Sample environments and equipment
All sample positioners and sample environments for the PXRD2D instrument are aligned using the main hexapod. Specifications of the hexapod can be found here: https://symetrie.fr/en/hexapods/breva/
To simplify mounting and exchanging different setups we have designed a bespoke kinematic mount. Detailed drawings for designing you own sample environment can be found at the bottom of this page.
At DanMAX we strive to develop a large portfolio of positioners and sample environments to allow a wide range of experiments. Here is the once currently available at the beamline:
A spinner directly driven by a stepper motor. Can rotate with up to 5 Hz. Uses manual Huber 1002 goniometer heads for alignment. Samples are mounted using SPINE magnetic caps.
The spinner can be configured in three different ways: Rotation around the vertical axis (minimum SDD ~170 mm), rotation around the horizontal axis centered on the hexapod (minimum SDD ~170 mm), and rotation around the horizontal axis downstream end on the hexapod (PDF configuration, minimum SDD ~ 95 mm). The PDF configuration can unfortunately not be used with the Cryostream.
Rotation and XRD-CT:
A Huber 408 goniometer mounted with the rotation axis in vertical orientation on top of a linear stage (X). Manual Huber 1002 goniometer heads are used for alignment of the sample. The goniometer is not equipped with an encoder. For XRD-CT the linear stage is scanned continuously and rotation is done in steps.
The recommended sample mount on the PXRD2D instrument is the SPINE magnetic base system developed for macromolecular crystallography. These bases can be used as is for capillaries up to Ø 0.5 mm. If larger capillaries are needed it is possible to drill a larger hole in the base.
We have successfully used CrystalCap SPINE HT (Hampton Research HR8-112) at DanMAX, but other vendors (e.g. Mitegen or Molecular Dimensions) have similar products.
The hexapod allows for flexibility when aligning the capillary to the beam position and allows the beam to intersect the capillary all the way from the top of the base and up to 50 mm along the capillary.
The recommended length of the capillaries are approximately 25 mm from the top of the base (this will allow the use of the protective SPINE caps as well). If the capillary will be used with the Cryostream positioned co-axially the capillary should be longer to limit the cooling of the base and goniometer head.
2D scanning stage based on two Standa 8MT50 stages https://www.standa.lt/products/catalog/motorised_positioners?item=308&prod=motorized_translation_stages with rotary encodes and a full step resolution of 5 µm. Scan area 150 mm by 100 mm. One of the two axis can be used for continuous scans. The stage is equipped with a Newport M-BKL-4 kinematic base for easy exchange of the sample holder.
Available sample holders:
- Holder for 6 AMPIX (REF) cells (2 pieces available at DanMAX).
- Holder for mapping flat samples. Holds two 44 mm by 44 mm plates (~0.5-1 mm thick) with various aperture designs for thin samples.
- Empty kinematic top plates for user equipment.
X scanning stage:
1D scanning based on a Standa 8MT50 stages https://www.standa.lt/products/catalog/motorised_positioners?item=308&prod=motorized_translation_stages with rotary encodes and a full step resolution of 5 µm. Scan length 200 mm. Can be used for continuous scans. The stage is equipped with a Newport M-BKL-4 kinematic base for easy exchange of the sample holder.
To position other equipment in the beam we have a generic M6 25 mm pitch breadboard that can be mounted on the hexapod.
Diamond Anvil Cell holder:
RY + XZ motion to align a diamond anvil cell (DAC) precisely in the X-ray beam. The holder is mounted on a kinematic base to allow off-line Raman spectroscopy. It further supports gas membranes for pressure control.
Capillary reactor setup for in-situ solvothermal experiments. The pressure is provided by an HPLC pump and heat with the HyBec heater. The system is enclosed in a splash box to prevent spills. The system is compatible with both PXRD and PDF (Qmax; ~17 Å-1).
Oxford Cryosystems Cryostream 800plus:
Liquid nitrogen cryostream capable of operating from 80 to 500 K (https://www.oxcryo.com/product/cryostream-800). Ramp rates from 1 to 360 K/h (0.0166 to 6 K/min). The cryostream can be used with the capillary spinner in horizontal and vertical geometry (but not in PDF configuration) and with the rotation stage.
Automatic refill is possible ensuring continuous operation. Control, monitoring, and metadata collection is implemented in the control system. Positioning of the cryostream is flexible but manual.
HyBec Heater (RT – 1000 K):
Heat gun with resistive heating of air or nitrogen gas. Placed below the sample through the hole in the hexapod.
Building / interfacing your own sample environments to DanMAX:
To minimise the time used to install and align user supplied sample environments we propose that users design their setups to match the kinematic mount installed on the large hexapod on the instrument. A detailed drawing of the interface and SE envelope can be found here, and a reference CAD model of the user supplied interface plate is available here. Any equipment must be approved by MAX IV and DanMAX staff before use. Please contact the DanMAXstaff for information about interfacing to other systems, e.g. control system, motion control, compressed air etc.
Lakeshore model 336 (https://www.lakeshore.com/products/categories/overview/temperature-products/cryogenic-temperature-controllers/model-336-cryogenic-temperature-controller) temperature controller with thermocouple card. Temperatures are recorded by the control system.
Biologic VMP3 potentiostat (https://www.biologic.net/products/vmp3/) with 14 channels (meta data not collected by control system yet).
PandABox (https://quantumdetectors.com/n/products/pandabox/) used for handling triggering in- and outputs (TTL signals) in addition to facilitating continuous scans. Please contact the DanMAX staff before submitting you proposal requiring TTL triggering.
Gas mixing panel (under construction). The panel makes it possible to mix two different gases and use these in either flow or static conditions up to 200 bar. The system can be purged via a vacuum line. Only non-toxic and non-flammable gases are permitted at this time. Please contact DanMAX staff before submitting you proposal requiring the use of gas.
Sample Environments and Detector Support (SEDS) group at MAX IV
The SEDS group maintain a pool of shared sample environments – check out their pages for details of what is available: Sample Environment and Detector Support (SEDS)
In the Sample Environment area adjacent to the control room, it is possible to manipulate benign samples. Dangerous and/or toxic samples must be handled in the chemistry laboratory across the hall. Please contact the DanMAX staff to book the chemistry lab if needed.
Equipment in the Sample Environment area:
- Microscope: Olympus SZX16 microscope with 0.5x and 1.0x objectives. Digital camera and encoder on zoom.
- Capillary filling equipment (may be moved to the chemistry lab if needed)
- Soldering iron and heat gun – please consult the DanMAX staff for safety guidelines before using the equipment.
- 10 ton press
Equipment in the chemistry laboratory
- Polishing equipment
- Vacuum oven