scholarly journals Optimizing laboratory X-ray diffraction contrast tomography for grain structure characterization of pure iron

2021 ◽  
Vol 54 (1) ◽  
Author(s):  
Adam Lindkvist ◽  
Haixing Fang ◽  
Dorte Juul Jensen ◽  
Yubin Zhang

Laboratory diffraction contrast tomography (LabDCT) is a recently developed technique for 3D nondestructive grain mapping using a conical polychromatic beam from a laboratory-based X-ray source. The effects of experimental parameters, including accelerating voltage, exposure time and number of projections used for reconstruction, on the characterization of the 3D grain structure in an iron sample are quantified. The experiments were conducted using a commercial X-ray tomography system, ZEISS Xradia 520 Versa, equipped with a LabDCT module; and the data analysis was performed using the software package GrainMapper3D, which produces a 3D reconstruction from binarized 2D diffraction patterns. It is found that the exposure time directly affects the background noise level and thus the ability to distinguish weak spots of small grains from the background. With the assistance of forward simulations, it is found that spots from the first three strongest {hkl} families of a large grain can be seen with as few as 30–40 projections, which is sufficient for indexing the crystallographic orientation and resolving the grain shape with a reasonably high accuracy. It is also shown that the electron current is a more important factor than the accelerating voltage to be considered for optimizing the photon numbers with energies in the range of 20–60 keV. This energy range is the most important one for diffraction of common metals, e.g. iron and aluminium. Several suggestions for optimizing LabDCT experiments and 3D volume reconstruction are finally provided.

IUCrJ ◽  
2021 ◽  
Vol 8 (4) ◽  
Author(s):  
H. Fang ◽  
D. Juul Jensen ◽  
Y. Zhang

Laboratory diffraction contrast tomography (LabDCT) is a novel technique for non-destructive imaging of the grain structure within polycrystalline samples. To further broaden the use of this technique to a wider range of materials, both the spatial resolution and detection limit achieved in the commonly used Laue focusing geometry have to be improved. In this work, the possibility of improving both grain indexing and shape reconstruction was investigated by increasing the sample-to-detector distance to facilitate geometrical magnification of diffraction spots in the LabDCT projections. LabDCT grain reconstructions of a fully recrystallized iron sample, obtained in the conventional Laue focusing geometry and in a magnified geometry, are compared to one characterized by synchrotron X-ray diffraction contrast tomography, with the latter serving as the ground truth. It is shown that grain indexing can be significantly improved in the magnified geometry. It is also found that the magnified geometry improves the spatial resolution and the accuracy of the reconstructed grain shapes. The improvement is shown to be more evident for grains smaller than 40 µm than for larger grains. The underlying reasons are clarified by comparing spot features for different LabDCT datasets using a forward simulation tool.


2019 ◽  
Vol 52 (3) ◽  
pp. 643-651 ◽  
Author(s):  
Florian Bachmann ◽  
Hrishikesh Bale ◽  
Nicolas Gueninchault ◽  
Christian Holzner ◽  
Erik Mejdal Lauridsen

A method for reconstructing the three-dimensional grain structure from data collected with a recently introduced laboratory-based X-ray diffraction contrast tomography system is presented. Diffraction contrast patterns are recorded in Laue-focusing geometry. The diffraction geometry exposes shape information within recorded diffraction spots. In order to yield the three-dimensional crystallographic microstructure, diffraction spots are extracted and fed into a reconstruction scheme. The scheme successively traverses and refines solution space until a reasonable reconstruction is reached. This unique reconstruction approach produces results efficiently and fast for well suited samples.


Author(s):  
Fikri Alatas ◽  
Fahmi Abdul Azizsidiq ◽  
Titta Hartyana Sutarna ◽  
Hestyari Ratih ◽  
Sundani Nurono Soewandhi

An effort to improve the solubility of albendazole (ABZ), an anthelmintic drug has been successfully carried out through the formation of multicomponent crystal with dl-malic acid (MAL). Construction of phase solubility curve of ABZ in MAL solution and crystal morphological observations after recrystallization in the acetone-ethanol (9:1) mixture were performed for initial prediction of multicomponent crystal formation. ABZ-MAL multicomponent crystal was prepared by wet grinding or also known as solvent-drop grinding (SDG) with acetone-ethanol (9:1) mixture as a solvent followed by characterization of the multicomponent crystal formation by powder X-ray diffraction and Fourier transform infrared (FTIR) methods. The solubility of ABZ-MAL multicomponent crystal was tested in water at ambient temperature and in pH 1.2, 4.5 and 6.8 of buffered solutions at 37°C. The phase solubility curve of the ABZ in the MAL solution showed type Bs. The ABZ-MAL mixture has a different crystalline morphology than pure ABZ and MAL after recrystallization in the acetone-ethanol mixture (9:1). The powder X-ray diffraction pattern and the FTIR spectrum of ABZ-MAL from SDG different from intact ABZ and MAL powder X-ray diffraction patterns and these results can indicate the ABZ-MAL multicomponent crystal formation. The ABZ-MAL multicomponent crystal has better solubility than pure ABZ in all media used. These results can be concluded that ABZ-MAL multicomponent crystal can be prepared by solvent-drop grinding method with acetone-ethanol (9:1) mixture as a solvent and can increase the solubility of albendazole.


2005 ◽  
Vol 03 (2) ◽  
pp. 24-29
Author(s):  
P.M. PIMENTEL ◽  
A.M.G. PEDROSA ◽  
H.K.S. SOUZA ◽  
C.N.S. JÚNIOR ◽  
R.C.A. PINTO ◽  
...  

Spinel oxides with the composition ZnCo2O4 and ZnCo2O4:Eu3+ have been synthesized by the Pechini method and characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures. The formation of monophase cubic spinel structure was confirmed by X-ray diffraction patterns. Extra lines corresponding to other phase has been observed in the powders calcined at 900 ºC. The results showed the extremely lower synthesis temperature than those presents in conventional methods.


2014 ◽  
Vol 782 ◽  
pp. 603-606 ◽  
Author(s):  
Ondrej Milkovič ◽  
Karel Saksl ◽  
Mária Hagarová ◽  
Štefan Michalik ◽  
Jana Gamcová

This paper is focused to structure characterization of two differently electrodeposited Ni-Co alloys on the copper surface. The chemical composition of the layers was determined by the EDX analysis in the scanning electron microscope. Phase analysis was realized by diffraction in the transmission mode using synchrotron radiation. Diffraction patterns also show the preferred orientation in the coating with saccharine addition.


2004 ◽  
Vol 831 ◽  
Author(s):  
Phanikumar Konkapaka ◽  
Huaqiang Wu ◽  
Yuri Makarov ◽  
Michael G. Spencer

ABSTRACTBulk GaN crystals of dimensions 8.5 mm × 8.5 mm were grown at growth rates greater than 200μm/hr using Gallium Vapor Transport technique. GaN powder and Ammonia were used as the precursors for growing bulk GaN. Nitrogen is used as the carrier gas to transport the Ga vapor that was obtained from the decomposition of GaN powder. During the process, the source GaN powder was kept at 1155°C and the seed at 1180°C. Using this process, it was possible to achieve growth rates of above 200 microns/hr. The GaN layers thus obtained were characterized using X-Ray diffraction [XRD], scanning electron microscopy [SEM], and atomic force microscopy [AFM]. X-ray diffraction patterns showed that the grown GaN layers are single crystals oriented along c direction. AFM studies indicated that the dominant growth mode was dislocation mediated spiral growth. Electrical and Optical characterization were also performed on these samples. Hall mobility measurements indicated a mobility of 550 cm2/V.s and a carrier concentration of 6.67 × 1018/cm3


2013 ◽  
Vol 834-836 ◽  
pp. 309-314
Author(s):  
Zi Fan Xiao ◽  
Jin Shu Cheng ◽  
Jun Xie

A glass-ceramic belonging to the CaO-Al2O3-SiO2(CAS) system with different composition of spodumene and doping the Li2O with amount between 0~2.5 % (mass fraction) were prepared by onestage heat treatment, under sintering and crystallization temperature at 1120 °C for two hours. In this paper, differential thermal analysis, X-ray diffraction, scanning electron microscopy, energy dispersive spectrometry and bending strength test were employed to investigate the microstructure and properties of all samples. β-wollastonite crystals were identified as the major crystalline phases, and increasing Li2O was found to be benefit for the crystallization and tiny crystalline phases remelting, resulting in the content of major crystalline phases increased first and then decreased with increasing the expense of spodumene. Meanwhile, the crystal size can be positively related with the content of Li2O. The preferable admixed dosage of spodumene can be obtained, besides the strength of glass-ceramics can be more than 90 MPa.


2021 ◽  
Vol 1039 ◽  
pp. 307-312
Author(s):  
Mohammad Malik Abood ◽  
Osama Abdul Azeez Dakhil ◽  
Aref Saleh Baron

Methyl ammonium lead iodide CH3NH3PbI3 Perovskite was synthesized by a new method mixing between one and two steps, in addition, the ethanol solvent was used to dissolve CH3NH3I and compared with isopropanol solvent. The characterizations of synthesized perovskite samples included the structural properties, morphological characteristics and optical properties. The intensity and orientation in X-ray diffraction patterns appear clearly in ethanol solvent while disappearing at a peak at 12o due to the speed reaction of perovskite in this solvent. Additionally, the ethanol solvent increasing the grain size of perovskite which homogeneity of the surface morphology. the ethanol solvent cause a decrease in the wavelength of absorbance edge in addition to an increase in the energy bandgap value. Keywords: Ethanol Solvent, Perovskite, Photovoltaic Technologies, X-ray diffraction.


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