• Title/Summary/Keyword: XRD patterns

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Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

Characterization and Conversion Electron Mössbauer Spectroscopy of HoMn1-x-FexO3 Thin Films by Pulsed Laser Deposition (PLD를 이용한 HoMn1-x-FexO3 박막 제조 및 후방 산란형 뫼스바우어 분광 연구)

  • Choi, Dong-Hyeok;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.18-21
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    • 2007
  • The hexagonal $HoMn_{1-x}-Fe_xO_3$(x=0.00, 0.05) thin films were prepared using pulsed laser deposition(PLD) method on $Pt/Ti/SiO_2/Si$ substrate. The microstructure and magnetic properties have been studied by x-ray diffraction(XRD), atomic force microscopy (AFH), scanning electron microscope(SEM:), x-ray photoelectron spectroscopy(XPS), and conversion electron $M\"{o}ssbauer$ spectroscopy(CEMS). From the analysis of the x-ray diffraction patterns, the crystal structure for all films was found to be a hexagonal($P6_3cm$), which was preferentially grown along(110) direction. The lattice constant $c_0$ of the film with x=0.05 was close to that of single crystal, whereas lattice constant $a_0$ with respect to single crystal shows a slight decrease. This difference of lattice parameters between film and single crystal was caused by the lattice mismatch between the film and $Pt/Ti/SiO_2/Si$ substrate. Conversion electron $M\"{o}ssbauer$ spectrum of $HoMn_{0.95}Fe_{0.05}O_3$ thin film shows an asymmetry doublet absorption ratio at room temperature, which is due to the oriented direction of crystallographic domains. This is corresponding with analysis of x-ray diffraction. The quadrupole splitting(${\Delta}E_Q$) at room temperature is found to be $1.62{\pm}0.01mm/s$. This large ${\Delta}E_Q$ was caused by asymmetry environment surrounding Fe ion.

Synthesis and Characterization of Layered Copper Hydroxides in Highly Concentrated Solution (고농도 용액에서 Layered Copper Hydroxides의 합성 및 특성)

  • Nam, Dae-Hyean;Choi, Choong-Lyeal;Kim, Kwang-Seop;Seo, Young-Jin;Park, Man
    • Korean Journal of Soil Science and Fertilizer
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    • v.43 no.6
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    • pp.872-879
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    • 2010
  • Layered copper hydroxides [LCHs, $Cu_2(OH)_3{\cdot}NO_3$] has the agricultural potentials as a fungicide because of its high crystallinity, excellent anion exchange capacity, and its regular layered particle size. The study, for the first time, has synthesized LCHs in highly concentrated solution and evaluated its physicochemical properties including the crystallinity and suspension stability. Optimal synthetic condition of LCHs was determined by crystallinity and stability of suspension as follow; 1) concentrations of $Cu(NO_3)_2$ and NaOH solutions were 3.0 M respectively, 2) reaction temperature and solution pH were $25^{\circ}C$ and 6.0, respectively, and 3) aging time after reaction was 2hr. Crystallinity of LCHs enhanced with increase in pH up to 9.0. Whereas, stability of suspension was decrease by increase in crystal size. Especially, increase in reaction temperature decreased stability of suspension. XRD patterns and SEM images exhibited that LCHs had regular layered particle size with 0.2~0.8 ${\mu}m$ and high crystallinity in optimal synthetic condition. The particle size was increased with increase in reaction temperature and pH. These results showed that LCHs synthesized in highly concentrated solution exhibited high stability of suspension as well as high crystallinity suitable to their potential as a fungicide.

A Study on Production Kiln Site Estimation, based on Historical Ceramic Characteristics and Scientific Analysis of the Celadons Excavated From the Beopcheon Temple Site and Son-gok 2-ri 4th Kiln Site (법천사지 청자와 손곡2리 4호 가마터 청자의 도자사적 성격과 과학적 분석을 통한 생산 가마터 추정 연구)

  • Lee, Byeong-hoon;Yun, Seok-in
    • Korean Journal of Heritage: History & Science
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    • v.47 no.3
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    • pp.24-41
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    • 2014
  • Since the celadons excavated from the Son-gok 2-ri 4th kiln site are located in the Beopcheon temple site and at close range, the similarity to the celadons excavated from the Beopcheon temple site is being raised. Thus, this study examined the correlation using a natural-scientific method. In this study, historical ceramic properties of total 19 celadons were examined and they were scientifically analyzed. First of all, according to the scientific analysis, chemical compositions of celadon clay showed a dispersed distribution at RO2 3.79-7.77mole and RO+R2O 0.33-0.49mole. When the microstructure was analyzed, most celadons excavated from the Beopcheon temple site, Wonju, which are estimated to be used in real life, had a favorable state, and some celadons from the Son-gok 2-ri 4th kiln site were found not to be glazed and sintered properly. When analyzing body crystalline phases of the celadons using the XRD method, quartz and mullite were extracted from all of the samples. And corundum was extracted from sg4 sample. Though firing temperature of each sample was different, they were mostly fired to temperatures between 1150 and $1200^{\circ}C$ and some of them experienced a low temperature of $1100^{\circ}C$ or a high temperature above $1200^{\circ}C$. Various chemical compositions and producing techniques were observed in the celadons from the Beopcheon temple site and Son-gok 2-ri 4th kiln site and it is hard to assure that the Son-gok 2-ri 4th kiln site was the production kiln site of the celadons used in the Beopcheon temple site. But according to the analysis of rare earth elements, some of the celadons from the Beopcheon temple site and Son-gok 2-ri 4th kiln site displayed a distribution pattern with certain regularity and this implies there is a possibility that the raw materials used in producing the ceramics might have come from the same origin. From the perspective of ceramic history, the celadons excavated from the Beopcheon temple site and Son-gok 2-ri 4th kiln site were produced using the same molding and sintering technique. Also, it is estimated that they were produced in the 12th or 13th century, judging from the overall shapes and patterns of the celadons.

Influences of the Composition on Spectroscopic Characteristics of AlxGa1-xN Thin Films (AlxGa1-xN 박막의 조성이 분광학적 특성에 미치는 영향)

  • Kim, Dae Jung;Kim, Bong Jin;Kim, Duk Hyeon;Lee, Jong Won
    • New Physics: Sae Mulli
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    • v.68 no.12
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    • pp.1281-1287
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    • 2018
  • In this study, $Al_xGa_{1-x}N$ films were grown on (0001) sapphire substrates by using metal-organic chemical vapor deposition (MOCVD). The crystallinity of the grown films was examined with X-ray diffraction (XRD) patterns. The surfaces and the chemical properties of the $Al_xGa_{1-x}N$ films were investigated using atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS), respectively. The optical properties of the $Al_xGa_{1-x}N$ film were studied in a wide photon energy range between 2.0 ~ 8.7 eV by using spectroscopic ellipsometry (SE) at room temperature. The data obtained by using SE were analyzed to find the critical points of the pseudodielectric function spectra, $<{\varepsilon}(E)>=<{\varepsilon}_1(E)>+i<{\varepsilon}_2(E)>$. In addition, the second derivative spectra, $d^2<{\varepsilon}(E)>/dE^2$, of the pseudodielectric function for the $Al_xGa_{1-x}N$ films were numerically calculated to determine the critical points (CPs), such as the $E_0$, $E_1$, and $E_2$ structure. For the four samples (x = 0.18, 0.21, 0.25, 0.29) between a composition of x = 0.18 and x = 0.29, changes in the critical points (blue-shifts) with increasing Al composition at 300 K for the $Al_xGa_{1-x}N$ film were observed via ellipsometric measurements for the first time.

Preparation of Organophilic MMT Modified with Various Aromatic Amines and Characterization of Polyimide Nanocomposite Films (다양한 구조의 방향족 아민으로 개질된 친유기성 MMT의 제조와 이를 이용한 폴리이미드 나노복합필름의 특성)

  • Han, Seung San;Choi, Kil-Yeong;Im, Seung Soon;Kim, Yong Seok
    • Applied Chemistry for Engineering
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    • v.17 no.2
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    • pp.177-182
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    • 2006
  • In this work, we have prepared organophilic MMT having thermal stability by ion exchange reaction of various aromatic ammonium salts with MMT containing sodium ion. The organic modifiers having alkyl side chains and amine functional group were successfully synthesized by effectively introducing the surfaces of MMT via ion exchange reaction to form organophilic MMTs with a view to improve the reactivity and thermal stability. The WAXD patterns of organophilic MMT showed the more increased gallery spacing by $3.3{\AA}$ than that of the pristine MMT and also the onset of initial decomposition of organophilic MMT was $275^{\circ}C$ as determined by a thermogravimetric analysis. The polyimide (PI) nanocomposite films based on poly(amic acid) and organophilic MMT were prepared by a solution blending followed by cyclodehydration reaction. We have investigated the dispersity of organophilic MMTs in PI matrix by using WAXD and the effect of the organophilic MMT content on the mechanical properties of PI nanocomposite films was studied.

A Study on Distribution of Mössbauer Spectroscopy in Al Doped Garnet (Al을 치환한 Garnet의 Mössbauer분포 함수 연구)

  • Min, Byoung-Ki;Kim, Sam-Jin;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.12 no.1
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    • pp.1-6
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    • 2002
  • Al$\^$3+/ substituted garnet Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ (x=0.0, 0.25, 0.5, 0.75, 1.0) was fabricated by sol-gel method. The crystallographic and magnetic properties of Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ have been studied with Mossbauer spectroscopy, x-ray diffraction (XRD), thermogravimetry analysis (TGA), differential thermal analysis (DTA), and vibrating samples magnetometer (VSM). The crystal structure of Y$_3$Fe$\_$5/O$\_$12/ is found to be a cubic with the lattice constant a$\_$0/= 12.381$\pm$0.005 $\AA$. The lattice constants a$\_$0/ decreases linearly from 12.381 to 12.304 A as the Al concentration (x) increases from x=0.0 to 1.0. Mossbauer spectra of measured at Y$_3$Fe$\_$5-x/A1$\_$x/O$\_$12/ various absorber temperatures of 13 to 600 K. Mossbauer spectrum for x = 0.0 is consist of well resolved two sets of six line patterns. While with increasing Al concentration outer sextet patters, which is originating from octahedral sites, broadens widely. These phenomena are interpreted in terms of random probability distributions of Fe$\^$3+/ and Al$\^$3+/ in tetrahedral site.

Solid state reactive sintering of cold pressed thermoelectric Mg3Sb2 (냉간 압축 성형한 Mg3Sb2 열전재료의 고상 반응 소결)

  • Kim, In-Ki;Jang, Kyung-Wook;Oh, Han-Jun
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.4
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    • pp.176-182
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    • 2014
  • We intended to prepare $Mg_3Sb_2$ compound bodies through solid state reactive sintering after cold-pressing mixtures of elementary Mg and Sb powders and investigated the crystal phases of the sintered bodies according to Mg/Sb mole ratios and reaction temperatures. The $Mg_3Sb_2$ bodies sintered at the temperatures of 773~843 K showed typical crystalline phases of $Mg_3Sb_2$ compounds, but their diffraction angles in XRD patterns were slightly different along with the vertical axis of the bodies obtained. All the bottom parts of the sintered $Mg_3Sb_2$ bodies were composed of the typical crystalline phases of $Mg_3Sb_2$ compounds and their diffraction angles were completely in accord with those of the ${\alpha}-Mg_3Sb_2$ phase, when Mg : Sb = 3.15 : 1.85 at 823 K, or when the Mg moles were greater than or equal to 3.10 at 843 K. It was considered that the slightly remaining Mg phases were formed by precipitation from ${\alpha}-Mg_3Sb_2$ phases during the solidification process of liquid phase.

Growth and Optical Properties of SnSe/BaF2 Single-Crystal Epilayers (SnSe/BaF2 단결정 박막의 성장과 광학적 특성)

  • Lee, II Hoon;Doo, Ha Young
    • Journal of Korean Ophthalmic Optics Society
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    • v.7 no.2
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    • pp.209-215
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    • 2002
  • This study investigated the crystal growth, crystalline structure and the basic optical properties of $SnSe/BaF_2$ epilayers. The SnSe epilayer was grown on $BaF_2$(111) insulating substrates using a hot wall epitaxy(HWE) technique. It was found from the analysis of X-ray diffraction patterns that $SnSe/BaF_2$ epilayer was growing to single crystal with orthorhombic structure oriented [111] along the growth direction. Using Rutherford back scattering(RBS), the atomic ratios of the SnSe was found to be stoichiometric, almost 50 : 50. The best values for the full width at half maximum (FWHM) of the DCXRD was 163 arcsec for SnSe epilarer. The epilayer-thickness dependence of the FWHM of the DCXRD shows that the quality of the $SnSe/BaF_2$ is as expected. The dielectric function ${\varepsilon}$(E) of a semiconductor is closely related to its electronic energy band structure and such relation can be drawn from features around the critical points in the optical spectra. The real and imaginary parts(${\varepsilon}_1$ and ${\varepsilon}_2$) of the dielectric function ${\varepsilon}$ of SnSe were measured. These data are analyzed using a theoretical model known as the model dielectric function(MDF). The optical constants related to dielectric function such as the complex refractive index(n*-n+ik), absorption coefficient (${\alpha}$) and normal- incidence reflectivity (R) are also presented for $SnSe/BaF_2$.

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Gas Sensing Behaviors of SnO2:Cu Nanostructures for CH4, CH3CH2CH3 Gas (SnO2:Cu 나노 구조물의 CH4, CH3CH2CH3 가스 감응 특성)

  • Lee, Ji-Young;Yu, Yoon-Sic;Yu, Il
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.12
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    • pp.974-978
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    • 2012
  • The effect of Cu coating on the sensing properties of nano $SnO_2:Cu$ based sensors for the $CH_4$, $CH_3CH_2CH_3$ gas was studied. This work was focussed on investigating the change of sensitivity of nano $SnO_2:Cu$ based sensors for $CH_4$, $CH_3CH_2CH_3$ gas by Cu coating. Nano sized $SnO_2$ powders were prepared by solution reduction method using stannous chloride($SnCl_2{\cdot}2H_2O$), hydrazine($N_2H_2$) and NaOH and subsequent heat treatment. XRD patterns showed that nano $SnO_2$ powders with rutile structure were grown with (110), (101), (211) dominant peak. The particle size of nano $SnO_2:Cu$ powders at 8 wt% Cu was about 50 nm. $SnO_2$ particles were found to contain many pores, according to SEM analysis. The sensitivity of nano $SnO_2:Cu$ based sensors was measured for 5 ppm $CH_4$ gas and $CH_3CH_2CH_3$ gas at room temperature by comparing the resistance in air with that in target gases. The sensitivity for both $CH_4$ and $CH_3CH_2CH_3$ gases was improved by Cu coating on the nano $SnO_2$ surface. The response time and recovery time of the $SnO_2:Cu$ gas sensors for the $CH_4$ and $CH_3CH_2CH_3$ gases were 18~20 seconds, and 13~15 seconds, respectively.