National Institute for Research and Development of Isotopic and Molecular Technologies

ROMANA


INCREASE OF THE COMPETITIVENESS OF THE EXISTING ESR LABORATORY FROM

 

THE MULTIFUNCTIONAL AND NANOSTRUCTURED SYSTEMS DEPARTMENT, INCDTIM

 

CLUJ-NAPOCA, FOR THE APPLICATION IN THE KNOWLEDGE BASED ECONOMY

 

CAPACITIES  PROGRAM    nr. 127 CP/1 / 14.09.2007

RES

ESR Spectrometer facilities

          Objectives

          Activities

          Results

          Personal

          Impact

 





Objectives:

The general objective of this project is the modernization of the existing ESR laboratory from the multifunctional and nanostructured systems department, INCDTIM Cluj-Napoca.

   The modernization of the existing ESR laboratory will give rise to:

(i) development of CD activity at INCDTIM Cluj-Napoca, since it will permit the development of the subjects which could be touched inside the top level research on European and national stage. These subjects imply the development and the characterization of new materials and multifunctional products

(ii) certification of the  ESR laboratory in order to be able to produce specific services

(iii) increase of the quality and diversification in the educational area through the partnerships with the universities by means of the training programs in magnetic resonance domain

(iv) involving of the young specialists in the magnetic resonance area who will represent and important reservoir of high qualified personal

(v) setting up of a magnetic resonance research base with multiple users in the Northwest region.

   The specific objectives staggered on the project’s time schedule:

I. Acquisition of a last generation and highly performant electron spin resonance (ESR) spectrometer and the necessarily accessories

II. Testing the spectrometer capacities and bringing it to a proper use.

   The project’s goal is to enhance the competitiveness of the CDI activities in the magnetic resonance spectroscopy area through the new scientific infrastucture.

This fact will permit:

(i) a fast integration in the European research area and particularly the increase of the competitiveness in the priority scientific domain- Nanosciences and Nanotechnologies, the multifunctional materials
(ii)
implication in the most advanced experimental techniques of the magnetic resonance area
(iii) maximum valorification of the very qualified human potential existing in this area at INCDTIM Cluj-Napoca  

     
Activities:     

   

In correlation with the above specific objectives, we propose the following activities which could ensure their achievement:

I. Acquisition of a electron spin resonance (ESR) spectrometer.

A.1.  Fitting out of the ESR laboratory.

A.2.  Aquisition of the ESR spectrometer.

II. Testing the spectrometer capacities and bringing it to a proper use.

A.3.  Assembling, testing of the spectrometer and the training of the specialists.    

   The above activities imply the following issues:

A.1. - assurance of the utilities necesarily to the most propitious conditions for the scientific research by means of the prologement of the water and electricity facilities, voltage stabilization and the laboratory air conditioning.

A.2.- getting in touch with the enterprises  which build the spectrometers 

- setting up of the legal procedures for the international auction

- signing up of the contract 

       - aquisition and the transport of the spectrometer.

A.3. - reception of the ESR spectrometeer and of the accesories 

        - assembling and bringing the spectrometer in to a proper use- will be done by the specialized team from the enterprise

        - testing of the specified performance parameters- will be done by the specialized team from the enterprise

        - demonstration of the spectrometer capacities and setting up the preliminary  experimental measurements

        - training of the specialized persons from the laboratory who will perform the experiments- will be done by the specialized team from the enterprise



Backi

Results:

(i) development and the modernization of the CD infrastructure in the ESR

spectroscopy area         

(ii) creation of the new working places. Two young physicists will be hired in order to cover the necesarily scientific activities as a result of the spectrometer aquisition.   

(iii) increase of the research capacities.

It will be setted up new applied research research topics in accordance with the European tendencies such as: nanotechnologies and nanosciences, multifunctional materials (nanometrology, spin dynamics, magnetic and crystalline interactions, structural morphology in nanomaterials applied in nanoelectronics,multifunctional materials for the efficient conversion of the solar energy, polymeric nanocomposites for shieding and sensors), protection of the environement (cantitative and qualitative analysis of the pollution factors and resulted products from the accidental        irradiation), control of the food quality (ESR spectroscopy is a standard method recognize by European Commission for the quality control of irradiated products which are exported), medicine and biology (characterization of the covered magnetic nanoparticles with different surfactants for very high temperature and of the drugs as a result of the molecular encapsulation).

(Iv) increase of the international visibility. The existence of the new infrastructure will gives new opportunities for the international cooperations and in this way we can deeply imply in the european research projects. The goal is to get 100000 EUR/ year.

(v) increase od the efficiency in the CD activities – by means of the enlargement of the scientific subjects and the number of projects in which it will be possible to be implied. 

(vi) setting up of modern facilities for the training and the formation of young researchers. We will contribute to the practical education of the PhD students in the ESR spectroscopy, its aplications and the development of new specific methods.

(vii) setting up of a magnetic resonance research base with multiple users in the North-West region.

(viii) new knowledges, methods and experimental procedures.

(ix) studies, analysies, mesurements, testings– as resulting from the demands of productive sector and  industrial beneficiaries.

   Obtained results::

The main objective of the project is the increase of the competitiveness of the existing ESR laboratory from the multifunctional and nanostructured systems department, INCDTIM Cluj-Napoca, through the acquisition of a last generation and high performant ESR spectrometer.

1. Digital electronics

Hall field controller

  • Operating range 50 G – 20 kG
  • Field setting resolution of 24 bit
  • Number of points for field sweep from 2 to 120000
  • Sweep range 0 – 20 kG in one scan
  • Stability better than 10 mG/h
  • Fast field scans with 320 sec/points
High resolution NMR field measuring unit
  • 1 mG resolution
  • 1.5 – 15 kG range
  • Probe diameter not more than 6 mm
  • High speed field tracking of 500 G / sec
Lock-in detector and modulation amplifier
  • Modulation frequency range 80 Hz – 100 kHz, continuously variable
  • Signal detection with amplitude resolution of 24 bit
  • Signal detection bandwidth of 300 kHz
  • Detection of 1st and 2nd harmonic
  • Detection of in- and out-of-phase signal
  • Double modulation techniques
  • Time constant from 0.01 msec to 5 sec
  • Modulation amplifier compatible with all resonators in all frequency bands

Rapid field scan generator
  • Sweep width 200 G
  • Scan speed 0.5 msec to 5 sec
High speed detector with 500 ns time resolution

2. Microwave units

X-band microwave bridge
  • Operating range 9.2 – 9.9 GHz
  • Tune picture width 10 – 80 MHz with electronic zoom
  • 600 mW maximum power
  • 200 mW levelled power in full operating range
  • 60 dB power attenuation in 1 dB steps
  • Signal amplifier with at least 6 MHz bandwidth
  • Integrated frequency counter with 1 kHz resolution
X-band universal high-Q waveguide cavity
  • Compatible with Helium and Nitrogen VT systems
  • Optical grid with more than 50 % transmission
  • 10 mm sample access
  • Integrated modulation coils
  • Modulation amplitude up to 20 G
  • Automatic tuning
  • Modulation amplitude of up to 20 G at 100 kHz
  • Weak-pitch sensitivity of 3000 : 1
  • Absolute sensitivity of 109 spins/G
X-band dual mode resonator
  • Perpendicular mode for measuring allowed transitions
  • Parallel mode for measuring forbidden transitions
  • 10 mm sample access
  • Integrated modulation coils
  • Modulation amplitude up to 10 G
  • Automatic tuning
  • Compatible with Helium and Nitrogen VT systems
X-band resonator for temperatures up to 700 K
  • 10 mm sample access
  • Automatic tuning
  • Compatible with Helium and Nitrogen VT systems
Q-band microwave bridge
  • Operating frequency 34 GHz +,- 150 MHz
  • 50 MHz tune picture width
  • 100 mW maximum power
  • 60 dB power attenuation in 1 dB steps
  • Signal amplifier with 6 MHz bandwidth
Q-band cavity
  • 3 mm sample access
  • Variable frequency
  • Variable coupling
  • Integrated modulation coils
  • Modulation amplitude up to 20 G
  • Variable temperature 3.8 – 300 K, continuously
  • Compatible with Helium and Nitrogen VT systems
  • Weak-pitch sensitivity of 2000 : 1
  • Oxygen in air sensitivity of 200 : 1

3. Magnetic Field Units

  • Electro magnet
  • 72 mm air gap
  • Maximum field of 14 kG
  • Homogeneity of 10 mG at 3400 G in a volume of 10x10x20 mm3
  • Weight less than 1900 kg
  • Pole tips for maximum field of 17 kG at 56 mm air gap
  • Magnet power supply of stability class 10-6
  • Heat exchanger for magnet and power supply

4. Instrument Control Software

Software to control all instrument parameters
Data acquisition with the following modes:
  • Field sweep
  • Time sweep
  • Rapid scan
  • Power sweep
  • Temperature sweep
2-dimensional acquisition modes:
  • Field vs. time
  • Field vs. power
  • Field vs. temperature
  • Time vs. field
  • Field vs. goniometer angle
  • Rapid scan vs. time

5. Data Analysis Software

Spectrum processing
  • Integration with automatic baseline subtraction
  • Integral normalization
  • Filtered differentiation
  • Smoothing routines
  • Peak-picking with position and distance indication
  • g-factor transformation
  • P1/2 analysis of saturation curves
  • Spectrum algebra for add, subtract, multiply, divide
  • Line shape fit for derivative and absorption signals
  • Time constant fit
  • Spectrum transformation with stretch and shift function
  • Baseline correction with polynom and spline functions
  • Quick and easy cursor read-out of line position, line width, signal amplitudes and g-factor
  • Spectrum display as line, points, histogram, contour, stack-plot
  • Spectrum export as ASCII, post script, TIFF, JPEG, PDF
Spectrum Simulation
  • Simulation package for liquids, powers and single crystals
  • Isolated spins systems
  • Coupled spin systems
  • Simulation of parallel mode spectra
  • Unlimited number of electron and nuclear spins
  • Spectrum optimization
  • Multiple isotopes
  • Spectrum calculation based on exact matrix diagonalization.

6. Variable Temperature Equipment

  • Helium base VT system compatible with X- and Q-band resonators Temperature range 3.8 – 300 K
  • Nitrogen based VT system compatible with X- and Q-band resonators Temperature range 100 – 700 K

7. Further Possible System Extensions

Upgrade to X- and Q-band ENDOR
Upgrade with L-, S-, K- and W-Band Microwave Frequencies
Upgrade to Pulse-EPR, Pulse-ENDOR and Pulse-ELDOR



img1 img2
img3 img4
img5 img6
img8 img12
img9 img1 img1

Disemination:

Articles:

1. O.Raita, D.Toloman, A.Popa, M.Stan, Al.Darabont and L.M.Giurgiu
EPR INVESTIGATIONS OF Sn1-xFexO2 NANOPOWDERS
Journal of Physics, in press

2.A.Popa, M. Jivanescu, D Toloman, O. Raita, L. M. Giurgiu
FERROMAGNETIC RESONANCE MEASUREMENTS ON Co NANOWIRES
Journal of Physics, in press

3.D Toloman, A R Biris, A Popa, O Raita, L M Giurgiu, I Ardelean
RAMAN and EPR STUDIES OF CALCIUM-PHOSPHATE GLASSES DOPED WITH MANGANESE IONS
Journal of Physics, in press

Conferences:

1. Adriana POPA, Dana TOLOMAN, Oana RAITA, Manuela STAN, Alexandru DARABONT, Liviu GIURGIU
MAGNETIC RESONANCE INVESTIGATION OF Co2+ IONS IN NANOPARTICLES OF ZnO PREPARED IN Air AND Ar ATMOSPHERE
Procc. 10-th“ International Balkan Workshop on Applied Physics”, Constanta, p.90, (2009)

2.D.Toloman, A.R.Biris, A.Popa, O.Raita, L.M.Giurgiu, I.Ardelean
RAMAN and EPR STUDIES of xMnO(1-x)[1.5P2O5 CaO] GLASS SYSTEM
Procc. 10-th“ International Balkan Workshop on Applied Physics”, Constanta, p.89, (2009)

3. O.Raita, A.Popa, D.Toloman, Al.Darabont, M.Stan and L.M.Giurgiu
MAGNETIC RESONANCE INVESTIGATIONSOF Sn1-XFeXO2 NANOPOWDERS
Procc. 10-th“ International Balkan Workshop on Applied Physics”, Constanta, p.89, (2009)

 

Back

Personal:
 

 

 

Nr crt

Institution

Name

Scientific title

Atribute in the project

Age

1.

INCDTIM Cluj-Napoca

Dr. Liviu Mihail Giurgiu

CS I

Project Director

63

2.

INCDTIM Cluj-Napoca

Dr. Sorin Farcas

CS II

Responsable  for new equipments buying

62

3.

INCDTIM Cluj-Napoca

Dr. Adriana Paula Popa

CS III

Responsable for instalation the new equipment

31

4.

INCDTIM Cluj-Napoca

Dr. Oana Raita

CS III

Assistent  for instalation  and

Performing testing of the spectrometer

Laboratory certification

30

5.

INCDTIM Cluj-Napoca

Dr. Ovidiu Pana

CS I

Responsable for performing testing

53

6.

INCDTIM Cluj-Napoca

Drd. Dana Toloman

CS III

Asistent for Q-band instalation and Unit Endor

 

30

7.

INCDTIM Cluj-Napoca

Drd. Izabella Craciunescu

CS III

Asistent for instalation variable temperature unit

30



Back
Impact:

   
        The scientific impact related to the aquisition of the ESR spectrometer
consists of:

(i) facilitiy to be implied in the following new research domains in accordance with the European tendencies:

- characterization by ESR of the nanometrology in nanoparticles and magnetic/metallic nanowires

- characterization of the spin dynamics and magnetic/cristalline interactions in the nanomaterials applied in nanoelectronics, the efficient conversion of the solar energy and those specific to the photosynthesis process

- investigation of the morphology and the structure of the nanocomposites resulting from the molecular encapsulation of the drugs and covered magnetic nanoparticles used in very high temperature

(ii) realization for the first time in Romania of the following new applications:

- ESR experiments at high frequency/magnetic field  (Q-band).

 The investigations will be directed towards: (i) the elucidation and the separation of the inner core- outer shell effects which are characteristics to the magnetic naoparticles (ii) the increase of the precision of the nanometrological characterization of metallic/magnetic nanoparticles (iii) the spin dynamics characterization as function of frequency and temperature in the nanostructures applied to spintronics in order to improuve the specific properties of the electronic components in nano range (iv) the precise identification and the characterization of the dynamical properties of the paramagnetic centers which appear in the new multifunctional materials during identificarea precisa si  caracterizarea proprietatilor dinamice ale centrilor (produsilor de the process of the solar energy conversion in electricity. These results will be compared with thwe obtained ones in the frame of the bilateral and intergovernemental agreements with the Physical-Chemistry Institute from Stuttgart University and the magnetic resonance department from the Demokritos Institute, Athens, respectively.

(iii) the achievement of a portofolio for the applications of ESR spectroscopy. 

With respect to this, we intend to set up the new ESR methods applied in the material, environmental and food control areas targeting to:

- the evaluation of hte mean size of fine naoparticles

- the evaluation of the concentration of the paramagnetic ions

- the quantitative determination of the concentration of the pollution factors as carbonic particles, heavy metal ions and so on

- the determination of the free radical concentration in the irradiated foods in order to prolonge their validity  period.

Economical/social impact for the regional socio-economical development.

  The north-western development region is one of the relatively developed zone from Romania with a great economical potential and whose future priority of the development

consists of the utilization of the new technologies based on knowledge. It is characterized by a high-qualified manpower, the developed academic medium, the high potential for the research and qualified high schools. The statistics show that the number of researchers as compared with the total population is smaller than the corresponding one in the European countries and also in other regions of our country. Based on these facts, we consider that the proposed project frames in the priority referring to the enhancement of CDI potential of the northwestern region. Therefore, the investments in the modernization of the infrastructure in the CDI system represents a priority for this region since it could contribute to the stabilization of the highly qualified man power and to the stimulation of the creation of new industrial entities.