Rietveld Analysis of Aurivillius-Type Structure Ceramics Synthesized from Precursors Prepared by Classical and HEBM Methods

2013 ◽  
Vol 203-204 ◽  
pp. 319-322
Author(s):  
Jolanta Dercz ◽  
Grzegorz Dercz ◽  
Krystian Prusik ◽  
Rafał Babilas

The aim of this study was to analyze the influence of the method of preparing the substrates in the form of simple oxides for the structure of the final Bi5Ti3FeO15ceramics. Milling of the substrates was carried out by two methods: the classical one by hand mixing in a porcelain mortar, and by high-energy. Structure studies were performed by the X-ray diffraction (XRD) method. XRD patterns were analyzed with the Rietveld method using the DBWS 9807a program. It was found out that the slightest deviation of the network parameters from the catalog data occurs for the sample obtained from simple oxides by free sintering (BTFs). Furthermore, it was also determined that the optimal high-energy time of the substrates is 5 hours. When compared to the ICDD catalog data, the resulting ceramics is a single phase one and has the lowest network parameters deviation among all samples which were subject to high-energy.

2015 ◽  
Vol 7 (1) ◽  
pp. 1346-1351
Author(s):  
Ch.Gopal Reddy ◽  
Ch. Venkateshwarlu ◽  
P. Vijaya Bhasker Reddy

Co-Zr substituted M-type hexagonal barium ferrites, with chemical formula BaCoxZrxFe12-2xO19 (where x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0), have been synthesized by double sintering ceramic method. The crystallographic properties, grain morphology and magnetic properties of these ferrites have been investigated by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Vibrating Sample Magnetometer (VSM). The XRD patterns confirm the single phase with hexagonal structure of prepared ferrites. The magnetic properties have been investigated as a function of Co and Zr ion composition at an applied field in the range of 20 KOe. These studies indicate that the saturation magnetization (Ms) in the samples increases initially up to the Co-Zr composition of x=0.6 and decreases thereafter. On the other hand, the coercivity (Hc) and Remanent magnetization (Mr) are found to decrease continuously with increasing Co-Zr content. This property is most useful in permanent magnetic recording. The observed results are explained on the basis of site occupation of Co and Zr ions in the samples.


2020 ◽  
Vol 10 (03) ◽  
pp. 2050003
Author(s):  
M. R. Hassan ◽  
M. T. Islam ◽  
M. N. I. Khan

In this research, influence of adding Li2CO3 (at 0%, 2%, 4%, 6%) on electrical and magnetic properties of [Formula: see text][Formula: see text]Fe2O4 (with 60% Ni and 40% Mg) ferrite has been studied. The samples are prepared by solid state reaction method and sintered at 1300∘C for 6[Formula: see text]h. X-ray diffraction (XRD) patterns show the samples belong to single-phase cubic structure without any impurity phase. The magnetic properties (saturation magnetization and coercivity) of the samples have been investigated by VSM and found that the higher concentration of Li2CO3 reduces the hysteresis loss. DC resistivity increases with Li2CO3 contents whereas it decreases initially and then becomes constant at lower value with temperature which indicates that the studied samples are semiconductor. The dielectric dispersion occurs at a low-frequency regime and the loss peaks are formed in a higher frequency regime, which are due to the presence of resonance between applied frequency and hopping frequency of charge carriers. Notably, the loss peaks are shifted to the lower frequency with Li2CO3 additions.


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.


Ceramics ◽  
2018 ◽  
Vol 1 (2) ◽  
pp. 343-352 ◽  
Author(s):  
Reginaldo Muccillo ◽  
Daniel de Florio ◽  
Eliana Muccillo

Compositions of (ZrO2)0.92(Y2O3)0.08 (zirconia: 8 mol % yttria—8YSZ) and (CeO2)0.8(Sm2O3)0.2 (ceria: 20 mol % samaria—SDC20) ceramic powders were prepared by attrition milling to form an equimolar powder mixture, followed by uniaxial and isostatic pressing. The pellets were quenched to room temperature from 1200 °C, 1300 °C, 1400 °C and 1500 °C to freeze the defects configuration attained at those temperatures. X-ray diffraction analyses, performed in all quenched pellets, show the evolution of the two (8YSZ and SDC20) cubic fluorite structural phases to a single phase at 1500 °C, identified by Rietveld analysis as a tetragonal phase. Impedance spectroscopy analyses were carried out in pellets either quenched or slowly cooled from 1500 °C. Heating the quenched pellets to 1000 °C decreases the electrical resistivity while it increases in the slowly cooled pellets; the decrease is ascribed to annealing of defects created by lattice micro-tensions during quenching while the increase to partial destabilization of the tetragonal phase.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1764-C1764
Author(s):  
Guilherme Calligaris ◽  
Ana Paula Ribeiro ◽  
Adenilson dos Santos ◽  
Lisandro Cardoso

The characterization of the fat components becomes very useful in the formulation of shortening, margarines and fatty products due to their unique properties of plasticity, texture, solubility and aeration. The qualitative analysis obtained by X-ray diffraction (XRD) can be further improved in order to fulfill the lack of information on the triacylglycerol (TAG) in the hardfat systems aiming a complete polymorph characterization. In this work, as an attempt to quantify the distinct β and β' TAG polymorphs, XRD was combined with Rietveld refinement method and applied to two types of samples: mixtures (M) and blended hardfats (B) samples involving fully hydrogenated of soybean (FHSO) and palm (FHPO) oils. M-samples were prepared with linear concentrations of FHSO (β) and FHPO (β') and their Rietveld analysis have provided the expected content trend through the involved polymorphic phases with a very good agreement (~5%). This result validates the Rietveld method applicability on this kind of materials. The Rietveld method applied for B-samples has shown that β' polymorphic form prevails over the β-form, even for samples originally prepared with FHSO (β)/FHPO (β') = 60/40 ratio (see figure). This result indicates the influence of the seeding process (earlier crystallization of β' phase). This first quantitative approach for blended samples represents a very useful contribution towards the full characterization of fats.


1998 ◽  
Vol 4 (S2) ◽  
pp. 342-343 ◽  
Author(s):  
S. D. Walck ◽  
P. Ruzakowski-Athey

The analysis of Selected Area Diffraction (SAD) patterns that are collected from a single phase material having sufficient crystallites to provide continuous rings is relatively straightforward. However, when this condition is not met and there may be several phases present having rings of a spotty nature, the pattern is complex and can be quite difficult to analyze manually because of the vast number of discrete spots. WinJade from MDI is an X-ray diffraction (XRD) analysis program with an Electron Diffraction Program Module (EDPM) that can be used to aid in the analysis of SAD patterns. The EDPM produces Integrated Circular Density Plots (ICDP), which are one-dimensional intensity profiles plotted as a function of equivalent XRD 20 values or crystal d-spacings. These ICDP's can be overlayed with XRD patterns or with reference lines from the NIST and JCPDS crystalline databases for direct comparisons.


2008 ◽  
Vol 368-372 ◽  
pp. 1187-1189
Author(s):  
Xu Ran ◽  
Jun Guo Ran ◽  
Li Gou ◽  
Ji Yong Chen ◽  
Jiao Min Luo

The crystalline structures of B-type carbonated hydroxyapatite (CHA) powders sintered at 700, 900 and 1100°C, respectively, were studied by Rietveld analysis of powder X-ray diffraction (XRD) data. A series of structure parameters, including lattice parameters (a and c), bond length and the distortion index of PO4 tetrahedron (Dind) were calculated by Rietveld method to characterize the fine structure of CHA. The broadening effect of XRD reflections was separated to calculate the micro-strain and crystalline size. The results showed that CHA become more stable with the increase of sintering temperature, but the CO3 2- is almost lost at temperature of 1100°C. The quantitative results about crystal structure of CHA based on crystalline structure simulated by Rietveld method are obtained.


2020 ◽  
Vol 19 (04) ◽  
pp. 1950034
Author(s):  
V. Balachandar ◽  
J. Brijitta ◽  
K. Viswanathan ◽  
R. Sampathkumar

In this study, ZnO–Fe2O3 nanocomposites were prepared by high-energy ball milling technique and characterized through X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), UV–visible spectroscopy and dielectric spectroscopy. The amount of Fe2O3 in the ZnO–Fe2O3 nanocomposites was varied at the rates of 1[Formula: see text]wt.%, 3[Formula: see text]wt.% and 5[Formula: see text]wt.% in order to investigate its influence on the structural, optical and dielectric properties of the nanocomposites. XRD patterns of nanocomposites revealed no shift in peak positions and hence confirmed the formation of composites after ball milling. Further, it was observed from FESEM analysis that Fe2O3 particles were distributed randomly on the ZnO matrix of the nanocomposites. ZnO–Fe2O3 nanocomposites reveal extended optical absorption in the range of 400–600[Formula: see text]nm from UV studies. The dielectric constant and loss of the nanocomposites decrease exponentially with increase in frequency. The composition and frequency dependences of the dielectric constant, dielectric loss and AC conductivity are explained based on the Maxwell–Wagner effect and Koop’s theory.


2003 ◽  
Vol 18 (1) ◽  
pp. 7-15 ◽  
Author(s):  
M. Courtial ◽  
M.-N. de Noirfontaine ◽  
F. Dunstetter ◽  
G. Gasecki ◽  
M. Signes-Frehel

So-called alite is a solid solution of tricalcium silicate Ca3SiO5 with a few percent of impurities. It constitutes the major phase of anhydrous Portland cement. In industrial compounds, alite crystallizes into two monoclinic forms designated M1 and M3. The possibility of correlation between the crystallographic structure of the clinker and its reactivity is still an open question. The answer of such a question involves a proper quantitative analysis of the various phases—including the exact alite polymorph—of the industrial product. The rather similar structure of the two alites makes it difficult to distinguish them from their XRD patterns. This paper shows that five angular windows in the X-ray diffraction patterns can be used with synthetic alites as well as industrial compounds, to identify the nature of the actual polymorph (M1 or M3) present and the structural model to be used (with or without superstructure) in subsequent Rietveld analysis of the data.


Cerâmica ◽  
2016 ◽  
Vol 62 (361) ◽  
pp. 1-8 ◽  
Author(s):  
J. L. Alves ◽  
A. E. Zanini ◽  
M. E. de Souza ◽  
M. L. F. Nascimento

Abstract Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitória da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8) μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale.


Sign in / Sign up

Export Citation Format

Share Document