• Title/Summary/Keyword: XRD Analysis

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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.C. Impedance Properties of HA/Ti Compound Layer coated Ti-30Ta-(3~15)Nb Alloys (Ti-30Ta-(3~15)Nb 합금에 HA/Ti 복합 코팅한 표면의 교류임피던스 특성)

  • Jeong, Y.H.;Lee, H.J.;Moong, Y.P;Park, G.H.;Jang, S.H.;Son, M.K.;Choe, H.C.
    • Journal of the Korean institute of surface engineering
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    • v.41 no.5
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    • pp.181-188
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    • 2008
  • A.C. impedance properties of HA/Ti compound layer coated Ti-30Ta-($3{\sim}15$)Nb alloys have been studied by electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10 and 15 wt% Nb were manufactured by the vacuum furnace system. And then specimen was homogenized at $1000^{\circ}C$ for 24 hrs. The sample was cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The non-coated and coated morphology of Ti alloy were analyzed by X-ray diffractometer (XRD), energy X-ray dispersive spectroscopy (EDX) and filed emission scanning electron microscope (FE-SEM). The corrosion behaviors were investigated using A.C. impedance test (PARSTAT 2273, USA) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Ti-30Ta-($3{\sim}15\;wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and $\beta$ phase peak was predominantly appeared in the case of increasingly Nb contents. The microstructures of Ti alloy were transformed from needle-like structure to equiaxed structure as Nb content increased. From the analysis of coating surface, HA/Ti composite surface uniformed coating layer with 750 nm thickness. The growth directions of film were (211), (112), (300) and (202) for HA/Ti composite coating on the surface after heat treatment at $550^{\circ}C$, whereas, the growth direction of film was (110) for Ti coating. The polarization resistance ($R_p$) of HA/Ti composite coated Ti-alloys were higher than those of the Ti and HA coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

Characteristics of By-product Ochre from Acid Mine Drainage (AMD) Treatment and Its Potential Use (산성광산배수 (AMD) 처리 부산물 ochre의 특성과 활용)

  • Jeong, Jung-Hwan;Kim, Ho-Jin;Kim, Young-Nam;Nam, Kwang-Soo;Kim, Kye-Hoon
    • Korean Journal of Soil Science and Fertilizer
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    • v.43 no.3
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    • pp.304-314
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    • 2010
  • This study was carried out to find out potential use of ochre as an agent to reduce phosphorus content in water. Ochre is a by-product from treatment of acid mine drainage (AMD) which is composed mostly of $Fe_2O_3$, $Fe_2O_3{\cdot}H_2O$, $FeO{\cdot}OH$ and $Fe(OH)_3$. Three ochre samples (ochre-H, ochre-D and ochre-S) were collected from three treatment facilities in Gangwon province. Physico-chemical characteristics of three ochre samples including pH, electrical conductivity, total phosphorus, available phosphorus, particle size distribution were analyzed. Scanning electron microscopy (SEM) energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis were also carried out. In addition, experiments for phosphorus removal from water was performed. Calcium content of ochre-H was higher than that of ochre-D and ochre-S, whereas iron content of ochre-H was lower than that of ochre-D and ochre-S. All the phosphorus in water up to maximum 191,411 mg $kg^{-1}$ per unit mass of ochre was removed with ochre-H. Ochre has immense potential as an agent to reduce phosphorus content in water.

Influence of Mixtures and Curing Conditions on Strength and Microstructure of Reactive Powder Concrete Using Ternary Pozzolanic Materials (배합 및 양생조건이 3성분계 포졸란재를 이용한 RPC의 강도발현 특성에 미치는 영향)

  • Janchivdorj, Khulgadai;Choi, Seung-Hoon;So, Hyoung-Seok;Seo, Ki-Seog;So, Seung-Young
    • Journal of the Korea Concrete Institute
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    • v.25 no.4
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    • pp.457-465
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    • 2013
  • This study discussed the influence of mixtures and curing conditions on the development of strength and microstructure of RPC using ternary pozzolanic materials. Through pilot experiment, various RPC was manufactured by adding single or mixed ternary pozzolanic materials such as silica fume, blast furnace slag and fly ash by mass of cement, up to 0~65%, and cured by using 4 types of method which are water and air-dried curing at $20^{\circ}C$, steam and hot-water curing at $90^{\circ}C$. The results show that the use of ternary pozzolanic materials and a suitable curing method are an effective method for improving development of strength and microstructure of RPC. The unit volume of cement was greatly reduced in RPC with ternary pozzolanic materials and unlike hydration reaction in cement, the pozzolanic reaction noticeably contributes to a reduction in hydration heat and dry shrinkage. A considerable improvement was found in the flexural strength of RPC using ternary pozzolanic materials, and then the utilization of a structural member subjected to bending was expected. The X-ray diffractometer (XRD) analysis and Scanning Electronic Microscope (SEM) revealed that the microstructure of RPC was denser by using the ternary pozzolanic materials than the original RPC containing silica fume only.

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.

The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-propanol (이소프로판올의 탈수반응에서 지르코니아 촉매의 결정상에 따른 영향)

  • Sim, Hye-In;Park, Jung-Hyun;Cho, Jun Hee;Ahn, Ji-Hye;Choi, Min-Seok;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.208-213
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    • 2013
  • Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

Oxidation behavior of (Mo1-xWx)Si2 high-temperature heating elements (초고온용 발열체 (Mo1-xWx)Si2의 산화거동에 대한 연구)

  • Lee, Sung-Chul;Myung, Jae-ha;Kim, Yong-Nam;Jeon, Minseok;Lee, Dong-won;Oh, Jong-Min;Kim, Bae-Yeon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.5
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    • pp.200-207
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    • 2020
  • MoSi2, (Mo1/2W1/2)Si2, and WSi2 powders were synthesized by self-propagating high-temperature synthesis (SHS) method. The synthesized powders were heat-treated at 500, 1,000, 1,200, 1,300, 1,400, 1,500 and 1,600℃ in ambient atmosphere. Oxidation of Mo-W silicide powder was found at low temperature of 500℃. XRD structure analysis and DTA/TG data showed that MoO3 was formed with 500℃ heat treatment for 1 hour, and that it was α-cristobalite phase that was formed with 1200℃ heat treatment, not α-quartz phase which is commonly found and stable at room temperature. Existence of W accelerated decomposition at both low and high temperature. Fully sintered MoSi2 and (Mo1/2W1/2)Si2 specimen did not show decomposition or weight loss by oxidation, with 1 hour heat treatment at either low or high temperature. Notably, it was difficult to sinter WSi2 because of oxidation reaction at low temperature.

Sol-Gel Synthesis, Crystal Structure, Magnetic and Optical Properties in ZnCo2O3 Oxide

  • Das, Bidhu Bhusan;Barman, Bittesh
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.453-458
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    • 2019
  • Synthesis of ZnCo2O3 oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo2O3. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O2 in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at giso ~2.230 and giso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co2+(3d7) in the oxide. DC conductivity value of 2.875 ×10-8 S/cm indicates very weakly semiconducting nature of ZnCo2O3 at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions 4T1g(4F)→2Eg(2G), 4T1g(4F)→4T1g(4P), 4T1g(4F)→4A2g(4F), 4T1g(4F)→4T2g(4F), respectively in octahedral ligand field around Co2+ ions. Direct band gap energy, Eg~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo2O3.

Effect of Surfactants on ZnO Synthesis by Hydrothermal Method and Photocatalytic Properties (계면활성제 첨가에 의한 산화아연의 수열합성과 광촉매 특성)

  • Hyeon, Hye-Hyeon;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.34 no.1
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    • pp.50-57
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    • 2017
  • Zinc oxide is, one of metal oxide semiconductor, harmless to human and environment-friendly. It has excellent chemical and thermal stability properties. Wurtzite-zinc oxide is a large band gap energy of 3.37 eV and high exciton binding energy of 60 meV. It can be applied to various fields, such as solar cells, degradation of the dye waste, the gas sensor. The photocatalytic activity of zinc oxide is varied according to the particle shape and change of crystallinity. Therefore, It is very important to specify the additives and the experimental variables. In this study, the zinc oxide were synthesized by using a microwave assisted hydrothermal synthesis. The precursor was used as the zinc nitrate, the pH value was controlled as 11 by NaOH. Surfactants are the ethanolamine, cetyltrimethylammonium bromide, sodium dodecyl sulfate, sorbitan monooleate was added by changing the concentration. The composite particles had the shape of a star-like, curcular cone, seed shape, flake-sphere. Physical and chemical properties of the obtained zinc oxide was characterized using x-ray diffractometer, field emission scanning electron microscopy, thermogravimetric analysis and optical properties was characterized using UV-visible spectroscopy, photoluminescence and raman spectroscopy.