• Title/Summary/Keyword: Dilatometry

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A preparation of hexacelsian powder by solution-polymerization route and its phase transformation behavior (Solution- polymerization 방법에 의한 hexacelsian 분말의 합성 및 상전이 공정에 의한 celsian 소결체의 제조)

  • Sang-Jin Lee;Young-Soo Yoon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.428-436
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    • 1997
  • Hexacelsian ($BaO{\cdot}Al_2O_3{\cdot}2SiO_2$) powder was prepared by a solution-polymerization route employing PVA solution as a polymeric carrier. A fine amorphous-type hexacelsian powder with an average particle size of 0.8 $\mu \textrm{m}$ and a BET specific surface area of $63 \textrm{m}^2$/g was made by a ball-milling the powder precursor for 12 h after calcination at $800^{\circ}C$ for :1 h. A densified hexacelsian was obtained through sintering at $1550^{\circ}C$ for 2 h under an air atmosphere. The $\alpha\longleftrightarrow\beta$ and $\beta\longleftrightarrow\gamma$ displacive phase transformation in polycrystalline hexacelsia,n was examined by using dilatometry and differential scanning calorimtry. The reconstructive transformation between hexacelsian and celsian was obtained by annealing at $1600^{\circ}C$ for 72h. Volume contraction of 5.6% was accompanied by the reconstructive transformation.

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Sintering Behavior and Electrical Properties of Strontium Titanate-Based Ceramic Interconnect Materials for Solid Oxide Fuel Cells (고체산화물 연료전지용 Strontium Titanate 세라믹 접속자 소재의 소결 거동 및 전기적 특성)

  • Park, Beom-Kyeong;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.11a
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    • pp.80.1-80.1
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    • 2010
  • A strontium titanate ($SrTiO_3$)-based material with a perovskite structure is considered to be one of the promising alternatives to $LaCrO_3$-based materials since $SrTiO_3$ perovskite shows a high chemical stability under both oxidizing and reducing atmospheres at high temperatures. $SrTiO_3$ materials exhibit an n-type semiconducting behavior when it is donor-doped and/or exposed to a reducing atmosphere. In this work, $Sr_{1-x}La_xTi_{1-y}M_yO_3$ materials doped with $La^{3+}$ in A-sites and aliovalent transition metal ions ($M^{n+}$) in B-sites were synthesized by the modified Pechini method. The X-ray diffraction analysis indicated that the materials synthesized by the Pechini process exhibited a single curbic perovskite-type structure without any impurity phases, and are tolerant, to some extent, to cation doping. The sintering behaviors of $Sr_{1-x}La_xTi_{1-y}M_yO_3$ in $H_2/N_2$ and air were characterized by dilatometry and microstructural observations. The electrical conduction mechanism and the dopant effect are discussed based on the defect structures and the electrical conductivities measured at various oxygen partial pressures and temperatures.

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Effect of Additive Size on the Densification and Thermal Conductivity of AlN Ceramics with MgO-CaO-Al2O3-SiO2 Additives

  • Lee, Hwa-Jun;Cho, Woo-Seok;Kim, Hyeong Jun;Kim, Hyung-Tae;Ryu, Sung-Soo
    • Journal of the Korean Ceramic Society
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    • v.54 no.1
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    • pp.43-48
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    • 2017
  • In this study, we investigate the effect of additive size on the densification and thermal conductivity of AlN ceramics with $MgO-CaO-Al_2O_3-SiO_2$ (MCAS) additives. Micro-sized MCAS powder prepared via melting and nano-sized MCAS powder synthesized via the polymeric complex method are used as sintering additives. We analyze the densification behavior of AlN added with 5 wt.% of MCAS by dilatometry as well as by isothermal sintering in the temperature range of $1300{\sim}1700^{\circ}C$. AlN exhibits higher sinterability with nano-MCAS than with micro-MCAS, and both specimens approach their maximum densities when sintered at $1600^{\circ}C$ for 4 h. The thermal conductivities of AlN with 5 wt% of nano- and micro-MCAS additives sintered at $1600^{\circ}C$ are 82.6 and 32.0 W/mK, respectively. We find that nano-MCAS is more effective in sintering of AlN ceramics at lower temperatures, and thus for enhancing their thermal conductivities.

Effect of Li3BO3 Additive on Densification and Ion Conductivity of Garnet-Type Li7La3Zr2O12 Solid Electrolytes of All-Solid-State Lithium-Ion Batteries

  • Shin, Ran-Hee;Son, Sam-Ick;Lee, Sung-Min;Han, Yoon Soo;Kim, Yong Do;Ryu, Sung-Soo
    • Journal of the Korean Ceramic Society
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    • v.53 no.6
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    • pp.712-718
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    • 2016
  • In this study, we investigate the effect of the$Li_3BO_3$ additive on the densification and ionic conductivity of garnet-type $Li_7La_3Zr_2O_{12}$ solid electrolytes for all-solid-state lithium batteries. We analyze their densification behavior with the addition of $Li_3BO_3$ in the range of 2-10 wt.% by dilatometer measurements and isothermal sintering. Dilatometry analysis reveals that the sintering of $Li_7La_3Zr_2O_{12}-Li_3BO_3$ composites is characterized by two stages, resulting in two peaks, which show a significant dependence on the $Li_3BO_3$ additive content, in the shrinkage rate curves. Sintered density and total ion conductivity of the system increases with increasing $Li_3BO_3$ content. After sintering at $1100^{\circ}C$ for 8 h, the $Li_7La_3Zr_2O_{12}-8$ wt.% $Li_3BO_3$ composite shows a total ionic conductivity of $1.61{\times}10^{-5}Scm^{-1}$, while that of the pure $Li_7La_3Zr_2O_{12}$ is only $5.98{\times}10^{-6}Scm^{-1}$.

Effect of the Addition of Aluminium Distearate on Manufacturing of $UO_2$ Nuclear Fuel (Aluminium Distearate 첨가가 $UO_2$ 핵연료 제조에 미치는 영향)

  • 박지연;정충환;김영석
    • Journal of the Korean Ceramic Society
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    • v.29 no.8
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    • pp.609-616
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    • 1992
  • This study has been investigated on the milling of Aluminium Distearate (ADS) powder and characteristics of the ADS-doped UO2 pellets. As-received ADS powder of the agglomerated particles has not shown any milling effect because of heat generated during planetary milling. But the use of coolant to effectively remove heat generated during milling has been found an effective way in breaking up the agglomerates of ADS powder. The green density of the UO2 pellet decreases with the amount of ADS powder doped. Therefore, in order to get the sintered density of 95% pellet decreases with the amount of ADS powder doped. Therefore, in order to get the sintered density of 95% theoretical density, the 200 ppm ADS-doped UO2 pellet has to be pressed under higher compacting pressure of 3500~4000 kgf/$\textrm{cm}^2$ compared with the ADS-undoped UO2 pellet pressed under around 3000 kgf/$\textrm{cm}^2$. The ADS-dpoed UO2 pellet with even relatively low sintered density of 10.27 g/㎤ exhibits open porosity of 1% while open porosity of the ADS-undoped UO2 pellet is reduced to around 1% only after its sintered density increases to 10.43g/㎤. It is, therefore, concluded that doping of ADS powder significantly contributes to the decrease in open porosity of the UO2 pellet. The dilatometry of the ADS doped UO2 pellet shows the sintering rate curve with the bimodal mode, which could be attributed to a phase reaction between UO2 and ADS. The X-ray diffraction analysis indicates that there occurs not any new phase formed but the shift of the peaks. It would be expected that a phase reaction resulting in solid solution would happen in the temperature range of 130$0^{\circ}C$ to 150$0^{\circ}C$ between UO2 and ADS.

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Effect of $TiO_2$ on Sintering Behavior of Mixed $UO_2$ and $U_3O_8$ Powder Compacts

  • Song, Kun-Woo;Kim, Keon-Sik;Kang, Ki-Won;Kim, Young-Min;Yang, Jae-Ho;Jung, Youn-Ho
    • Nuclear Engineering and Technology
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    • v.31 no.5
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    • pp.455-464
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    • 1999
  • The effect of TiO$_2$ on the sintering behavior of mixed UO$_2$-U$_3$O$_{8}$ Powder compacts has been investigated using the U$_{3}$O$_{8}$ powder made tv oxidation of defective UO$_{2}$ pellets. Without TiO$_2$, UO$_2$ pellet density is inversely proportional to U$_3$O$_{8}$ content and is below 94 %TD in the U$_3$O$_{8}$ range above 15 wt%. Using more than 0.1 wt % TiO$_2$, however, the density decreases slightly with U$_3$O$_{8}$ content and thus is higher than about 94% TD in the whole range of U$_3$O$_{8}$ content. The grain sizes of UO$_2$ pellets with more than 0.1 wt % TiO$_2$are larger than about 30${\mu}{\textrm}{m}$. Therefore, the U$_3$O$_{8}$ Powder can be reused without any restriction on its amount in UO$_2$ pellet fabrication by sintering the mixed UO$_2$-U$_3$O$_{8}$ compact with the aid of TiO$_2$. Mechanisms for densification and grain growth are proposed and discussed, based on a dilatometry study and an examination of microstructure. microstructure.

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The Nature of Water in Tactic Poly (2-Hydroxyethyl Methacrylate) Hydrogels

  • Kim, Eui-Hwan;Jeon, Sang-Il;Yoon, Sung-Chul;Jhon, Mu-Shik
    • Bulletin of the Korean Chemical Society
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    • v.2 no.2
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    • pp.60-66
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    • 1981
  • The hypothesis that three classes of water exist in hydrogels, namely X water (free water-like), Z-water (bound water-like), and Y water (interfacial water-like), has been verified and generally accepted. To further check the validity of this hypothesis and to study the nature of X, Y, and Z water as conformation changes, several experiments have been done using Tactic Poly(2-hydroxyethyl methacrylate) (P-HEMA) gels. Thermal expansively data for tactic P-HEMA gel was obtained. In each case of isotactic and syndiotactic P-HEMA, the higher water content gels showed an extremely sharp volume change at $0^{\circ}C$, indicating the presence of normal free water-like. Lower water content gels showed no anomalous change in thermal expansion, indicating that the water is bound water-like. The medium water content gels exhibited intermediate behavior. These results were also confirmed by bulk gel conductivity measurments. The differential scanning calorimeter(DSC) experiment was simply introduced to further verify the bound water-like quantities which was obtained by the method of dilatometry and specific conductivity. Observing the amounts of X, Y, and Z water with the change of tacticity, the similar content of bound water-like may be due to the same primary structure of isotactic and syndiotactic polymer and the difference in free and interfacial water-like content may be due to the difference in secondary and tertiary structure of tactic polymer. Therefore, as the polymer conformation varies, the free and interfacial water-like content will be varied. In order to demonstrate these concepts, Russel et al.'s CPK space-filling molecular models of isotactic and syndiotactic P-HEMA was utilized.

A Novel Method to Calculate the Carbides Fraction from Dilatometric Measurements During Cooling in Hot-Work Tool Steel

  • Zhao, Xiaoli;Li, Chuanwei;Han, Lizhan;Gu, Jianfeng
    • Metals and materials international
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    • v.24 no.6
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    • pp.1193-1201
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    • 2018
  • Dilatometry is a useful technique to obtain experimental data concerning transformation. In this paper, a dilation conversional model was established to calculate carbides fraction in AISI H13 hot-work tool steel based on the measured length changes. After carbides precipitation, the alloy contents in the matrix changed. In the usual models, the content of carbon atoms after precipitation is considered as the only element that affects the lattice constant and the content of the alloy elements such as Cr, Mo, Mn, V are often ignored. In the model introduced in this paper, the alloying elements (Cr, Mo, Mn, V) changes caused by carbides precipitation are incorporated. The carbides were identified using scanning electron microscope and transmission electron microscope. The relationship between lattice constant of carbides and temperature are measured by high-temperature X-ray diffraction. The results indicate that the carbides observed in all specimens cooled at different rates are V-rich MC and Cr-rich $M_{23}C_6$, and most of them are V-rich MC, only very few are Cr-rich $M_{23}C_6$. The model including the effects of substitutional alloying elements shows a good improvement on carbides fraction predictions. In addition, lower cooling rate advances the carbides precipitation for AISI H13 specimens. The results between experiments and mathematical model agree well.

Study on the Anisotropic Size Change by Austenitizing and Tempering Heat Treatment of STD11 Tool Steel Using Dilatometry (딜라토미터를 이용한 STD11 공구강의 오스테나이징 및 템퍼링 열처리에 따른 치수 변화 이방성 연구)

  • Hong, Ki-Jung;Kang, Won-Guk;Song, Jin-Hwa;Chung, In-Sang;Lee, Kee-Ahn
    • Korean Journal of Metals and Materials
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    • v.46 no.12
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    • pp.800-808
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    • 2008
  • Heat treatment is an important step for tool manufacture, but unavoidably generates dimensional distortion. This study investigated the continuous dimensional change and the anisotropic behavior of STD11 tool steel during austenitizing and tempering heat treatment especially using quenching dilatometer. Dilatometric results represented that the dimensional change along longitudinal direction was larger than that along transverse direction. Anisotropic phase transformation strain was produced in forged STD11 tool steel during heat treatment. Anisotropic dimensional change increased with increasing austenitizing temperature. After tempering, anisotropic distortion was partially reduced. FactSage thermodynamic equilibrium phase simulation and microstructural observation (FE-SEM, TEM) showed that large ($7{\sim}80{\mu}m$) elongated $M_7C_3$ carbides could be formed along rolling direction. The resolution of elongated carbides during austenitizing was found to be related with the change of martensite transformation temperature after heat treatment. Anisotropic size change of STD11 tool steel was mainly attributed to large elongated carbides produced during rolling process. Using dilatometric and metallographic examination, the possible mechanism of the anisotropic size change was also discussed.