Aller au menu principal Aller au contenu principal
Partager
logo SAMBA

SAMBA (Spectroscopy Applied to Material Based on Absorption) est une ligne d'absorption dans le domaine des rayons X durs. SAMBA est ouverte a une vaste communauté scientifique qui va de la physique à la chimie, les sciences des surfaces et de l'environnement.

SAMBA (Spectroscopy Applied to Material Based on Absorption) est une ligne d'absorption dans le domaine des rayons X durs. SAMBA est ouverte a une vaste communauté scientifique qui va de la physique à la chimie, les sciences des surfaces et de l'environnement. Le schéma optique de la ligne est optimisé pour être très versatile et couvrir l'interval 4.5-43keV avec un flux de photons élevé, stabilité et une résolution optimale. Un nouveau détecteur HPGe avec 35 pixels est disponible à partir de 2012 pour des mesures sur des espèces hautement dilué.

Veuillez noter que le dispositif Quick-EXAFS a été transféré à la ligne ROCK à lui dédié.

L'équipe

ALIZON
ALIZON Guillaume
Assistant Ingénieur de Ligne De Lumière
FONDA
FONDA Emiliano
Responsable Ligne De Lumière
IKOGOU
IKOGOU Maya
IRAR
LANDROT
LANDROT Gautier
Scientifique de Ligne De Lumière
ZITOLO
ZITOLO Andrea
Scientifique de Ligne De Lumière

Données techniques

Energy range

Between  6 to 35 keV

Energy Resolution (ΔE/E)

Si(111) : 1.2x10-4 @ 5 keV
Si(220) : 6x10-5 @ 15 keV

Source

Bending Magnet  Radiation (Ec = 8.65 keV)  1.5 mrd Horizontal x 1 mrd Vertical

Flux in the XAS hutch

Si(111) : 10+12 Phot/s/0.1%bw @ 10 keV 
Si(220) : 2.8x10+11 Phot/s/0.1%bw @ 15 keV 
Si(220) : 2.3x10+10 Phot/s/0.1%bw @ 35 keV

Optics

A sagittal focusing monochromator between two bendable cylindrical mirrors

Sample Environment

Many ancillary devices like cryostats (He liq and N2liq), furnaces, thermostated liquid cells and many sample-holders.

Raman Spectroscopy

UV-Visible Spectroscopy

Differential Scanning Calorimetry

(x-ray diffraction as a further developement)

Beam size at sample (EXAFS hutch)

200x300 μm2

Beam size at sample (SurfAs hutch)

300x300 μm2

Detectors

Ionisation chambers (Transmission)

Canberra 35-elements monolithic planar Ge pixel array detector, Multi-elements Germanium detector or a Vortex silicon drift detector (Fluorescence)

Total electron yield
SAMBA domaine énergie

Thématiques scientifiques

Material science 
Energy storage

Determination of structural and electronic properties and average size of nanosystems. Dynamic or static study of new anodic or cathodic materials. Understanding of magnetic phase transition of molecular system in coordination chemistry. Characterisation of glasses etc...
Physic Investigation of clusters embedded in matrices.
Biology, Biomaterials

Study of reactivity of biomimetic compounds which are used as simple model compounds to understand the mechanism of catalysis of more sophisticated systems like metallo-enzymes. Investigation of metal ions present in metallo-proteins and in bio-inorganic complexes.

Earth and environmental sciences

Local environment probe of any element in natural systems (soils, sediments, snow, plants, microorganisms ...).

Surface science

Characterisation of the local structure of thin films at the very first stages of growth. Study of the interfaces : metal/metal, metal/semiconductor and oxides/metal.

Catalysis

Structural and electronic characterisation of catalysts in order to understand/predict their catalytic activity/selectivity in a given reaction. (DeNOx catalysis, Fischer-Tropsch, hydrogenation of hydrocarbons ...).

Optical Hutch

optic SAMBA
Schéma de la cabane Optique

 

Mirrors

Two cylindrically bendable silicon mirrors (WinlightX) coated by a layer of 50 nm of Pd are used for providing:

  1. vertical collimation of the beam
  2. vertical focusing of the beam at the sample position
  3. harmonic rejection.

The mirrors are used over the whole 4-40 keV energy range available on the beamline by tilting the mirrors from 10 mrad to 1 mrad (i.e. 0.57° to 0.057°) depending on the desired cut-off energy for removing the harmonic X-rays.

Reflectivity SAMBA mirror
 

The reflective Pd surfaces are 1200 mm long per 88 mm wide allowing a horizontal acceptance of about 6.2 mrad on the first collimating mirror located at 14.1 m from the source. The surface of the mirrors was polished to a rms roughness less than 3 Ǻ rms and to a  longitudinal slope error less than 2µrad rms. The first mirror is water cooled using blades immersed in In-Ga eutectic in grooves in the mirror surface.

The focusing in the vertical direction is ensured by the M2 mirror, the resulting vertical spot size at the sample position is 110 µm (FWHM) with a foot size of about 300 µm.

cylindrical curvature for M2

Sagittal focusing double crystal monochromator

Sagittal focusing double crystal monochromator

Sagittal focusing double crystal monochromator


Sagittal focusing double crystal monochromator

The sagittally focusing Double Crystal Monochromator (DCM) provided by Oxford Danfysik is used in the so-called high flux mode. The DCM is installed at 16.1 m from the source. It deals of a first flat water-cooled Si(220) or Si(111) crystal and a sagittally bent 2nd crystal. The main Bragg axis of rotation passes through the centre of the diffracting face on the 1st crystal and perpendicular to the beam axis. In this way, the incident white beam is always centred on the axis of rotation. A fixed offset to the exit beam is achieved by moving the 2nd crystal perpendicularly to the first one according to the Bragg angle. In this case the beam moves along the axis of the sagittally-bent 2nd crystal. The first crystal is indirectly water-cooled by using a multi-channel water cooling support (SOLEIL original design) in contact with the crystal through a thin film of In-Ga eutectic. The 2nd crystal is uncooled.

The horizontal acceptance of the monochromator is limited by the efficiency of the sagittal bender. For a horizontal acceptance of 1.5 mrad, the typical beam size at the sample position is around 300 µm (H) x 200 µm (V) (FWHM).

In order to avoid possible radiation damage on the sample due to the high density of photons in a so small spot, the beamline is often slightly defocused in both directions to achieve a spot size of 2 mm (H) x 1mm (V).

 Flux at the sample position provided by the Si(220) and Si(111)

Flux at the sample position provided by the Si(220) and Si(111)

 Flux at the sample position provided by the Si(220) and Si(111)

Normalized flux at the sample position for the Si(220) and Si(111) sagittally DCM (400 mA stored current, 1.5 mrad horizontal and 1 mrad of grazing incidence on the mirrors).

Then the typical flux at the sample position at 8.5 keV is 5 1011 ph/s with the Si(220) DCM and 1.2 1012ph/s with the Si(111) DCM (6 mrad of vertical acceptance and 1.5 mrad of horizontal acceptance, I = 400 mA).

Related publications: 

SAMBA: The 4-40 keV X-ray Absorption Spectroscopy Beamline at SOLEIL. 
V. Briois, E. Fonda, S. Belin, L. Barthe, C. La Fontaine, F. Langlois, M. Ribbens, F. Villain 
UVX 2010 - 10e Colloque sur les Sources Cohérentes et Incohérentes UV, VUV et X ; Applications et Développements Récents: 41-47. EDP Sciences 2011

Quick-EXAFS monochromator (no longer available)

The SOLEIL designed Quick-EXAFS monochromators are made of two independent channel-cut crystals (Si(111) and Si(311)). 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 to 37 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 monochromatorQuick-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.

courbes absorption quick

(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.


(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 

EXAFS Hutch

Retrouvez ci-dessous les modes de détection de la station EXAFS ainsi que les différents couplages disponibles.

Accédez aux différents types de Setups disponibles sur la station EXAFS

 

Sagittal Mode

 

Crystal type : Si220 (4 to 42 keV)  Si111 (4 to 22 keV)
Beam size : 300μm x 200μm  /  75μm x 75μm using capillary

Detection

Transmission :

chambre ionisationOxford ionization chambers

Fluorescence :

fluorescence camberra Canberra 35-elements  monolithic planar Ge pixel array detector

Detector Silicon Drift : Vortex Detector Silicon Drift : Vortex

Total electron yield

No picture. The sample must be electrical conductor otherwise a thin layer of graphite may be evaporated. 

Beam size using capillary : 75μm x 75μm

Application in Environmental science as an example, but also microfluidic application and grazing incidence of thin films. 

capillary montage

Quick-exafs Mode


Crystal type : Si311 Si111 (4 to 37 keV)
Beam size : typically 0.5 mm x 1 mm
Flux ~ 1011 ph/s at 8 keV

Detection

Transmission

Oken ionization chambers

Oken ionization chambers

 Oken ionization chambers

Fluorescence

Avalanche Photo Diode (APD)

Avalanche Photo Diode (APD)

TEY

Tey absoption spectrum

Tey absoption spectrum

Ni K edge XAS signal (up) collected in a TEY detection mode on a Proton Exchange Membrane Fuel Cell thick film in the Quick-EXAFS mode after correction of glitches. The presented spectrum is not averaged (5s of time acquisition).The frequency of oscillation of the Si(111) channel-cut was 0.1 Hz (5s per spectrum) with an oscillation amplitude of 1.6°.

No picture. The sample must be electrical conductor otherwise a thin layer of graphite may be evaporated. 

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. 

XAS with edge jumping

The SAMBA quick-EXAFS monochromator: XAS with edge jumping

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°

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

Notice :

quick-exafs_anglais.pdf (1.4 Mo - pdf) (1.4 Mo)

CombinedTechniques

XAS with Raman spectroscopy

XAS with Raman spectroscopy

XAS with Raman spectroscopy

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 VARIANCary 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 Raman and UV-Visible spectroscopies

 

 

 

 

 

 

 

 

 

 

 

XAS with Differential Scanning Calorimeter (DSC)

DSC 111 Setaram :

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...)

 

 

 

 

 

Catalysis

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

polyvalent soleil four for ftr coupling

logo SAXOCharacteristics   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)

 

 

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 

high pressure cell transmission raman coupling

logo ifpCharacteristics  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)

high pressure cell
high pressure cell

 

 

 

 

 

Commercial cell Harrick for fluorescence and Raman coupling

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

commercial cell harrick for fluorescence raman coupling

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

Gas distribution systemGas distribution system control

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

 

 

 

Mass spectrometer

Mass spectrometerMKS Cirrus
LM99 Analyser

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

 

 

Energy Science

Setup for Li/Na batteries

Setup for Li/Na batterieslogo pulsseVMP3 Bio-logic Multi-channel Potentiostat 

 

16 independent channels, 6 already equipped whose one for impedance measurement

set up lina batteries

 

 

 

 

Low temperature

Helium Cryostat

Helium Cryostat

He cryostat suitable for transmission and fluorescence detection 
(20 K to Room Temperature)

 

 

 

 

 

Nitrogen Cryostat

nitrogene cryostatLiquid nitrogen (80 K) cryostat suitable for transmission and fluorescence detection

 

 

 

 

 

Liquid Cells

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 cell for transmissionLiquid cells PTFE with fixed optical paths
(0.5<o.p.<5mm)

 

 

 

 

 

 

Liquid cell for fluorescence mode

Liquid cell for fluorescence modeLiquid cell (PCTFE) for fluorescence detection
(design F. Villain)

 

 

 

 

 

 

 

Liquid cell for biological sample

Liquid cell for biological samplePTFE sample-holder for He cryostat 
(two samples ~ 50µl) available for 
transmission and fluorescence detection 

 

 

 

 

 

Thermostated liquid cell

Thermostated liquid cellThermostated 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)

 

 

 

 

 

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

 

 

 

 

 

 

SEXAFS Hutch

Préparation de surface et croissance de film mince in situ sous ultra-vide (10-10) pour mesures

Outils de préparation
Cellules de Knudsen, Source pour bombardement d'é Omicron, microbalance à Quartz

Détecteurs pour XAS
Dinode (TEY), 7-éléments Ge Canberra (fluorescence)

Caractérisation des surfaces
Auger, LEED, analyseur de gaz residuel

NB: le porte-échantillon peut être refroidit à -190°C et chauffé jusqu'à 1000°C suivant le type.

bâti SEXAFS HUVSEXAFS HUV

Vue du bâti SEXAFS HUV :
(A) canne de transfet échantillon ;
(B) carrousel de la chambre de transfert ;
(C) chambre principale d'analyse/croissance ;
(D) détecteur Ge 7 éléments (Canberra France)

Notices :

gnuplothowto.pdf (114.69 Ko)

new_holderpositions.pdf (84.22 Ko)

sputteringhowto.pdf (62.75 Ko)

tbt_cryostats.pdf (54.91 Ko)

augerhandbook.pdf (340.67 Ko)

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

Gas

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.

Sample positioning

Two schemas of implantation for new experimental set-up on the EXAFS table could be hold, but contact your local contact is mandatory.

schemas of implantation for new experimental set-up on the EXAFS tableschemas of implantation for new experimental set-up on the EXAFS table

Aide à la soumission de projets

Dépôt de projets 
Date limite (standard & BAG project) : 
15 Février - 15 septembre

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