The AILES beamline is conceived for absorption spectroscopy, applied to the study of molecular orsolid state systems. It covers the electromagnetic spectrum region ranging from the mid- to far infrared (IR) or THz range (4000 to 5 cm-1 ).

In addition to the increase in flux and brilliance made possible by the Synchrotron Radiation, the beamline has been designed for a high level of mechanical stability, to minimize the noise level. This was achieved using high stability optical mounts and chambers, compatible with the interferometers' optical throughput. Radiation emitted in a magnetic dipole is collected and refocused at the entrance of two Michelson-type interferometers (FTIR). These two spectroscopic workstations are, in general, dedicated to rovibrational studies of molecular systems (AILES A, with the highest resolution, 0.1
μeV or about 0.001 cm-1 ) and to studies of optical properties of condensed matter (AILES B, 0.007cm-1)

The two experimental workstations are complemented by various sampling devices, enabling the different studies of matter in gaseous, liquid and solid phases. Research projects on AILES concern different applications in physics, chemistry and biology.

The aim of the beamline is to answer the needs of scientific projects for which bridging the spectral gap between conventionel IR and microwave radiation is particularly important, and combining high flux and stability over a broad band source.

Beamline Energy Resolution
1 * 10-4 [meV] @ 100 [eV]
1 * 10-3 [meV] @ 1000 [eV]
1 * 10-3 [meV] @ 10 [eV]
Beamline Energy Range
5 - 5000 [eV]
Max Flux On Sample
1 * 1012 [ph/s] @ 10 [eV]
1 * 1014 [ph/s] @ 100 [eV]
5 * 1013 [ph/s] @ 1000 [eV]
Spot Size On Sample Hor
400 - 3000 [um]
Spot Size On Sample Vert
400 - 3000 [um]
Divergence Hor
100 [mrad]
Divergence Vert
10 - 100 [mrad]
Photon Sources

Bending Magnet

Type
Bending Magnet
Available Polarization
Linear variable
Variable Polarization
Yes
Source Divergence Sigma
X = 20000 [urad], Y = 80000 [urad]
Source Size Sigma
X = 1000 [um], Y = 1000 [um]
Source Spectral Flux
1 * 10-12 [ph/s/0.1%bw]
Additional Lightsources

Glowbar source

Type
Interferometer
Central Wavelength/Energy
1000 * 106 [nm]
Beam shape
Other...
Other beam shape
Rond
Polarisation
Unpolarized
Monochromators

Monochromators

Energy Range
10 - 5000 [eV]
Type
Interferometer
Resolving Power
1 * 10-3 [deltaE/E]
Number Of Gratings
3
Grating Type
Beamspliters
Pre-focusing Mirror Type
silver coated mirrors
Refocusing Mirror Type
silver coated mirrors
Other Optics

Spectrometers

Description
The AILES Beamline use two Bruker 125 Interferometers (Branch A and B) as stations for spectroscopic analysis. The collected Synchrotron Radiation (SR) can be steered by a movable mirror toward either one of these two interferometers.
The Branch B interferometer has a lower resolution (max unapodized resolution = 0.008 cm-1) and therefore should be the choice for condensed matter studies.

A complete range of optimized beam splitters and detectors is available to cover the whole near- to very far infrared range. The strong point of the AILES Beamline being experimentation in the far IR, a special effort has been the implementation of fast bolometers (ca. 1 kHz bandpass) enabling an increase in signal to noise ratio (S/N) with respect to standard detectors.
Endstations or Setup

ATR Set-up under vacuum

Description
Attenuated Total Reflection (ATR) is a sampling technique which enables solid, liquid or thin films samples to be examined directly in the infrared range. The ATR uses the evanescent wave, a property of total internal reflection to probe the sample. A beam of infrared light is passed through the ATR crystal in such a way that it reflects off the internal surface in contact with the sample.
This reflection gives rise to the evanescent wave which extends into the sample. The penetration depth into the sample is typically close to the wavelength of light, but is also affected by the angle of incidence and the indices of refraction for the ATR crystal and the medium being probed. This results in the technique to be adapted to the spectral range: a long path in the far infrared where the sample is usually less absorbing and a shorter path in the mid infrared where the sample usually absorbs more.

As the AILES beamline is working under vacuum, we have developed a mechanical device combining the ATR optics of a commercial set-up (Smart-Orbit, ThermoNicolet) and the sample compartment of the spectrometer under vacuum. With this configuration the entire optical path is under vacuum (preventing atmospheric water vapour absorption) except for the attenuated wave redirected toward the sample pressed at the diamond crystal interface. In addition, as the set-up optics only exploits reflective optics (no refocusing lenses are used) this configuration is adapted to the entire visible, infrared and THz ranges.
Furthermore, although the interferometer is evacuated and changing samples does not require breaking the vacuum system. Other advantages consist in the ability to obtain a reference by measuring a simple "total reflection" (without pressed sample).
Base Pressure
1000 [mbar]
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid
Other Sample Type
Solid
Mounting Type
Pressed on a diamond cristal

Close cycle highly stable cryostat

Description
A cryogenic system allowing infrared transmission measurements for samples at temperature ranging from 400K to 4K has been developed for the condensed matter measurements (branch B). This system includes a pulse tube Helium close cycle cryogenerator provided by Cryomech (PT 405) working with a closed loops of helium cooling down samples at 4K in 1h30.

A specific chamber connected to the spectrometer IFS125 BRUKER, the cold head and the sample holder of the cryostat were designed and developed at SOLEIL (see figure below). Specific optic reduces the spot size at the sample by a factor 2 allowing measurement of small sample (less than 1mm) as well as an optimal alignment under vacuum. The vacuum level of the spectrometer and the beam-line (less than 10-5 mbar) allows connecting directly (without supplementary windows) the cryostat chamber and the spectrometer thus avoiding absorption and/or multiple fringes by windows.
Base Pressure
1 * 10-3 [mbar]
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid
Other Sample Type
Solid
Mounting Type
Specifics sample holders adapted for solid samples, pellets and liquid samples have been developed.
Required Sample Size
X = 1 [mm], Y = 1 [mm]

Gas cells

Description
The AILES beamline is equipped with various cells. The goal is to generate optical paths up to a few hundred meters in a controlled enclosure cooled down between 350 and 100K, with vacuum systems capable of handling the appropriate gas mixtures without generating extraneous vibration, harmful to the quality of the measure.
The characteristics of the cells are:
• Allowing an optical path from 10 cm up to a few hundered meters with at least 10% transmission.
• Compatibility with a wide optical range (20-4000 cm-1).
• High stability and accuracy measurements even at low temperature and pressure.

The cool cell optical system allows for temperature in the 80-300 K ±1K. The pressure will be controlled from 100 to 0.1 with an accuracy of 0.001 mbar.
Spectrometer
10-3 mbar
Base Pressure
0.1 [mbar]
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Gas
Other Sample Type
cooles gas (down to 100K), corrosive gas (down to 100K)
Required Sample Volume
0.2 * 10-3 [mL]

High Pressure and Low Temperature

Description
This set-up is placed into a separated compartment and use two focusing Cassegrain optics. Infrared measurements can be made in transmission and reflectivity, using a diamond anvil cell.
A small quantity of the sample to study is mixed to a binder transparent in infrared (polyethylene in the FIR, KBr or NaBr in the MID) and then loaded in a 250 µm hole drilled in a pre-indented gasket. A ruby inserted in this space is used to calibrate pressure. The pressure is controlled in the range up to 80GPa and the set-up allow measurements by steps of 1 to 2 GPa . The sample can be cooled down to 20K thanks to a helium closed cycle cryostat.
Microscopes
x 25
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid
Other Sample Type
Solid

Hydration Cell

Description
This copper designed cell allow: (i) temperature control between 380 K and 40 K; (ii) dosage of the desired amount of adsorbed gas; (iii) pumping down to 10-6 mbar for reference measurements free from molecular adsorption. The cell was designed to study the modifications to the infrared spectra following molecular adsorption. The use of a unique cell, in a wide spectral domain, provides complementary information and insures the reproducibility of the adsorption and gas dosage.

The cell is made in copper in order to allow for good thermal exchange and has a volume of ~1 cm3 to limit gas absorption at ambient pressure. It is UHV-compatible (leak rate > 1·10-9 mbar·l/s). The cell is connected to a closed-cycle cryostat by a copper braid for cooling and temperature resolved experiments (from 40 K to 380 K). A thermocouple and a resistive heater allow controlling the sample temperature during measurements with a precision of ± 0.1 K. The cell is equipped with two diamond windows (10 mm in diameter, 0.5 mm in thickness at center, 0.5° wedge) allowing to measure the transmission of material from the THz to the mid infrared region with reduced spectral channelling effects. The sample is fixed on a sample holder at precise normal incidence relative to the incident beam. An entry for the gas input/output or the vacuum pump is also present in the body of cell. Gas dosage can be done in static conditions.

During hydration measurements, the system is studied at equilibrium for a given value of relative humidity (defined as the ratio of partial water vapour pressure p and water vapour pressure p0 (31.7 mbar at 25°C) at a given temperature, RH=(p/p0)*100). A tube containing outgassed deionized liquid water (18.2 MΩ·cm-1 at 25°C) provides the vapour source. The vapour pressure is monitored by a thermostated gauge (0-100 mbar at ±0.02 mbar) and, once at equilibrium, the measurements are performed.
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Gas
Other Sample Type
Porous materials, adsorbed gas

Optical Set-up

Description
The A513/Q Bruker reflection accessory allows the measurement of the solids (or liquids) reflectivity for variable incidence angles between 13 and 85 degrees. The sample is placed in the horizontal plan of the set. The development of a motorized translation stage allows the simultaneous positioning and then the successive measurement of reflectance for 3 different samples. This setup is particularly well adapted for the study of non-transparent materials (Infrared Refection Absorption Spectroscopy of monolayers or sub-monolayers, Langmuir-Blodgett films, corrosion analysis, semiconductors,…). The control of the angle of incidence is made directly through the acquisition software, without breaking the vacuum in the spectrometer. The coupling with a motorized polarizer (also computer controlled) is possible.

The unit A510/Q-T is an accessory designed for both transmission and reflection measurements mainly in the MIR region. The great advantage of this unit is that the sample can be measured in transmittance and reflectance at exactly the same spot without the need of interrupting the spectrometer purge or venting the sprectometer (when working under vacuum condition). Typical applications are the spectroscopic analysis of solids (e.g. crystals, semiconductors), optical filters and window materials, accurate absorbance determination as well as low temperature transmittance and reflectance studies.

The motorized polarizer holder A121 allows a computer-controlled operation of the polarizer, i.e. measurement at different polarization angles without the necessity of opening the spectrometer sample compartment are possible. The polarizer holder can be rotated by 360° with an angle resolution of 0.25°.
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid
Other Sample Type
Solid

Temperature controlled Liquid cell

Description
The transmission studies of liquids as a function of the temperature in the range -75°C to 100°C is offered on the AILES beamline. The set-up is composed of a motorized tree axis motion, which allows the adjustment of the cell containing the sample without breaking the vacuum.
This cell is in contact with the cold tip of a closed cycle cryostat system for cooling the sample. Various windows (Diamond, Polyethylene, TPX, CaF2, ZnSe) allow spectroscopic studies in all the infrared range from 5cm-1 to 5000cm-1.
The thickness of the sample is defined by Mylar spacers ranging from 1 μm to 100 μm. In order to measure the temperature of the sample a Pt100 sensor is connected to the liquid cell containing the sample.
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid
Other Sample Type
Frozen liquid

Thin path electrochemical cell

Description
This set-up has been adapted for use with the synchrotron beamline AILES spectrometers. In particular, it can work under vacuum a necessary condition to increase the stability of the optics, the sensitivity of the measurements (less than 10-4 unity of absorbance), and hence the spectral resolution.
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Liquid

White-type cell dedicated to the study of stable molecules

Description
This multipass cell consists in a stainless steel cylindrical vacuum chamber of 2853 mm length and 600 mm diameter equipped with three mirrors in a White-type arrangement. The hard gold coated optics are spherical concave mirrors with 2526 mm radius of curvature and diameters of about 200 mm. An absorption path length of about 10 up to 180 m can be reached in this cell. Using this set-up one can perform gas-phase absorption spectroscopy in the FIR region for several kinds of samples. Thanks to the relatively long absorption pathlength, pure rotation as well as rovibration transitions of low frequency modes were obtained for samples with low vapor pressure at room temperature. Since 2009, 17 external projects have been successfully realized with that set-up (8 publications, 2 accepted papers). For more absorbing compounds, a smaller cell is available to cover the 0.8- 8 meter path length range.
Detectors Available
Bolometers
MCT detectors
InSb detectors
Endstation Operative
Yes

Sample

Sample Type
Gas
Detectors

Bolometers

Type
Adapted to the THz and far infrared
Description
Detectors response in the nsec (Bolometer Scontel) up to 10 ms, 1 microsec (hot electrons Bolometer), 1 msec (Bolometer Si)
Pixel Size
X = 1000 [um], Y = 1000 [um]
Array Size
X = 1 [pixel], Y = 1 [pixel]
Signal/NoiseRatio
1 * 10-6
Atomic Composition
Si, Pt layer

Detection

Detected Particle
Photon

InSb detectors

Type
Adapted to Near infrared
Pixel Size
X = 1000 [um], Y = 1000 [um]
Array Size
X = 1 [pixel], Y = 1 [pixel]
Signal/NoiseRatio
1 * 10-6
Atomic Composition
InSb

Detection

Detected Particle
Photon

MCT detectors

Type
Adated to Mid-infrared
Description
Detectors response 10 microsec (Rapid MCT)
Pixel Size
X = 1000 [um], Y = 1000 [um]
Array Size
X = 1 [pixel], Y = 1 [pixel]
Signal/NoiseRatio
1 * 10-6
Atomic Composition
Mercury Cadmium Telluride (MCT)

Detection

Detected Particle
Photon
contacts
ROY Pascale
BRUBACH Jean-Blaise
Techniques
Absorption
  • IR spectroscopy
  • THz spectroscopy
Emission or Reflection
  • Reflectrometry
Imaging
  • IR Microscopy
  • THz near-field microscopy
Scattering
  • Reflectivity
Disciplines
Chemistry
  • Atoms, molecules, clusters and gas-phase chemistry
  • Catalysis
  • Electrochemistry
  • Green Chemistry
  • Other - Chemistry
  • Physical Chemistry
  • Technique Development - Chemistry
Earth Sciences & Environment
  • Global change & Climate observation
  • Other - Earth Sciences & Environment
  • Technique Development - Earth Sciences & Environment
  • Water sciences/Hydrology
Energy
  • Technique Development - Energy
Engineering & Technology
  • Detectors
  • Technique Development - Engineering & Technology
Material Sciences
  • Knowledge based multifunctional materials
  • Other - Material Sciences
  • Technique Development - Material Sciences
Physics
  • Astronomy/Astrophysics/Astroparticles
  • Atomic & molecular physics
  • Hard condensed matter - electronic properties
  • Hard condensed matter - structures
  • Matter under extreme conditions, warm dense matter, plasmas
  • Nanophysics & physics of confined matter
  • Optics
  • Other - Physics
  • Soft condensed matter physics
  • Surfaces, interfaces and thin films
control/Data analysis
Control Software Type
  • OPUS LabView
Data Output Type
  • spectra
Data Output Format
  • ascii
Softwares For Data Analysis
  • OPUS Igor Origin