Tomography - 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:

Technical University Cluj-Napoca (Prof. Dr. Traian PETRISOR)
National Institute Of Materials Physics (Dr. Valentin TEODORESCU)
Accent Pro 2000 S.R.L. (Dr. Mihai IOVEA)

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)

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)

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

Scientific report 2006 (Romanian)

Stage 2 - 2007:	Complex numerical modelling (physics, mechanics, imaging), scanning configuration and tomographic reconstruction configuration calibration. Realization of tomographic subsystems.

Scientific report 2007 (Romanian)

Stage 4 - Sept 2008:

Laboratory setup for submicronic digital radiography.
Fabrication of TEM tomograph subsystems.

Scientific report June 2008 (Romanian)

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

Scientific report Sept 2008 (Romanian)

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. 24^th 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, 8^th 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
.
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, 24^th Symposium on Fusion Technology, 15-19 Sept. 2008, Rostock, Germany.

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