• Title/Summary/Keyword: recrystallization temperature

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High-temperature Thermal Decomposition of Cs-adsorbed CHA-Cs and CHA-PCFC-Cs Zeolite System, and Sr-adsorbed 4A-Sr and BaA-Sr Zeolite System (Cs-흡착 CHA-Cs 및 CHA-PCFC-Cs 제올라이트계와 Sr-흡착 4A-Sr 및 BaA-Sr 제올라이트계의 고온 열분해)

  • Lee, Eil-Hee;Kim, Ji-Min;Kim, Hyung-Ju;Kim, Ik-Soo;Chung, Dong-Yong;Kim, Kwang-Wook;Lee, Keun-Young;Seo, Bum-Kyoung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.16 no.1
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    • pp.49-58
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    • 2018
  • For the immobilization of high-radioactive nuclides such as Cs and Sr by high-temperature thermal decomposition, this study was carried out to investigate the phase transformation with calcined temperature by using TGA (thermogravimetric analysis) and XRD (X-ray diffraction) in the Cs-adsorbed CHA (chabazite zeolite of K type)-Cs and CHA-PCFC (potassium cobalt ferrocyanide)-Cs zeolite system, and Sr-adsorbed 4A-Sr and BaA-Sr zeolite system, respectively. In the case of CHA-Cs zeolite system, the structure of CHA-Cs remained at up to $900^{\circ}C$ and recrystallized to pollucite ($CsAlSi_2O_6$) at $1,100^{\circ}C$ after undergoing amorphous phase at $1,000^{\circ}C$. However, the CHA-CFC-Cs zeolite system retained the CHA-PCFC-Cs structure up to $700^{\circ}C$, but its structure collapsed in $900{\sim}1,000^{\circ}C$, and then transformed to amorphous phase, and recrystallized to pollucite at $1,100^{\circ}C$. In the case of 4A-Sr zeolite system, on the other hand, the structure of 4A-Sr maintained up to $700^{\circ}C$ and its phase transformed to amorphous at $800^{\circ}C$, and recrystallized to Sr-feldspar ($SrAl_2Si_2O_8$, hexagonal) at $900^{\circ}C$ and to $SrAl_2Si_2O_8$ (triclinic) at $1,100^{\circ}C$. However, the BaA-Sr zeolite system structure began to break down at below $500^{\circ}C$, and then transformed to amorphous phase in $500{\sim}900^{\circ}C$ and recrystallized to Ba/Sr-feldspar (coexistence of $Ba_{0.9}Sr_{0.1}Al_2Si_2O_8$ and $Ba_{0.5}Sr_{0.5}Al_2Si_2O_8$) at $1,100^{\circ}C$. All of the above zeolite systems recrystallized to mineral phase through the dehydration/(decomposition) ${\rightarrow}$ amorphous ${\rightarrow}$ recrystallization with increasing temperature. Although further study of the volatility and leachability of Cs and Sr in the high-temperature thermal decomposition process is required, Cs and Sr adsorbed in each zeolite system are mineralized as pollucite, Sr-feldspar and Ba/Sr-feldspar. Therefore, Cs and Sr seen to be able to completely immobilize in the calcining wasteform/(solidified wasteform).

Studies on Preparation of Boron Compounds from Colemanite Ore : Preparation of Boric Acid and Reaction Mechanism (I) (Colemanite 광물로부터 붕소화합물의 제조에 관한 연구 : 붕산제조 및 반응기구 (I))

  • Choi, Byung-Hyun;Lim, Hyung-Mi;Jee, Mi-Jung;Jang, Jae-Hun;Paik, Song-Hoo;Lee, Mi-Jai
    • Journal of the Korean Ceramic Society
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    • v.41 no.10 s.269
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    • pp.756-765
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    • 2004
  • We present extraction process and reaction mechanism of boric acid from one of calcium borate ores, colemanite by reaction with sulfuric acid. Colemanite has been fully decomposed under pH 5 with sufficiency amount of sulfuric acid, more than the amount stoichiometrically required. Calcium sulfate was separated out, leaving boron in the liquid phase after sulfuric acid addition. The extraction process of boric acid was affected by dissolution temperature and time, amount of sulfuric acid and ammonium sulfate, pH and a degree of concentration before recrystallization. The $SiO_2$ of the impurities which colemanite contains was insoluble so that it was separated out with calcium sulfate from liquid phase. The species of $CaO,\;Al_2O_3,\;Fe_2O_3,\;MgO$ were remained in a liquid phase after reaction with sulfuric acid. These impurities were separated out by addition of ammonia to the liquid phase, funhermore, boric acid was produced by process of pH adjustments and acidification, concentration, and recrystallization.

The Microstructure and physical properties of electroplated Cu films (열처리에 따른 Cu 전해도금막의 미세구조 및 물리적성질 변화)

  • 권덕렬;박현아;김충모;이종무
    • Journal of the Korean Vacuum Society
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    • v.13 no.2
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    • pp.72-78
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    • 2004
  • Cu seed layers deposited by magnetron sputtering onto tantalum nitride barrier films were treated with ECR plasma and then the copper films were electroplated and rapid thermal annealed in an argon or nitrogen atmosphere at various temperatures ranging from 200 to $500^{\circ}C$. Changes in the microstructure and physical properties of the copper films electroplated on the hydrogen ECR plasma cleaned copper seed layers were investigated using X-ray diffraction (XRD), electron back-scattered diffraction (EBSD), and atomic force microscopy (AFM) analyses. It was found that the copper film undergoes complete recrystallization during annealing at a temperature higher than $400^{\circ}C$. The resistivity of the Cu film tends to decrease and the degree of (111) preferred orientation tends to increase as the annealing temperature increases. Theoptimum annealing condition for obtaining the film with the lowest resistivity, the smoothest surface and the highest degree of the (111) preferred orientation is rapid thermal annealing in a nitrogen atmosphere at $400^{\circ}C$ for 120 s. The resistivity and the surface roughness of the electroplated copper film annealed under this condition are 1.98 $\mu$O-cm and 17.77 nm, respectively.

Preparation and Characterization of Porous and Composite Nanoparticulate Films of CdS at the Air/Water Interface

  • Ji, Guanglei;Chen, Kuang-Cai;Yang, Yan-Gang;Xin, Guoqing;Lee, Yong-Ill;Liu, Hong-Guo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2547-2552
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    • 2010
  • CdS nano-particulate films were prepared at the air/water interface under Langmuir monolayers of arachidic acid (AA) via interfacial reaction between $Cd^{2+}$ ions in the subphase and $H_2S$ molecules in the gaseous phase. The films were made up of fine CdS nanoparticles with hexagonal Wurtzite crystal structure after reaction. It was revealed that the formation of CdS nano-particulate films depends largely on the experimental conditions. When the films were ripened at room temperature or an increased temperature ($60^{\circ}C$) for one day, numerous holes were appeared due to the dissolution of smaller nanoparticles and the growth of bigger nanoparticles with an improved crystallinity. When the films were ripened further, CdS rodlike nanoparticles with cubic zinc blende crystal structure appeared due to the re-nucleation and growth of CdS nanoparticles at the stacking faults and defect structures of the hexagonal CdS grains. These structures were characterized by transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and X-ray diffraction (XRD). These results declare that CdS semiconductor nanoparticles formed at the air/water interface change their morphologies and crystal structures during the ripening process due to dissolution and recrystallization of the particles.

The Study on the CEC Increase and Granulation of Natural Zeolite -2. Effects of Temperature and Time on the Recrystallization of Natural Zeolite (천연(天然)Zeolite의 CEC 증가(增加)와 입단화(粒團化)에 관(關)한 연구(硏究) -2. 반응(反應) 온도(溫度)와 반응(反應) 시간(時間)의 영향(影響))

  • Choi, Jyung;Hur, Nam-Ho;Lee, Dung-Hoon
    • Korean Journal of Soil Science and Fertilizer
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    • v.26 no.3
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    • pp.151-154
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    • 1993
  • The magnitute of CEC of the reaction product which was produced by the treatment of the natural zeolite power(CEC : 67me/100g) with 3N-NaOH at $80^{\circ}C$ for 30 hours was determined to be about 260me/100g, which was the highest value in all reaction products. By the NaOH-treatment the contents of major clay minerals in natural zeolite was shown to be decreased and it is apparent that new phillipsite was synthesized. Furthermore it is interesting that the phillipsite contents was increased with longer reaction time and higher temperature. After 30 hours treatment the dorminant clay mineral in the reaction product was found to be phillipsite.

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Characterization of Microstructure and Mechanical Properties of High-Purity Iron Added with Copper

  • Taguchi, O.;Lee, Su Yeon;Uchikoshi, M.;Isshiki, M.;Lee, Chan Gyu;Suzuki, S.;Gornakov, Vladimir S.
    • Journal of the Korean Society for Heat Treatment
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    • v.25 no.1
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    • pp.22-26
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    • 2012
  • An influence of the addition of copper (0.5, 1.0 and 1.5 mass% Cu) on the microstructure and mechanical properties of high purity iron (99.998 mass%) was characterized. The microstructure and microhardness of high-purity iron based samples, which were rolled at room temperature and subsequently annealed, were investigated in this work. The microstructure of the samples has been observed by electron back scattering diffraction (EBSD) and the mechanical properties have been studied by using micro-Vickers hardness test. The results of microstructural observation showed that deformation band was formed in high purity iron by rolling at room temperature, and it was recovered by annealing up to about 900 K. The microhardness results showed that the softening of high-purity iron occurred by annealing up to about 900 K, while the hardness of iron added with about 0.5-1.5 mass% copper was kept over 100 Hv and at the early time of annealing reached a maximum. The hardness of iron added with a small amount of copper may be attributed to precipitation hardening as well as solution hardening. The orientation of crystal in recrystallized grain was almost same as that of deformed grain.

Texture Formation of Eletroplated Nickel and Nickel Alloy on Cu Substrate (구리 기판에 전착시킨 니켈과 니켈합금의 집합조직 형성)

  • Kim, Jae-Geun;Lee, Sun-Wang;Kim, Ho-Jin;Hong, Gye-Won;Lee, Hee-Gyoun
    • Progress in Superconductivity
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    • v.7 no.2
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    • pp.145-151
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    • 2006
  • Nickel and nickel-tungsten alloy were electroplated on a cold rolled and heat treated copper(Cu) substrate. 4 mm-thick high purity commercial grade Cu was rolled to various thicknesses of 50, 70, 100 and 150 micron. High reduction ratio of 30% was applied down to 150 micron. Rolled texture was converted into cube texture via high temperature heat treatment at $400-800^{\circ}C$. Grain size of Cu was about 50 micron which is much smaller compared to >300 micron for the Cu prepared using smaller reduction pass of 5%. 1.5 km-long 150 micron Cu was fabricated with a rolling speed of 33 m/min and texture of Cu was uniform along length. Abnormal grain growth and non-cube texture appeared for the specimen anneal above $900^{\circ}C$. 1-10 micron thick Ni and Ni-W film was electroplated onto an annealed cube-textured Cu or directly on a cold rolled Cu. Both specimens were annealed and the degree of texture was measured. For electroplating of Ni on annealed Cu, Ni layer duplicated the cube-texture of Cu substrate and the FWHM of in plane XRD measurement for annealed Cu layer and electroplated layer was $9.9^{\circ}\;and\;13.4^{\irc}$, respectively. But the FWHM of in plane XRD measurement of the specimen which electroplated Ni directly on cold rolled Cu was $8.6^{\circ}$, which is better texture than that of nickel electroplated on annealed Cu and it might be caused by the suppression of secondary recrystallization and abnormal grain growth of Cu at high temperature above $900^{\circ}C$ by electroplated nickel.

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Characteristics Comparison of Prepared Films According to Influence of Adsorption Inhibitor in the Condition of Deposition (PVD증착용 흡착인히비터의 영향에 따른 제작막의 특성 비교)

  • 이찬식;윤용섭;권식철;김기준;이명훈
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2001.11a
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    • pp.67-67
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    • 2001
  • The structure zone model has been used to provide an overview of the relationship between the microstructure of the films deposited by PVD and the most prominent deposition condition.s. B.AMovchan and AV.Demchishin have proposed it firstls such model. They concluded that the general features of the resulting structures could be correlated into three zones depending on $T/T_m$. Here T m is the melting point of the coating material and T is the substrate temperature in kelvines. Zone 1 ($T/Tm_) is dominated by tapered macrograins with domed tops, zone 2 ($O.3) by columnar grains with denser boundaries and zone 3 ($T/T_m>O.5$) by equiaxed grains formed by recrystallization. J.AThomton has extended this model to include the effect of the sputtering gas pressure and found a fourth zone termed zone T(transition zone) consisting of a dense array of poorly defined fibrous grains. R.Messier found that the zone I-T boundary (fourth zone of Thorton) varies in a fashion similar to the film bias potential as a function of gas pressure. However, there has not nearly enough model for explaining the change in morphology with crystal orientation of the films. The structure zone model only provide an information about the morphology of the deposited film. In general, the nucleation and growth mechanism for granular and fine structure of the deposited films are very complex in an PVD technique because the morphology and orientation depend not only on the substrate temperature but also on the energy of deposition of the atoms or ions, the kinetic mechanism between metal atoms and argon or nitrogen gas, and even on the presence of impurities. In order to clarify these relationship, AI and Mg thin films were prepared on SPCC steel substrates by PVD techniques. The influence of gas pressures and bias voltages on their crystal orientation and morphology of the prepared films were investigated by SEM and XRD, respectively. And the effect of crystal orientation and morphology of the prepared films on corrosion resistance was estimated by measuring polarization curves in 3% NaCI solution.

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Evaluation of Granite Melting Technique for Deep Borehole Sealing (심부시추공 밀봉을 위한 화강암 용융거동 평가)

  • Lee, Minsoo;Lee, Jongyoul;Ji, Sung-Hoon
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.16 no.4
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    • pp.479-490
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    • 2018
  • The granite melting concept, which was suggested by Gibb's group for the closing of a deep borehole, was experimentally checked for KURT granite. The granite melting experiments were performed in two pressure conditions of atmospheric melting with certain inorganic additives and high pressure melting formed by water vaporization. The results of atmospheric tests showed that KURT granite started to melt at a lower temperature of $1,000^{\circ}C$ with NaOH addition and that needle shaped crystals were formed around partially melted crystals. In high pressure tests, vapor pressure was increased by adding water with maximum pressure of about 400 bars. KURT granite was partially melted at $1,000^{\circ}C$ when vapor pressure was low. However, it was not melted at vapor pressures higher than 200 bars. Therefore, it was determined that high pressure with a small amount of water vapor more effectively decreased the melting point of granite. Meanwhile, high temperature and high pressure vapor caused severe corrosion of the reactor wall.

Characteristics of Precipitation Hardened Extra Low Carbon Steels (석출강화형 극저탄소강의 특성에 대한 고찰)

  • Yoon, Jeong-Bong;Kim, Sung-il;Kim, In-Bae
    • Korean Journal of Metals and Materials
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    • v.46 no.10
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    • pp.609-616
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    • 2008
  • Conventional bake-hardenable(BH) steels should be annealed at higher temperatures because of the addition of Ti or/and Nb which forms carbides and raises recrystallization start temperature. In this study, the development of new BH steels without Ti or Nb addition has been reviewed. The new BH steels have nearly same mechanical properties as the conventional BH steels even though it is annealed at lower temperature. The steels also show smaller deviation of the mechanical properties than that of the conventional BH steels because of the conarol of solute carbon content during steel making processes. The deviation of mechanical properties in conventional BH steels is directly dependent on the deviation of solute carbon which is greatly influenced by the amount of the carbide formers in conventional BH steels. Less alloy addition in the newly developed BH steels gives economical benefits. By taking the advantage of sulfur and/or nitrogen which scarenge in Interstitial-Free or conventional BH steels, fine manganese sulfides or nano size copper sulfides were designed to precipitate, and result in refined ferrite grains. Aluminum nitrides used as a precipitation hardening element in the developed steels were also and resull in fine and well dispersed. As a result, the developed steels with less production cost and reduced deviation of mechanical properties are under commercial production. Note that the developed BH steels are registered as a brand name of MAFE(R) and/or MAF-E(R).