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BL04 - MSPD
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Sample environments & preparation
Sample Environments

Although updated regularly, information on this page might be incomplete. Please, refer to the User Office Portal for the latest equipment lists. If you have any doubts, would like to integrate user cells or additional equipment as well as to verify availability of the sample environment, please contact the beamline staff.

Powder Diffraction

FMB Oxford hot air blower

Temperature range: RT – 1223K (RT – 950°C).

To be used with samples in capillaries (quartz ones for temperatures above 700°C)

Detailed description of the equipment can be found at the manufacturer's website

FMB Oxford hot air blower.png

Oxford cryostream 700 series

Temperature range: 80K – 450K

To be used with samples in capillaries

Detailed description of the equipment can be found at the manufacturer's website

Oxford cryostream 700 series.png

Dynaflow liquid He cryostat

Temperature range: 10 – 300K

To be used with samples in capillaries and MAD detection setup

For detailed description refer to Van der Linden et al. Review of Scientific Instruments 87, 115103 (2016).

Dynaflow liquid He cryostat.png

Capillary flow cell

Based on the design described in Chupas et al. J. Appl. Cryst. (2008) 41, 822-824.

Heating and cooling using either Oxford Cryostream or FMB Oxford hot air blower. Available in the constant pressure (0 – 50 bar) or constant flow (0.1 – 5 ml/min, Bronkhorst gas flow controller) mode.

Can be used either with thick wall quartz capillaries (OD 1mm / ID 0.8mm) or with 0.8 mm flexible fused silica capillaries. The capillary is mounted using standard 1/16" x 1.0mm or 1/16" x 0.8mm graphite ferrules.

Convenient to fill capillaries can be purchased from Hilgenberg (ref 4000104, Glass capillaries made of quartz glass, one end cut, one end funnel formed approx. Ø 2,0 +1,0/-0,5 mm,L= 100 ± 2 OD= 1 ± 0,1 ID= 0,58 ± 0,1 S= 0,21 mm)

Capillary flow cell.png

Equipment for the electrochemical studies

2 x 4 channels BioLogic VSP potentiostat/galvanostat

4/8 coin cells holder for CR2032, CR2025 or CR2016 cells

holder for up to 3 Leriche type cells

MTI MSK-110 coin cell crimping tool is available in the chemistry laboratory (Ar glove 

Equipment for the electrochemical studies_1.png

Equipment for the electrochemical studies_2.png

High Pressure

On-line pressure calibration set-up (ruby luminescence method)

Pressure can be controlled using BETSA PDS-200 manual pressure drive system or Sanchez APD-200 automatic pressure drive

On-line pressure calibration set-up.jpeg

In-air external ring heater (50 & 60 mm diameter)

Temperature range: RT – 600 K

BETSA external ring heater.jpeg

External heating vacuum system

 Temperature range: RT – 900K

External heating vacuum system.jpeg

lHe Cryostat

Temperature range: 15K – RT

lHe Cryostat.jpeg

Navitar 12X online visualization system

The distance between the Navitar light and the sample at the focus position is around 18mm. For bulky
samples the ring light can be removed (and put an external light) increasing the distance up to ~35mm. The graphical user interface allows to measure any set of the predefined points, perform line scans or grid scans. The Navitar 12X is equipped with an analyzer for the polarized light in reflection.

Navitar 12X online visualization system.jpeg

Sample Preparation
Powder Diffraction

Absorption should be considered since it might be an issue for samples which contain heavy elements. Calculate the linear absorption coefficient, μ (in cm-1), of the sample at the wavelength at which data will be acquired. Note, to minimise absorption correction μ*r should be <1, where r = radius of capillary (in cm) and μ must take into account the packing density (generally 40-60%). The following web pages provide tools to calculate it: APS absorption tool and NIST scattering tables.

Standard set-up consists of powder samples loaded into glass capillaries. Next, a video that gives an idea for the first time users. Quartz and borosilicate capillaries of diameter 0.3, 0.5, 0.7, 1.0 and 1.5 mm are available at the beamline. For other dimensions, massive usage or if preferred to fill capillaries at home, capillaries can be ordered from e.g; www.hilgenberg-gmbh.de, www.wjm-glas.de, www.capillarytubes.co.uk

The composition of the samples should be made known to the local contact since fluorescence reduces the signal-to-noise ratio of the MYTHEN detector considerably. This problem can be avoided (in most cases) with the correct beamline configuration.

Battery Lab

Find out more details of the equipment available for you

High Pressure

We have several types of Diamond Anvil Cell (DAC) available:

  • piston-cylinder LeToullec-type with a gas-driven membrane for pressure generation (available commercially @Betsa).
  • plate DAC (Almax Boehler-type).
  • pneumatic DAC membrane-free for low pressure regime.

Depending on the material of the DAC the working temperature range goes from room temperature to low and high temperatures.

For all the DACs the working pressure depends on the diamond culet size installed.

DAC_1.jpg

DAC_2.jpg

DAC_3.jpg

The diamond anvil cells (DACs) should be requested by the users 4 weeks prior to experiment. Please contact beamline staff to verify availability of DACs.

Users should be aware they are responsible of the delicate equipment used during the experiments and must strictly follow the beamline staff instructions.

Misuse of DAC is particularly addressed since it can lead to diamond breakage!!!

Instrumental Resolution
Powder Diffraction

The instrumental resolution on the Powder Diffraction station depends on the detection setup, capillary size and incoming beam divergence. Angle dependence of the peak FWHMs for various configurations at 20 keV is illustrated. The instrumental resolution has been determined by refining a Na2Ca3Al2F14 sample. This compound is known for not introducing sample induced broadening and owing to its low density can be measured at soft energies in transmission mode. The crystal structure is described in Courbion and Ferey, Journal of Solid State Chemistry (1988) 76, 426 10.1016/0022-4596(88)90239-3

Angle dependence of the peak FWHMs HP.png

GSAS and FullProf instrument parameter files for some typical photon energies and capillary diameters can be downloaded using the links below. Additional information on this topic can be found at Kaduk, J. A., & Reid, J. (2011). Typical values of Rietveld instrument profile coefficients. Powder Diffraction, 26(1), 88–93 and references therein.

Detector

Energy

Capillary diameter

GSAS parameter file

FullProf parameter file

MYTHEN

13 keV

0.3 mm

Mythen_13keV_03mm.prm

BL04_MYTHEN_13keV_03mm.irf

  

0.5 mm

Mythen_13keV_05mm.prm

BL04_MYTHEN_13keV_05mm.irf

  

0.7 mm

Mythen_13keV_07mm.prm

BL04_MYTHEN_13keV_07mm.irf

  

1.0 mm

Mythen_13keV_10mm.prm

BL04_MYTHEN_13keV_10mm.irf

 

20 keV

0.3 mm

Mythen_20keV_03mm.prm

BL04_MYTHEN_20keV_03mm.irf

  

0.5 mm

Mythen_20keV_05mm.prm

BL04_MYTHEN_20keV_05mm.irf

  

0.7 mm

Mythen_20keV_07mm.prm

BL04_MYTHEN_20keV_07mm.irf

  

1.0 mm

Mythen_20keV_10mm.prm

BL04_MYTHEN_20keV_10mm.irf

 

30 keV

0.3 mm

Mythen_30keV_03mm.prm

BL04_MYTHEN_30keV_03mm.irf

  

0.5 mm

Mythen_30keV_05mm.prm

BL04_MYTHEN_30keV_05mm.irf

  

0.7 mm

Mythen_30keV_07mm.prm

BL04_MYTHEN_30keV_07mm.irf

  

1.0 mm

Mythen_30keV_10mm.prm

BL04_MYTHEN_30keV_10mm.irf

MAD

13 keV

1.0 mm

MAD_13keV_10mm.prm

BL04_MAD_13keV_10mm.irf

 

20 keV

 

MAD_20keV_10mm.prm

BL04_MAD_20keV_10mm.irf

 

38 keV

 

MAD_38keV_10mm.prm

BL04_MAD_38keV_10mm.irf

High Pressure

The instrumental resolution on High Pressure Endstation is angular resolution dependent. Powder diffraction patterns on a standard LaB6 (NIST standard 660b) were collected for this purpose. Angle dependence of the peak FWHMs for various configurations at different energies is illustrated below. Angular dependence of the peak FWHM at Powder Diffraction Endstation using Mythen detector is represented for comparison purposes. One can notice that the angular resolution at the HP station is inferior to the PD station counterpart due to angular limitations.

Angle dependence of the peak FWHMs HP.png

Recommended FullProf and GSAS instrument parameters for some typical photon energies and sample-to-detector distances are given below. Note that due to low angular range of the HP station these values are less reliable than those of the PD station.

Energy

Sample-to-detector distance

gsas parameters

  

fullprof parameters

  
  

GV

GW

LY

V

W

X

29.2 keV

180 mm

-8.82

6.20

18.0

-0.00489

0.00344

0.180

 

220 mm

-7.71

5.69

11.5

-0.00428

0.00316

0.115

 

260 mm

-5.82

4.79

10.9

-0.00323

0.00266

0.109

 

300 mm

-2.92

3.93

10.8

-0.00162

0.00218

0.108

23.2 keV

300 mm

-2.69

3.68

11.4

-0.00149

0.00204

0.114

38.9 keV

170 mm

-8.92

6.40

22.4

-0.00495

0.00355

0.224

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