allowing to measure currents as low as 10 fA.

Agilent and Hioki RC bridges for capacitance measurements in the frequency range from      20 Hz  to 5 MHz.

Probe-station CPX-VFequipped with4 probe arms, each with 3-axis adjustments and      ±5° theta planarization, and a 25 kOe vertical field superconducting magnet. The temperature range for the probe station is from 4.2 K to 400 K and the measuring frequencies from DC to 67 GHz. The system can operate with external equipment, such as oscilloscopes, RC bridges, electrometers, etc.

TF Analyzer 2000for measuring properties of non-linear dielectrics such as: Hysteresis, Fatigue, Retention, Static hysteresis, Imprint, Leakage current. The system can operate with external equipment, such as oscilloscopes, temperature units, probing stations, high voltage amplifiers, etc.
The last two characterization facilities were purchased in 2009 and were fully supported from the infrastructure POS-CCE Project of NIMP "Euro-Regional Centre for Advanced Materials, for Surfaces and Interfaces", Project-No. 141/2009, acronym CEUREMAVSU.

HERA-DLTS HE-1030 and TSC Systems for detection and characterization of electrically active defects in materials and structures. The electrically active defects generated during the growth, implantation, processing or irradiation are those with direct impact on the electrical properties of the materials, multilayer structures and complex devices. Their detection and characterization is essential for improving the growth and processing technologies. The system is sensitive to defects generated in concentration down to 108 cm-3 and it is a unique facility in Romania. The HERA-DLTS HE-1030 system was installed in 2009 and was fully supported from the Core program contract 45N/2009.
Dr. Ioana Pintilie
         National Institute of Materials Physics, Atomistilor 105b, 077125 Magurele-Ilfov, Romania

„Continutul acestui material nu reprezinta în mod obligatoriu pozitia oficiala a Uniunii Europene sau a Guvernului României”

UNIUNEA EUROPEANA	GUVERNUL ROMNIEI	Instrumente Structurale