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 Flow Cell

Provides temperatures up to 1073 K (+800ºC) with gas flow for capillary format samples. Based on the design of P. Chupas (P. J. Chupas et al., J. Appl. Cryst. 41, 822 (2008)). Quartz capillaries are available at the BXDS beamlines. This cell can be used on all three beamlines.

(Above) High temperature flow cell operating on the Huber endstation.

 

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.