National Institute Of Materials Physics - Romania

Atomic Structures and Defects in Advanced Materials Laboratory

TEM: Main




Introduction Equipment Techniques Results


Introduction

The Electron Microscopy facilities in our lab include two TEMs, an SEM-FIB dual system and a fully equipped room for specimen preparation.

Among the two TEMs, JEOL 200CX is used for conventional analytical TEM investigations and JEM ARM 200F for high-resolution analytical TEM investigations including HRTEM, STEM, EELS, EDS, EFTEM.

The TESCAN Lyra 3 XMU SEM-FIB system TESCAN Lyra 3 XMU SEM-FIB is used for thin lamella preparations, but also for morphological, analytical and structural investigations via SEM, EDS and EBSD.

Investigation Possibilities:

  • Microstructural and morphological characterization of nanostructured materials (powders, nanowires), thin films, ceramics, alloys by TEM/HRTEM and SEM.
  • Structural characterization down to atomic resolution of extended defects in crystalline materials.
  • Characterization of strain fields associated with extended defects and interfaces.
  • Chemical elemental composition measurements by EDS and EELS.



Introduction Equipment Techniques Results


JEM ARM200F JEM 2100 TESCAN Lyra3 Specimen Preparation

JEM ARM 200F Configuration Specifications
Working modes: CTEM, HRTEM, STEM BF, STEM ADF, STEM HAADF, SAED, nano-ED, CBED, EDS, EELS, EFTEM, EELS-SI
  • FEG Field Emission Gun
  • STEM unit with CS-corrector
  • EDS Unit: JEOL JED-2300T
  • GIF (Gatan Image Filter): Gatan Quantum SE
  • CCD Cameras :
    • wide angle: Gatan Orius 200D
    • bottom mounted: Gatan Ultrascan 1000XP
    • GIF camera: Gatan Ultrascan 1000FT
  • Accelerating voltages: max. 200 kV
  • TEM magnification: 50 – 2 000 000 ×
  • TEM resolution: 0.19 nm
  • STEM magnification: 200 – 150 000 000 ×
  • STEM-HAADF resolution: 0.08 nm
  • EDS:
    • energy resolution EDS: 131,4 eV (Mn-Ka)
    • in TEM mode
    • in STEM mode: spot, line profile or 2D mapping
  • EELS – energy resolution 0.7 eV




Introduction Equipment Results


JEM ARM200F JEM 2100 TESCAN Lyra3 Specimen Preparation

JEM 2100 Configuration: Technical specifications:
Working modes: CTEM, HRTEM, STEM BF, STEM ADF, STEM HAADF, SAED, nano-ED, CBED, EDS
  • LaB6 Gun
  • STEM Unit
  • EDS Unit:
    • JEOL JED-2300T
    • with Dry SDD
    • detection area of 30 mm2
  • NanoMEGAS ASTAR system
  • CCD Camera: emSIS Tengra
  • Accelerating voltages: max. 200 kV
  • TEM magnification: 1 500 – 1 500 000 ×
  • TEM resolution:
    • 0.19 nm (UHR pole piece)
    • 0.25 nm (HT pole piece)
  • STEM magnification: 200 – 150 000 000 ×
  • STEM-HAADF resolution: 0.08 nm
  • EDS :
    • energy resolution EDS: 131,4 eV (Mn-Ka)
    • in TEM mode
    • in STEM mode: spot, line profile or 2D mapping




Introduction Equipment Results


JEM ARM200F JEM 2100 TESCAN Lyra3 Specimen Preparation

TESCAN Lyra3 Configuration: Technical specifications:
Working modes: SEM, FIB, EDS, SEM-FIB, SEM-EDS, EBSD, low vacuum mode
  • SEM: FEG Gun (0.2-30 kV)
  • Detectors: secondary electrons (SE), backscattered electrons (BE)
  • FIB: Ga ion source (0.5-30 kV / 2nA max)
  • Gas Insertion System: Pt
  • EDS: Viewfiels spectrum/ SEM mapping
  • EBSD: Bruker e-Flash 1000
  • nano-manipulator for TEM lamella extraction
  • wide range sample-stage
  • SEM resolution:
    • High Vacuum Mode: 1.2 nm at 30 kV
    • Low Vacuum Mode: 1.5 nm at 30 kV
  • FIB Resolution: 5 nm at 30 kV
  • EBSD acquisition/indexing rate (single phase):
    • acquisition: up to 880 patterns/s
    • indexing : up to 770 patterns/s




Introduction Equipment Techniques Results


JEM ARM200F JEM 2100 TESCAN Lyra3 Specimen Preparation

Specimen Preparation Machines:
  • Wire saw
  • Lapping machines
  • Zeiss Axio Observer reversed metallographic microscope for monitoring the thinning/polishing stages
  • Zeiss Stemi 2000 stereoscopic optical microscope for TEM specimen manipulation
  • Gatan PIPS ion milling installations
  • JEOL JEE 4C vacuum evaporator
  • Gatan ultrasound disc cutter
  • Gatan Dimple Grinder




Introduction Equipment Techniques Results


Techniques

Morphological and structural characterization:
Conventional TEM & SAED High resolution TEM/STEM
TEM Spectroscopy:
Energy Dispersive X-ray Spectroscopy (EDS) & Electron Energy Loss Spectroscopy (EELS) Electron Energy Loss Spectroscopy – Spectrum Imaging (EELS-SI)
Energy Dispersive X-ray Spectroscopy mapping Energy Filtered Transmission Electron Microscopy (EFTEM)




Introduction Equipment Techniques Results


Results

  1. A. Tamion; M. Hillenkamp; A. Hillion; V.A. Maraloiu; I.D. Vlaicu; M. Stefan; D. Ghica; H. Rositi; F. Chauveau; M.-G. Blanchin; M. Wiart; V. Dupuis; Ferritin surplus in mouse spleen 14 months after intravenous injection of iron oxide nanoparticles at clinical dose; Nano Research; 9 (8), 2398-2410 (2016)
  2. Scarisoreanu N.D, Craciun F., Birjega R., Ion V., Teodorescu V.S, Ghica C., Negrea R., Dinescu M.; Joining Chemical Pressure and Epitaxial Strain to Yield Y-doped BiFeO3 Thin Films with High Dielectric Response; Scientific Reports, 6 (2016)
  3. VA Maraloiu, F Appaix, A Broisat, D Le Guellec, VS Teodorescu, C Ghezzi, Bvd Sanden, MG Blanchin; Multiscale investigation of USPIO nanoparticles in atherosclerotic plaques and their catabolism and storage in vivo; Nanomedicine: Nanotechnology, Biology and Medicine 12 (1), 191-200 (2016)
  4. M. Stefan, D. Ghica, S. V. Nistor, A. V. Maraloiu, R. Plugaru; Mn2+ions distribution in doped sol–gel deposited ZnO films; Applied Surface Science; (2016); doi : 10.1016/j.apsusc.2016.02.167
  5. VS Teodorescu, AV Maraloiu, RF Negrea, D Ghica, ND Scarisoreanu, M Dinescu, M Gartner, M-G Blanchin, High atomic diffusivity during pulsed laser irradiation of TiON quasi-amorphous films, Applied Surface Science; 374, 248-251 (2016)
  6. Rusen E., Diacon A., Mocanu A., Gavrila R., Nistor L.C, Dinescu A.; CdSe (quantum dots)-graphene oxide system for thiophene polymerization: a new strategy, a new material; Rsc Advances, 6(30):25577-25583 (2016)
  7. Nistor S.V, Stefan M., Nistor L.C, Ghica D., Vlaicu I.; Distribution and interaction of Mn2+ ions incorporated in cubic ZnS quantum dots over a broad concentration range; Journal of Alloys and Compounds, 662:193-199 (2016)
  8. Rusen E., Diacon A., Mocanu A., Nistor L.C.; Novel facile method for obtaining CdSe/polyaniline/C-60 composite materials; Scientific Reports, 6 (2016)
  9. Trinca L., Galca A.C, Aldica G.V, Radu R., Mercioniu I., Pintilie L.; On the growth of conductive aluminum doped zinc oxide on 001 strontium titanate single crystals; Applied Surface Science, 364:365-370 (2016)
  10. Teodorescu, V. S. ; Ghica, C.; Maraloiu, A.V.; Vlaicu, M.; Kuncser, A.; Ciurea, M. L.; Stavarache, I.; Lepadatu, A. M.; Scarisoreanu, N.D.; Andrei, A.; Ion, V.; Dinescu, M.; Nanostructuring of GeTiO amorphous films by pulsed laser irradiation; BEILSTEIN JOURNAL OF NANOTECHNOLOGY; 6; 893-900 (2015)
  11. Rusen E., Mocanu A., Nistor L.C, Hudhomme P., Diacon A.; Anionic polymerization by an electron transfer process from a CdSe quantum dot-perylenediimide (PDI) system; Rsc Advances, 5:28228-28232 (2015)
  12. Negrea R.F, Teodorescu V.S, Ghica C.; Atomic scale elemental mapping of light elements in multilayered perovskite coatings. Applied Surface Science. 355:250-255 (2015)
  13. Acsente T., Negrea R.F, Nistor L.C, Logofatu C., Matei E., Birjega R., Grisolia C., Dinescu G; Synthesis of flower-like tungsten nanoparticles by magnetron sputtering combined with gas aggregation; European Physical Journal D. 69 (2015)
  14. Vajda K., Kasa Z., Dombi A., Nemeth Z., Kovacs G., Danciu V., Radu T., Ghica C., Baia L., Hernadi K. et al.; “Crystallographic” holes: new insights for a beneficial structural feature for photocatalytic applications; Nanoscale, 7:5776-5786 (2015)
  15. Ghica C., Negrea R.F, Nistor L.C, Chirila C., Pintilie L.; Nanoscale monoclinic domains in epitaxial SrRuO3 thin films deposited by pulsed laser deposition; Journal of Applied Physics, 116 (2014)
  16. Krishnan G., Negrea R.F, Ghica C., Brink G.H ten, Kooi B.J, Palasantzas G.; Synthesis and exceptional thermal stability of Mg-based bimetallic nanoparticles during hydrogenation; Nanoscale, 6:11963-11970 (2014)
  17. Rusen E., Mocanu A., Nistor L.C, Dinescu A., Calinescu L., Mustatea G., Voicu S.I, Andronescu C., Diacon A.; Design of Antimicrobial Membrane Based on Polymer Colloids/Multiwall Carbon Nanotubes Hybrid Material with Silver Nanoparticles; ACS Applied Materials & Interfaces, 6:17384-17393 (2014)

Introduction Equipment Techniques Results



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