Ultra-low-temperature X-ray data collection with a newly developed 0.1 mm Kapton-film cylinder for a closed-cycle helium cryostat

2003 ◽  
Vol 36 (6) ◽  
pp. 1452-1454 ◽  
Author(s):  
Marc Meserschmidt ◽  
Mathias Meyer ◽  
Peter Luger
Keyword(s):  
Low Temperature ◽  
Data Collection ◽  
Vacuum Chamber ◽  
Closed Cycle ◽  
X Ray ◽  
Helium Cryostat ◽  
Fine Pitch ◽  
Low Costs ◽  
Data Collections ◽  
Ccd Detectors

A 0.1 mm Kapton-film vacuum chamber was constructed to be mounted on the cold head of a closed-cycle helium cryostat. The use of Kapton instead of beryllium results in a low and practically non-structured background, which is thus tolerable on the area-detection frames of modern CCD detectors. The Kapton chamber is only fixed at the upper and lower holders of the cryostat and its counterweight, and is stabilized by spanning with fine pitch threads, holding constant the necessary vacuum of 10−6 mbar for at least several days. Low costs and non-toxicity are further advantages of this material; moreover, the sample remains visible even after cooling. Data collections on strychnine single crystals at 15 K showed improvedI/σ ratios of high-order reflections compared with 100 K data, most favourably when synchrotron primary radiation was used.

Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis

1998 ◽  
Vol 53 (12) ◽  
pp. 1528-1530 ◽  
Author(s):  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Data Collection ◽  
Single Crystals ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Mecn Solution

Abstract Benzo-18 -crown-6 -Acetonitrile (1/2), Crystal Structure Single crystals of the title complex resulted fortuitously during an attempt to co-crystallise MeN(SO2Me)2 with benzo-18-crown-6 from an MeCN solution at -30 °C. The crystal structure has been determined via data collection at -100 °C (monoclinic, space group P21/n, Z = 4). The nitrile molecules are located with their me­ thyl groups above and below the plane of the 18-membered crown ring, the Me hydrogen atoms being rotationally disordered about the MeCN axes; C(methyl)···O(crown) distances range from 309.4(3) to 384.9(3) pm.

Low Temperature X-Ray Diffractometer with Closed Cycle Refrigeration System

1978 ◽  
Vol 22 ◽  
pp. 89-99
Author(s):  
U. Benedict ◽  
Y. Cornay ◽  
C. Dufour
Keyword(s):  
Phase Transformation ◽  
Low Temperature ◽  
Thermal Gradient ◽  
Quartz Crystal ◽  
Powdered Sample ◽  
Closed Cycle ◽  
Refrigeration System ◽  
Lattice Contraction ◽  
X Ray ◽  
Metallic Foils

An assembly consisting of an X-ray tube, a quartz crystal monochromator, and a vertical X-ray goniometer with proportional counter was mounted in a glove box for work with actinide metals and compounds. An evacuated camera containing the expander tube of a closed-cycle cryogenic system was fitted onto the goniometer. A thin layer of the powdered sample was fixed on the end-plate of the expander tube. Beryllium windows were provided in the camera wall for the incident and for the diffracted beam.The cooling camera is suitable for use with thin powder layers or metallic foils. Thicker layers can be studied, but a strong thermal gradient perpendicular to the specimen surface is expected. The camera has been applied to the study of lattice contraction and phase transformation at low temperature In actinide metals and compounds .

scholarly journals Gaining information at low temperature with laboratory capillary X-ray powder data collection

2004 ◽  
Vol 60 (a1) ◽  
pp. s226-s226
Author(s):  
P. Fernandes ◽  
A. Florence ◽  
N. Shankland ◽  
W. I. F. David ◽  
K. Shankland
Keyword(s):  
Low Temperature ◽  
Data Collection ◽  
X Ray

A novel low-temperature X-ray goniometer with closed-cycle cooling to about 18 K

1980 ◽  
Vol 13 (5) ◽  
pp. 425-432 ◽  
Author(s):  
S. Samson ◽  
E. Goldish ◽  
C. J. Dick
Keyword(s):  
Low Temperature ◽  
Closed Cycle ◽  
X Ray

New high- and low-temperature apparatus for synchrotron polycrystalline X-ray diffraction

1998 ◽  
Vol 5 (3) ◽  
pp. 929-931 ◽  
Author(s):  
C. C. Tang ◽  
G. Bushnell-Wye ◽  
R. J. Cernik
Keyword(s):  
High Temperature ◽  
Low Temperature ◽  
Closed Cycle ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Temperature Furnace ◽  
Wide Range ◽  
Powder Samples ◽  
Heater Coil ◽  
Temperature Furnace

A high-temperature furnace with an induction heater coil and a cryogenic system based on closed-cycle refrigeration have been assembled to enhance the non-ambient powder diffraction facilities at the Synchrotron Radiation Source, Daresbury Laboratory. The commissioning of the high- and low-temperature devices on the high-resolution powder diffractometer of Station 2.3 is described. The combined temperature range provided by the furnace/cryostat is 10–1500 K. Results from Fe and NH4Br powder samples are presented to demonstrate the operation of the apparatus. The developments presented in this paper are applicable to a wide range of other experiments and diffraction geometries.

Low Temperature Attachment For X-Ray Powder Diffractometry

1993 ◽  
Vol 37 ◽  
pp. 457-463 ◽  
Author(s):  
H.W. King ◽  
M.A. Peters ◽  
E.A. Payzant ◽  
M.B. Stanley
Keyword(s):  
High Temperature ◽  
Barium Titanate ◽  
Low Temperature ◽  
Phase Transformations ◽  
Vacuum Chamber ◽  
X Ray ◽  
Temperature Range ◽  
Beryllium Window ◽  
Open Cycle

AbstractA low temperature attachment based on a miniature open-cycle Joule-Thomson refrigerator has been developed for x-ray diffractometry measurements over the temperature range from 65 - 400 K, By use of a special mounting plate, the device can be substituted for the heater assembly of a high temperature attachment and thereby utilize the available vacuum chamber and x-ray transparent beryllium window. The device is demonstrated by investigating the polymorphic phase transformations that occur in barium titanate.

A low-temperature X-ray Weissenberg goniometer with closed-cycle cooling to about 28 K

1982 ◽  
Vol 15 (2) ◽  
pp. 241-244 ◽  
Author(s):  
W. Adlhart ◽  
H. Huber
Keyword(s):  
Heat Transfer ◽  
Low Temperature ◽  
Single Crystal ◽  
Scattered Radiation ◽  
Angular Range ◽  
Closed Cycle ◽  
Cold Finger ◽  
X Ray ◽  
Crystal Rotation

A low-temperature camera for single-crystal X-ray investigation between 28 and 350 K has been developed for a modified Weissenberg goniometer. Cooling is provided by a double-stage cryorefrigerator which is firmly attached to the low-temperature camera. Stranded copper cables ensure a flexible heat transfer between crystal and cold finger allowing a crystal rotation of 180°. Compared to the usual Weissenberg technique almost no further limitation is given on the accessible angular range of the scattered radiation.

Magnetically coupled crystal holder and liquid-helium cryostat for X-ray four-circle diffractometer studies between 5 and 300 K

1989 ◽  
Vol 22 (6) ◽  
pp. 584-591 ◽  
Author(s):  
R. Argoud ◽  
J. Muller
Keyword(s):  
High Pressure ◽  
Low Temperature ◽  
Liquid Helium ◽  
Controlled Atmosphere ◽  
Helium Flow ◽  
X Ray ◽  
Cell Parameters ◽  
Data Collections ◽  
Crystal Holder ◽  
Goniometer Head

A new low-temperature system for X-ray four-circle diffractometer studies down to 5 K has been developed. The crystal is mounted on a new holder which is magnetically coupled to the diffractometer. This coupling is achieved by mounting a master magnet in place of the classical goniometer head. This master magnet drives a slave magnet fixed on the new crystal holder, and therefore the crystal is indirectly oriented by the master magnet. This magnetically coupled crystal holder (MCCH) is enclosed in a helium-flow cryostat which remains stationary during the φ, χ and to movements. The χ value is limited to ±65° and ω to 40° for a 150 mm diameter χ circle. All the tests and data collections (from 5 to 15 d) gave accuracies on the intensities, cell parameters and atomic positions identical to those obtained with a classical goniometer head. No frost problem occurs with this apparatus. The MCCH may also have applications in controlled-atmosphere, high-pressure or vacuum investigations.

Simple Method for the Handling of Crystals at Low Temperature: Application to the X-Ray Structure Determination of But2P(=NSiMe3)NHSiMe3 and [But2P(NSiMe3)2]Li·(thf)2

2002 ◽  
Vol 55 (4) ◽  
pp. 249 ◽  
Author(s):  
A. J. Edwards ◽  
E. Wenger
Keyword(s):  
Low Temperature ◽  
Data Collection ◽  
Structure Determination ◽  
Molecular Structures ◽  
Simple Method ◽  
Dry Ice ◽  
X Ray ◽  
Temperature Application

Crystals of the very soluble iminophosphonamide species But2P(=NSiMe3)NHSiMe3 (1) and [But2P(NSiMe3)2]Li�(thf)2 (2) have been obtained and were mounted at dry-ice temperature using a propan-2-ol matrix for X-ray data collection at 100 K. This very simple method for handling the crystals at low temperature is described together with the resulting molecular structures of (1) and (2).

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