• Fibers and Polymers
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• v.6 no.3
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• pp.206-218
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• 2005

Structural studies of series of 'as spun' and drawn PEEK fibers have been carried out using X-ray diffraction and optical microscopy techniques. The analysis of results suggest that fibers produced at a constant draw ratio with increasing draw temperatures show enhanced orientation and crystalline behaviour. The resolved equatorial and meridional traces provide additional structural parameters in terms of crystallinity, crystallite size, and crystallite thickness. It is concluded that drawing at a temperature below $T_g(i.e.,\;144^{\circ}C)$ results in poorly oriented non-crystalline materials, whereas drawing above $T_g$ results in highly oriented semi crystalline materials. Additional drawing proved to increase the overall orientation with slight improvements in lateral order of the chain molecules. Quantitative analysis revealed that the crystallite size increases with increasing drawing temperature. The results also revealed the increased crystallite size upon additional drawing. Crystalline orientation parameter, $_c$, suggests almost perfect orientation. In all cases, the amorphous orientation is found to be lower than the overall orientation parameter obtained from the optical birefringence. As a result of additional drawing, crystalline orientation was found to increase slightly but the increase in the orientation of non-crystalline material was found to be substantial. An average crystalline density was determined from the orthorhombic unit cell dimensions. It was found to vary as a result of processing conditions. It was also found that the value of the maximum birefringence shows heavy dependence on the chain conformation.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2002.11a
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• pp.97-117
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• 2002

A chemoinfometrical method for quantitative determination of crystal content of indomethacin (IMC) polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the conventional powder X-ray diffraction method was performed. Pure $\alpha$ and ${\gamma}$ forms of IMC were prepared using published methods. Powder X-ray diffraction profiles and NIR spectra were recorded for six kinds of standard materials with various content of ${\gamma}$ form IMC. The principal component regression (PCR) analyses were performed based on normalized NIR spectra sets of standard samples of known content of IMC ${\gamma}$ form. A calibration equation was determined to minimize the root mean square error of the prediction. The predicted ${\gamma}$ form content values were reproducible and had a relatively small standard deviation. The values of ${\gamma}$ form content predicted by two methods were in close agreement. The results were indicated that NIR spectroscopy provides for an accurate quantitative analysis of crystallinity in polymorphs compared with the results obtained by conventional powder X-ray diffractometry.

• Journal of the Korean Society for Heat Treatment
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• v.30 no.5
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• pp.215-221
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• 2017

The effect of austenitizing temperature on the degree of carbides re-solutionizing, mean graine size, hardness and the volume fraction of retaind austenite ($V_{\gamma}$) etc., has been studied by means of metallography, X-ray diffractometry and hardness measurement in STD 11 tool steel. As austenitizing temperature increases, the amount of alloying elements which is re-dissolved into matrix increases, resulting in increase of $V_{\gamma}$, due to the chemical stabilization of austenite. The Vickers hardness value decreases with increasing austenitizing temperature, which is attributed to grain size as well the volume fractions of $V_{\gamma}$ and carbides. Theoretical diffraction intensity of (200) ${\alpha}^{\prime}$, (211) ${\alpha}^{\prime}$ (200) ${\gamma}$ and (220) ${\gamma}$ peaks obtained by $CuK_{\alpha}$ chracteristics X-ray (${\lambda}=0.15429nm$) was calculated, and quantitative analysis of $V_{\gamma}$ could be carried out by X-ray diffraction method. The resultant value is well coincided with the value obtained by image analysis method. When the quenched specimen is tempered above $200{\sim}400^{\circ}C$ for 30 min, the transition carbides i.e., MC and $M_2C$ in the size of about 20 nm begin to precipitate at $300^{\circ}C$.

• Journal of the Mineralogical Society of Korea
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• v.19 no.4 s.50
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• pp.363-381
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• 2006

Mineral compositions of granitic rocks from Geochang, Pocheon, Iksan, and China were obtained by the modal analysis, CIPW norm calculations, and Rietveld quantitative analysis for stone specification of the Geochang granitic rocks. The Geochang granitic rocks show grey to dark in color and medium grained porphyritic texture. They mainly consist of quartz, plagioclase, alkali feldspar, and biotite. Among three different method for determining the mineral compositions of granitic rocks, normative compositions using X-ray fluorescence data are not appropriate for representing real mineral composition. Rietveld quantitative analysis using X-ray powder diffraction data is proved better method to determine exact mineral compositions than modal analysis using microscopic observation. Q-A-P diagram shows that the Geochang granitic rocks are typical granodiorite, whereas the granitic rocks of Pocheon, Iksan, and China are monzogranite, monzogranite to granodiorite, and granodiorite, respectively. Compared to China ones, the Geochang granitic rocks are nearly close to each other in mineral composition.

• Proceedings of the Korean Ceranic Society Conference
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• 2000.04a
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• pp.21.1-21.1
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• 2000

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.10
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• pp.97-101
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• 2017

X-ray diffractometers are used to characterize material properties, such as the phase, texture, lattice constant and residual stress, based on the diffracted beams obtained from specimens. Quantitative analyses using X-rays are typically conducted by measuring the peak positions of the diffracted beams. However, the long-term use of the diffractomer, like any other machine, results in errors associated with the mechanical parts, which can deteriorate the accuracy of the quantitative analyses. In this study, the process of correcting systematic errors in the $2{\theta}$ range of $30{\sim}90^{\circ}$ is discussed, for which strain-free Si powders from NIST were used as the standard specimens. For the evaluation of the impact of such error correction, we conducted a quantitative analysis of the true lattice constant for tungsten thin films.

• The Journal of Advanced Prosthodontics
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• v.11 no.5
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• pp.253-261
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• 2019

PURPOSE. To evaluate the influence of cyclic loading on phase transformation of zirconia abutments and to compare the effectiveness of three different quantitative ageing assessment techniques. MATERIALS AND METHODS. Thirty two Y-TZP prostheses fabricated from two brands, InCoris ZI and Ceramill ZI, were cemented to titanium bases and equally divided into two subgroups (n=8): control group without any treatment and aged group with cyclic loading between 20 N and 98 N for 100,000 cycles at 4 Hz in distilled water at $37^{\circ}C$. The tetragonal-to-monoclinic phase transformation was assessed by (i) conventional x-ray diffraction (XRD), (ii) micro x-ray diffraction (${\mu}XRD$), and (iii) micro-Raman spectroscopy. The monoclinic-phase fractions (M%) were compared by two-way ANOVA. RESULTS. InCoris Zi presented significantly higher M% than Ceramill Zi in both control and aged groups (P<.001). Both materials exhibited significant phase transformation with monoclinicphase of 1 to 3% more in aged groups than controls for all three assessment techniques. The comparable M% was quantified by both ${\mu}XRD$ and XRD. The highest M% was assessed with micro-Raman. CONCLUSION. Cyclic loading produced significant phase transformation in tested Y-TZP prostheses. The micro-Raman spectroscopy could be used as an alternative to XRD and ${\mu}XRD$.

• Journal of the Korean Society of Radiology
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• v.6 no.6
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• pp.477-481
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• 2012

An X-ray diffractometer which has various X-ray optics can give qualitative and quantitative information for a sample using a nondestructive analysis method. A parallel beam optic passes the parallel beam and removes divergent beam generated from an X-ray tube. The parallel beam optic used in the X-ray diffractometer was fabricated by wire cut and grading of stainless steel plates and was evaluated its performance using an X-ray imaging system. The measured parallelization of 6.6 mrad for the fabricated the parallel beam optic was a very close to the expected value of 6 mrad. An X-ray imaging technique for evaluating the parallel beam optics can estimate parallelization for each plate and can be used to other X-ray optics.

• Journal of the Korean Society of Costume
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• v.58 no.5
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• pp.211-231
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• 2008

To conserve historic textiles, analyses of textile materials, pollutants and deterioration are prerequisite steps. Based upon analytical results, guides for conservation of historic textiles are established. In analyses of textile materials, pollutants and deterioration, there are chemical methods(burning, solubility and staining), physical methods(microscopy and density) and instrumental analysis(Fourier Transform Infrared Spectroscopy (FT-IR), Fourier Transform Raman Spectroscopy(FT-Raman), Gas Chromatography(GC), Mass Spectroscopy(MS), X-Ray Fluorescence (EDXRF, WDXRF), Energy Dispersive Spectroscopy(EDS), and X-Ray Diffraction(XRD), Tensile Testing Machine etc.). Combination of qualitative and quantitative analyses makes accurate diagnosis of textile condition possible. As examples of analyses and conservation of historic textiles, Chuninsan(19 century) similar to sunshade with handing down historic textile and golden decorative skirt(17 century) with excavated costume are taken.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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• pp.2111-2111
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• 2001

A chemoinfometrical method for evaluating the quantitative determination of crystallinity one polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the and compared with the conventional powder X-ray diffraction method was performed. [Method] The pPure a and g forms of indomethacin (IMC) were prepared by reportedusing published methods. Six kinds of standard samples obtained by physically mixing of a and g forms. After the powder X-ray diffraction profiles of samples have been measured, the intensity values were normalized to against the intensity of silicon powder as the as an external standard. The calibration curves for quantification of crystal content were based upon the total relative intensity of four diffraction peaks from of the form g crystal. FT-NIR spectra of six calibration sample sets were recorded 5 times with the NIR spectrometer (BRAN+LUEBBE). Chemoinfometric analysis was performed on the NIR spectral data sets by applying the principal component regression (PCR). [Results] The relation between the actual and predicted polymorphic contents of form g IMC measured using by the X-ray diffraction method shows a good straight linen linear relation., and it has slope of 0.023, an intercept of 0.131 and a correlation coefficient of 0.986. PCR analyses wereis was performed based on normalized NIR spectra sets offer standard samples of known content of IMC g form. IMC. A calibration equation was determined to minimize the root mean square error of the predictionthe prediction. Figure 1 shows a plot of the calibration data obtained by NIR method between the actual and predicted contents of form g IMC. The predicted values were reproducible and had a smaller standard deviation. Figure 2 shows that the plot for the predicted transformation rate (%) of form a IMC to form g as measured by X-ray diffractomeoy against to those as measured by NIR method. The plot has a slope of 1.296, an intercept of 1,109, and a correlation coefficient of 0.992. The line represents a satisfactory correlation between the two predicted values of form g IMC content. Thus NIR spectroscopy is an effective method for the evaluation to the pharmaceutical products of quantitative of polymorph.