Electronic Resource
Copenhagen
:
International Union of Crystallography (IUCr)
Applied crystallography online
13 (1980), S. 425-432
ISSN:
1600-5767
Source:
Crystallography Journals Online : IUCR Backfile Archive 1948-2001
Topics:
Geosciences
,
Physics
Notes:
A unique low-temperature, full-circle goniometer for single-crystal X-ray diffraction has been constructed with the novel adaptation of a closed-cycle refrigerator in such a manner that the cold finger remains stationary during the φ and χ rotations. This has been made possible through the development of a flexible heat-transfer link between the top of the φ shaft and the cold station. The new design concept incorporates several important features: (1) the vacuum shroud and radiation shields also remain stationary so as to reduce the X-ray windows to narrow slots; (2) the sample crystal is enclosed in a black, nearly isothermal cavity (Hohlraum); and (3) the φ shaft is mechanically decoupled from the thermal contraction of the cold finger and other parts. The new system has considerable advantages over presently existing low-temperature adaptations for X-ray diffraction: (1) the goniometer operates between 300 and 18 K without expenditure of liquid cryogen and with minimal attendance; (2) the system is capable of operating for long periods of time with minimal risk of interruption of the cooling cycle; (3) absorption of X-rays by the windows is minimal and independent of the Bragg angle; and (4) data collection at any temperature down to its present lowest limit of 18 K is virtually as easy as with any conventional room-temperature diffractometer. At the time of writing the instrument has been in use for over 10000 h and has measured over 100000 X-ray reflections from single crystals.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1107/S0021889880012484
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