A near-ambient-temperature-control cell for use with synchrotron X-ray powder diffraction

1995 ◽  
Vol 28 (5) ◽  
pp. 651-653 ◽  
Author(s):  
R. J. Cernik ◽  
S. R. Craig ◽  
K. J. Roberts ◽  
J. N. Sherwood
Keyword(s):  
Powder Diffraction ◽  
Temperature Control ◽  
Low Cost ◽  
Control Cell ◽  
Temperature Stability ◽  
Free Rotation ◽  
Melting Points ◽  
X Ray ◽  
Rotator Phase ◽  
Better Than

A low-cost cell has been designed and built for synchrotron X-ray powder diffraction studies of materials with low melting points. The cell has been operated between 253 and 323 K with a temperature stability of better than 0.1 K. The construction of the cell allows free rotation of the sample during a scan in order to maximize the number of powder grains in the reflecting position. The cell has been used to study a transition from an ordered to a rotator phase in hexadecane occurring at 278 K and the results from that study are reported.

A scanning CCD detector for powder diffraction measurements

2013 ◽  
Vol 46 (4) ◽  
pp. 1058-1063
Author(s):  
B. H. Toby ◽  
T. J. Madden ◽  
M. R. Suchomel ◽  
J. D. Baldwin ◽  
R. B. Von Dreele
Keyword(s):  
Data Collection ◽  
Powder Diffraction ◽  
Low Cost ◽  
Source Image ◽  
X Ray ◽  
Analyzer Crystal ◽  
Ccd Detector ◽  
Position Sensitive ◽  
Position Sensitive Detectors ◽  
Better Than

Several different approaches have traditionally been used for detection of X-ray powder diffraction patterns, including area detectors, point detectors and position-sensitive detectors. Each has advantages. This paper discusses use of a low-cost CCD detector attached to a diffractometer arm, where line-by-line readout of the CCD is coupled to continuous motion of the arm. When this type of detector is used and where X-ray optics are employed to focus the source image onto the detector plane both high-resolution and rapid measurements can be performed, with data collection over a complete 2θ range. This is particularly advantageous for synchrotron applications but valuable also for Guinier diffractometer laboratory instruments. Peak resolutions are shown to be moderately better than what can be obtained with a position-sensitive detector and significantly better than with an area detector. Many samples have intrinsically broadened peak shapes for which little improvement in data quality could be obtained with an analyzer-crystal detector. With comparable numbers of modules, these CCD data collection speeds can be close to those with position-sensitive detectors, but without the low-angle asymmetry seen in the latter.

Automated pressure and temperature control apparatus for x‐ray powder diffraction studies

1992 ◽  
Vol 63 (2) ◽  
pp. 1763-1770 ◽  
Author(s):  
P. T. C. So ◽  
S. M. Gruner ◽  
E. Shyamsunder
Keyword(s):  
Powder Diffraction ◽  
Temperature Control ◽  
X Ray ◽  
Control Apparatus

New X-ray powder diffraction data for two triborates CsB3O5(CBO) and TlB3O5(TBO)

1999 ◽  
Vol 14 (3) ◽  
pp. 234-236 ◽  
Author(s):  
M. Touboul ◽  
N. Pénin ◽  
L. Seguin
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Powder Diffraction Data ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray ◽  
Figures Of Merit ◽  
Diffraction Patterns ◽  
Better Than

Precise X-ray powder diffraction patterns of two isostructural triborates, CsB3O5(CBO) and TlB3O5(TBO), have been collected on a D5000 diffractometer with a primary monochromated beam (λ CuKα1=1.5406 Å). Refinement of indexed reflections in the space group P212121 led to: a=6.201(1) Å, b=8.514(2) Å, c=9.176(2) Å, Z=4, Dx=3.363 for CBO and a=5.2156(4) Å, b=8.2659(6) Å, c=10.2240(9) Å, Z=4, Dx=4.773 for TBO. The Smith–Snyder figures of merit are F30=53.0 (0.0101, 56) for CBO and F30=112.9 (0.0074, 36) for TBO. These values are much better than the previous ones published in Powder Diffraction File.

Liquid Metal Based Stretchable Radiation-Shielding Film

2015 ◽  
Vol 9 (1) ◽  
Author(s):  
Yueguang Deng ◽  
Jing Liu
Keyword(s):  
Liquid Metal ◽  
Metal Film ◽  
Low Cost ◽  
Practical Method ◽  
Radiation Shielding ◽  
X Ray ◽  
Lead Particle ◽  
Temperature Liquid ◽  
Shielding Material ◽  
Better Than

We reported a stretchable and flexible radiation-shielding film based on room-temperature liquid metal. Conceptual experiments showed that the liquid metal based printing technology can achieve an ultrathin flexible radiation-shielding film with a thickness of 0.3 mm. Moreover, the yield strength and ultimate strength of the liquid metal film appear much better than those of a conventional lead-particle-containing radiation-shielding material. In order to evaluate the radiation-shielding performance of the liquid metal material, X-ray radiation experiments to compare the liquid metal film and conventional lead-particle-based shielding material under different stretching conditions were performed. The results indicate that the liquid metal shielding film could achieve a certain radiation-shielding performance. Furthermore, because of the screen-printing properties of liquid metal, a low-cost X-ray mask method using a liquid metal selective radiation-shielding film was also studied, which could serve as a highly efficient and practical method for the medical X-ray shielding applications or semiconductor lithography industry.

A Sample Holder for X-Ray Powder Diffraction Studies of Flakiness and Block Sample

2013 ◽  
Vol 544 ◽  
pp. 433-436
Author(s):  
Hua Yong Zhang ◽  
Xiao Jian Liu ◽  
Hai Yan Sun ◽  
Chun Sheng Fan
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Low Cost ◽  
Sample Holder ◽  
X Ray Diffraction ◽  
X Ray ◽  
Block Sample ◽  
Powder Diffractometer ◽  
Analytical Results ◽  
Sample Carrier

Powder X-ray diffraction (XRD) is one of the primary techniques used to characterize solid state materials. But there is not a sample holder which can be fit into the sample carrier of the Bruker D8-Advance x-ray powder diffractometer for flakiness and block samples test. In this article, we will design, manufacture and evaluate a sample holder for flakiness and block samples. Materials of the holder are steel, glass and plasticine etc. The holder is low cost, easy to be processed, convenience to prepare the samples, and accurately obtain the best analytical results.

Physico-Chemical Characterization of Some 5,5-Disubstituted-1,3-Dixanthyl Barbituric Acids

1967 ◽  
Vol 21 (4) ◽  
pp. 225-231 ◽  
Author(s):  
B. C. Flann ◽  
J. A. R. Cloutier
Keyword(s):  
Experimental Data ◽  
Powder Diffraction ◽  
Infrared Spectra ◽  
Chemical Characterization ◽  
Melting Points ◽  
X Ray ◽  
Physico Chemical ◽  
Diffraction Patterns ◽  
Derivatives Of

The dixanthyl derivatives of 21 clinically important barbituric acids have been prepared. Melting points, infrared spectra, and x-ray powder-diffraction patterns of the purified compounds are presented. Infrared evidence is used to discuss the position of the linkage between the xanthyl and barbiturate portions of the derivatives. The experimental data should prove of particular value for the microchemical identification of barbiturates.

Préparation, Identification et Radiocristallographie d'un Hétérocycle Cétonique à Intérêt Médicinal: l'Isopropyl-3, phényl-2, diaza-1,3, one-5 bicyclo [3,3,0] octène-1

1990 ◽  
Vol 5 (1) ◽  
pp. 48-49
Author(s):  
Par Mme C. Caranoni ◽  
M.J.P. Reboul ◽  
Melle C. Soula
Keyword(s):  
Chemical Analysis ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Better Than

AbstractThe heterocycle of a functionalized 2-imidazoline, C15N2OH18, was obtained by reaction when 2-bromo, 2-alkenoïc ketone was allowed to react with a monosubstituted benzamidine. The compound presents a R*R* configuration. X-ray powder diffraction data have been obtained from single multifaceted brown crystals prepared at 273 K in benzene with triethylamine as catalyst. Chemical analysis gives a purity better than 99%. This compound crystallizes in the monoclinic space group P21/c [14]. The cell parameters were determined by employing single-crystal diffraction methods (Bragg and precession patterns) and were refined from accurate powder diffractometer data recorded at T = 293 (1) K.

Obtaining optimal structural data from X-ray powder diffraction using the Rietveld method

2014 ◽  
Vol 29 (4) ◽  
pp. 396-403 ◽  
Author(s):  
Shanke Liu ◽  
He Li ◽  
Jianming Liu
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Low Cost ◽  
Structural Data ◽  
Preferred Orientation ◽  
X Ray

Diffraction data of calcite were collected using a conventional Bragg–Brentano diffractometer, which is a convenient, low-cost, and highly popular in-house instrument, and its crystal structure was refined by the Rietveld method. This paper shows how one treats preferred orientation and how different refinement strategies affect the accuracy of the result.

scholarly journals Investigation of high-pressure planetary ices by cryo-recovery. I. An apparatus for X-ray powder diffraction from 40 to 315 K, allowing `cold loading' of samples

2018 ◽  
Vol 51 (3) ◽  
pp. 685-691 ◽  
Author(s):  
Ian G. Wood ◽  
A. Dominic Fortes ◽  
David P. Dobson ◽  
Weiwei Wang ◽  
Lucjan Pajdzik ◽  
...  
Keyword(s):  
High Pressure ◽  
Low Temperature ◽  
Powder Diffraction ◽  
Ambient Pressure ◽  
Temperature Stability ◽  
Extended Period ◽  
Turnaround Time ◽  
Normal Operation ◽  
X Ray ◽  
Sample Chamber

A low-temperature stage for X-ray powder diffraction in Bragg–Brentano reflection geometry is described. The temperature range covered is 40–315 K, with a temperature stability at the sample within ±0.1 K of the set point. The stage operates by means of a Gifford–McMahon (GM) closed-cycle He refrigerator; it requires no refrigerants and so can run for an extended period (in practice at least 5 d) without intervention by the user. The sample is cooled both by thermal conduction through the metal sample holder and by the presence of He exchange gas, at ambient pressure, within the sample chamber; the consumption of He gas is extremely low, being only 0.1 l min−1 during normal operation. A unique feature of this cold stage is that samples may be introduced into (and removed from) the stage at any temperature in the range 80–300 K, and thus materials which are not stable at room temperature, such as high-pressure phases that are recoverable to ambient pressure after quenching to liquid nitrogen temperatures, can be readily examined. A further advantage of this arrangement is that, by enabling the use of pre-cooled samples, it greatly reduces the turnaround time when making measurements on a series of specimens at low temperature.

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