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ROCKRocking Optics for Chemical Kinetics
ROCK est une ligne de spectroscopie d’absorption X en mode quick-EXAFS dans le domaine 4 - 40 keV

 

This acknowledgement is mandatory for all publications from ROCK  beamline :
This work was supported by a public grant overseen by the French National Research Agency (ANR) as part of the “Investissements d’Avenir” program (reference : ANR-10-EQPX-45).

 

Publications majeures :
La Fontaine C., Belin S., Barthe L., Roudenko O., and Briois V. "ROCK : A Beamline Tailored for Catalysis and Energy-Related Materials from ms Time Resolution to µm Spatial Resolution" Synchrotron Radiation News, 33(1):20-25. (2020).

Briois V., La Fontaine C., Belin S., Barthe L., Moreno T., Pinty V., Carcy A., Giradot R. and Fonda E. "ROCK : the new Quick-EXAFS beamline at SOLEIL" Journal of Pysics Conferences Series, 712:art n° 012149 (2016).

La ligne de lumière ROCK est une ligne de spectroscopie d’absorption X en mode quick-EXAFS dans le domaine 4 - 40 keV.

label investissement d'avenirFinancée par l’ANR dans le cadre des Projets Investissements d’Avenir (Equipex 2010), ROCK  est dédiée à l'étude des processus cinétiques rapides sur des nanomatériaux utilisés principalement dans le domaine de la catalyse et des batteries. Le but de cet EQUIPEX est de contribuer au développement de catalyseurs et de batteries plus performants qui devraient trouver des applications industrielles dans le domaine de la production et du stockage de l'énergie en conformité avec la protection de la santé publique et de l’environnement.

L'équipe

BRIOIS
BRIOIS Valerie
Responsable Ligne De Lumière
BEAUVOIS
BEAUVOIS Anthony
Scientifique de Ligne De Lumière
BELIN
BELIN Stephanie
Scientifique de Ligne De Lumière
BARTHE
BARTHE Laurent
Assistant Ingénieur de Ligne De Lumière
JIANG
JIANG Lei
LA-PORTA
LA-PORTA Francesco
Ribeiro Passos Aline
Postdoc
Plais Lucie
Doctorante

Collaboratrice associée

IADECOLA Antonella (RS2E CNRS)
    01 69 35 94 68
antonella.iadecola@synchrotron-soleil.fr

Données techniques

Gamme d'énergie

4.5 à 40 keV

Résolution en énergie (∆E/E)

2 10-4 à 5 10-5

Source

Aimant de courbure (Ec = 8.65 keV)

Flux

Si(111) @ 8.0 keV : 2 1012ph/s
Si(220) @ 20 keV : 5 1011ph/s

Optiques

Miroir toroïdal courbable en Si recouvert de 50nm d'Ir ;

2 monochromateurs QuEXAFS (Si111 et Si220) entre un miroir plan et un miroir courbable en Si à trois pistes (Pd, Pt et B4C) assurant le rejet des harmoniques

Environnement de l'échantillon

Dispositifs ancillaires pour la catalyse (Fours, rack distribution gaz, spectromètre de masse ...)
Cellules électrochimiques thermostatable, multipotentiomètre
Spectromètres Raman et UV-visible
Calorimétrie différentielle à balayage

Taille du faisceau

350 µm à 4.9 mm de large (FWHM)
79 µm à 2.2 mm de hauteur (FWHM)

Détecteurs

Chambres à ionisation OKEN
Photodiode à avalanche

Thématiques scientifiques

Nanomatériaux utilisés principalement dans le domaine de la catalyse et des batteries

 

Des informations détaillées sur les miroirs et monochromateurs de la cabane optique, sur la station EXAFS. Retrouvez également les Setups disponibles sur ROCK, les techniques couplées et les particularités de la ligne.

Cabane optique

Schéma de la cabane Optique

Storage ring : Toroidal collimating mirror M1 (CINEL/Winlight X)

enceinte M1 anneau ROCK

M1

Fixed Grazing Incidence : 2.5 mrad
Ir (50 nm)
Roughness 5 Å <
Tangential slope error: 0.5 μrad RMS
Sagittal slope error : 20 μrad RMS
Water Cooled
Total absorbed power : 87 W
Absorbed power density : 4 mW/mm 2

Collimating principeCollimating principe :

 

 

Optical hutch :  Mirrors M2a and M2b harmonic rejection and vertical focusing (IRELECALCEN/Winlight X)

 

M2aM2a

M2bM2b

Acceptance 1.5 (H) x 1.0 (V) mrad2 1.5 (H) x 1.0 (V) mrad2
Source distance 16.82 m 22.44 m
Optical active area 47 mm x 1100 mm 47 mm x 1100 mm
Coating 3 stripes Pt layer 50 nm, Pd layer 50 nm and B4C layer 5 nm  3 stripes Pt layer 50 nm, Pd layer 50 nm and B4C layer 5 nm
Roughness less than 3 Ǻ RMS less than 3 Ǻ RMS
Longitudinal slope error 1 µrad RMS/best spherical fit 1 µrad RMS/best spherical fit
Sagittal slope error 5 µrad RMS 5 µrad RMS
Orientation Reflecting vertically upward Reflecting vertically qownward
Working pitch angle

1.75 mrad to 5.2 mrad

1.75 mrad to 5.2 mrad
Shape Flat mirror : R > 20 km Bending radius range : 1.5 km < R < 20 km
Cooling system Water cooling No cooling
Maximum total absorbed power 78 W -
Maximum absorbed power density 19 mW/mm2 -

 

Quick-EXAFS monochromator

Expected flux at the focusing point

The SOLEIL designed Quick-EXAFS monochromators are made of two independent channel-cut crystals (Si(111) and Si(220)) and was first used on SAMBA beamline. Each channel-cut crystal is mounted on a cam driven tilt table allowing it to oscillate periodically with amplitude θ(t) around an average fixed Bragg angle θB. The amplitude can be tune from 0.1 to 4° by an original SOLEIL in vacuum variable cam design. The θB Bragg angle is selected by one of the two goniometers holding the oscillating tilt tables. The 4.5 to 40 keV energy range is available using both Quick-EXAFS monochromators. The channel-cut crystal can be changed by the other one in few seconds during an experiment allowing to record quick-EXAFS data at absorption edges very far in energy. For instance the XAS study of a bimetallic catalyst at both edges during the same catalytic reaction is now possible with the SAMBA’s QuEXAFS set-up, even if the edge energies of those elements are covered by two distinct crystals.

Quick-exafs monochromator

Maximum performance of the Quick-EXAFS mechanics in terms of oscillation frequency of the channel-cut is 40 Hz for two recorded spectra: one with the Bragg angle collection in the downward direction and the other with the Bragg angle collection in the upward direction. Due to the photon flux available at the sample position at the SAMBA beamline in QuEXAFS configuration ((flux ~ 1011 ph/s at 8 keV) the optimal time resolution of experiments on real concentrated and not too absorbing samples is around 100 ms. On ROCK we expect to reach 1012 ph/s in 50 ms.

(left) Absorption of stacked Cr and Mn metallic foils measured over an amplitude of 3.6 °. Data are the average of 10 spectra each collected at 1Hz. (right) k2 weighted Quick-EXAFS are compared to standard scans taken in almost 15 min.

 

Related publications:

The SAMBA Quick-EXAFS monochromator: XAS with edge jumping
E. Fonda, A. Rochet, M. Ribbens, S. Belin, L. Barthe, V. Briois
Journal of Synchrotron Radiation (2012), 19, p 417 - 424

 

Cabane EXAFS

 ►Quick-exafs Mode

 

Crystal type : Si111 Si220 (4 to 40 keV)
Beam size : from 350 x 79 µm2 to 4.9 x 2.2 mm2
Flux ~ 1012 ph/s at 8 keV


Transmission

Oken ionization chambers

Fluorescence APD ou PIPS

Avalanche Photo Diode (APD)

PIPS

PIPS

Edge Jump

Large energie range from 4 keV (Si111) to 37 keV (Si311) in 30s
The remote selection of the monochromator crystals, Si(111) or Si(311), allowing users to permanently access energies between 4 and 37 keV in Quick-exafs mode. 

E. Fonda, A. Rochet, M. Ribbens, S. Belin, V. Briois The SAMBA quick-EXAFS monochromator: XAS with edge jumping J. Synchrotron Rad. 2012, 19, 417 – 424.

Example of the energy range accessible with Si111 cam=4°

Setups disponibles

 

Couplages

ROCK's experimental station EXAFS is characterised by a lot of techniques combined to XAS, such as Differential Scanning Calorimetry, Raman Spectroscopy and UV-Visible Spectroscopy.

XAS with Raman spectroscopyRaman_SAXO_oven

                                                             Kosi RXN1-785 Kaiser

Iexc. = 785 nm or 532 nm 
CCD: 100-3450cm-1 or 200-4000 cm-1 
Optical fibers
with probehead 
Seceral Long Working Distance
objectives (150 mm to 35 mm)

XAS with UV-visible spectroscopy

Cary 50 VARIAN

                   

With optical fibers
190 < I < 1100 nm
VScan < 24000 nm/min
XAS cell with mylar or PP windows for optical fiber used in transmission
or immersion probe : 2 or 10 mm
or cuvettes Quartz, Glass, PMMA, PS
XAS with Raman and UV-Visible spectroscopies  
XAS with Differential Scanning Calorimeter (DSC) 
DSC 111 Setaram :

Calvet type differential scanning calorimeter 
-120 to 800°C 

* Phase transition (fusion, crystallization, glass transition, polymerization, degradation)
*  Cp Evaluation
*  Monitoring of reactions (oxidation, reduction, dehydration...)

 

Catalyse

Retrouvez ci-dessous les différents environnements échantillons catalyseurs à votre disposition sur la station EXAFS.

Polyvalent SOLEIL development for fluorescence, transmission and Raman coupling

La Fontaine, C., Barthe, L., Rochet, A., & Briois, V.
X-ray absorption spectroscopy and heterogeneous catalysis: Performances at the SOLEIL's SAMBA beamline. Catalysis Today, 2013, 205: 148–158

Two ovens/capillaries set-up collaboration MAX IV/SOLEIL designed by L. Barthe

Characteristics    Lytle-type cell

  • RT 600°C +/- 0.5°C
  • Atmospheric pressure
  • Powdered catalyst gently pressed into the cavity of the sample hoolder (thickness 2, 4 and 6 mm, 0.10 - 0.25 cm3)

 

 

 

 

 

Characteristics 2 capillaries oven

  • RT 1000°C +/-0.5°C

High pressure cell for transmission and Raman coupling

A. Rochet et al. Catalysis Today (2011) vol 171 186-191 
A. Rochet et al. Diamond Light Source Proceedings (2011) 1, e130 1-4

Characteristics  Lytle-type cell

  • RT 600°C +/- 0.5°C
  • 50 bar
  • Powdered catalyst gently pressed into the cavity of the sample holder (thickness 2 mm)


Commercial cell Harrick for fluorescence and Raman coupling

C. La Fontaine et al. Harrick Scientific Products (Ed.), Application Note n°91201 (2010).

Characteristics

  • RT 500°C
  • Atmospheric pressure
  • Powdered catalyst (≈50 mg) gently pressed into the sample holder cavity
  • Catalyst pellet (6 mm dia.) disposed onto a BN bed

Gas distribution system

  • Complex mixtures
  • Saturator for liquid reactants
  • Heated lines (120°C)
  • Patm --> 20 bar
  • Remote control

Mass spectrometer

MKS Cirrus
LM99 Analyser

  • Tripple mass filter, 1-200amu or 1-300amu
  • Faraday and SEM detector
  • Maximum operating pressure Faraday 2x10-5 mBar

Basse temperature

With the courtesy of SAMBA beamline

Helium Cryostat He cryostat suitable for transmission and fluorescence detection 
(20 K to Room Temperature)
Nitrogen Cryostat Liquid nitrogen (80 K) cryostat suitable for transmission and fluorescence detection

Cellules liquides

We have different cells with fixed or variable optical path available for basic or acidic solution. Two of them are thermostatically controlled. Note Kapton, Mylar, PP or PTFE can be used as windows depending of the nature of the solution.

Liquid cell with variable optical path for transmission Thermostated liquid cell (PTFE) with  adjustable optical paths (10 µm to 6 mm)  suitable for the combination of  transmission XAS with UV-Vis spectroscopies (design SPECA)
Liquid cell for transmission Liquid cells PTFE with fixed optical paths
(0.5<o.p.<5mm)
Liquid cell for fluorescence mode Liquid cell (PCTFE) for fluorescence detection
(design F. Villain)
Liquid cell for biological sample

PTFE sample-holder for He cryostat 
(two samples ~ 50µl) available for 
transmission and fluorescence detection

With the courtesy of SAMBA beamline

Thermostated liquid cell

Thermostated liquid cell (PCTFE) with adjustable optical paths (100µm to 10mm) suitable for the combination of transmission XAS with Raman and/or UV-Vis spectroscopies
(design F. Villain)

 

 

Thermostated liquid cell (PTFE) with adjustable optical paths (10µm to 6mm) suitable for the combination of transmission XAS with UV-Vis spectroscopies (design SPECA) 

Science de l'Energie

Setup for Li/Na batteries

VMP3 Bio-logic Multi-channel Potentiostat 

16 independent channels, 6 already equipped (+/-400mA) whose one for impedance measurement

ANR  Electrochemical cell dedicated to operando XAS
J. B. Leriche et al. J. Electrochem. Soc., 157, (5) A606-A610 2010
Multicell support
Furnace RT to 90°C
for 2 electrochemical cells for example
Thermostated support

 

Notices

EXAFS :                                    

PDF icon gnuplothowto.pdf (114.69 Ko - pdf) (114.69 Ko)
Media Folder: 
GnuplotHOWTO.pdf                 

QuickExafs        

         

TBT_cryostats.pdf 

Informations aux utilisateurs, préparation des échantillons, la charte SOLEIL des utilisateurs et une aide à la soumission de projets sont disponibles en ligne. 

Aide à la soumission de projets

 Comment préparer votre demande de temps de faisceau ?

Les soumissions de projet doivent suivre le modèle prédéfini suivant : Renseignement du "formulaire" en ligne, concernant la partie générale du projet.

  1. Description scientifique et expérimentale
  2. Annexes des images (format .jpeg .png)
  3. Description des conditions expérimentales nécessitant des précautions spéciales de sécurité
  4. Soumission du projet

(S'il s'agit de la continuation d'un projet, il est nécessaire de soumettre un rapport d'expérience(s) passée(s) dans le SUN set et inclure la (les) publication(s) correspondante(s) avant de soumettre votre nouveau projet)

L'ensemble de la demande doit être rédigé en anglais

De plus,

- Il est nécessaire de contacter un des scientifiques de la ligne, pour discuter de l'adéquation du projet avec les spécificités de la ligne de lumière en particuliers au sujet des environnements échantillons, du mode de détection ou d'acquisition.
- La justification du temps de faisceau demandé est indispensable.

N'oubliez pas de mentionner vos publications liées à la ligne dans le sunset.

Pour plus d'informations : Le guide général des Utilisateurs

 

 

Préparation des échantillons

Gaz

The application for the use of specialty gases must be stipulated in your proposal in order that the security service can assess the associated risks. Specialty gases must be commanded 8 weeks before your experiment, also you have to prevent your local contact well in advance, for common gases (helium, argon, nitrogen, hydrogen, air and oxygen) only 2 weeks are sufficient.  

Helium liquid

The application for the use of helium liquid must be stipulated in your proposal and recalled to your local contact in such a way to order sufficiently in advance the suitable volume.