scholarly journals Designing a synchrotron micro-focusing beamline for macromolecular crystallography

2016 ◽  
Vol 62 (3) ◽  
pp. 395-400
Author(s):  
Paweł Grochulski ◽  
Mirosław Cygler ◽  
Brian Yates

After a successful 10 years of operation, the Canadian Macromolecular Crystallography Facility 08ID-1 beamline will undergo an upgrade to establish micro-beam capability. This paper is mostly focussed on optics and computer simulations for ray tracing of the beamline. After completion, the focussed beam at the sample will have a much smaller size of 50 × 5 μm2 (H x V), allowing measurement of X-ray diffraction patterns from much smaller crystals than possible presently. The beamline will be equipped with a fast sample changer and an ultra-low noise photon counting detector, allowing shutter-less operation of the beamline. Additionally, it will be possible to perform in-situ room-temperature experiments.

2017 ◽  
Vol 371 ◽  
pp. 73-77 ◽  
Author(s):  
Adriano Gonçalves Reis ◽  
Danieli Aparecida Pereira Reis ◽  
Antônio Jorge Abdalla ◽  
Antônio Augusto Couto ◽  
Jorge Otubo

An in situ high-temperature X-ray diffraction (HTXRD) study in maraging 300 steel was carried out to study the martensite to austenite transformation and effect of time of exposure in the austenite reversion below austenite start temperature. Solution annealed materials were subjected to controlled heating-holding cycles. The first sample was heated at a rate of 10 oC/min from room temperature to 800 oC, showing that the microstructure is completely martensitic (α’110) until 600 oC. From 650 oC until 800 oC, the microstructure is gradually changing from martensitic to austenitic, showed by the increasing peaks of γ111 and reducing peaks of α’110. At 800 oC the microstructure is completely austenitic (γ111). Another sample was heated at 10 oC/min from room temperature to 600 oC and held for 4 hours. At 600 oC, at 0 h time of exposure, only a martensitic peak was observed. An austenite peak can be observed after some time of exposure at this temperature. The volume fraction of austenite increased with increasing time of exposure at 600 oC, reaching 50/50 volume fraction after 4 hours of exposure. XRD diffraction patterns for the same sample that was held for 4 hours at 600 oC and then cooled down in air to room temperature showed the same intensity of austenite and martensitic peaks found in situ at 600 oC for 4 hours (retained austenite), with the volume fraction of 50/50 of austenite and martensite phases. The HTXRD technique can be used to identify and quantify martensite to austenite transformation and austenite retention.


2002 ◽  
Vol 35 (4) ◽  
pp. 471-476 ◽  
Author(s):  
J.-F. Bérar ◽  
L. Blanquart ◽  
N. Boudet ◽  
P. Breugnon ◽  
B. Caillot ◽  
...  

In this paper, results obtained from a prototype photon counting detector are presented. The pixel size is 330 µm × 330 µm for a total area of 16 µm × 40 mm. The detector works at room temperature and its dynamic response ranges from 0.01 up to 106photons pixel−1s−1. An energy resolution of about 1.5 keV has been measured. Very encouraging small-angle X-ray scattering (SAXS) and diffraction patterns were obtained, demonstrating the success of the prototype. Plans for future developments based on this study are presented.


2012 ◽  
Vol 512-515 ◽  
pp. 1511-1515
Author(s):  
Chun Lin Zhao ◽  
Li Xing ◽  
Xiao Hong Liang ◽  
Jun Hui Xiang ◽  
Fu Shi Zhang ◽  
...  

Cadmium sulfide (CdS) nanocrystals (NCs) were self-assembled and in-situ immobilized on the dithiocarbamate (DTCs)-functionalized polyethylene glycol terephthalate (PET) substrates between the organic (carbon disulfide diffused in n-hexane) –aqueous (ethylenediamine and Cd2+ dissolved in water) interface at room temperature. Powder X-ray diffraction measurement revealed the hexagonal structure of CdS nanocrystals. Morphological studies performed by scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) showed the island-like structure of CdS nanocrystals on PET substrates, as well as energy-dispersive X-ray spectroscopy (EDS) confirmed the stoichiometries of CdS nanocrystals. The optical properties of DTCs modified CdS nanocrystals were thoroughly investigated by ultraviolet-visible absorption spectroscopy (UV-vis) and fluorescence spectroscopy. The as-prepared DTCs present intrinsic hydrophobicity and strong affinity for CdS nanocrystals.


2017 ◽  
Vol 866 ◽  
pp. 199-203
Author(s):  
Chidchanok Chainej ◽  
Suparut Narksitipan ◽  
Nittaya Jaitanong

The aims of this research were study the microstructures and mechanical properties for partial replacement of cement with Fly ash (FA) and kaolin waste (KW). Ordinary Portland cement were partially replaced with FA and KW in the range of 25-35% and 10-25% by weight of cement powder. The kaolin waste was ground for 180 minutes before using. The specimen was packing into an iron mold which sample size of 5×5×5 cm3. Then, the specimens were kept at room temperature for 24 hours and were moist cured in the incubation lime water bath at age of 3 days. After that the specimens were dry cured with plastic wrap at age of 3, 7, 14 and 28 days. After that the compounds were examined by x-ray diffraction patterns (XRD) and the microstructures were examined by scanning electron microscopy (SEM). The compressive strength was then investigated.


1974 ◽  
Vol 29 (12) ◽  
pp. 1771-1777 ◽  
Author(s):  
N. C. Haider ◽  
S. H. Hunter

Powder Cd of 99.999% purity was prepared at room temperature (25 °C) and x-ray diffraction patterns were obtained using CuKaα radiation with Ni-filter. The line broadening was analyzed after incorporating the appropriate correction factors. At room temperature Cd was found to have large particle size (653 A), small root mean square strain (.001), small deformation fault probability a (.003). and negligible growth fault probability β(0). Compared to other hep metals which have been studied earlier and which have higher melting temperatures, metal Cd is much less affected by mechanical deformation at room temperature.


2016 ◽  
Vol 850 ◽  
pp. 191-196 ◽  
Author(s):  
Wei Wang ◽  
Cun Lei Zou ◽  
Ren Geng Li ◽  
Wen Wen ◽  
Hui Jun Kang ◽  
...  

In situ synchrotron X-ray diffraction was used to study a deformed Cu-0.88 Fe-0.24 P alloy during heating process. The measurements were performed at room temperature and also at high temperatures up to 893 K in order to determine the recovery, ageing and recrystallization process. With the increase of temperature, the angles of copper matrix peaks moved left and the FWHM (full width at half maximum) decreased slightly. Fe3P precipitates were first detected at 533 K, reached the maximum at 673 K, and re-dissolved into matrix at 853 K. A dramatic decrease in FWHM was observed accompanied by the precipitation of Fe3P phases, indicating the reduction of lattice distortion of copper matrix.


Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.


1964 ◽  
Vol 42 (10) ◽  
pp. 1886-1889 ◽  
Author(s):  
B. Swaroop ◽  
S. N. Flengas

The crystal structure of zirconium trichloride was determined from X-ray diffraction patterns. Zirconium trichloride belongs to the [Formula: see text]space group. The dimensions of the main cell at room temperature are: a = 5.961 ± 0.005 Å and c = 9.669 ± 0.005 Å.The density of zirconium trichloride was measured and gave the value of 2.281 ± 0.075 g/cm3 while, from the X-ray calculations, the value was found to be 2.205 g/cm3.


2012 ◽  
Vol 29 (1) ◽  
pp. 50
Author(s):  
D.N Ba ◽  
L.T Tai ◽  
N.T Trung ◽  
N.T Huy

The influences of the substitution of Ni with Mg on crystallographic and magnetic properties of the intermetallic alloys LaNi5-xMgx (x ≤ 0.4) were investigated. The X-ray diffraction patterns showed that all samples were of single phase, and the lattice parameters, a and c, decreased slightly upon chemical doping. LaNi5 is well known as an exchange-enhanced Pauli paramagnet. Interestingly, in LaNi5-xMgx, the ferromagnetic order existed even with a small amount of dopants; the Curie temperature reached the value of room temperature for x = 0.2, and enhanced with increasing x.


2014 ◽  
Vol 1712 ◽  
Author(s):  
Thomas W. Cornelius ◽  
Zhe Ren ◽  
Francesca Mastropietro ◽  
Simon Langlais ◽  
Anton Davydok ◽  
...  

ABSTRACTA scanning force microscope for in situ nanofocused X-ray studies (SFINX) has been developed which can be installed on diffractometers at synchrotron beamlines allowing for the combination with various techniques such as coherent X-ray diffraction and fluorescence. The capabilities of this device are demonstrated on Cu nanowires and on Au islands grown on sapphire (0001). The sample topography, crystallinity, and elemental distribution of the same area are investigated by recording simultaneously an AFM image, a scanning X-ray diffraction map, and a fluorescence map. Additionally, the mechanical response of Au islands is studied by in situ indentation tests employing the AFM-tip and recording 2D X-ray diffraction patterns during mechanical loading.


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