BESSY II
KMC-2 Diffraction and XANES

KMC-2 Beamline

The beamline provides an experimental set-up for EXAFS, XANES, and X-Ray fluorescence measurements at-air in the energy range of 4 keV – 15 keV. Beam intensity is stabilized by MOSTAB electronics with an accuracy of 0.3 %.

ENDSTATIONS

 

DIFFRACTION STATION

For X-Ray diffractometry and reflectometry the experimental hutch is equipped with a 6-axis HUBER goniometer and a VANTEC 2000 area detector. An alternative point detector for high angular resolution is available.

Applications

•    Grazing incidence diffraction (GID);
•    Reciprocal space mapping of single crystal Bragg reflections
•    Diffuse scattering
•    Powder diffraction
•    Anomalous diffraction
•    Reflectometry

 

XANES STATION

The KMC-2 XANES is a dedicated endstation to investigate the short-range environment around selected atomic species in condensed matter by X-ray Absorption Spectroscopy. This end-station provides possibility for EXAFS, XANES and X-ray fluorescence measurements at-air.

Applications

•    liquids, molecular solutions, liquid crystals;
•    single- and poly-crystalline materials;
•    amorphous and highly disordered solids;
•    molecules and macromolecules containing metallic atoms or partially substituted with heavy atoms.

 

For both endstations a variable suite of sample enviroment equipment is available, as well as a central user support by the sample environment department.

 

Beamline Resolving Power
2.5 * 10-4 [deltaE/E] @ 8000 [eV]
Beamline Energy Range
4 - 15 [eV]
Max Flux On Sample
1 * 1010 [ph/s] @ 8 [keV]
Spot Size On Sample Hor
5 - 250 [um]
Spot Size On Sample Vert
5 - 600 [um]
Photon Sources

Dipole DIP-09-2

Type
Bending Magnet
Source Divergence Sigma
X = 2.5 [urad], Y = 0.5 [urad]
Monochromators

Monochromator KMC

Energy Range
4000 - 15000 [eV]
Type
Double-crystal monochromator, first crystal water cooled, 2 SiGe 111 graded crystals, angular range 2.16° - 70°, feedback stabilization for EXAFS measurements
Refocusing Mirror Type
Rh-coated cylinder mirror with bending mechanics
Endstations or Setup

Diffraction

Description
The basis of the Diffraction endstation is a 6-circle goniometer in psi-geometry. The samples can be mounted on a motorized xyz-stage that allows movement in all directions as well as on variable sample holders for specialized sample environments (cryostats, furnaces, gas pressures). Two detectors are available: A scintillation detector (Cyberstar) and an area detector (Bruker Vantec). 2Θ angles up to 140° are accessible with the area detector. The instrument is located at the KMC-2 beamline, which provides X-ray radiation with very stable energies in the range between 4 and 14 keV.
Diffractometer
HUBER 6-circle goniometer in psi-geometry
Detectors Available
area detector
point detector
Endstation Operative
Yes

Sample

Sample Type
Crystal, Amorphous, Powder
Other Sample Type
Condensed Matter
Mounting Type
variable sample holders

Techniques usage

Diffraction / Crystallography
Yes
Diffraction / Powder diffraction
Yes
Diffraction / Surface diffraction
Yes
Scattering / Anomalous scattering
yes
Scattering / Elastic scattering
yes
Scattering / Wide angle scattering
Yes

Manipulator or Sample stage

Description
HUBER xyz translation insert for GM-cryocooler.
Degrees Of Freedom
3
Translator Stages
3
Degrees Of Freedom
3
Translator Stages
3

Sample Environment

Description
By this stage different capillary samples can be rotated about the capillary axis, which allows minimizing preferred sample orientations in powders or texture effects. The sample temperature can be regulated either by a cold air jet in the range from 240 K to 300 K, or alternatively by a hot air blower from 297 K to 850 K. The gas pressure in the sealed quartz or Kapton capillaries can be controlled by connecting them to a suitable gas dosing system. The gas pressure in the sealed quartz or Kapton capillaries can be controlled by connecting them to a suitable gas dosing system.
Pressure (Max)
100 [bar]
Temperature
240 - 850 [K]
Description
GM-cryocooler with heater stage for samples in vacuum or under controlled gas atmospheres at temperatures from 15K to 450K. Optional sample holders for reflection and transmission measurements are available, as well as a positioning stage for the cryo-cooler allowing finest sample adjustments.
Pressure (Max)
1.5 [bar]
Temperature
15 - 450 [K]
Description
N-Helix closed cycle operated cryo-jet to cool down small samples or sample capillaries in a temperature-controlled gas stream.
Temperature
20 - 300 [K]
Description
Anton Paar DHS 1100 furnace for experiments up to 1100 °C in air, inert gas or mild vacuum (10 mbar) without limitations on the movement of the goniometer.
Pressure (min)
10 [mbar]
Pressure (Max)
1013 [mbar]
Temperature
297 - 1373 [K]
Description
A custom-build Be-domed furnace with in-build turbopump for experiments up to 950 °C in high vacuum; this furnace is restricted to Θ-2Θ geometry.
Pressure (min)
1 * 10-5 [mbar]
Temperature
297 - 1223 [K]
Description
Custom build fully automated high-pressure volumetric gas dosing system for combined in-situ gas adsorption isotherm measurements at high pressures.
Pressure (Max)
200 [bar]
Description
BELSORP MAX fully automated low-pressure volumetric gas dosing system for combined in-situ gas adsorption isotherm measurements at low pressures.
Pressure (Max)
1.3 [bar]
Description
Custom built controller unit for continuous gas flow and pressure equipped with two independent flow controller 10 to 1000 mL/min and three independent pressure controllers for low- and high-pressure applications.
Pressure (min)
0.01 [bar]
Pressure (Max)
300 [bar]
Description
Teledyne ISCO 260D is able to pump (hazardous) gases and fluids independent at controlled constant flow rates and high pressures. Teledyne ISCO 260D for pumping (hazardous) gases and fluids independent at controlled constant flow rates and high pressures. The cylinder is equipped with a temperature-control jacket for optional thermal stabilization in the range from 10°C to 70°C. With its 260 ml cylinder volume the pump can deliver a precise 1 ml/minute for over 4 hours on a single fill. The 260D is ideal for a wide range of chemical feed applications up to 100 mL/min.
Pressure (Max)
517 [bar]

Sample Holders

Description
Polyimid tubes for liquid or powder samples under controlled gas atmospheres
Type
Powder sample holder for reflection geometry
Description
Sample can be placed in a variable 0.2 mm - 1.0 mm deep groove (10 mm diameter) of a flat Aluminum sample holder for Bragg-Brentano Scattering.
Type
Powder sample holder for transmission geometry
Description
Sample can be placed between two thin Kapton sheets of variable distance (0.2mm - 2mm).
Type
Hilgenberg Markröhrchen
Description
thin-walled quartz tubes for liquid or powder samples under controlled gas atmospheres

XANES

Description
The KMC-2 XANES is a dedicated endstation to investigate the short-range environment around selected atomic species in condensed matter by X-ray Absorption Spectroscopy. This end-station provides possibility for EXAFS, XANES and X-ray fluorescence measurements at-air. The detector system consists of three ionization chambers, Si-PIN photodiode, energy-dispersive detector (Bruker X-Flash 6|60) and scintillation counter. The experimental setup allows for a parallel monitoring of the transmitted through the sample X-ray beam intensity as well as for fluorescence yield measurements. This end-station attached to the KMC-2 beamline is providing medium photon flux between 4000 eV and 15000 eV and linear photon polarization, necessary to exploit the potential of X-ray absorption spectroscopy.
Base Pressure
1013 [mbar]
Detectors Available
energy-dispersive detector
photodiodes Si-PIN
ionization chambers
Endstation Operative
Yes

Sample

Sample Type
Crystal, Amorphous, Fiber, Powder, Gel, Liquid, Gas

Techniques usage

Absorption / EXAFS
Yes
Absorption / NEXAFS
Yes
Emission or Reflection / Micro XRF
Yes
Emission or Reflection / X-ray fluorescence (XRF)
Yes

Manipulator or Sample stage

Description
xyz translation and z-rotation
Degrees Of Freedom
4
Translator Stages
3

Sample Environment

Description
The furnace can host sample capillaries for XANES investigations in transmission and fluorescence mode. The sample temperature can be regulated by a hot air blower. The gas pressure in the sealed quartz or Kapton capillaries can be controlled by connecting them to a suitable gas dosing system.
Pressure (Max)
100 [bar]
Temperature
297 - 700 [K]
Description
GM-cryocooler with heater stage for samples in vacuum or under controlled gas atmospheres at temperatures from 15K to 450K. Optional sample holders for reflection and transmission measurements are available, as well as a positioning stage for the cryo-cooler allowing finest sample adjustments.
Pressure (Max)
1.5 [bar]
Temperature
15 - 450 [K]
Description
Custom build fully automated high-pressure volumetric gas dosing system for combined in-situ gas adsorption isotherm measurements at high pressures.
Pressure (Max)
200 [bar]
Description
BELSORP MAX fully automated low-pressure volumetric gas dosing system for combined in-situ gas adsorption isotherm measurements at low pressures.
Pressure (Max)
1.5 [bar]
Description
Custom built controller unit for continuous gas flow and pressure equipped with two independent flow controller 10 to 1000 mL/min and three independent pressure controllers for low- and high-pressure applications.
Pressure (min)
0.01 [bar]
Pressure (Max)
300 [bar]
Description
Teledyne ISCO 260D is able to pump (hazardous) gases and fluids independent at controlled constant flow rates and high pressures. Teledyne ISCO 260D for pumping (hazardous) gases and fluids independent at controlled constant flow rates and high pressures. The cylinder is equipped with a temperature-control jacket for optional thermal stabilization in the range from 10°C to 70°C. With its 260 ml cylinder volume the pump can deliver a precise 1 ml/minute for over 4 hours on a single fill. The 260D is ideal for a wide range of chemical feed applications up to 100 mL/min.
Pressure (Max)
517 [bar]

Sample Holders

Type
Polyimid
Description
Clip sample holder with Kapton windows for powder or flat samples.
Description
Polyimid tubes for liquid or powder samples under controlled gas atmospheres
Type
Hilgenberg Markröhrchen
Description
thin-walled quartz tubes for liquid or powder samples under controlled gas atmospheres
Detectors

area detector

Type
VANTEC 2000
Description
Scintillator

Detection

Detected Particle
Electron

energy-dispersive detector

Type
Bruker X-Flash 6|60
Description
scintillation counter

Detection

Detected Particle
Photon

ionization chambers

Detection

Detected Particle
Ion

photodiodes Si-PIN

Detection

Detected Particle
Photon

point detector

Detection

Detected Particle
Photon
Support Laboratories

DEGAS (GasLab)

Description

The DEGAS laboratory offers a suite of modular experimental equipment dedicated to supplementing sample characterization by gas adsorption analysis or sample preparation issues, i.e. degassing.


X-ray Corelab

Description

The X-ray Corelab covers different X-Ray diffraction methods at HZB locations Adlershof (WCR) and Wannsee (LMC) and makes them available to all interested co-workers of HZB as well as for guests.


contacts
Dr. Daniel Többens
Dr. Götz Schuck
Techniques
Absorption
  • EXAFS
  • NEXAFS
Diffraction
  • Crystallography
  • Powder diffraction
  • Surface diffraction
Emission or Reflection
  • Micro XRF
  • Reflectrometry
  • X-ray fluorescence (XRF)
Scattering
  • Anomalous scattering
  • Elastic scattering
  • Wide angle scattering
Disciplines
Chemistry
  • Catalysis
  • Other - Chemistry
  • Physical Chemistry
Earth Sciences & Environment
  • Geology
  • Mineralogy
  • Other - Earth Sciences & Environment
Energy
  • Other - Energy
  • Sustainable energy systems
Material Sciences
  • Knowledge based multifunctional materials
  • Metallurgy
  • Other - Material Sciences
Physics
  • Hard condensed matter - structures
  • Nanophysics & physics of confined matter
  • Other - Physics
  • Soft condensed matter physics
  • Surfaces, interfaces and thin films
control/Data analysis
Control Software Type
  • PC-based BESSY monochromator control system EMP/2
Data Output Type
  • tbc
Data Output Format
  • tbc
Softwares For Data Analysis
  • Windows-NT, RADICON RDPW software
Other Equipment Available On Site
Glovebox for sample preparation under dry Argon atmosphere.
in partnership with