Structures and Properties

The Structures and Properties platform provides research groups with tools for characterising the physicochemical properties of materials developed in the laboratory. In addition to the maintenance and management of the instrumental equipment, its role is to provide real expertise in advanced characterisation techniques. The platform is also heavily involved in instrumental development projects under extreme conditions. The diversity of the characterisation instruments proposed allows the physico-chemical properties of matter to be probed from the macroscopic scale (magnetic, electrical, optical and mechanical properties) to the nanometric and atomic scales (structure of materials, imaging of magnetic fields on the nanometric scale, etc.). The experimental techniques used to characterise these properties call on skills in plasmonics, diffraction (X-rays and electrons) and radiation-matter interaction in the broad sense.

Sébastien Weber, leader

Departments

TEM, FIB & sample preparation 

The Transmission Electron Microscopy (TEM), Focused Ion Beam (FIB) and Sample Preparation department is composed of three complementary and inseparable entities: TEM/SEM sample preparation, FIB/SEM and TEM.

This service offers all users in the laboratory and also outside the laboratory the possibility of carrying out an in-depth study of a material by electron microscopy.

Our fields of activity:

– Classical preparation for TEM (thin section) and SEM (scanning electron microscopy)
– FIB preparation of localized thin sections
– Multi-scale imaging (Optical, SEM, TEM, HRTEM)
– Orientation and chemical mapping (EDSD, ASTAR, EDS, EELS)

Our strengths:

– Expertise in mechanical, electrolytic and ionic thinning
– Expertise in imaging, spectroscopy, diffraction
– Wide range of TEM holders for in situ observations (temperature, traction, multi-contact, …)
– Maintenance and training on all the department’s equipment
– External services (local, national, European…)

The sample preparation department is the essential activity that precedes electron microscopy observation. Conventional methods consist of surface polishing for scanning electron microscopy (SEM) observations, or thinning the samples to a few tens of nanometres thick for transmission electron microscopy (TEM) observations. However, sample preparation can become more exotic depending on the problem at hand.

The department provides the laboratory with numerous tools and different preparation techniques, which are taught to students and those wishing to be trained.

Whether conventional or more modern, sample preparation requires great precision, skill and patience on the part of the operator!

This department is composed of two members Catherine Crestou TCE CNRS (specialist in ion thinning) and Dominique Lamirault TCN ITRF (specialist in electrolytic jet thinning)

Ion beam thinning: GATAN PIPS Model 691

Plane view of a  BaTiO3 sample

Cross-section of a BaTiO3 sample

Electrolytic jet thinning: STRUERS TenuPol-5

Sample of a metal alloy on a copper grid

Cutting tools :

ONA AF25 wire EDM machine

ESCIL Well diamond wire saws

BUEHLER IsoMet 4000 saw

Mechanical thinning :

ESCIL 300GTL, 200GTL polishers

ALLIED Multiprep semi-automatic polisher

BUEHLER Phoenix 4000 polisher

BUEHLER vibratory polisher

VibroMet2 GATAN Grinder

SOUTH BAY TECHNOLOGY Tripod Polisher Model 590

GATAN Dimpler Grinder Model 656

The FIB/SEM dual beam systems consist of two microscopes: a SEM (Scanning Electron Microscope) column and a FIB (Focused Ion Beam) column. They allow the observation and abrasion of matter at the scale of ten nanometres. They can also accommodate numerous other pieces of equipment for depositing material (Pt, W, Au, C), moving objects or performing chemical or crystallographic analysis, always on a submicrometre scale.

We use these machines at CEMES to carry out numerous experiments on all types of materials: preparation of thin slides for transmission electron microscopy (TEM), EDS and EBSD analyses, etching of pillars and beams for in situ compression and bending tests, etching of stencil gratings on Si3N4 membranes, electrical contact by localised metal deposition, etc.

This department is composed of one person: Robin Cours, CNRS Research Engineer.

Helios NanoLab600i

Strengths: TEM thin foil preparation, EDS EBSD, MEB FEG analysis

  • SEM FEG column
  • FIB column: LMIS Ga source
  • Omniprobe micromanipulator
  • Five GIS (gas injection system): Pt, W, C, Co et O2
  • Detectors: SE, BSE, EBSD, EDS, STEM

Microscope Helios

Microscope Helios NanoLab600i

Zeiss CrossBeam 1540 XB

Strenghts: Electron lithography, SEM FEG

  • SEM FEG column
  • FIB column: LMIS Ga, AuGe or aussi sources
  • In a clean room
  • Raith electron lithography modul
  • Four GIS: Pt, W, XeF2, H2O
  • Micro-pinces Kleindieck micro clamps

Microscope Zeiss CrossBeam 1540

Installation of a carbon nanocone on an AFM cantilever head

Transmission electron microscopes (TEM) consist of an electron gun (source), electromagnetic lenses that act on the electron beam and various detectors. These detectors allow images to be obtained, diffraction images that provide information on the shape and structure of the sample, but also on its chemical composition or its mechanical, magnetic or electrical properties…. TEMs allow very local observation of materials (from a few µm2 to a few Å2). For the electron beam to pass through the sample, the latter must be very fine (of the order of 100nm).

There are 6 TEMs available for internal or external users at CEMES, 4 conventional (CM20, JEM2010, CM20FEG, HF2000) and 2 corrected for image mode aberrations (TECNAIF20 and HF3300 I2TEM). A very wide range of sample holders is also proposed in order to act in-situ (i.e. in the microscope) on the materials studied. It is then possible to orientate, heat, deform and apply fields to our samples in order to determine their intrinsic properties.

The department provides training for users who wish to become autonomous in all the techniques offered by the park (conventional imaging, parallel mode and precession diffraction, ASTAR, high resolution, STEM, EELS/EDX spectroscopy, EFTEM, etc.), and provides services in one of the techniques mentioned above.

The department is composed of two members: Sébastien Joulié, CNRS engineer in charge of the CM20, JEM2010 and TECNAIF20 microscopes, and Cécile Marcelot, CNRS engineer in charge of the CM20FEG, HF200 and I2TEM microscopes.

CM20 (200kV)

  • LaB6 thermionic gun
  • TEM/STEM
  • BF/DF detector
  • Homemade camera

Microscope CM20

Cobalt nano wires

JEOL 2010 (200kV)

Strengths: dark field, in situ video

  • LaB6 thermionic gun
  • High contrast pole piece
  • View III SYS camera

Microscope JEOL 2010

Dislocations in a nickel-base superalloy

CM20 FEG

Strengths: EDX spectroscopy, Astar precession

  • Schottky gun
  • TEM/STEM
  • BF/DF detector
  • Orius Gatan camera
  • EDX SDD Bruker detector
  • ASTAR NanoMegas precession

Microscope CM20 FEG

EDX mapping of a Al-Cu alloy

Orientation mapping of an iron oxide dendrite

TECNAI F20 (200kV)

Strengths: high resolution, EELS spectroscopy

  • Schottky gun
  • TEM/STEM
  • HAADF, BF/DF detector
  • Cs C-corr CEOS image corrector
  • Gatan camera
  • GIF Gatan

Microscope Tecnai F20

Fe3O4 nanoparticle

HF2000 (200kV)

  • Cold FEG gun
  • TEM/STEM
  • BF/DF detector
  • US1000 Gatan camera

Microscope HF2000

Growing of nano wires of Co on Al2O3

I2TEM (HF3300) 300kV

Strengths: electron holography, in operando, high resolution, EELS spectroscopy

  • Cold FEG gun
  • Double Stage (Normal, Lorentz)
  • Large gap objective pole pieces
  • B-corr CEOS image corrector
  • TEM/STEM
  • BF/DF detector
  • DDE K3 Gatan camera
  • Multibiprisms
  • Quantum Gatan GIF

Microscope I2TEM (HF3300)

Hologram on a  CoFe2O4 nano flower

Optics and Magnetism

The optics and magnetism department brings together all the laboratory’s experimental capabilities in optics and magnetism. It provides users inside and outside the laboratory with tools for characterising the optical/magnetic properties of materials. The optical part includes near- and far-field Raman spectroscopy devices as well as temporal measurement capabilities from femtosecond to millisecond. Spatial mapping of the properties measured on structured samples is available on all devices. The magnetism section includes macro- and microscopic Kerr magneto-optical, radio-frequency and magneto-transport measurements under cryostat.

The service’s devices are either directly accessible by users (after training) or in collaboration with the researchers who “set up” the device.

Sébastien Moyano, Frédéric Neumayer, Sébastien Weber (leader)

Microscope à Force Atomique couplé à un spectromètre Raman constituant notre TERS (Tip Enhanced Raman Spectrometer)

Atomic Force Microscope coupled to a Raman spectrometer constituting our TERS (Tip Enhanced Raman Spectrometer)

– Spectral analysis in reflectance, fluorescence and Raman emission

– UV, visible and near infrared analysis

– Micrometer resolution hyper-spectral mapping

– Nano tip excitation spectrometry: 10/20 nm resolution spectro-spatial mapping

– Fluorescence lifetime mapping: micrometer resolution and >100 picoseconds

– Pump-probe measurements of femtosecond/picosecond dynamics

– Non-linear microscopy

– Quantum plasmonics: single photon counting (intensity time correlation)

– Ultrafast Transmission Electron Microscopy, stationary and time-resolved cathodoluminescence (joint CNRS Hitachi laboratory: HC-IUMI)

– Broadband ferromagnetic resonance measurements (0-20 GHz) in stripline configuration

– Spin dynamics measurements on micro-antennas, by synchronous detection (field modulation), vector analysis (network analyser) or spectral analysis (spectrum analyser).

– Magnetometry and magneto-transport 0 – 9T, 2 – 400 K.  

 

Strenghts:

    • Development of computer interfaces for the control and automation of experimental devices (PyMoDAQ, fig. 2)
    • Development of test/prototype benches around spectroscopy and optics in general (e.g. fig. 3: Micro-MOKE)

Diagramme de fonctionnement de la librairie PyMoDAQ pour le contrôle de dispositifs expérimentaux et l'acquisition de données

Functional diagram of the PyMoDAQ library for the control of experimental devices and data acquisition

a) Micro-MOKE: Dispositif de caractérisation de l'aimantation sous microscope par effet MOKE (Magneto-optical Kerr Effect). b) Image de domaines magnétiques acquise en utilisant le Micro-MOKE et son logiciel sous PyMoDAQ.

a) Micro-MOKE: Device for characterising magnetisation under a microscope using the MOKE (Magneto-optical Kerr Effect).

b) Image of magnetic domains acquired using the Micro-MOKE and its software under PyMoDAQ.

The department has different types of lasers (continuous, pulsed, gas, solid-state…) used on the different experimental devices according to the needs as well as lasers attached to particular devices:

– Continuous, fixed and fibre-coupled lasers:

◦ Krypton [406-676 nm] emission on atomic lines

◦ Argon [457-514 nm] emission on atomic lines

◦ Titanium: Sapphire [700-1050 nm] tunable emission

Table optique (Spectro T64000) regroupant un ensemble de LASER à gaz (Argon, Krypton et solid-state : Ti-Sa). Ces sources peuvent être délivrée dans les différentes salles d’expérimentation par fibre optique

Optical table (Spectro T64000) with a set of gas LASERs (Argon, Krypton and solid-state: Ti-Sa). These sources can be delivered to the different experimental rooms by optical fibre.

  • – Mobile lasers:

    ◦ Super-continuum [450-2500 nm], [250-40000 kHz]

    ◦ DPSS diode @488nm

    ◦ Diode Continuous or pulsed lasers (20 picoseconds):

           ▪ Aurea: 405nm, 632nm, 785nm

           ▪ PicoQuant: 532nm, …

    ◦ Helium Neon

    ◦ …

  • – Horiba/Jobin Yvon T64000 Spectrometer. The most versatile spectrometer:

     Single monochromator or triple monochromator

     Near UV and visible range

     Arrays: 2400, 1800 and 150 rpm

     

    – Dilor UV Spectrometer

     Triple monochromator

     Laser: Ar [275-364 nm]

     Array: 2400 rpm

     

    – X-Plora Horiba/Jobin Yvon. The most used spectrometer

     Lasers: DPSS @ 532 nm, diode lasers @ 638 and 785 nm

     Arrays 2400, 1800, 600 and 300 rpm

     Reflection and transmission white lamps

     

    – TERS: Tip Enhanced Raman Spectrometer. Coupling of a LABRAM spectrometer, a TRIOS AFM and silver tips

     DPSS laser at 532nm and He:Ne at 632nm

     1800 and 300tr/mm gratings

     

    – FLIM: Fluorescence Life-time Imaging Spectrometer

     Uses pulsed diode lasers or fibre gas lasers

     Micrometric spatial and temporal resolution greater than 20 picoseconds

     Hyper-spectral or hyper-temporal mapping

     

    – Femtosecond bench

     Coherent Chameleon Ultra II femtosecond oscillator, 80 MHz, 100 fs, 680-1080 nm

     Frequency doubler/tripler

     Femtosecond time probe pump measurements in transmission or reflection

     Micrometric spatial resolution

     

    – FemtoTEM ultrafast electron microscope:

     Amplified femtosecond laser source Amplitude Satsuma systems, single shot to MHz, 20 uJ/pulse, 250 fs

     Electron imaging, EELS spectrum and time-resolved cathodoluminescence

  • Macro-MOKE
  • Micro-MOKE
  • PPMS
  • Radio-frequency
Characterisation

The Characterisation Department brings together several complementary activities with a single aim: to offer a multidisciplinary approach to the characterisation of materials. It has a very large number of instruments that enable it to explore numerous properties of materials such as those related to their interfaces, morphologies, mechanical or crystallographic characteristics. This equipment is complemented by various means of sample preparation, including a set of high-temperature furnaces (up to 1500°C).

The department offers its skills for both simple measurements and more in-depth studies of many types of materials, sometimes requiring instrumental and/or methodological development.  

It relies on the specific skills of its staff members: David Neumeyer, for granular materials and their characterizations, Christophe Deshayes for mechanical tests and scanning electron microscopy observations. The X-ray diffraction activity completes and extends the department’s means of investigation.

 A large part of the department’s equipment is accessible to users after theoretical and practical training in the techniques and interpretation of the results.

Contact : david.neumeyer@cemes.fr

Quelques exemples de moyens disponibles et résultats : a-1 et a-2 Diffractomètre Brucker Discover (2D), exemple de résultat obtenu pour une pâte de tesson poterie chinoise ancienne (Clément Hole) b-1 mésoporosité mesurée et c-1 à 3, Malvern NanoZS, poten-tiel Zeta et Phase Plot (Alumine commerciale – CE NanoDesk)

Some examples of available means and results: a-1 and a-2 Brucker Discover Diffractometer (2D), example of result obtained for an ancient Chinese pottery shard paste (Clément Hole) b-1 measured mesoporosity and c-1 to 3, Malvern NanoZS, Zeta potential and Phase Plot (Commercial Alumina – CE NanoDesk)

The strong development of techniques for the elaboration of granular materials (Spray Pyrolysis, CVD, Sol-Gel, etc.) has led to the joint development of specific powder characterisation means within CEMES.

Supported by more than two decades of activities within the framework of numerous collaborations, services or projects, concerning a great diversity of materials, the activity has been enriched by the experience acquired on the specificities linked to the understanding and implementation of divided materials.

It now offers access to various techniques, such as gas adsorption-desorption, dynamic light scattering, laser granulometry, spectrofluorescence, etc.

These techniques allow macroscopic access to various properties essential to the understanding of the behaviour of divided solids.

Combined with other techniques available within the CEMES platform, they allow very complete studies of powders and dispersions.

Contact : david.neumeyer@cemes.fr

Non-exhaustive list of available techniques:

– Gas adsorption/desorption (Nitrogen and Argon) (Belsorp)

– pHmeter chain (SI Analytics)

– Conductivity chain (

– UV-Visible spectrofluorometry (Hitachi)

– Pycnometry (Micromeritics)

– Laser granulometry (Malvern)

– Dynamic light scattering (DLS) (Malvern)

– Zeta potential (Malvern)

– ….

The department is equipped with two Bruker D8 diffractometers which allow complementary studies of crystallised materials. 

The first, the D8 Advance, is equipped with a copper source and a LynxEye detector (1D) in a Bragg-Brentano configuration. It is highly resolving and is suitable for phase identification and the study of refinement processes.

Contact : david.neumeyer@cemes.fr

The second, the D8 Discover, is equipped with a Cobalt micro source and a 2D detector. It is dedicated to stress and texture measurements as well as to the study of samples that do not have a flat surface.

Contact : christophe.deshayes@cemes.fr

The department is equipped with two mechanical testing machines:

– A 30 kN Zwick tensile machine used at room temperature to determine the strength and deformation behaviour of materials until failure.

– A high-temperature creep machine (up to 800°C) used, for example, to study aeronautical alloys such as TiAl.

Contact : christophe.deshayes@cemes.fr

[1] – Microstructure, Plasticity and Ductility of a TNM+ Alloy Densified by Spark Plasma Sintering -Michael Musi, Christophe Deshayes, Guy Molénat, Louise Toualbi, Benjamin Galy, Petra Spoerk-Erdely, Muriel Hantcherli, Jean-Philippe Monchoux, Marc Thomas, Helmut Clemens and Alain Couret*– 2022- https://doi.org/10.3390/met12111915

[2] – Remarkable corrosion resumption of archaeological bronzes, induced by the oxidation of ternary Cu-Sn-S phases in atmosphere, after long-term burial with sulfidesCéline Rémazeilles*, Véronique Langlet-Marzloff, Juan Creus, Guillaume Lotte, Christophe Deshayes, François Baleux, Luc Robbiola – 2020 – https://doi.org/10.1016/j.corsci.2020.108865

[3] – Simple and economic elaboration of high purity CaCO3 particles for bone graft applications using a spray pyrolysis techniqueDavid Neumeyer*, Chiara Venturini, Nicolas Ratel-Ramond, Marc Verelst and Andre Gourdon – 2017 – https://doi-org.inp.bib.cnrs.fr/10.1039/C7TB00586E

[4] – Influence of salts and humic acid on 2,4-dichlorophenoxyacetic acid removing from aqueous solution by peanut shell activated carbonJacques K. Fatombi*, Ignace Agani, Sèmiyou A. Osseni, Esta A. Idohou, David Neumeyer, Marc Verelst, Robert Mauricot, Taofiki Aminou – 2020 – https://doi.org/10.5004/dwt.2020.25597

[5] – Optimizing metal-support interphase for efficient fuel cell oxygen reduction reaction catalyst -Divya Nechiyil, Meenakshi Seshadhri Garapati, Rashmi Chandrabhan Shende, Sébastien Joulié, David Neumeyer, Revathi Bacsa, Pascal Puech, Sundara Ramaprabhu, Wolfgang Bacsa* – 2020 – https://doi.org/10.1016/j.jcis.2019.11.015

MEMBERS

PROJECTS

  • FLIM, Micro-MOKE, Metheor, Fourier transform interferometer, Infrared spectroscopy

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