Ingénierie et Architectures Macromoléculaires

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Own equipment

Specialised in polymer science from the synthesis up to the final application, IAM team is equipped with different techniques to support its research studies.

These equipments that are helpul at the different stages of the R&D, can be classified according to different categories in polymer chemistry, physicochemistry or transformation.

- Spectroscopy
- Thermal analysis
- Separative techniques
- Mechanical and viscoelastic analyses
- Films characterization
- Reactors
- Others techniques


Spectroscopy

  • FTIR spectrophotometers (Nexus - Nicolet and Spectrum 100 - Perkin Elmer)

Applications : Characterization of the chemical structure of organic/inorganic molecules, polymers…

Mode :
- Reflexion
- Transmission in KBr or with ATR equipment (Zn-Se / diamond crystal)

Additional :
- Possibility of irrradiation under UV lamp
- Registering under temperature change (-100 °C to 200 °C)

Contacts : Olivia Giani & Claire Negrell

  • UV/Vis spectrometers (Lambda 35-Perkin-Elmer and Cary50 – Varian)

Options :
- Peltier
- Optical fiber support

Contacts : Sophie Monge & Claire Negrell

  • Spectrofluorophotometer (Shimadzu RF 5301 PC)

Applications : Measurement parameters of fluorescence (intensity and wavelength distribution of emission spectrum after excitation by a certain spectrum of light).

Contact : Vincent Lapinte


Thermal analysis

  • 2 Thermogravimetric Analysis (Q50 - TA Instruments)

Applications : Analysis of chemical componds (molecules, polymers…) to evaluate their thermostability or their filler content (composites).

Mode :
- Dynamic from ambient up to 1000 °C
- Kinetic

Atmospher :
- Inert (gaseous nitrogen)
- Oxydant (air)

Contacts : Joël Couve & Claire Negrell

  • 3 Differential Scanning Calorimeters (2 Maia – Netzsch and DSC StarOne – Mettler)

Applications :
- Characterisation of calorimetric behaviour of molecules, polymers and materials.
- Determination of endothermic or exothermic phenomena (melting, glass transition, crystallisation, polymerisation, degradation…)

Mode :
- Dynamic from -150°C up to 700 °C with linear or modulated signal
- Kinetic
- Photocalorimetry (UV) under Hg-Xe lamp

Atmospher :
- Inert (gaseous nitrogen)
- Oxydant (air)

Contacts : Abdelatif Manseri & Joel Couve pour la DSC du plateau technique


Separative techniques

  • Flash chromatography (1 Unit)

Applications : Flash column chromatography is a quick and (usually) easy way to separate complex mixtures of compounds.

Eluents : all solvents

Detectors : UV (2 l), Evaporative Light Scattering Detection

Contact : Claire Negrell

  • Gel Permeation Chromatography (8 units of Varian-Agilent)

Applications :
- Determination of polymer Molecular weight
- Interest of the triple detection : assessment of the true molar mass, the study of the structure and the conformation of macromolecules directly, without using any standards, nor extrapolation of the results.

Eluents : THF, DMF , DMAc, MeOH/Water, Chloroform

Detectors : Refractive Index, UV, Viscosimeter and Light scattering

Columns : for high and low molecular weights / for polar functions

Software : Sirhus

Reference contacts : Olinda Gimello & Claire Negrell


Mechanical and viscoelastic analyses

  • 3 Rheometers (AR1000 & AR2000 EX - TA Instruments, MCR102 - Anton Paar)

Applications :
- Characterization of the viscoelastic properties of polymers in solution, molten or solid state according to a large range of possible influence parameters : temperature (thermomechanical behavior), frequency (spectromechanical analyses – master curves), time (kinetic, stress relation, creep…)

Mode :
- from – 150 °C up to 600 °C :
- Dynamic, steady or transient mode
- Air or inert atmospher

Geometries :
- parallel plates,
- cone-plane,
- couette,
- rectangular torsion

Contacts : Jean-Pierre Habas & Christine Joly-Duhamel

  • 2 Dynamic Mechanical Analyses (DMA50 - ACOEM Metravib)

Applications :
- Study of viscoelastic behavior of polymers and composites in the solid state. A sinusoidal stress is applied and the strain in the material is measured, allowing one to determine the complex modulus. The temperature of the sample or the frequency of the stress are often varied, leading to variations in the complex modulus. This approach can be used to locate the glass transition temperature of the material, as well as to identify transitions corresponding to other molecular motions.

Mode :
- From – 150 °C up to 550 °C
- Modulation of hygrometric conditions
- Dynamic, steady or transient mode

Large range of geometries suitable for the mechanical characterization of polymers, foams, composites and fibres (tension/traction, compression, bending…)

Contacts : Rémi Auvergne, Christine Joly-Duhamel, Vincent Lapinte & Jean-Pierre Habas

  • Microrheometer (Formulaction)

Applications :
- Passive Microrheology consists in using micron sized particles to measure the local deformation of a sample due to thermal energy (Brownian motion). This local probing method enables the measurement of the evolution of viscosity and elasticity, in bulk samples or in films.

Contact : Claire Negrell

  • Viscosimeter (Brookfield DV2T)

Applications :
- Viscosimeter measures fluid viscosity at given shear rates

Mode :
- Room temperature
- 0.1 to 200 rpm

Contact : Vincent Lapinte

  • Traction Apparatus (Instron 5533)

Applications : Mechanical technique for plastics, composites, films

Mode :
- 100 N and 10 kN sensor
- extensometer

Contact : Vincent Lapinte

Films characterization

  • Shore A and D Durometers

Standard testing of material hardness (ISO 868 et 7619, ASTM D 2240 et DIN 53505)

2 common scales : A scale for softer plastics D scale is for harder ones

Contacts : Jean-Jacques Robin & Claire Negrell

Reactors

  • 3 CO2sc reactors

1 variable-volume view-cell (3mL-15mL) with one sapphire window and circulating heating fluid, equipped with pressure transducer, rupture disks, internal thermocouple, and magnetic stirring ; 2 circulating heating fluid baths ; 1 ISCO 260D syringe pump ; polycarbonate shield.

Contact : Patrick Lacroix-Desmazes

  • 2 UV reactors

Volumes : 18 ml, 188 ml and 600 ml Light sources : 253,7 nm – 184,9/253,7 nm – 300 nm Options : Magnetic stirrer and Cooling fan

Contacts : Jean-Jacques Robin & Claire Negrell

  • Autoclaves (or pressure reactors)

Feeding the Autoclaves from F-gases/alkenes from lines

Specific set up to feed thick borosilicate Carius Tubes with 0.50 to 2.00 g of F-alkenes

10 high pressure-Hastelloy Autoclaves equipped with security disk, valves, manometer, and mechanical stirrer (from 50 ml to 600 ml)

  • Plasma reactor

Used for surface modification, grafting and functionalization. Gas and vapors of monomers ; Flowmeter : sccm ; Radio-frequency : 13,56 MHz ; Max power : 200 W ; Pirani pressure gauge

Contact : André Mas

  • Microwave reactor

Contact : Sophie Monge

  • Glovebox

Experiments in controlled or anhydrous medium ; Inert Gases (such as Argon or Nitrogen) ; Lock chamber

Contact : André Mas

Others techniques

  • 2 Dynamic Contact Angle Measuring System

Measurement the surface tension and interfacial tension of a liquid using the pendant or sessile drop methods.

Contacts : Olivia Giani & Claire Negrell

  • Tensiometer (DCAT11-Data Physics)

Study of the surface chemistry : measurement of the surface tension and liquid interface, determination of the CMC of a surfactant and a density of a liquid.

Contact : Claire Negrell

  • Granulometer-Zetasizer (Nano ZS-Malvern), Granulometer (Vasco3 - Cordouan) and Zetsizer (Wallis – Cordouan)

Characterization of nanoparticles, colloids and proteins (particle size, zeta potential..).

Contact : Sophie Monge & Claire Negrell

  • Salt spray test (ASCOTT)

Standardized test method used to check corrosion resistance of coated samples

Contact : Abdelatif Manseri

  • Microcompounder (Xplore)

Production of injection-moulded specimens in research scale (minimum required amounts of 5 g only) ; co- and counter-rotating twin screws. Three temperature zones can be controlled individually (max. 300 °C).

Adress : Ecole des mines, Alès (30) Contact : Sylvain Buonomo

  • Cryomill (Spex)

The cryomilling uses a cryogenic fluid (liquid nitrogen) to cool exactly (until -196 °C) materials (amounts of 1-5 g) up to their point of embrittlement to facilitate the mechanical reduction.

Contact : Claire Negrell

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