• Title/Summary/Keyword: High-temperature XRD

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BCTZ Addition on the Microstructure, Piezoelectric/Dielectric Properties and Phase Transition of NKLN-AS Piezoelectric Ceramics (BCTZ첨가가 NKLN-AS계 압전세라믹스의 미세구조와 압전/유전특성 및 상전이현상에 미치는 효과)

  • Lee, Woong-Jae;Ur, Soon-Chul;Lee, Young-Geun;Yoon, Man-Soon
    • Korean Journal of Materials Research
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    • v.22 no.1
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    • pp.35-41
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    • 2012
  • Presently, the most promising family of lead-free piezoelectric ceramics is based on $K_{0.5}Na_{0.5}NbO_3$(KNN). Lithium, silver and antimony co-doped KNN ceramics show high piezoelectric properties at room temperature, but often suffer from abnormal grain growth. In the present work, the $(Ba_{0.85}Ca_{0.15})(Ti_{0.88}Zr_{0.12})O_3$ component, which has relaxor ferroelectric characteristics, was doped to suppress the abnormal grain growth. To investigate this effect, Lead-Free $0.95(K_{0.5}Na_{0.5})_{0.95}Li_{0.05}NbO_3-(0.05-x)AgSbO_3-x(Ba_{0.85}Ca_{0.15})(Ti_{0.88}Zr_{0.12})O_3$[KNLN-AS-xBCTZ] piezoelectric ceramics were synthesized by ball mill and nanosized-milling processes in lead-Free $0.95(K_{0.5}Na_{0.5})_{0.95}Li_{0.05}NbO_3-(0.05-x)AgSbO_3$ in order to suppress the abnormal grain growth. The nanosized milling process of calcined powders enhanced the sintering density. The phase structure, microstructure, and ferroelectric and piezoelectric properties of the KNLN-AS ceramics were systematically investigated. XRD patterns for the doped and undoped samples showed perovskite phase while tetragonality was increased with increasing BCZT content, which increase was closely related to the decrease of TO-T. Dense and uniform microstructures were observed for all of the doped BCZT ceramics. After the addition of BCTZ, the tetragonal-cubic and orthorhombic-tetragonal phase transitions shifted to lower temperatures compared to those for the pure KNNL-AS. A coexistence of the orthorhombic and tetragonal phases was hence formed in the ceramics with x = 0.02 mol at room temperature, leading to a significant enhancement of the piezoelectric properties. For the composition with x = 0.02 mol, the piezoelectric properties showed optimum values of: $d_{33}$ = 185 pC/N, $k_P$ = 41%, $T_C=325^{\circ}C$, $T_{O-T}=-4^{\circ}C$.

The Study on the Crystal Growing of Mn-Zn Ferrite Single Crystals by Floating Zone Method (Floating Zone법에 의한 Mn-Zn Ferrite 단결정성장에 관한 연구)

  • 정재우;오근호
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.2 no.1
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    • pp.10-19
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    • 1992
  • Mn - Zn Ferrite has physical properties of the high initial permeability, saturation magnetic flux density, and low loss factor as a representative magnetic material of soft ferrites, in addition the mechanical property is excellent as a single crystal. Therefore it is important electronic components and used for VTR Head. Mn - Zn Ferrite single crystals with the diameter 8mm were grown in atmosphere mixed with $O_2$ and Ar gas by the Floating Zone(FZ) method that impurities can not be incorporated to the crystals because of not-using the crucible to put in the melt, and the sharp temperature gradient results from making a focus at one point utilizing the infrared ray emitted from the halogen lamp as a heat source. During the crystal growing, the highest temperature of melting area was maintained to be $1650^{\circ}C$, growth rate and rotation rate were 10 mm/hr, 20 rpm respectively. The phases and the growth directions of crystals were determined from the analysis of X RD patterns, Laue, TEM diffraction patterns and etch pit shapes were observed by the optical microscope through the chemical etching. The corelation of optimum conditions for acquiring the better crystals was found out with the growth rate, the length and diameter of melt at the interface according to the diameter of feed rod, and the patterns of growing interface also studied.

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Electrical Properties of $Ba_{1-x}(Bi_{0.5}K_{0.5})TiO_3$ according to $(Bi_{0.5}K_{0.5})TiO_3$ for Pb-free PTC (Pb-free PTC에 있어서 $(Bi_{0.5}K_{0.5})TiO_3$ 첨가에 따른 $Ba_{1-x}(Bi_{0.5}K_{0.5})TiO_3$의 전기적특성)

  • Lee, Mi-Jai;Choi, Byung-Hyun;Paik, Jong-Hoo;Kim, Bip-Nam;Lee, Woo-Yong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.35-36
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    • 2008
  • PTC thermistor are characterized by an increase in the electrical resistance with temperature. The PTC materials of middle Curie point were produced or that of high Curie point (above $200^{\circ}C$), it was determined that compositional modifications of $Pb^{2+}$ for $Ba^{2+}$ produce change sin the Curie point to higher temperature. PTC ceramic materials with the Curie point above $120^{\circ}C$ were prepared by adding $PbTiO_3$, PbO or $Pb_3O_4$ into $BaTiO_3$. Thereby, adding $Pb^{2+}$ into $BaTiO_3$-based PTC material to improve Tc was studied broadly, however, weal know that PbO was poisonous and prone to volatilize, then to pollute the circumstance and hurt to people, so we should dope other innocuous additives instead of lead to increase Tc of composite PTC material. In order to prepare lead-free $BaTiO_3$-based PTC with middle Curie point, the incorporation on $Bi_{1/2}K_{1/2}TiO_3$ into $BaTiO_3$-based ceramics was investigated on samples containing 0, 1, 2, 3, 4, and 50mol% of $Bi_{1/2}K_{1/2}TiO_3$. $Bi_{1/2}K_{1/2}TiO_3$ was compounded as standby material by conventional solid-state reaction technique. The starting materials were $Bi_2O_3$, $K_2CO_3$, $BaCO_3$ and $TiO_2$ powder, and using solid-state reaction method, too. The microstructures of samples were investigated by SEM, DSC, XRD and dielectric properties. Phase composition and lattice parameters were investigated by X-ray diffraction.

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Characterization and Formation Mechanism of Zr-Cu and Zr-Cu-Al Metallic Glass Thin Film by Sputtering Process

  • Lee, Chang-Hun;Sun, Ju-Hyun;Moon, Kyoung-Il;Shin, Seung-Yong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.271-272
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    • 2012
  • Bulk Metallic Glasses (BMGs or amorphous alloy) exhibit high strength and good corrosion resistance. Applications of thin films and micro parts of BMGs have been used a lot since its inception in the research of BMGs. However, Application and fabrication of BMGs are limited to make structural materials. Thin films of BMGs which is sputtered on the surface of structural materials by sputtering process is used to improve limits about application of BMGs. In order to investigate the difference of properties between designed alloys and thin films, we identified that thin films deposited on the surface that have the characteristic of the amorphous films and the composition of designed alloys. Zr-Cu (Cu=30, 35, 38, 40, 50 at.%) and Zr-Cu-Al (Al=10 at.% fixed, Cu=26, 30, 34, 38 at.%) alloys were fabricated with Zr (99.7% purity), Cu (99.997% purity), and Al (99.99% purity) as melting 5 times by arc melting method before rods 2mm in diameter was manufactured. In order to analyze GFA (Glass Forming Ability), rods were observed by Optical Microscopy and SEM and $T_g$, $T_x$, ($T_x$ is crystallization temperature and $T_g$ is the glass transition temperature) and Tm were measured by DTA and DSC. Powder was manufactured by Gas Atomizer and target was sintered using powder in large supercooled liquid region ($=T_x-T_g$) by SPS(Spark Plasma Sintering). Amorphous foil was prepared by RSP process with 5 gram alloy button. The composition of the foil and sputtered thin film was analyzed by EDS and EPMA. In the result of DSC curve, binary alloys ($Zr_{62}Cu_{38}$, $Zr_{60}Cu_{40}$, $Zr_{50}Cu_{50}$) and ternary alloys ($Zr_{64}Al_{10}Cu_{26}$, $Zr_{56}Al_{10}Cu_{34}$, $Zr_{52}Al_{10}Cu_{38}$) have $T_g$ except for $Zr_{70}Cu_{30}$ and $Zr_{60}Al_{10}Cu_{30}$. The compositions with $T_g$ made into powders. Figure shows XRD data of thin film showed similar hollow peak.

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Effect of $BaTiO_3$ according to $(Bi_{0.5}Na_{0.5})TiO_3$ for Pb-free PTC (Pb-free PTC에 있어서 $(Bi_{0.5}Na_{0.5})TiO_3$ 첨가에 따른 $BaTiO_3$ 효과)

  • Lee, Mi-Jai;Paik, Jong-Hoo;Kim, Sei-Ki;Kim, Bip-Nam;Lee, Woo-Yong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.57-58
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    • 2008
  • PTC thermistor are characterized by an increase in the electrical resistance with temperature. The PTC materials of middle Curie point were produced or that of high Curie point (above $200^{\circ}C$), it was determined that compositional modifications of $Pb^{2+}$ for $Ba^{2+}$ produce change sin the Curie point to higher temperature. PTC ceramic materials with the Curie point above $120^{\circ}C$ were prepared by adding $PbTiO_3$, PbO or $Pb_3O_4$ into $BaTiO_3$. Thereby, adding $Pb^{2+}$ into $BaTiO_3$-based PTC material to improve Tc was studied broadly, however, weal know that PbO was poisonous and prone to volatilize, then to pollute the circumstance and hurt to people, so we should dope other innocuous additives instead of lead to increase Tc of composite PTC material. In order to prepare lead-free $BaTiO_3$-based PTC with middle Curie point, the incorporation on $Bi_{1/2}Na_{1/2}TiO_3$ into $BaTiO_3$-based ceramics was investigated on samples containing 0, 1, 2, 3, 4, and 50mol% of $Bi_{1/2}Na_{1/2}TiO_3$. $Bi_{1/2}Na_{1/2}TiO_3$ was compounded as standby material by conventional solid-state reaction technique. The starting materials were $Bi_{1/2}Na_{1/2}TiO_3$, $BaCO_3$, $TiO_2$ and $Y_2O_3$ powder, and using solid-state reaction method, too. The microstructures of samples were investigated by SEM, DSC, XRD and dielectric properties. Phase composition and lattice parameters were investigated by X-ray diffraction.

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Effect of RTA Temperature on the Structural and Optical Properties of HfO2 Thin Films (급속 열처리 온도가 HfO2 박막의 구조적 및 광학적 특성에 미치는 효과)

  • Chung, Yeun-Gun;Joung, Yang-Hee;Kang, Seong-Jun
    • The Journal of the Korea institute of electronic communication sciences
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    • v.14 no.3
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    • pp.497-504
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    • 2019
  • We fabricated $HfO_2$ thin films using RF magnetron sputtering method, and investigated structural and optical properties of $HfO_2$ thin films with RTA temperatures in $N_2$ ambient. $HfO_2$ thin films exhibited polycrystalline structure regardless of annealing process, FWHM of M (-111) showed reduction trend. The surface roughness showed the smallest of 3.454 nm at a annealing temperature of $600^{\circ}C$ in result of AFM. All $HfO_2$ thin films showed the transmittance of about 80% in visible light range. By fitting the refractive index from the transmittance and reflectance to the Sellmeir dispersion relation, we can predict the refractive index of the $HfO_2$ thin film according to the wavelength. The $HfO_2$ thin film annealed at $600^{\circ}C$ exhibited a high refractive index of 2.0223 (${\lambda}=632nm$) and an excellent packing factor of 0.963.

Catalytic Effects on Graphitized Carbon Fibers of Graphitization Catalysts Introduced during Hot-Water Stretching (열수 연신시 흑연화 촉매 도입에 따른 탄소섬유의 흑연화 촉진효과)

  • Hyun-Jae Cho;Hye Rin Lee;Byoung-Suhk, Kim;Yong-Sik, Chung
    • Composites Research
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    • v.37 no.3
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    • pp.162-169
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    • 2024
  • In this study, PAN(polyacrylonitrile)-based precursor fibers were produced through a wet-spinning process, and their morphologies and graphitization behavior were investigated in the presence of two graphitization catalysts (Ca, Ni). The graphitization catalysts were introduced into the formed pores during hot-water stretching of wet-spun PAN-based precursor fibers. The catalytic effects of graphitization catalysts were examined through crystal structure and Raman analysis. At a relatively low temperature of 1500℃, the graphitization was not significantly affected, whereas at a high temperature of 2400℃, the obtained ID/IG value of graphite fiber (GF-Ni100) was decreased by about twice (~0.28) compared to the untreated fibers (GF-AS~0.54). By comparing the ID/IG values (GF-Ca100~0.42: GF-Ni100~0.28) of Ca and Ni graphitization catalyst, it was found that the degree of graphitization of Ni graphitization catalyst showed higher influence than that of Ca graphitization catalyst. Moreover, 2D band was also observed, indicating that the graphite plane structures composed of multiple layers were developed. XRD results confirmed that the crystal inter-planar distance (d002) of the graphite crystal was slightly decreased after the treatment with the graphitization catalyst, But, the crystal size of Ca-treated graphite fiber (GF-Ca100) was increased by up to ~5 nm.

Investigation of physicochemical properties, sustainability and environmental evaluation of metakaolin- granulated blast furnace slag geopolymer concrete

  • Anas Driouich;Safae El Alami El Hassani;Zakia Zmirli;Slimane El Harfaoui;Nadhim Hamah Sor;Ayoub Aziz;Jong Wan Hu;Haytham F. Isleem;Hadee Mohammed Najm;Hassan Chaair
    • Computers and Concrete
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    • v.34 no.4
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    • pp.489-501
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    • 2024
  • Geopolymers are part of a class of materials characterized by properties combining polymers, ceramics, and cement. These include exceptionally high thermal and chemical stability, excellent mechanical strength and durability in aggressive environments. This work deals with the synthesis, characterization, and sustainability evaluation of GPGBFS-MK geopolymers by alkaline activation of a granulated blast furnace slag-metakaolin mixture. In the first step, elemental and oxide analyses by XRF and EDS showed that the main constituents of GPGBFS-MK geopolymers are silicon, sodium, and aluminium oxides. The structural analyses by XRD and FTIR confirmed that the geopolymerization for GPGBFS-MK geopolymers did occur, accompanied by the formation of disordered networks from the blends and a modification to the microstructure by the geopolymerization process. Similarly, the microstructural study made by SEM showed that the GPGBFS-MK geopolymers are constituted by aluminosilicates in the form of dense clusters on which are adsorbed particles of unreacted GBFS in the form of spheroids and white residues of the alkaline activating solution. In addition, the study of the sustainability evaluation of GPGBFS-MK geopolymers showed that the water absorption of geopolymeric materials is lower than that of OPC cement. As for the elevated temperature resistance, the analyses indicated an excellent elevated temperature resistance of GPGBFS-MK. In the same way, the study of the resistance to chemical aggressions showed that the GPGBFS-MK geopolymeric materials are unattackable, contrary to the OPC cement-based materials which are strongly altered.

Crystallographic and Magnetic Properties of Brownmillerite Ca1-xSrxFeO2.5(x=0, 0.3, 0.5, 0.7, 1.0) (Brownmillerite Ca1-xSrxFeO2.5(x=0, 0.3, 0.5, 0.7, 1.0)의 결정학적 및 자기적 성질에 관한 연구)

  • Yoon, Sung-Hyun;Yang, Ju-Il;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.14 no.2
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    • pp.76-82
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    • 2004
  • Crystallographic and magnetic properties for Brownmillerite-type oxides $Ca_{1-x}$Sr$_{x}$FeO$_{2.5}$ (x = 0, 0.3, 0.5, 0.7, 1.0) were investigated using x-ray diffraction (XRD) and Mossbauer spectroscopy. Polycrystalline samples were prepared by conventional solid-state reaction method. Information on exact crystalline structures, lattice parameters, bond lengths and bond angles were obtained by refining their XRD profiles using a Rietveld method. The crystal structures were found to be all orthorhombic with space group Icmm (x = 0, 0.3) and Icmm (x = 0.5, 0.7, 1.0) The lattice parameters increased monotonically with increasing Sr concentration. Both the tetrahedral and the octahedral sites were considerably distorted and elongated along b-axis. While bond lengths and bond angles O-Fe-O tend to increase minutely with the increase of Sr content, bond angles Fe-O-Fe decreased accordingly. The Mossbauer spectra showed two sets of sharp sextets originating from ferric ions occupying the tetrahedral and the octahedral sites under the magnetic transition temperature T$_{N}$. Regardless of the compositions x, the electric quadrupole splittings were -0.3 mm/s and 0.4 mm/s for the octahedral and the tetrahedral site, respectively. Above T$_{N}$, the Mossbauer spectra showed the paramagnetic doublets whose electric quadrupole splittings were about 1.6 mm/s, irrespective of compositions x. T$_{N}$ was found to decrease monotonically with the increase of Sr concentration. Ratios of absorption area for the two sites were almost 1:1 up to as high as 0.95 T$_{N}$ for all x. The result of the Debye temperature indicated that the inter-atomic binding force for the Fe atoms in the tetrahedral site was stronger than that for the octahedral site.hedral site.

Dealumination of $NH_4Y$-Zeolite to Convert to the Hydrophobic Zeolite by High-Temperature Steam Treatment (소수성 제올라이트로의 변환을 위한 고온 수증기처리에 의한 $NH_4Y$-제올라이트의 탈알루미늄)

  • Kim, Jin-Young;Jeon, Dong-Hwan;Chung, Byung-Hwan;Mo, Se-Young
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.4
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    • pp.420-430
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    • 2005
  • This study was performed to change the hydrophilic $NH_4Y$-zeolite to the hydrophobic one for removal of VOCs by removing the $Al^{3+}$ in the zeolite-structure to increase the Si/Al ratio, for which the three pelleted $NH_4Y$-zeolite samples were contacted separately with the steam of $400^{\circ}C$, $500^{\circ}C$ and $600^{\circ}C$, respectively, in a stainless steel column for 4 hours. Then extraction of the ex-structure aluminum of the hydrolyzed zeolites with the nitric acids of 0.25, 0.50, 0.75, and 0.10 M at $90^{\circ}C$ in 500 mL-flasks, respectively, according to steam temperature were followed. XRD analysises of the dealuminated zeolites showed that the peaks of the zeolites that had been hydrolyzed with the steams of both $500^{\circ}C$ and $600^{\circ}C$ are distorted more with the increase of the concentration of nitric acid used for extraction of the ex-structure aluminums, however, those hydrolyzed with steam of $400^{\circ}C$ became amorphous phase when treated with the all nitric acids of four concentrations. Also the EDX analysises showed that the BET surface areas and TPVS of the zeolites that had been hydrolyzed with the steam of $600^{\circ}C$ were increased with the concentration of the nitric acid when the nitric acids of 0.25 M and 0.5 M had been used but decreased when the nitric acids of 0.75 M and 1.0 M had been used. These results led to the conclusion that both the $600^{\circ}C$ and $500^{\circ}C$-steam and the 0.5 M-nitric acid are appropriate to change the hydrophilic $NH_4Y$-zeolites to the hydrophobic one, which were proven by the measurement of the benzene and tolune-adsorbing capacities showing the same trend as the BET surface area and TPV The Si/Al ratios and water-adsorbing capacities of the dealuminated zeolites were increased and decreased, respectively, with the concentration of the nitric acids so that it showed that the hydrophobicity is increased.