Les spectromètres disponibles au laboratoire sont:

 
 
 

 

 

  • Temperature resolved second harmnic generation (TR-SHG)

 

   

suppliers:         

Principle: Second harmonic generation is a non-linear optical process occurring exclusively in non-centrosymmetric crystals and leading to a doubling of the frequency of the incident beam as it passes through the sample. The setup based on the “Kurtz and Perry” method permits the measurements of the SHG intensity generated by of a powder sample versus temperature.

Type of analyses:

  • Conglomerate detection [1] and verification of non-centrosymetry
  • Detection of solid impurity at ppm [2]
  • Study of polymorphic transitions (monotropic or enantiotropic [3] as well as disorder order [4]) involving at least one non-centrosymmetric phase.
  • Phase diagram study involving at least one non-centrosymmetric phase [5,6]

Main publications :

  1. A. Galland, V. Dupray, B. Berton, S. Morin-Grognet, M. Sanselme, H. Atmani and G. Coquerel, Cryst. Growth Des., 2009, 9, 2713–2718.
  2. S. Clevers, F. Simon, V. Dupray and G. Coquerel, J. Therm. Anal. Calorim., 2013, 112, 271–277.
  3. S. Clevers, F. Simon, M. Sanselme, V. Dupray and G. Coquerel, Cryst. Growth Des., 2013, 13, 3697–3704.
  4. S. Clevers, C. Rougeot, F. Simon, M. Sanselme, V. Dupray and G. Coquerel, J. Mol. Struct., 2014, 1078, 61–67.
  5. L. Yuan, S. Clevers, N. Couvrat, Y. Cartigny, V. Dupray and G. Coquerel, Chem. Eng. Technol., 2016, 39, 1326–1332.

 

 
  • 2-Photon Microscopy – SHG/THG Microscopy

 

   

Suppliers : Leica, Spectra-Physics and Linkam

         

Principle: The Leica SP8 confocal microscope, coupled with a femtosecond laser (Insight X3, spectaphysics) tunable over a wide range of wavelengths (680-1300 nm) allows sample analyses by microscopy: SHG (second harmonic generation), THG (third harmonic generation) and TPF (two-photon fluorescence).  It provides access to spatially localized information by recording SHG/THG/TPF-2D maps and building SHG/THG/TPF-3D profiles at the scale of a few micrometers with minimal sample preparation. The SHG is sensitive to the non-centrosymmetry of the medium and the THG signal is obtained for any heterogeneity of the optical properties of the medium. It is also possible to tune the temperature of the samples between -150 and 800 °C.

  • Type of analyses:

    Detection of non-centrosymmetric impurities (chemical or structural impurities), optical properties of new materials, resolution of ambiguities when assigning space groups, study of phase transitions, determination of transition temperature, assistance in the construction of phase diagrams, study of chiral discrimination in the solid state, ...

    The use of the Linkam stage makes possible to follow the evolution of the samples vs temperature and the visualization of various types of phase transitions (recrystallizations, desolvations, polymorphic transitions, melting).

SHG and THG microscopy image during crystallization of a Formic Acid/Water mixture. In green, formic acid crystals (SHG signal), in red ice crystals (THG signal)

Image d’un monocristal (phénanthrène) au cours de la transition polymorphique (En vert signal SHG de la phase noncentrosymétrique)

Main publications:

  1. Batoul Almoussawi, Marielle Huvé, Valérie Dupray, Simon Clevers, Victor Duffort, et al.. The Oxy-sulfide Ba 5 (VO 2 S 2 ) 2 (S 2 ) 2 Combining Disulfide Channels and Mixed Anion Tetrahedra andits Third Harmonic Generation Properties. Inorganic Chemistry, American Chemical Society, 2020,59 (9), pp.5907-5917. 10.1021/acs.inorgchem.9b03674
  2. Dong Fan, Nicolas Barrier, Aurélie Vicente, Jean-Pierre Gilson, Simon Clevers, et al.. Organictemplate-free synthesis of an open framework silicoaluminophoshate (SAPO) with high thermal sta-bility and high ion conductivity. Inorganic Chemistry Frontiers, Royal Society of Chemistry, 2020, 7(2), pp.542-553.
  3. Veronica Ianno, Simon Clevers, Philippe Négrier, Valerie Dupray, Gérard Coquerel, et al.. p -Synephrine enantiomers: binary phase diagram, crystal structure and kinetic stability of a metastable conglomerate monitored by nonlinear optics. CrystEngComm, Royal Society of Chemistry, 2020, 22 (36), pp.6071-6080. ⟨10.1039/D0CE00841A⟩. ⟨hal-03006854⟩.
 
 
  • Spectrophotomètre ATR-FTIR Alpha-P

 

   

Fournisseur:         

Principe: La configuration de cet appareil permet de mesurer en routine les spectres infra-rouges des matériaux

Type d'analyses effectuées: Mesure de spectres IR en routine sur des échantillons solides et liquides - Identification chimique et discrimination de polymorphes.