Sample Environments
The Brockhouse beamlines share several sample environments. If you'd like to use one in your next run, please mention it in your proposal.
Oxford Cryostream 800 Plus
Provides temperature control from 80 – 500 K (-193 – +226ºC) by blowing nitrogen gas over the sample. Maximum ramp rate is 6º/minute. We have two of these on mobile carts. They can be used on all three beamlines.
(Above left) Cryostream running on the Bruker endstation. (Above right) Following a phase change in KNO3, from orthorhombic to trigonal, using X-ray powder diffraction. Diffraction patterns were collected from 124ºC to 144ºC in 2º steps with the cryostream on the Huber endstation.
High Temperature Gas Flow Furnace
Temperatures up to 1473K (1200ºC) with gas flow. Samples are loaded in quartz capillaries with outer diameters of up to 3 mm. Based on the P. Chupas design (P. J. Chupas et al., J. Appl. Cryst. 41, 822, 2008). For details on setting up the furnace, refer to the BXDS High Temperature Gas Flow Furnace manual. Please reach out to the beamline staff for the manual.
(Above left) Setup of the high temperature gas flow furnace. (Above right) In-situ heating X-ray diffraction patterns of nickel oxide electrodes (N Zhang et al 2023 J. Electrochem. Soc. 2023, 170, 070515).
Dual Sample Higher Temperature Flow Cell
Temperatures up to 1273 K (+1000ºC) with gas flow. Samples are in capillary format, and two can be loaded at a time. Quartz capillaries are available at the BXDS beamlines. Also based on the P. Chupas design (P. J. Chupas et al., J. Appl. Cryst. 41, 822, 2008).
(Above left) Dual sample higher temperature flow cell. (Above right) Demonstrated temperature setpoint accuracy.
Helium Cryostat
Advanced Research Systems, Model DE202A-G-T. Enables low temperature experiments down to 10 K (-263ºC), with a beryllium dome over the sample. Samples can also be heated to 450 K (+177ºC). The mounting is very specific to the Huber diffractometer in the IVU beamline. Other implementations may be possible with advanced notice.
(Above left) The helium cryostat set up to measure PXRD on the Huber endstation. (Above right) A view of the powder sample with the beryllium domes removed.
Heating/cooling stage with gas atmosphere
Linkam HFSX350-GI. This stage is quite flexible. It can be oriented horizontally for use with planar samples and grazing incidence measurements. It can also mount vertically and accept standard capillary samples. There is a flush-mounted heating/cooling element. The body can be water cooled. It has gas-in and gas-out ports, and a controlled environment is possible by fabricating a custom lid. It is fully integrated to BXDS beamline software, SPEC.
- Temperature range: 77 to 623 K (-196 to 350°C). Integrated 100 ohm platinum resistor sensor
- Heating rate: 30°C per minute
- Temperature stability: <0.1°C
(Above left) Heating a planar sample in grazing incidence, WLE beamline. (Above right) Heating a capillary sample in transmission. (Below right) Cooling a planar sample in Bragg-Brentano. (Below left) Heating a sample in trasnmission, WHE beamline.