Accueil > Plateformes > Microscopie électronique avancée > Le super TEM : Aberration-corrected ARM 200F Cold-FEG Microscope


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The recent development of the aberration correctors and highly coherent electron sources has boosted the impact of electron microscopy on the characterization of matter at the atomic scale. Indeed, the last generation of instruments attains picometer-order spatial resolution, with an energy resolution of tenth of an eV. Both, high resolution imaging and analytical microscopy have enormously benefited from these technological advances, resulting in enhanced structural and chemical analysis of nanomaterials. Here we describe the performances and main results of the Super TEM : a JEOL ARM 80 – 200 kV microscope, employing a Cold FEG and two aberration-correctors for the objective and condenser lens systems. The Super TEM was installed for the first time, in September 2011 at Paris Diderot University. In 2014, in situ sample holders were implemented on the super TEM, offering unprecedented perspectives to study nanomaterials in liquid and gaseous environments at the atomic scale. The STEM corrector were installed in 2019 with high solid-angle EDX detectors.
This new generation of instrument is open to the scientific community through the Paris Diderot University Platform and the METSA national network.



Size dependent reactivity of gold nanocatalysts under hydrogen

(a) HR STEM images showing a phase transition in sub-3 nm gold nanoparticles under hydrogen while Sup-3 nm nanoparticles remain stable.

Revealing Size Dependent Structural Transitions in Supported Gold Nanoparticles in Hydrogen at Atmospheric Pressure
A. Nassereddine, Q. Wang, D. Loffreda, C. Ricolleau, D. Alloyeau, C. Louis, L. Delannoy, J. Nelayah and H. Guesmi
Small 17, 2104571 (2021)

Temperature effects on the nucleation & growth of gold nanoparticles in water

(a) Time-lapse STEM images showing nucleation and growth of gold nanoparticles at 25°C and 85°C. Scale bar is 1 µm on all images.

Quantitative In Situ Visualization of Thermal Effects on the Formation of Gold Nanocrystals in Solution
A. Khelfa, J. Nelayah, H. Amara, G. Wang, C. Ricolleau, D. Alloyeau
Advanced Materials 33 (38), 2102514, 2021

Growth mechanisms of Au@Ag nanorods from the bench-scale down to the single nanoparticle level

(a) Time-lapse STEM images showing the anisotropic deposition of silver on a gold bipyramid in aqueous media. Scale bar is 50 nm on all images. (b) Contour plots of the AuAg rods extracted every second from image analysis

Real-Time In Situ Observations Reveal a Double Role for Ascorbic Acid in the Anisotropic Growth of Silver on Gold
Kinanti Aliyah, Jieli Lyu, Claire Goldmann, Thomas Bizien,Cyrille Hamon, Damien Alloyeau, Doru Constantin
J. Phys. Chem. Lett. 2020, 11, 2830-2837

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Nucleation and growth of nanopores in hexagonal Boron Nitride

Reconciling theoretical and experimental studies on the growth mechanisms of nanopores in h-BN

Quantitative insights into the growth mechanisms of nanopores in hexagonal boron nitride
Ouafi Mouhoub, Rafael Martinez-Gordillo, Jaysen Nelayah, Guillaume Wang, Ji-Hoon Park, Ki Kang Kim, Young Hee Lee, Christophe Bichara, Annick Loiseau, Christian Ricolleau, Hakim Amara, Damien Alloyeau
Physical Review Materials 4, 014005 (2020)

Reavealing the biodegradation mechanisms of gold nanoparticles in vivo

TEM image of a lysosome in which injected and degraded gold nanoparticles are identified. The degradation products are made up of gold crystals measuring 2 nm in diameter self-organized in nanoleaves

Unexpected intracellular biodegradation and recrystallization of gold nanoparticles
Alice Balfourier, Nathalie Luciani, Guillaume Wang, Gerald Lelong, Ovidiu Ersen, Abdelali Khelfa, Damien Alloyeau, Florence Gazeau and Florent Carn
PNAS 2019

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Probing the dynamics of nanocatalysts at atmospheric pressure

octahedron-to round morphology transition of Au nanoparticles under O2 at atmospheric pressure

Reshaping Dynamics of Gold Nanoparticles under H2 and O2 at Atmospheric Pressure
Adrian Chmielewski, Jun Meng, Beien Zhu, Yi Gao, Hazar Guesmi, Hélène Prunier, Damien Alloyeau, Guillaume Wang, Catherine Louis, Laurent Delannoy, Pavel Afanasiev, Christian Ricolleau, Jaysen Nelayah
ACS Nano 13, 2024-2033

Measuring the surface energy of nanoalloys with in situ heating TEM experiments

Evaporation of CuAu3 Nanoparticles at 750°C with time. The variation of nanoparticle radii allows calculating their surface energies

Direct Measurement of the Surface Energy of Bimetallic Nanoparticles : Evidence of Vegard’s Rulelike Dependence
A. Chmielewski, J. Nelayah, H. Amara, J. Creuze, D. Alloyeau, G. Wang, C. Ricolleau
Phys. Rev. Lett. 120, 025901

Visualizing the dynamics of extracellular vesicles

Extracellular vesicles observed directly in cell-buffer with nanometer resolution by liquid-cell TEM

Monitoring the dynamics of cell-derived extracellular vesicles at the nanoscale by liquid-cell transmission electron microscopy
M. Piffoux, N. Ahmad, J. Nelayah, C. Wilhelm A. Silva, F. Gazeau, D. Alloyeau Nanoscale 10, 1234 - 1244

Exploring the formation of gold nanostar

Formation of a gold Nanostar followed by Liquid cell TEM showing the transformation of an icosahedral seed into a well symmetric nanostar with 20 arms induced by dimethylamine molecules.

Exploring the Formation of Symmetric Gold Nanostars by Liquid-Cell Transmission Electron Microscopy
Nabeel Ahmad, Guillaume Wang, Jaysen Nelayah, Christian Ricolleau, and Damien Alloyeau
Nano Lett. 17 (7), 4194–4201

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Monitoring the oxidative transformations of carbon nanotubes as a guideline for understanding their biodegradation in macrophages

Degradation of a multi-walled carbon nanotube (MWCNT) induced by hydroxyl radicals studied at the nanoscale by using liquid STEM imaging. Iron-oxide nanoparticles encapsulated inside the MWCNT are liberated after the rupture of the tubes, illustrating the potential of biodegradable MWCNTs for drug delivery applications.

Carbon Nanotube Degradation in Macrophages : Live Nanoscale Monitoring and Understanding of Biological Pathway
Dan Elgrabli, Walid Dachraoui, Cécilia Ménard-Moyon, Xiao Jie Liu, Dominique Bégin, Sylvie Bégin-Colin, Alberto Bianco, Florence Gazeau, and Damien Alloyeau
ACS Nano, DOI : 10.1021/acsnano.5b03708

Following the growth mechanisms of gold nanoplates in liquid

In situ liquid STEM characterization of the growth of 2D gold nanoparticles

Unravelling Kinetic and Thermodynamic Effects on the Growth of Gold Nanoplates by Liquid Transmission Electron Microscopy
Damien Alloyeau, Walid Dachraoui, Yasir Javed, Hannen Belkahla, Guillaume Wang, Hélène Lecoq, Souad Ammar, Ovidiu Ersen, Andreas Wisnet, Florence Gazeau, and Christian Ricolleau
Nano Letters 15, 2574−2581

Growth of Cu nanorods

3D structural analysis of Cu Nanorods with a 2-fold symmetry by using electron tomography and diffraction

Original Anisotropic Growth Mode of Copper Nanorods by Vapor Phase Deposition
H Prunier, C Ricolleau, J Nelayah, G Wang, D Alloyeau
Crystal Growth & Design 14 (12), 6350-6356

Discovering a new phase diagram in AuPd nanoalloys

Ultra HRTEM images of L10 Au–Pd nanoparticles

Long-range chemical orders in Au–Pd nanoparticles revealed by aberration-corrected electron microscopy
J Nelayah, NT Nguyen, D Alloyeau, GY Wang, C Ricolleau
Nanoscale 6 (17), 10423-10430

Monitoring at high resolution the biodegradation of iron oxyde nanocubes in vivo

High resolution electron microscopy follow-up of the degradation of iron oxide nanocubes in intracellular lysosomes extracted from the spleen of mice 14 days after in vivo injection (left picture). The structural analysis on the right picture allows identifying the atomic structure of the injected nanocubes (white frame) and the ferritin protein (red frame)

Biodegradation of iron oxide nanocubes : high-resolution in situ monitoring
Lénaic Lartigue, Damien Alloyeau, Jelena Kolosnjaj-Tabi, Yasir Javed, Pablo Guardia, Andreas Riedinger, Christine Péchoux, Teresa Pellegrino, Claire Wilhelm, Florence Gazeau
ACS nano 7 (5), 3939-3952

Gold nanoshield against the biodegradation of magnetic nanoparticles

Bragg filltered high resolution images of iron oxide NFs (in red) covered by a gold
layer (in green) deposited by PLD technique. The nominal thickness of the gold layer is (a) 3 nm, isolated cluster are formed, (b) 5 nm, a percolated fi lm is formed and (c) 7 nm, acontinuous layer is formed.

Biodegradation Mechanisms of Iron Oxide Monocrystalline Nanoflowers and Tunable Shield Effect of Gold Coating
Yasir Javed, Lénaic Lartigue, Pierre Hugounenq, Quoc Lam Vuong, Yves Gossuin, Rana Bazzi, Claire Wilhelm, Christian Ricolleau, Florence Gazeau, Damien Alloyeau

Detection and chemical analysis of single atoms diffusing on a surface using aberration corrected HRTEM

HRTEM images of CoPt nanoparticles. Individual Co and Pt atoms coming from beam induced Ostwald ripening, appear as additional black contrast on the carbon substrate. Signal to noise ratio (SNR) measured between the two corresponding arrows in the HRTEM image for both Co and Pt atoms : (1) SNR profile showing two Co atoms (SNR of –2.32). (2-3) SNR profiles showing one Pt atom (SNR of –3.59).

Following Ostwald ripening in nanoalloys by high-resolution imaging with single-atom chemical sensitivity
D. Alloyeau, T. Oikawa, J. Nelayah, G. Wang, C. Ricolleau
Applied Physics Letters. 101, 121920

Aberration-corrected HRTEM study of 2D materials

HRTEM image of single layer graphene acquired at 80 kV.

Synthesis of graphene by cobalt-catalyzed decomposition of methane in plasma-enhanced CVD : Optimization of experimental parameters with Taguchi method
H-A Mehedi, B Baudrillart, D Alloyeau, O Mouhoub, C Ricolleau, VD Pham, C Chacon, A Gicquel, J Lagoute, S Farhat
Journal of Applied Physics, 120 (6), 065304(1-11)

Determination of the iron valence state in iron oxide nanostructures by EELS fine structure

Comparison of (a) the Fe L2,3-edge and (b) the O K-edge electron energy-loss near-edge structures of a-Fe2O3 (plain lines) and FeO (black dots). The pre-edge background for each edge has been subtracted using a power-law function. The contribution from transitions to the continuum states has not been removed.

Performances of an 80 – 200 kV microscope employing a cold-FEG and an aberration-corrected objective lens
C. Ricolleau, J. Nelayah, T. Oikawa, Y. Kohno, N. Braidy, G. Wang, F. Hue and D. Alloyeau
Journal of Electron Microscopy doi : 10.1093/jmicro/dfs072

Mapping of surface plasmon resonance in nanoalloys

(a) HAADF image of a dimer of Au3Cu nanocubes. The red dots indicate five distinct positions at which spatially-resolved EEL spectra were acquired on the dimer (b) Comparison of the five spectra acquired at the positions indicated in (a). The energy resolution of the microscope allows us to detect the hybridized surface plasmon resonances associated to the interparticles interactions.

High resolution imaging and spectroscopy using Cs corrected TEM with cold FEG JEM-ARM 200F
C. Ricolleau, J. Nelayah, T. Oikawa, Y. Kohno, N. Braidy, G. Wang, F. Hue and D. Alloyeau
Jeol News, 47, 2-8

Magneto-structural studies of iron-oxide nanoflowers

Three-dimensional analysis of the Multi-Cores maghemite nanoparticles by bright-field TEM tomography. Bright-field
images acquired with a tilt angle of (A) -60, (B) 0, and (C) -60-. (D) Three-dimensional representation of the particles
(tomogram). Two-dimensional slices extracted from the tomogram : (E) 2D slice parallel to the substrate, corresponding to the
blue (x,y) plane in the 3D representation ; (F) 2D slice perpendicular to the substrate, corresponding to the blue (y,z) plane in
the 3D representation.

Cooperative Organization in Iron Oxide Multi-Core Nanoparticles Potentiates their Efficiency as Heating Mediators and MRI Contrast Agents
Lenaic Lartigue, Pierre Hugounenq, Damien Alloyeau, Sarah P Clarke, Michael Levy, Jean-Claude Bacri, Rana Bazzi, Dermot F Brougham, Claire Wilhelm, Florence Gazeau
ACS Nano 6, 10935

Spatial and energy resolutions

(a) Measured zero-loss peaks in various emission current (IE) conditions measured at 200 kV. The energy spread was defined by
FWHM of the zero-loss peak. (b) Energy spread as a function of emission current measured at 200 kV (red and 80 kV (blue).

(a) Young’s fringes pattern obtained at 200 kV showing a point resolution of 75 pm. (b) Fast fourier transformation of a
high-resolution image obtained at 200 kV on a (100) gold single crystal. The observation of the [048] peak of the gold crystal highlights that
the lattice resolution of the microscope is below 50 pm (d048 = 0.046 nm). (c) Young’s fringes pattern obtained at 80 kV showing a point
resolution of 80 pm.

Performances of an 80 – 200 kV microscope employing a cold-FEG and an aberration-corrected objective lens
C. Ricolleau, J. Nelayah, T. Oikawa, Y. Kohno, N. Braidy, G. Wang, F. Hue and D. Alloyeau
Journal of Electron Microscopy doi : 10.1093/jmicro/dfs072