ceex
NIMETIM - Nano/Micro-Scale Imaging And Metrology By Electron And X-Ray 3-D Tomography Of Innovative Materials 
Project CEEX 06-D11-23/2006-2008
 

 

PROJECT MANAGER: Dr. Ion TISEANU, e-mail: tiseanu@infim.ro

PROJECT DURATION: 2006-2008

PROJECT COORDINATOR: National Institute For Lasers Plasma And Radiation Physics

 

PARTNERS:

 

 

 

 

MAIN OBJECTIVES:

 

  •  Development of sub-micron X-ray quantitative tomography techniques; design and fabrication of a nanoCT facility; development of standards for performances assessment of sub-micron spatial resolution tomography facility.

  •  Extension of the functionality of the TEM facility to 3D tomography with spatial resolution of tens of nanometres for polymeric composites and mesoporous materials.

  •  Advanced modelling (physics, mechanics, imaging) of new laminographic/tomographic scanning configurations.

  •  Application of the newly developed methods and instruments to the characterization of advanced materials and devices (superconductors, biomaterials, ceramics, nano/microelectronic devices, etc.).

  •  Build-up of a high-performance imagery laboratory network for a wide range of applications, implying a broad range of compositions, dimensions and spatial resolutions (<20 nm / ~500 nm / ~10 µm / >300 µm)
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    The tomographic investigation capabilities to be reached are quantified in the following table:

     

    Items

    Main specifications for current X-ray microtomography configuration

    Main specifications to be reached at the end of the project for X-ray nanotomography

    X-ray source

    Max. high voltage: 160 kVp
    Max power: 20 W
    Feature recognition: ~ 5 µm

    Maximum high voltage: 160 kVp
    Maximum power: 15 W
    Feature recognition: ~ 300 nm

    Detector elements

    768 x 576 image intensifier (XII)
    1248 x 1248 a-Si flat panel

    Same + 2048 x 2048 camera, 25 µm/pixel

    Digital Output

    10 bits XII, 12 bits a-Si

    Same + 16 bits XII

    Effective Area of Detector

    169x169 mm2 XII, 120x120 mm2 a-Si

     

    Micrometric manipulator

    X stage

     

    Z stage

    θ stage

    Sample fine adjustment

     

     

    travel 500mm, loading cap. 30kg

     

    travel 300mm, loading capacity 6kg

    accuracy 0.03°, loading cap. 20kg

    -

     

     

     

    travel 800mm, loading capacity 30kg

    travel 1200mm, loading capacity 50kg

    travel 300mm, loading capacity 6kg

    accuracy 0.02°, loading capacity 30kg

    accuracy 10µm, repeatability 5µm,

    loading capacity 2kg

    Magnification Factor

    < 1000

    < 2000

    Spatial Resolution

    aprox. 10µm

    ≥500 nm

    Scanning Time

    < 15min. (720 angles)

    < 15min. (720 angles)

    3D Reconstruction Time

    < 2min. (256x256, 256 lines)
    < 20min. (1024x1024, 512 lines)

    < 30min. (2048x2048, 1024lines)

    Scaning Method

    Cone beam CT
    Full scan (360deg.)

    Cone beam CT
    Short Scan (180deg.+1/2 fan angle)
    Oblique View Cone Beam

     

    Main characteristics of the electron tomography
    that will be developed in this project

    Microscope

    TEM Jeol 200CX

    Detector

    CCD camera 2048x2048 pixels

    Goniometer range

    ±60°, 120 projection angles

    Magnification factor

    104-105

    Spatial resolution

    aprox. 10-20 nm

    Reconstruction methods

    FBP, Maximum Entropy, ART

    3D reconstruction time

    < 30min. (volume 512x512x512 voxels)

    Stage 1 - 2006:  Sub-micron imaging of advanced materials

    Stage 2 - 2007: Complex numerical modelling (physics, mechanics, imaging), scanning configuration and tomographic reconstruction configuration calibration. Realization of tomographic subsystems.
     
    Stage 4 - Sept 2008: Laboratory setup for submicronic digital radiography.
    Fabrication of TEM tomograph subsystems.

    Stage 4 - Sept 2008:  Nano/micro electron and X-ray tomography - experimental validation.

     

    Final report (English)

     

    Publications:

    Journals:

    • I. Tiseanu, T. Craciunescu, T. Petrisor, A. della Corte. 3D X-ray micro-tomography for modeling of NB3SN multifilamentary superconducting wires. Fusion Engineering and Design, 82, p. 1447–1453, 2007

    • T. Kai, N. Okada, M. Baba, T. Takahashi, M. Misawa, I. Tiseanu, N. Ichikawa, Structure of effective catalyst layers around bubbles in a fluidized catalyst bed, Chemical Engineering Journal 130(2007)119-124.

    • Augieri, G. Celentano, L. Ciontea, V. Galluzzi, U. Gambardella, J. Halbritter, T. Petrisor, A. Rufoloni, A. Vannozzi, Angular properties of pure and Ca-substituted YBa2Cu3O7-δ Superconducting thin films grown on SrTiO3 and CeO2 buffered Al2O3 substrates, Physica C: Superconductivity and its Applications Volume 460-462 II, Issue SPEC. ISS., 1 September 2007, Pages 829-830

    • N. Pompeo, E. Silva, R. Marcon, V. Galluzzi, G. Celentano, A. Augieri, T. Petrisor,  Microwave properties of YBa2Cu3O7-δ films with BaZrO3 nanoinclusions, Physica C: Superconductivity and its Applications, Volume 460-462 I, Issue SPEC. ISS., 1 September 2007, Pages 412-413

    • Vannozzi, A. Augieri, G. Celentano, L. Ciontea, F. Fabbri, V. Galluzzi, U. Gambardella, A. Mancini, T. Petrisor, A. Rufoloni, Cube textured substrates for YBCO coated conductors: Influence of initial grain size and strain conditions during tape rolling, IEEE Transactions on Applied Superconductivity, 17-2(2007) 3436-3439

    • V. Galluzzi, A. Augieri, L. Ciontea, G. Celentano, F. Fabbri, U. Gambardella, A. Mancini, T. Petrisor, N. Pompeo, A. Rufoloni, E. Silva, A. Vannozzi, YBa2Cu3O7-δ films with BaZrO3 inclusions for strong-pinning in superconducting films on single crystal substrate, IEEE Transactions on Applied Superconductivity 17-2(2007)3628-3631.

    • G. Augieri, G. Celentano, U. Gambardella, J. Halbritter, T. Petrisor,  Analysis of angular dependence of pinning mechanisms on Ca-substituted YBa2Cu3O7-δ epitaxial thin films, Superconductor Science and Technology 20-4(2007) 381-385

    • I. Tiseanu, T. Craciunescu, G. V. Aldica, M. Iovea. X-ray micro-tomography as a tool for quantitative characterization of advanced materials manufacturing processes. Advanced Materials Research, 47-50, pp. 698-701, 2008.

    • Gh. V. Aldica, P. Nita, I. Tiseanu, T. Craciunescu, P. Badica. High density MgB2 superconductor: structure and SEM investigations. Journal of Optoelectronics and Advanced Materials, 4, pp. 929 - 932, 2008.

    • A. Barau, V. Budarin,  A. Caragheorgheopol, R. Luque,  D.J. Macquarrie, A. Prelle, V. S. Teodorescu, M. Zaharescu, A Simple and Efficient Route to Active and Dispersed Silica Supported Palladium Nanoparticles, Catalysis Letters, 2008, 124:204–214, DOI 10.1007/s10562-008-9465-x

    • I. Tiseanu, T. Craciunescu, Assessment of the Aplicability of X-Ray Tomography for Irradiated Samples, in curs de publicare in Fusion Engineering and Design

    •  P. Badica, G. Aldica, T. Craciunescu, I. Tiseanu, Y. Ma, K. Togano, Microstructure of MgB2 samples observed through X-ray Microtomography, in curs de publicare in Superconducting Science and Technology

     
    Conferences:

    • I. Tiseanu, T. Craciunescu, T. Petrisor, A. della Corte. 3D X-ray micro-tomography for modeling of NB3SN multifilamentary superconducting wires. 24th Symposium on Fusion Technology, 11-15 Sept. 2006, Varsovia, Polonia

    • Gh.V. Aldica, P. Nita, I. Tiseanu, T. Craciunescu, P. Badica, High Density MgB2 Superconductor: Structure and Morphology through Microtomography and SEM Investigations, 5th International Conference, “New Research Trends In Material Science”, ARM-5, Sibiu, Romania, 5 – 7September, 2007

    • I. Tiseanu, T. Craciunescu, X-ray Microtomography Experience at National Institute for Laser, Plasma and Radiation Physics, Bucharest, Romania, Prezenata la Fachtagung Prozessnahe Röntgenanalytik Berlin, Germany, 15-16 November 2007

    • M. Simon, I. Tiseanu, C. Sauerwein, S.-M. Yoo, I.-S. Cho, Development of multi sensor and multi source computed tomography Systems,  DIR 2007 - International Symposium on Digital industrial Radiology and Computed Tomography, June 25-27, 2007, Lyon, France

    • M. Simon, I. Tiseanu, C. Sauerwein: Characterization of Automotive Parts by a Novel Multi-Scan Tomography System, 4th International Conference Emerging Technologies in Non-Destructive Testing, April 2-4, 2007, Stuttgart, Germany.

    • L. Ciontea, G. Celentano, A. Augieri, T. Ristoiu , R. Suciu,  M. S. Gabor, A. Rufoloni, A Vannozzi, V Galluzzi, T Petrisor, Chemically  Processed  BaZrO3 Nanopowders as Artificial Pinning Centres, 8th European Conference on Applied Superconductivity, EUCAS’07 Bruxelles 16-20 September 2007.

    • L. Ciontea, A. Angrisani, G. Celentano, T. Petrisor jr., A. Rufoloni, A. Vannozzi, A. Augieri, V. Galuzzi, A. Mancini, T. Petrisor,  Metal Propionate Synthesis of Epitaxial YBa2Cu3O7-x Films, Prezentata la  8th European Conference on Applied Superconductivity, EUCAS’07 Bruxelles 16-20 September 2007

    • Gh.V. Aldica, P. Nita, I. Tiseanu, T. Craciunescu, P. Badica, X-ray micro-tomography as a tool for quantitative characterization of advanced materials manufacturing processes, "International Conference on Multi-functional Materials and Structures” 28-31July 2008, Hong Kong SAR, China
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    • I. Tiseanu, T. Craciunescu, P. Badica, G.V. Aldica, M. Rindfleisch, Characterization of Superconducting Wires by Cone-Beam  Micro-Tomography, acceptata pentru prezentare la IEEE 2008Workshop on X-Ray Micro Imaging of Materials, Devices, and Organisms, 22-24 October 2008 Dresden, Germany

    •  M. Iovea, O.Duliu, G.Mateiasi, M. Neagu, M. Mangu, I. Tiseanu, T. Craciunescu, Preliminary experiments for X-Ray dual-energy Micro-Tomography quantitative analysis.

    • Badica, G. Aldica, T. Craciunescu, I. Tiseanu, Y. Ma, K. Togano, Microstructure of MgB2 samples observed through X-ray Microtomography, acceptata pentru prezentare la IEEE 2008 Workshop on X-Ray Micro Imaging of Materials, Devices, and Organisms, 22-24 October 2008 Dresden, Germany

    •  M. Iovea, G.Mateiasi, M. Neagu, M. Mangu, O. Duliu, I. Tiseanu, T. Craciunescu, Materials microanalysis technique by dual-energy X-ray Tomography and Radioscopy, NDT 2008 15-18 September, Shrigley Hall Hotel, Nr Macclesfield, Cheshire, UK

    •  I. Tiseanu, T. Craciunescu, Assessment of the Aplicability of X-Ray Tomography for Irradiated Samples, 24th Symposium on Fusion Technology, 15-19 Sept. 2008, Rostock, Germany.

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