The X-ray diffraction facilities of ISIC comprise 8 instruments dedicated to powder, thin film and single crystal X-ray diffraction.
- Available Instrumentation
- Sample Environments
Diffractometers available at ISIC
Single Crystal diffraction:
- 2 Supernovas (Oxford Diffraction, Rigaku) – BCH 2117 and 2118
- Venture (Bruker) – I17 0 I2
- Apex II (Bruker Nonius) – BCH 2118
Powder and thin film diffraction:
- D8 Advance (Bruker) – I17 0 I2
- D8 Discover (Bruker) – I17 0 I2
- D8 Discover Vario (Bruker) – BCH 2118
- D8 Discover Plus TXS (Bruker) – BCH 2118 – to be installed 05/2020
Surface analytics at ISIC
- Supra XPS (Kratos) – I17 -1 L6
- Raman microscope (Renishaw) – I17 -1 L6
2 Supernovas (Oxford Diffraction, Rigaku)
Both Supernovas are equipped with low temperature devices (Oxford Cryosystems) allowing to perform measurements between 80 K and 400 K. Each instrument has a dual microsource (Copper and Molybdenum) to optimize measurement strategies in terms of absorption and data collection time. The spot size on the sample is approximately 100 micron. Open access measurements are possible on one of the supernovas after a thorough training in data collection and basic analysis.
The D8 Venture single crystal diffraction setup is placed in a much larger enclosure compared to the Supernovas, allowing for more space to work with non-ambient sample cells and related configurations such as gas systems or lasers. This setup can also be used to measure thin films in basic 2D Grazing Incidence configuration. Our Venture is currently laid out for samples with significant absorption and is powered by a Mo-microsource, the beam spot is 120 micron in the goniometer center.
The D8 Advance is our full open-access high throughput powder diffractometer. A robotic sample changer is available allowing to run automized serial measurements on different samples. The D8 Advance runs on a standard Cu-source that can be switched between line and point focus, and acquires data with and energy dispersive Si-strip detector (Lynxeye XE) that allows for energy discrimination due to sample fluorescence. The integrated Twin-Twin optics enable fast, user-friendly and reproducible change of optics for different instrumental configurations.
This allows to routinely perform powder diffraction in reflection and transmission, as well as grazing incidence diffraction on thin films. Transmission measurements can be performed between room temperature and approx 1000 K.
We host two Bruker D8 Discover systems. The first is dedicated to high-throughput measure- ments using a dwell plate using a double-laser system and an XYZ stage for automated sample allignment. Up to 96 samples of millimeter size can be measured in one run, sw. The XYZ stage allows to perform Grazing Incidence X-ray diffraction (out-of-plane) on thin films, using parallel beam or focussing optics.
The second D8 Discover is dedicated to in-situ studies of powder samples in reflection and transmission geometry. The instrument is run on a Cu-source and a Vantec-1 gas detector for high speed diffraction, allowing to obtain time resolutions well below one second (accessible two-theta range in snap-shot mode approx. 10° 2T). Various home-made non-ambient sample cells are available and continuously extended. An example of such a cell is shown on the right, designed to measure under gas pressures up to 200 bar within a temperature range of approx 100 K to 800 K.
A variety of sample environments are available on the different open-access and restricted-access instruments, allowing to carry out “in-situ” studies of materials under external stimulus. In particular, the XRD Platform is continuously developing novel sample chambers in collaboration with its users and the ISIC workshops in order to meet specific needs. Please do not hesitate to contact Dr. Pascal Schouwink to discuss your ideas and projects or if you do not find the specific sample environment here. It is possible that it already exists, but has not been updated on this page yet. As of October 2016 the available sample environments are:
- Temperature range 80 – 400 K (-193 – 127 °C)
- Possibilities do exist to perform single crystal measurements under vacuum or a specific gas atmopshere in glas capillaries, provided the crystals diffract well enough. The options need to be discussed with users case by case.
Powder samples/Thin films
- Transmission measurements (glass capillary) between 25 and 1000 °C.
- Transmission and reflection measurements under protective gas atmosphere or in liquid.
- Transmission measurement under static gas pressure (Pmax about 50 bar) or vacuum.
- Reflection measurements between 25 and 400 °C.
- Reflection measurements under cryogenic conditions (currently developed).
- Reflection measurements under gas pressure or flow/atmosphere (Pmax about 200 bar, currently in development).
The different instrumental setups allow to measure a large variety of samples. These include all kinds of polycrystalline materials, such as powder samples, nanoparticles, thin films, polymers but also printed materials, heterostructures, mechanical parts or devices. Usually mg amounts of a respective sample are sufficient. A large number of samples can also be screened to evaluate the feasibility of further experiments. In general the specific requirements and the desired information are discussed together prior to experiment.
Samples: some examples of commonly measured samples are shown on top, from left to right: Metalorganic framework (MOF) powder sample, polymer beads, perovskite thin film, perovskite film with electrode. bottom, left to right: Solid Oxide Fuel Cell (SOFC), high throughput sample changer for synthesis robot (before and after loading), powder under Argon atmosphere in glass capillary.