scholarly journals Structural Analysis of Interstratified Illite-Smectite by the Rietveld Method

Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 244
Author(s):  
Xiaoli Wang ◽  
Hejing Wang

Rietveld method is a powerful tool in obtaining structural information of clay minerals by using of X-ray diffraction (XRD) patterns. However, the interstratified illite-smectites (I-S) show various stacking defects preventing the direct application of this method. It was shown that the Rietveld method combined with a recursive structure-factor calculation can be used for describing the stacking disorder of I-S. In this study, a series of samples with different stacking sequences and different proportions of layer types were chosen to verify the applicability of Rietveld method in determination of structural parameters of I-S. The Rietveld refinements were carried out on powder samples and oriented specimens in air-dry (AD) and ethylene glycol (EG) state. The structural information obtained by X-ray fluorescence (XRF) and thermal analysis were used as an independent test of the reliability of the refinements. The refined and experimental results were compared systematically and the relationship between structural parameter was discussed. For powder and oriented specimens, the refined results of occupancies of potassium and iron and the proportion of illitic layers showed consistent results. The refined value of cis-vacant layers was in good agreement with the experimental data. The reliability of the refinements increased with increasing proportion of illitic layers.

Author(s):  
Peng Liu ◽  
Hongbin Zhang ◽  
Sinong Wang ◽  
Hui Yu ◽  
Bingjie Lu ◽  
...  

AbstractThe crystallinity indices (CrI) of Chinese handmade papers were investigated using the X-ray diffraction (XRD) method. Four Chinese handmade papers, Yingchun, Zhuma, Yuanshu and Longxucao papers were used as model substrates of mulberry bark, ramie, bamboo and Eulaliopsis binata papers, respectively. Two forms of the paper samples, paper sheets and their comminuted powders, were used in this study. The results showed that their XRD patterns belong to the cellulose-I type and Iβ dominates the cellulose microstructure of these paper samples. Moreover, it was found that the microstructures and CrIs of cellulose of these papers were changed by the grinding treatment. This work suggested that the sheet form of the handmade papers is suitable to determine CrI by XRD, despite the contribution of non-cellulosic components in the papers. The order of CrIs for these paper sheet samples was Yingchun, Zhuma, Longxucao and Yuanshu papers. Besides CrIs, differences in cross-sectional areas of the crystalline zone of cellulose can be used for comparing different types of handmade papers. It was also found that the CrIs and crystallite size of paper cellulose varied between the sheet samples and the powder samples, illustrating that the pulverisation has a negative influence on the microstructure of the handmade papers.


2013 ◽  
Vol 12 (01) ◽  
pp. 1350006
Author(s):  
AHMED E. HANNORA ◽  
FARIED F. HANNA ◽  
LOTFY K. MAREI

Mechanical alloying (MA) method has been used to produce nanocrystallite Mn -15at.% Al alloy. X-ray diffraction (XRD) patterns for the as-milled elemental α- Mn and aluminum powder samples show a mixture of α + β- MnAl phases after 20 h of milling and changes to a dominant β- MnAl phase structure after 50 h. An average crystallite size of 40 nm was determined from Hall–Williamson method analysis after 5 h of milling. Moreover, the thermal analysis results using differential thermal analysis (DTA), suggested a possible phase transformation after 20 h of milling. Isothermal treatments are carried in the temperature range of 450°C to 1000°C. Room-temperature vibrating sample magnetometer (VSM) measurements of the hysteretic response revealed that the saturation magnetization Bs and coercivity Hc for 10 h ball milled sample are ~ 2.1 emu/g and ~ 92 Oe, respectively.


2007 ◽  
Vol 22 (1) ◽  
pp. 59-63 ◽  
Author(s):  
Min Li ◽  
Wenxia Yuan ◽  
Jingfang Wang ◽  
Cong Gu ◽  
Huaizhou Zhao

Trigonal rare-earth dioxymonocyanamides Ln2O2CN2 (Ln=Dy, Ho, Er, Tm, Yb) were synthesized by the modified solid-state metathesis (SSM) method, in which Ln2O3 and melamine C3N6H6 were mixed and heated at 850 °C in vacuumed silica ampoules. Possible chemical reaction pathways are proposed. X-ray diffraction (XRD) patterns of Ln2O2CN2 were refined using the Rietveld method. Compounds Ln2O2CN2 crystallize in the trigonal system with space group P3m1, Z=1, and cell parameters of a and c varying from 3.7267(1) to 3.6407(1) Å and from 8.1848(3) to 8.1152(3) Å, respectively, as Ln atoms change from Dy to Yb. These compounds have stacking structures of Ln2O22+ and CN22− layers, similar to those of previously reported compounds Ln2O2CN2 (Ln=Ce, Pr, Nd, Sm, Eu, Gd). The presence of CN22− ions has been confirmed by infrared spectroscopy, with two characteristic peaks in the vicinity of 651 and 2075 cm−1.


2002 ◽  
Vol 35 (5) ◽  
pp. 577-580 ◽  
Author(s):  
Zein Heiba ◽  
Hasan Okuyucu ◽  
Y. S. Hascicek

Nanosized polycrystalline samples of (Er1−uGdu)2O3(0 ≤u≤ 1.0) were synthesized by a sol–gel technique. X-ray diffraction data were collected and the crystal structures were refined by the Rietveld method. All samples are found to have the same crystal system and formed solid solutions over the whole range ofu. The Er3+and Gd3+ions were randomly distributed over two cationic sites, 8band 24d, in the space groupIa\bar{3} (206) in all refined structures. The lattice parameter was found to vary non-linearly with the composition (u). The average microstrain and average crystallite size have been calculated from the Williamson–Hall plots for each sample. The average size ranges from 50 to 70 nm, and the microstrain from 0.4 to 1.7%.


Clay Minerals ◽  
1990 ◽  
Vol 25 (3) ◽  
pp. 249-260 ◽  
Author(s):  
A. Plançon ◽  
C. Zacharie

AbstractUntil recently, the determination of the defect structures (previously referred to incorrectly as “crystallinity”) of kaolinites has been obtained in one of two ways: (1) measurement of the Hinckley index, or (2) by comparing calculated X-ray diffraction patterns based on a model of the defect structure (including types of defects and abundances) with experimental diffraction profiles. The Hinckley method is simple and easy to perform but contains no real information about the defect structure. Calculated XRD patterns are based on real defects but these calculations are time consuming and require some skill in application. Another approach is proposed: an expert system which will accurately describe the defect structure of kaolinites based on a few measurements taken from a normal powder diffraction profile. This system has been verified for nine kaolinite samples for which the defect structure was previously determined by comparison of calculated and observed diffraction profiles. The expert system reproduced the correct defect structure for each of the samples.


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