European Synchrotron Radiation Facility
ID02 - Time-resolved SAXS/WAXS/USAXS

The beamline ID02 is primarily a combined small-angle, wide-angle, and ultra small-angle scattering instrument (SAXS, WAXS, USAXS, respectively). The high brilliance of an undulator source is exploited to probe the microstructure and non-equilibrium dynamics of soft matter and related systems from a few Angstroms to micron scale, and down to sub-millisecond time range. On specific systems, it is now possible to perform ultra-small-angle X-ray photon correlation spectroscopy USA-XPCS which allows probing equilibrium dynamics in the micron range.

The scientific application of the ID02 beamline can be broadly divided into three domains; (1) soft condensed matter, (2) noncrystalline structural biology, and (3) interdisciplinary areas of soft matter, biology, and nanoscience. Soft matter studies most often involve probing the equilibrium and the nonequilibrium microstructure, while the structural biology work is largely centered around the structure-function relationship. In the interdisciplinary topics, the hierarchical structure of the self-assembled exotic nanostructures is elucidated.

Some of the techniques used in softmatter research can be directly applied to industrial research and development problems.

Beamline Energy Resolution
2 * 10-4 [eV] @ 12400 [eV]
Beamline Energy Range
8000 - 20000 [eV]
Max Flux On Sample
1 * 1014 [ph/s] @ 12400 [eV]
Spot Size On Sample Hor
20 - 900 [um]
Spot Size On Sample Vert
10 - 100 [um]
Divergence Hor
0.01 - 0.025 [mrad]
Divergence Vert
0.006 - 0.01 [mrad]
Transverse Coherence Length At Sample Position Vert Value
10 - 30 [um]
Transverse Coherence Length At Sample Position Hor Value
10 - 20 [um]
Endstations or Setup

Default

Sample

Sample Type
Other:

Manipulator or Sample stage

Description
This set-up allows to mount 8 sealed capillaries of diameter ranging from 1 to 2mm. The temperature can be varied from 5 to 120 °C. Best adapted for measurements around 12.4keV are quartz capillaries with a diameter of 1.5 or 2.0mm. Please make also sure to carefully verify the diameter of the capillaries before using. This ensures faster loading of the samples and facilitates intensity calibration of the scattering curves.
The set-up is less adapted for the study of low scattering liquid samples due the difficult background subtraction using different capillaries for sample and solvent.
Description
Four position sample changer:
The temperature (5 to 100 °C) is controlled by a Peltier element. The samples are contained in liquid tight aluminium cells with thin mica or mylar windows. The sample thickness can be 0.5, 1.0 or 2.0 mm. The setup is available for all users. However, windows have to be provided by the users (supplier info).
Description
Industrial sample changer:
A more advanced version of the above setup is available explicitly for industrial experiments. 30 sample cells can be placed at the same time. The temperature is controlled by Peltier elements and can be varied from 10 to 120 °C in less than 30 minutes. The gas tight sample cells are made of aluminum with nickel coating and mica windows.

Sample Environment

Description
High pressure cell:
It is based on a high force piezo stack (Piezo Systems Jena) which can dynamically compress a small volume (~50 ml) and reach a pressure up to 1 kbar in less than 1 ms. Smaller amplitudes of a few 100 bar can be reached in a few 100 ms. This cell also permits to perform static SAXS/WAXS experiment up to 1.5 kbar and 100°C. The pressure windows are polished diamond (thickness ≈ 1 mm) and the stability is within a few bars.
Description
Linkam heating stage:
(THMS600/TMS94) It can perform faster temperature ramping and quenching (up to 80 °C/min, nominal stability of 1 °C) primarily in crystallization studies. This setup can also be used to change the sample temperature over a wide temperature range (-100 to 600 °C). An adaptor to mount solid samples (in the form of a circular disc - diameter 3 to 10 mm) and liquid samples (in sealed capillaries of diameter 1 mm) is available
Description
Mettler heating stage:
(FP90/FP84HT) : It is used to perform programmed temperature ramping and quenching (20 °C/min, nominal stability of 0.1 °C) primarily in crystallization studies. In addition, this setup can be used to change the sample temperature over a wide range (25 to 350 °C depending on the sample container availability). The solid samples (in the form of a circular disc - diameter 3 to 10 mm) can be mounted directly and the liquid samples can be contained in sealed capillaries (diameter 1 to 2 mm).
Description
Peltier controlled flow-through cell:
This flow-through capillary cell is operated in air. Two types of capillary are available: one made from bio-compatible polycarbonate with a wall-thickness of either 0.1 mm or 0.05 mm and a diameter of 2.0 mm. The second type is a quartz-capillary, of which a range of different diameters is available (1.0 mm - 2.0 mm). Using the flow-through cell allows reliable measurement of sample and solvent scattering of low scattering liquid samples (reliable background subtraction!). A temperature range between 5 to 80 °C is accessible.
Description
Stopped-flow rapid mixing device:
The device is based on a commercial instrument (BioLogic, SFM-400) with four stepper motor driven syringes and three mixers. A home-made SAXS/WAXS flow-through capillary cell (diameter ~1.6 mm) is adapted to the mixing chamber. The flow can be stopped with millisecond accuracy using a solenoid driven hard-stop. The dead time of mixing is about 2 ms for flow rates exceeding 7 ml/sec. This device can also be used to effect a temperature jump over the range 5 - 70 °C with a few millisecond deadtime.
Description
Stress controlled Rheometer:
The stress controlled rheometer is a commercial Haake RS6000 and the shaft drives an X-ray transparent couette cell. The concentric cylinders (inner diameter 20 mm, outer diameter 22 mm, and height 40 mm) are machined out of polycarbonate (lower background) or aluminum (for higher temperatures up to 170 °C and good organic solvents) with wall thickness around the beam position ~100 µm. Minimum sample volume required is about 2.5 ml. For highly viscous samples, a plate-plate type shearing geometry is available.

Magnetic Fields

AC Fields
Magnetic field system:
It is based on permanent magnets arranged periodically as in the undulator. The field can be varied from 0.1 mT to 1.5 T. The direction of the magnetic field can be either perpendicular or parallel to the beam direction. An oven adapted for both capillaries and flat cells is also available to perform measurements in the range of temperature (25 to 300 °C). This setup can be used as an alternative to shear flow in the case of mineral liquid crystals.
Max AC Field
1 [T]
contacts
Peter BOESECKE
Michael Sztucki
Narayan THEYENCHERI
Techniques
Scattering
  • Coherent scattering
  • Small angle scattering
  • Time-resolved scattering
  • Wide angle scattering
control/Data analysis
Control Software Type
  • SPEC
Data Output Type
  • Normalized 2D scattering pattern with all beamline meta data in the header
Data Output Format
  • ESRF data format and HDF5 for 2D and ASCII for azimuthally averaged data
Softwares For Data Analysis
  • SAXS Utilities, SPD, PyFAI, Fit2D, etc.
in partnership with