• Title/Summary/Keyword: Quantitative X-ray diffraction

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QUANTITATIVE ANALYSIS OF CRYOMILLED NANOCRYSTALLINE Ti-6Al-4V ALLOY POWDER BY X-RAY DIFFRACTION

  • M. OH;H.K. YU;J.-H. LEE;M.C. OH;S.-H. JUNG;B. AHN
    • Archives of Metallurgy and Materials
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    • v.63 no.3
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    • pp.1439-1442
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    • 2018
  • A nanocrystalline Ti alloy powder was fabricated using cryomilling. The grain size and lattice strain evolution during cryomilling were quantitatively analyzed using X-ray diffraction (XRD) based on the Scherrer equation, Williamson-Hall (W-H) plotting method, and size-strain (S-S) method assuming uniform deformation. Other physical parameters including stress and strain have been calculated. The average crystallite size and the lattice strain evaluated from XRD analysis are in good agreement with the result of transmission electron microscopy (TEM).

Study on the Orientation of Particles in Tablets (정제내부의 입자배열에 관한 연구)

  • Sohn, Young-Taek
    • Journal of Pharmaceutical Investigation
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    • v.21 no.3
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    • pp.125-132
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    • 1991
  • Using X-ray crystallography powder diffraction, the quantitative representation method of preferred orientation of particles ill tablets was developed. Selected faces of a tablet. the upper surface and faces cut parallel and normal to the upper surface, were presented to an X-ray beam and X-ray diffraction patterns for these faces were measured. The effects of particle size. tableting pressure, and particle form on the preferred orientation were also investigated. It was also recognized that the degree of anisotropy in terms of capping tendency was influenced by the preferred orientation of particles in tablets.

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Structure of Ni and NiO Nanoparticles Observed by X-ray Coherent Diffraction Imaging

  • Kim, Chan;Kim, Yoon-Hee;Hamh, Sun-Young;Son, Jun-Gon;Khakurel, Krishna Prasad;Iqbal, Mazhar;Noh, Do-Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.542-543
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    • 2012
  • Coherent diffraction imaging (CDI) method using hard x-ray at 5.46 keV was applied to study assembly of Ni and Ni oxide nano structures formed on a Si3N4 membrane. Density distribution of Ni nano-particles was obtained quantitatively with about 15 nm lateral resolution by reconstructing images from the speckle diffraction pattern. In addition, reconstructed images of nickel oxide particles indicated that Ni atoms diffuse out during the oxidation process leaving pores inside the nickel oxide crust. Furthermore, we recognize that really weak phase object, less than 5 nm thickness of Ni residues, can be reconstructed due to the reference particles. We achieved quantitative information of nanometer sized materials and demonstrate the effect of reference particles by using hard x-ray coherent diffractive imaging method.

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Application Study of Chemoinfometrical Near-Infrared Spectroscopic Method to Evaluate for Polymorphic Content of Pharmaceutical Powders (일본의 근적외선분광법에 대한 제약회사 응용 및 현황)

  • Otsuka, Makoto
    • 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.

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Determination of mixing ratios in a mixture via non-negative independent component analysis using XRD spectrum (XRD 스펙트럼의 비음독립성분분석을 통한 혼합물 구성비 결정)

  • You, Hanmin;Jun, Chi-Hyuck;Lee, Hyeseon;Hong, Jae-Hwa
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.502-507
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    • 2007
  • X-ray diffraction method has been widely used for qualitative and quantitative analysis of a mixture of materials since every crystalline material gives a unique X-ray diffraction pattern independently of others, with the intensity of each pattern proportional to that material's concentration in a mixture. For determination of mixing ratios, extracting source spectra correctly is important and crucial. Based on the source spectra extracted, a regression model with non-negativity constraint is applied for determining mixing ratios. In some mixtures, however, X-ray diffraction spectrum has sharp and narrow peaks, which may result in partial negative source spectrum from independent component analysis. We propose several procedures of extracting non-negative source spectra and determining mixing ratios. The proposed method is validated with experimental data on powder mixtures.

A Study of the Crystal Structure of the Fine S-Phase Precipitate in Al-Cu-Mg Alloy by Electron Diffraction Experiments (전자회절실험에 의한 알루미늄 합금 (Al-Cu-Mg)의 미세 S-상 석출입자에 대한 결정구조 연구)

  • Kim, Hwang-Su
    • Applied Microscopy
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    • v.35 no.4
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    • pp.1-9
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    • 2005
  • In this paper it is reported that a comprehensive study of the crystal structure of the fine size S-phase ($Al_2CuMg$) precipitate in Al-Cu-Mg alloy by electron diffraction experiments. The experiments involve taking the selected area diffraction pattern for a S-phase particle, simulations of the pattern based on the kinematical diffraction theory and quantitative data collection from the zone axis diffraction patterns for the comparison with calculated diffraction intensity using both the kinematical and the dynamical diffraction theory. As a result, a good fitting model of the S-phase structure turns out to be the model reported early by X-ray methods (Perlitz & Westgren, 1943), not the new model determined by HRTEM methods (Radmilovic et al., 1999).

X-ray Diffraction Studies of Poly(aryl ether ether ketone) Fibers with Different Degrees of Crystallinity and Orientation

  • Karacan Ismail
    • 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.

7$\AA$ Phase in the Sancheong Kaolin : 7$\AA$-Halloysite or Kaolinite\ulcorner (산청 고령토중의 7$\AA$ 상에 대한 연구 : 7$\AA$-할로이사이트 또는 캐올리나이트\ulcorner)

  • 정기영;김수진
    • Journal of the Mineralogical Society of Korea
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    • v.2 no.1
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    • pp.18-25
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    • 1989
  • The X-ray diffraction and electron microscopy study of the kaolin sample from Sancheong area show that the halloysite occurs as hydrated 10$\AA$ form. It implies that the 7$\AA$ reflection and hk-line splitting in the X-ray diffractogram are ascribed to kaolinite. Kaolinite in Sancheong kaolin is of a disordered type. It tends to be enriched in the colored part of kaolin samples. Quantitative analyses show that kaolin contains 16-57% halloysite and 10-55%kaolinite.

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Improvement of Measurement Accuracy by Correcting Systematic Error Associated with the X-ray Diffractometer (X-선 회절 장비의 기계적 오차 수정을 통한 분석 정확도 향상)

  • Choi, Dooho
    • 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.

Quantitative Analysis of Metallographic Characteristics with Austenitizing Temperature in STD 11 Steel (STD 11 강의 오스테나이트화 온도에 따른 제 특성의 정량 분석)

  • Kim, J.E.;Ju, Y.H.;Jang, W.Y.
    • 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 $300^{\circ}C$.