Closed-cycle helium refrigeration system

Fig. 1. Schematic representation of vacuum furnace closed-cycle helium refrigeration system used for metal vapor microsolution optical spectroscopy, as well as conventional metal vapor-matrix isolation experiments. (A) NaCl or Suprasil optical window, horizontal configuration (B) stainless steel vacuum shroud (C) NaCl or Suprasil optical viewing ports (D) cajon-rubber septum, liquid or solution injection port (E) gas deposition ports (F) vacuum furnace quartz crystal microbalance assembly. With the optical window in a fixed horizontal configuration, liquid or solution sample injection onto the window at any desired temperature in the range 12-300 K is performed in position 1A, metal deposition is conducted in position IB, and optical spectra are recorded in position 1C see Procedure).

Most previous attempts to obtain X-ray diffraction data at very low temperatures (< 80 K) have used custom built systems with closed cycle helium refrigerators mounted on large, robust four circle diffractometers. In order to remove the inherent disadvantages of these systems - cost, single application, absorption and scattering of the windows - we have built an open flow system from mainly off-the-shelf components which uses liquid helium as the cryogen. This is not the first open flow helium system [19, 20] but is the first that is mainly off-the-shelf and is mountable on any diffractometer. It is based on an ADP Helitran ESR cryostat with modifications to the nozzle assembly and to the direction of the gas flow. The lowest temperature is estimated to be <30K. At the current price for liquid helium in... 

Nowadays, the standard cryostats are closed-cycle helium refrigerators. They are commercially available. We use either the Displex Closed-Cycle System CSA from Air Products or the Closed-Cycle Compressor Unit RW 2 with Coldhead Base Unit 210 and Extension Module ROK from Leybold. These systems can run for thousands of hours with minimal maintenance. The sample holder can be cooled to temperatures from room temperature to about 10 K. A typical example of a closed-cycle helium matrix apparatus is shown in Figure 1.1. 

The X-ray diffraction studies at 13 K were performed by a Weissenberg-type low-temperature IP system equipped with closed cycle helium refrigerator. The oscillation photographs were taken around the >-axis. Figure 5.39(a) shows X-ray reflection spots in the (101) plane. At 300 K no satellite reflections were observed. Around 100 K very faint extra diffuse reflections were observed and at 80 K clear satellite reflections were observable. The satellite reflections grew at low temperature. Figure 5.39(b) shows P, Q satellite... 

The cryogenic adsorption system was specially developed to measure adsorption isotherms of H2 and D2. This system is equipped with a closed helium cycle two-stage Gifford McMahon refrigerator to operate under cryogenic conditions. The adsorption temperature can be kept constant within 0.03 K at 20 K. Adsorption isotherms are obtained by gas adsorption manometry. This method is based on the measurement of the gas pressure in a calibrated, constant volume, at a known temperature. The dead space volume was calculated from a helium calibration measurement at the temperature of interest. Thermal transpiration effect was calibrated according to the work by Takaishi and Sensui [41]. 

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