If you want to submit a proposal to perform an experiment at NCD-SWEET, we encourage you to read the general ALBA user website and the beamline section 'proposal submission' to find useful information. Do not hesitate to contact the beamline staff for any inquiries.

 

DESCRIPTION

NCD-SWEET beamline is devoted to:

  • Small and Wide Angle X-ray Scattering in transmission (SAXS & WAXS)
  • Grazing Incidence Small and Wide Angle X-ray Scattering (GISAXS & GIWAXS)

SAXS  is a technique used to study the structure and morphology of materials at the nanoscale. It involves scattering X-rays at small angles (< 5 degrees) and analyzing the scattered pattern to determine information about particle size, shape, and arrangement. Complementarily, WAXS provides information about crystal structures, phase transitions, and atomic ordering in materials by recording large scattering angles (> 5 degrees). Recording simultaneously SAXS and WAXS results in a length scale which ranges from a few microns to a few angstroms.

By its part, the grazing incidence configuration fulfills the necessity to investigate nanoscale objects at surfaces, buried interfaces or in thin films using a grazing incidence X-ray beam (< 1 degree). GISAXS provides information about the size, shape, and arrangement of nanoscale structures, while GIWAXS provides detailed information about the crystallographic structure, orientation, and phase transitions within the material.

These techniques are commonly used in various fields, including materials science, chemistry and biology. As illustration, a non-comprehensive list of examples of systems and materials that can be studied at NCD-SWEET beamline using the X-ray scattering technique are: biomaterials, biological macromolecules, catalysts, ceramic materials, colloids, energy materials (solar cells, batteries), fibers, geological materials (minerals, rocks), inorganic nanomaterials, lipid bilayers, liquid crystals, membranes, mesoporous materials, nanocomposites, nanoparticles, paints and coatings, pharmaceuticals (amorphous and crystalline forms), porous materials, self-assembled monolayers, soft matter systems, supramolecular assemblies, surfactants and emulsions,thin films and multilayers.

 

IM_NCDSWEET-BeamlineInfo1  IM_NCDSWEET-BeamlineInfo2 

 

BEAMLINE OPTICAL LAYOUT

NCD-SWEET beamline optical layout with the main components. Below, a more detailed information is provided. 

NCD-SWEET optical layout

TECHNICAL SPECIFICATIONS

General specifications for the NCD-SWEET beamline. The actual values were matching the expected theoretical calculations.

Wavelength range/Energy range   0.62 - 1.90 Å / 6.5 -20 keV
Flux at sample position > 1.5·1012 ph/s at 12.4 keV @ 150 mA
Bandpass (ΔE/E) 2.7 10-4 at 10.0 keV
Beam size at sample position 130 µm x 130 µm (H x V)
Sample detector distance 2.1 - 7.2 m (SAXS) | < 300 mm (WAXS)

COMPONENTS

Source: In-vacuum undulator (IVU21)

The NCD-SWEET beamline is tunable over a wavelength range of 0.62Å - 1.90Å and delivers a high-photon flux onto the sample, the beam has an excellent beam collimation and photon density, and is also highly stable. For this purpose the photon source of this beamline is an undulator, IVU21, placed in a medium 4 m straight section.
Here some parameters of the IVU21 are presented:

Material Sm5Co17 Pure Permanent Magnet
Period 21.6 mm
Number of periods 92
K at minimum gap 1.6
Photon source size (FWHM) 309 x 18 µm2 (H x V)
Photon source divergence (FWHM) 112 x 28-22 µrad2 (H x V)

Optics

The chosen optical layout is aimed at delivering high-photon flux onto the sample: A channel cut Si (111) monochromator is used to obtain the monochromatic X-ray beam with a ∆E/E of 2.7·10-4 at 10.0 keV. Then, the X-ray beam is collimated with an array of 3, 6, or 9 Be lenses. A set of microfocussing Be lenses is also available to focus the X-ray beam on the sample position, obtaining a beam size of 4 × 10 µm2 (V × H) at 12.4 keV. Along the beamline, several 4 sets of slits vertical and horizontal slits are used to define and clean the X-ray beam. Before the sample, an in vacuo fast shutter is placed that only opens if data acquisition is demanded, minimizing the sample irradiation unless needed.

Centre of ID U21 0 m
Trigger unit separating Optics hutch and Front End 17 m
Channel cut monochromator Si (111) 22 m
Collimating Be lenses 24.3 m
Microfocussing Be lenses 32 m
Sample position 32.5 m
SAXS Sample-Detector distance 2.1 m up to 7.2 m

DETECTORS

The beamline currently uses a single hybrid-pixel photon counting detector for (GI)SAXS and a CDD detector for (GI)WAXS experiments. The SAXS detector is supplied by Dectris (Pilatus3 S 1M) and the WAXS detector by Rayonix (LX255-HS). 

Visitors to the line must consider the actual sample-to-detector distance and choose it correctly in order to record the data of interest. In this context you need to consider the active area of the detector that will allow you to record the q-range of interest. Moreover, you must bear in mind that the accessible q-range for both SAXS and WAXS recordings is a function not only of the sample-to-detector distance, but also of the energy of the monochromatic photon beam.

Detectors specifications

 

Pilatus3 S 1M (Dectris)

LX255-HS (Rayonix)

Mode (GI)SAXS (GI)WAXS
Active image area 168.7 x 179.4 mm2 (H x V) 85 x 255 mm2 (H x V)
Total number of pixels 981 x 1043 pixels (H x V) 1920 pixels x 5760 pixels (H x V)
Pixel size (not binned) 172 x 172 µm2 44.27 x 44.27 µm
Frame rate 25 frames/s 10 - 140 frames/s (binning dependent)
Dynamic range 20 bits 16 bits

Working distances: The Pilatus detector can be placed from 2.1 to 7.2 m from the sample position, while the Rayonix detector has a maximum distance of 300 mm in GIWAXS configuration.

A micro ion chamber monitors the incoming beam intensity (I0) after the available fast shutter and before the sample, while the transmitted beam intensity (I1) is monitored using a photodiode on the corresponding beamstop.

SAMPLE ENVIRONMENT

NCD-SWEET beamline is a flexible multipurpose beamline that can accommodate a large variety of sample environments for in situ experiments (for example: spin coating systems, 3D printers, ALD reactors, electrochemical, battery or shear cells, furnaces, etc.). Here below you will find more information about the modular sample positioning system and some sample environment devices already available at NCD-SWEET beamline. Users are encouraged to bring their own equipment always following the safety regulations. 

Sample positioning

NCD-SWEET provides a sample positioning system that allows to move and tilt the sample position for performing your experiment. This is a modular setup that can be adapted for a specific experiment.

SamplePositioning

User sample environment

This modular configuration allows NCD-SWEET beamline to accommodate a large variety of user sample environments. If you would like to bring your own sample environment for an experiment, we strongly recommend discussing it with a member of the beamline team well in advance of submitting your proposal and coming to your experiment. The NCD-SWEET beamline staff can help you during the design phase of your setup to ensure a full compatibility with the beamline. 

Here below, some common sample environments available at NCD-SWEET beamline are described.

Linkam stages

Several linkam stages are available with temperature and force control (stretcher).

Linkam specifications
Linkam type Capillary - THMS350  Film - THMS600 Stretcher - TST350
Min Temp (ºC) -196 -196 -196
Max Temp (ºC) 350 600 350
Min Rate (ºC /min) 0.01 0.01 0.01
Max Rate (ºC /min) 30 150 60
Min speed (µm/s)     1
Max speed (µm/s)     1000
Force resolution (N)     0.01

Temperature control:

In addition to the different Linkam stages described, there is a NanoDAC temperature controller also available at the beamline to read/control the temperature of a system from the beamline.

Cooling system:

A chiller (-10  to 80 ºC) is available with manual control. General water cooling lines with a pressure regulator and flow sensor from ALBA are also available. The connections follow the metric using 10 mm OD tubes as main tube for cooling systems.

Gas system:

NCD-SWEET beamline provides a gas injection and exhaust system for using gases for an experiment. Please, contact the beamline staff to ensure that the gas of interest (pressure, composition, volume) can be used for your experiment and that is delivered on time (2 months before your experiment).

  • Exhaust: 2 x KF40 connections are available to connect the sample environment to an independent ATEX certified extraction system
  • Injection: Limited with a pressure up to 10 bar, there are 8 pressure regulators with 1/8" or 1/4" connections for: 2 inert, 2 mix, 3 flammable mix, 1 oxygen gas bottles. 

Pneumatic valve controller:

A pneumatic controller is available to open/close pneumatic valves from the beamline controls system. It can control up to 8 pneumatic lines (max. 6 bars) but it can be extended in the future.

Sample holders:

Some pictures of the available sample holders for in situ and ex situ experiments at NCD-SWEET beamline.

  • SAXS & WAXS
 

Non thermo-stated ladder for 38 capillaries

(1mm, 1.5mm or 2mm diameter)

Thermo-stated ladder for 38 capillaries

(1 mm or 2mm diameter) 

CapillaryRack ThermostatedMultiCapillaryRack
Film holder for 176 samplesLinkam stretcher - TST350
Film Holder LinkamStretcher
Linkam capillary  - THMS350Linkam film - THMS600
LinkamCapillary LinkamFilm

 

  • GISAXS & GIWAXS
 
Rotation rodLarge sample holder
rotationrod sampleholder
Multiple samples holderTemperature control - Adapted THMS600
multisampleholder LinkamGI
Temperature controlled solvent annealing 
Annealing