Low Temperature X-Ray Diffractometer with Closed Cycle Refrigeration System

1979 ◽  
pp. 89-99 ◽  
Author(s):  
U. Benedict ◽  
Y. Cornay ◽  
C. Dufour
Keyword(s):  
Low Temperature ◽  
Closed Cycle ◽  
Refrigeration System ◽  
X Ray

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 .

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

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.

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.

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.

Low temperature x-ray microanalysis of frozen-hydrated tobacco leaves

1984 ◽  
Vol 42 ◽  
pp. 284-285
Author(s):  
S. Edith Taylor ◽  
Patrick Echlin ◽  
May McKoon ◽  
Thomas L. Hayes
Keyword(s):  
Low Temperature ◽  
Lemna Minor ◽  
Root Tips ◽  
Tobacco Leaves ◽  
X Ray ◽  
Whole Cells ◽  
Carbon Coated ◽  
The Right ◽  
Beam Currents ◽  
The University

Low temperature x-ray microanalysis (LTXM) of solid biological materials has been documented for Lemna minor L. root tips. This discussion will be limited to a demonstration of LTXM for measuring relative elemental distributions of P,S,Cl and K species within whole cells of tobacco leaves.Mature Wisconsin-38 tobacco was grown in the greenhouse at the University of California, Berkeley and picked daily from the mid-stalk position (leaf #9). The tissue was excised from the right of the mid rib and rapidly frozen in liquid nitrogen slush. It was then placed into an Amray biochamber and maintained at 103K. Fracture faces of the tissue were prepared and carbon-coated in the biochamber. The prepared sample was transferred from the biochamber to the Amray 1000A SEM equipped with a cold stage to maintain low temperatures at 103K. Analyses were performed using a tungsten source with accelerating voltages of 17.5 to 20 KV and beam currents from 1-2nA.

Bulk standards for low-temperature biological x-ray microanalysis

1984 ◽  
Vol 42 ◽  
pp. 282-283
Author(s):  
P. Echlin ◽  
M. McKoon ◽  
E.S. Taylor ◽  
C.E. Thomas ◽  
K.L. Maloney ◽  
...  
Keyword(s):  
Phase Separation ◽  
Low Temperature ◽  
Analytical Method ◽  
Salt Solutions ◽  
Absolute Concentration ◽  
Cooling Process ◽  
X Ray ◽  
The Absolute ◽  
Analytical Procedures ◽  
Electrical Conductors

Although sections of frozen salt solutions have been used as standards for x-ray microanalysis, such solutions are less useful when analysed in the bulk form. They are poor thermal and electrical conductors and severe phase separation occurs during the cooling process. Following a suggestion by Whitecross et al we have made up a series of salt solutions containing a small amount of graphite to improve the sample conductivity. In addition, we have incorporated a polymer to ensure the formation of microcrystalline ice and a consequent homogenity of salt dispersion within the frozen matrix. The mixtures have been used to standardize the analytical procedures applied to frozen hydrated bulk specimens based on the peak/background analytical method and to measure the absolute concentration of elements in developing roots.

Micro X-Ray Diffraction Study of Polycrystalline MgB 2 Wire and Evaluation of Carbon Doping Effect Via Low-Temperature Sintering

2019 ◽  
Author(s):  
Minoru Maeda ◽  
Dipak Patel, Dr. ◽  
Hiroaki Kumakura, Dr. ◽  
Gen Nishijima, Dr. ◽  
Akiyoshi Matsumoto, Dr. ◽  
...  
Keyword(s):  
Low Temperature ◽  
Diffraction Study ◽  
Carbon Doping ◽  
Doping Effect ◽  
Low Temperature Sintering ◽  
X Ray Diffraction ◽  
X Ray

The Application of X-Ray Diffraction at Elevated Temperatures to Study the Mechanism of Formation of Sodium Tripolyphosphate

1961 ◽  
Vol 5 ◽  
pp. 276-284
Author(s):  
E. L. Moore ◽  
J. S. Metcalf
Keyword(s):  
High Temperature ◽  
Low Temperature ◽  
Amorphous Phase ◽  
Elevated Temperatures ◽  
Sodium Tripolyphosphate ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Temperature Form ◽  
High Temperature Form

AbstractHigh-temperature X-ray diffraction techniques were employed to study the condensation reactions which occur when sodium orthophosphates are heated to 380°C. Crystalline Na4P2O7 and an amorphous phase were formed first from an equimolar mixture of Na2HPO4·NaH2PO4 and Na2HPO4 at temperatures above 150°C. Further heating resulted in the formation of Na5P3O10-I (high-temperature form) at the expense of the crystalline Na4P4O7 and amorphous phase. Crystalline Na5P3O10-II (low-temperature form) appears after Na5P3O10-I.Conditions which affect the yield of crystalline Na4P2O7 and amorphous phase as intermediates and their effect on the yield of Na5P3O10 are also presented.

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