• Journal of the Mineralogical Society of Korea
• /
• v.7 no.1
• /
• pp.62-79
• /
• 1994

The quanttative and structural analysis of the binary standard mixtures of albite and quartz, and microcline and albite were carried out using the Rietveld refinement method in order to investigate the accuracy and precision of the method. The quantitative analysis using the Rietveld method results in a standard deviation of 4 wt % for the albite-quartz standard mixtures and 1 wt % for the microcline-albite standard mixtures, suggesting that its accuracy is far better than that of the conventional XRD method in which only a few selected peaks are utilized. Furthermore, the unit-cell parameters of component minerals in mixtures were also estimated accurately during the analysis. It was observed that the refined weight fractions deviate systematically from their measured values when the method is applied to the mixtures that contain minerals with different degrees of preferred orientation, such as albite-quartz mixtures. The preferred orientation parameters and R-values suggest that the systematic deviation is caused as a result of the preferred orientation effect of feldspar crystallites. It is evident that the preferred orientation corrections are of help for the accurate determination of unit-cell parameters, although they may not improve the result of quantitative analysis significantly. The refined weight fraction of the mineral with higher degree of preferred orientation in mixture is greater than the measured one. This is apparently caused by the effect of geometry of feldspar crystallites in the surface of the mounted sample. The Rietveld refinement method minimizes the problems inherent in the traditional XRD methods, such as the line overlap, primary extinction, and preferred orientation effect, by fitting every data point in a whole pattern explicitly. Furthermore, accurate unit-cell parameters as well as scale factors that can be obtained from the Rietveld refinement are used for the quqantification. The present stdudy demonstrates that the Rietveld method yields far more accurate analytical result than the conventional XRD quantitative analysis method does.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.31 no.3
• /
• pp.116-126
• /
• 2021

Diesel particulate filter (DPF) is a typical application field of cordierite (Mg₂Al₄Si₅O₁₈) honeycomb. Green body for DPF honeycomb was extruded using slurry paste and sintered at the temperature range of 980~1450℃. Quantitative crystal phase analysis was carried out by using Rietveld refinement method for powder XRD data. In conjunction with the quantitative Rietveld analysis, SEM-EDS analysis was carried for the crystal phases (indialite, cordierite, cristobalite, alumina, spinel, mullite, pro-enstatite). After removing amorphous phase on the sintered surfaces by chemical etching method, the shape and composition of the crystal phases can be clearly identified by SEM-EDS method. By combining the Rietveld refinement method and SEM-EDS analysis, crystal phase evolution process in DPF cordierite ceramics could be clarified. In addition, the coefficient of thermal expansion (CTE) of the DPF honeycombs were measured and compared with the calculated CTEs based on the quantitative crystal phase analysis results.

• Journal of the Korean Ceramic Society
• /
• v.35 no.10
• /
• pp.1113-1119
• /
• 1998

Crystal structure of needle-shaped maghemite(${\gamma}$-{{{{ { {Fe }_{2 }O }_{3 } }}) has been studied by the Rieveld analysis of powder X-ray diffraction patterns. The tetragonal space group P41,.3212 and cubic space group P41,.32 have been have been used for the refinement of X-ray diffraction patterns. The crystal system of maghemite is closed to tetragonal more than cubic. The tetragonal lattice parameters are a=8.3460$\AA$ and c=25.034$\AA$ The standard X-ray diffraction pattern of the tetragonal maghemite analyzed with space group P41,.3212 is proposed.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.12 no.2
• /
• pp.87-90
• /
• 2002

$LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

• Computers and Concrete
• /
• v.19 no.1
• /
• pp.19-31
• /
• 2017

This paper uses modelling and experiment to perform a quantitative analysis for the gypsum and ettringite formations in cement pastes subjected to sulfate attack. Firstly, based on Fick's law and chemical reaction kinetics, a diffusion model of sulfate ions in cement pastes is proposed, and then the model of the gypsum and ettringite formations is established to analyze its contents in cement pastes with corrosion time. Secondly, the corrosion experiment of the specimens with cement pastes immersed into 2.5%, 5.0% and 10.0% $Na_2SO_4$ solutions are carried out, and by using XRD-Rietveld method, the phases of powder samples from the specimens are quantitatively analyzed to obtain the contents of gypsum and ettringite in different surface depth, solution concentration and corrosion time. Finally, the contents of gypsum and ettringite calculated by the models are compared with the results from the XRD experiments, and then the effects of surface depth, corrosion time and solution concentration on the gypsum and ettringite formations in cement pastes are discussed.

• Journal of the Korean Recycled Construction Resources Institute
• /
• v.8 no.4
• /
• pp.514-519
• /
• 2020

In this study, cement clinkers were sintered at each temperature by replacing some of the clay components of cement clinkers with coal materials. The mineral phase change of sintered cement clinker was quantitatively analyzed by XRD-Rietveld method. As the sintering temperature of cement clinker increased, the amount of belite decreased, the amount of alite increased, and the amount of free-CaO decreased. The form of alite and belite could be distinguished at sintering temperature of 1450℃ or higher. The crystal size was greatly increased at 1500℃ sintering. It was confirmed that the excessive sintering was progressed. Free-CaO decreased with the increase of sintering temperature. At 1450 ℃ or higher, it was less than 0.5%. In 1450℃ or greater, it is determined that enough sintering is included. Therefore, the application of fly ash as a raw material of cement clinker was judged to be usable as a source of chemical components of alumina and iron raw materials.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.7 no.2
• /
• pp.244-252
• /
• 1997

The pseudo-spinel type solid solution, $LiAl_{2.5}/Fe_{2.5}O_8$ was prepared by reaction of $LiCO_3, Al_2O_3, Fe_2O_3$ mixture at 1620K, which can be used for cathode material in lithium batteries. Its structure was investigated by Rietveld profile-analysis of XRD in detail. The space group of solid solution is $P4_3$32(a=8.1293$\AA$) and the final residual index of structure refinement was about 5%. Cations $Al^{3+}, Fe^{3+}$ are located at both tetra- and octahedral-coordination and $Li^+$ ions are occupied in the octahedral 4b-, 12d-site of the inverse spinel.

• Computers and Concrete
• /
• v.13 no.6
• /
• pp.695-707
• /
• 2014

This study investigated the chloride binding isotherms of various cement types, especially the contributions of C-S-H and AFm hydrates to the chloride binding isotherms were determined. Ordinary Portland cement (OPC), Modified cement (MC), Rapid-hardening Portland cement (RHC) and Low-heat Portland cement (LHC) were used. The total chloride contents and free chloride contents were analyzed by ASTM. The contents of C-S-H, AFm hydrates and Friedel's salt were determined by X-ray diffraction Rietveld (XRD Rietveld) analysis. The results showed that OPC had the highest chloride binding capacity, and, LHC had the lowest binding capacity of chloride ions. MC and RHC had very similar capacities to bind chloride ions. Experimental equations which distinguish the chemically bound chloride and physically bound chloride were formulated to determine amounts of the bound chloride basing on chloride binding capacity of hydrates.

• Journal of the Korea Institute of Building Construction
• /
• v.20 no.1
• /
• pp.11-18
• /
• 2020

Carbon nanotubes are used in various industries with their excellent mechanical properties and electrical conductivity. In the construction industry, research is being conducted to give self-sensing capabilities to structures, but the results of experiments vary among researchers, and the analysis is insufficient. Therefore, in this study, the hydration and electrical properties of MWCNT-added cement pastes were measured. The electrical resistance values of hydration heat, porosity, Rietveld quantitative analysis, compressive strength, and distance were measured.. The heat resistance, porosity, Rietvelt quantitative analysis, compressive strength and distance were measured according to electrical resistance. Experimental results showed that the heat of hydration decreased with increasing MWCNT. XRD Rietveld quantitative analysis showed that there was no significant difference in the amount of hydration products with increasing addition rate of MWCNT. As a result of SEM analysis, the MWCNT is agglomerated by van der Waals forces, and this area is considered to be caused by voids and weak areas. The electrical resistance value decreases as the addition rate is increased, and thus may play a role for magnetic sensing in the future.

• Proceedings of the Korean Institute of Building Construction Conference
• /
• 2021.11a
• /
• pp.74-75
• /
• 2021

This study attempted to study the setting time and compressive strength according to the sugar type through XRD. Setting time was found to be delayed the most when mixing white sugar, and setting time was promoted when mixing Saccharin and Aspartame. It was found that when white sugar and Grosvener siraitia were mixed, the compressive strength was higher than that of Control. Aspartame the age passed, C₃S decreased and Ca(OH)₂ increased.