• Title/Summary/Keyword: zirconium hydroxide

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Corrosion Characteristics and Oxide Microstructure of Zirconium Alloys for Nuclear Fuel Cladding (핵연료피복관용 Zr 합금의 부식특성 및 산화막 미세구조)

  • Jeong, Yong-Hwan;Baek, Jong-Hyeok;Kim, Seon-Jae;Kim, Gyeong-Ho;Choi, Byeong-Gwon;Jung, Yeon-Ho
    • Korean Journal of Materials Research
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    • v.8 no.4
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    • pp.368-374
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    • 1998
  • The corrosion characteristics of zirconium alloys have been investigated in various aqueous solutions of LiOH. NaOH, KOH, RbOH. and CsOH at 3S$0^{\circ}C$. The concentrations of solutions were set to 4.3 mmol and 32.Smmol with equimolar $M^+$ and OH . The oxide characterization was performed using TEM on the samples corroded in 32. Smmol LiOH, NaOH, and KOH solution. The samples were prepared to have the same oxide thickness for the pretransition and post- transition regimes. Considering the trend of experimental data, the cation would playa major role in the corrosion process of Zr alloys in alkali hydroxide solutions. The microstructures of the oxides formed in various solutions were quite different. In LiOH solution the oxides grown in pre-transition as well as post-transition had the equiaxed structures with many pores and open grain boundaries. The oxides grown in NaOH solution had the protective columnar structures in pre-transition and the equiaxed structures with many open grain boundaries in post- transition. On the other hand. in KOH solution the columnar structure was maintained from pre- transition to post- transition. It was considered that the cation incorporation into zirconium oxide controlled the oxide characteristics and the corrosion acceleration in alkali hydroxide solutions.

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A Study on the Constituents of Pyrolusitum by XRD and XRF (XRD와 XRF를 이용한 무명이(無名異)의 구성 성분 연구)

  • Lee, Minwoo;Choi, Goya;Lee, Young-Jong
    • The Korea Journal of Herbology
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    • v.33 no.6
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    • pp.87-92
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    • 2018
  • Objectives: The aim of the study was to analyze the constituents of Pyrolusitum, which was used to eliminate static blood and inflammation, to establish the basis of clinical application. Methods: Qualitative analysis was performed by X-Ray Diffraction (XRD) using the sample as a powder, and the elemental content of granular sample was measured by X-Ray Fluorescence (XRF). 1 M hydrochloric acid and 5% sodium hydroxide aqueous solution were added to observe the changing shape, respectively. Results: Qualitative analysis by XRD revealed that the Pyrolusitum samples used in the study contained quarts and kaolinite. Quantitative analysis by XRF revealed that the manganese content in the samples used in the study was 6.16% on average, while iron was contained the highest amount of 22.99%. The minor constituents include 1.08% of titanium, 0.30% of barium, 0.18% of lead, 0.06% of zirconium, 0.05% of chromium, 0.04% of zinc, 0.03% of cadnium, 0.02% of nickel, 0.01% of arsenic, 0.01% of copper, 0.01% of rubidium, 0.01% of strontium, 0.00% of molybdenum, respectively. And cobalt, which is reported to be a constituent of Pyrolusitum, was not detected at all in the samples of the study. Pyrolusitum was dissolved in dark brown when it was put into 1 M hydrochlorid acid, and there was brown precipitate when sodium hydroxide solution was added to Pyrolusitum and stirred. Conclusions: It was found that manganese and iron were the major constituents of Pyrolusitum, and it could be identified by using concentrated hydrochloric acid and sodium hydroxide solution.

Preparation of Zirconia-Coated NiO Powder and its Microstructure ($ZrO_2$를 피복한 NiO 분말의 제조 및 미세구조)

  • 문지웅;이홍림;김구대;김재동;이동아;이해원
    • Journal of the Korean Ceramic Society
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    • v.35 no.7
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    • pp.653-658
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    • 1998
  • Zirconia coated NiO powders were prepared by the thermal hydrolysis of $Zro(NO_3)_2$.$6H_2O$ in a mixed solvent of alcohol and water. Amorphous zirconium hydroxide was uniformly coated on the surface of NiO powder with the thickness of 20nm. The $ZrO_2$ coating layer was crystallized to tetragonal $ZrO_2$ with the size of 40-60nm at $900^{\circ}C$. The coated NiO powder containing 15 vol% $ZrO_2$ was found to have a similar isoelectric point to that of the $ZrO_2$ The grain growth inhibition effect of the coated powders was superior to the mechanically mixed powders.

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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.

Microshear bond strength of dual-cure resin cement in zirconia after different cleaning techniques: an in vitro study

  • Atoche-Socola, Katherine Joselyn;Arriola-Guillen, Luis Ernesto;Lopez-Flores, Ana Isabel;Garcia, Isadora Martini;Huertas-Mogollon, Gustavo;Collares, Fabricio Mezzomo;Leitune, Vicente Castelo Branco
    • The Journal of Advanced Prosthodontics
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    • v.13 no.4
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    • pp.237-245
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    • 2021
  • PURPOSE. This study aimed to compare the microshear bond strength (µSBS) of dual-cure resin cement in CAD-CAM zirconia after different cleaning techniques. MATERIALS AND METHODS. Fifty discs of zirconia-based ceramic from Ivoclar Vivadent were embedded in acrylic resin. The discs were divided into five groups according to the cleaning methods used: Group 1: drying with spraying + sandblasting with Al2O3; Group 2: washed with water and dried with spraying + sandblasting with Al2O3;Group 3: washed with distilled water and dried with spraying + sandblasting with Al2O3 + zirconium oxide (Ivoclean); Group 4: washed with distilled water and dried with spraying + sandblasting with Al2O3 + potassium hydroxide (Zirclean); and Group 5: washed with distilled water and dried with spraying + sandblasting with Al2O3 + 1% NaClO. All of the groups were contaminated with artificial saliva for 1 minute and then cleaned. Statistical analyses were performed using ANOVA and Tukey's tests. RESULTS. There were statistically significant differences among all groups for µSBS (P < .05). The group treated with zirconium oxide (Group 3) showed the highest µSBS (18.75 ± 0.23 MPa). CONCLUSION. When applied to zirconia, the cleaning methods affected the bonding with resin cement differently.

A Study of Cleaning Technology for Zirconium Scrap Recycling in the Nuclear Industry (원자력산업에서 지르코늄 스크랩 재활용을 위한 세정기술에 관한 연구)

  • Lee, Ji-Eun;Cho, Nam-Chan;An, Chang-Mo;Noh, Jae-Soo;Moon, Jong-Han
    • Clean Technology
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    • v.19 no.3
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    • pp.264-271
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    • 2013
  • In this study, we optimized the removal condition of contaminants attached on the scrap surface to recycle the scrap generated from the Zr alloy tube manufacturing process back to the nuclear grade. The main contaminant is remnant of watersoluble cooling lubricant that is used in the pilgering manufacture during the tube production, and it is assumed to be compressed and carbonized on the surface of tube. Zirlo alloy tube of ${\phi}9.50mm$, which has high occurrence frequency of scrap, was selected as the object to be cleaned, and cleaning abilities of reagents were evaluated by measuring the characteristics of contaminants remained and by analyzing the surface of the tube after cleaning process. For evaluation of each cleaning agent, we selected two types of sodium hydroxide series and three types of potassium hydroxide series. Furthermore, to confirm dependence on tempe-rature and ultrasonic intensities, cleaning at the room temperature, $40^{\circ}C$, and $60^{\circ}C$ was conducted, and results showed that higher the cleaning temperature and higher the ultrasonic intensity, better the cleaning effect. As a result of the bare-eye inspection, while the use of sodium hydroxide provided satisfactory condition on the tube surface, the use of potassium hydroxide series provided satisfactory condition on the tube surface only when the ultrasonic intensity was over 120 W. In the cleaning effect analysis using the gravimetric method, cleaning efficiency of sodium hydroxide series was as high as 97.6% ($60^{\circ}C$, 120 W), but since the tube surface condition was poor after the use of potassium hydroxide, the gravimetric method was not appropriate. In the analytical result of surface contaminants on the tube surface, C, O, Ca, and Zr were detected, and mainly C and O dominated the proportion of contaminants. It was also found that the degree of cleaning on the tube affected the componential ratio of C and O; if the degree of cleaning is high, or if cleaning is well-conducted, the proportion of C is decreased, and the proportion of O is increased. Based on these results, optimal cleaning for application in the industry can be expected by categorizing cleaning process into three steps of Alkali cleaning, Rinsing, and Drying and by adjusting cleaning parameters in each step.

Characteristics of Al2O3/ZrO2 Ceramics by the Dispersion Process of ZrO2 Particles (ZrO2 입자의 분산방법에 따른 Al2O3/ZrO2 요업체의 특성)

  • Youn, Sang-Hum;Kim, Jae-Jun;Hwang, Kyu-Hong;Lee, Jong-Kook;Kim, Hwan
    • Journal of the Korean Ceramic Society
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    • v.42 no.8 s.279
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    • pp.561-566
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    • 2005
  • For the homogeneous dispersion of $ZrO_2$ particles in $Al_2O_3/ZrO_2$ceramics, Zr-precusors were mixed with oxide $Al_2O_3$powders by chemical routes such as partial precipitation or partial polymerization of Zr-nitrate solutions. In case of the mechanical mixing of ultrafine $Al_2O_3$ and $ZrO_2$ oxide powders, relatively homogeneous dispersion was difficult to achieve so that the particle size and distributions of $ZrO_2$ were relatively inhomogeneous after sintering at high temperature. But when the Zr-Y-hydroxide were co-precipitated to ultrafine $Al_2O_3$ oxide powders followed by calcinations, homogeneous dispersion of nano-sized $ZrO_2$ particles in $Al_2O_3/ZrO_2$ composite ceramics were obtained. But because of the coalescence of dispersed $ZrO_2$ particles, dispersed $ZrO_2$ was grown up to more than 0.2${mu}m$ (200 nm) when sintered at the temperature of higher than $1500^{\circ}C$ But when the sintering temperature was kept to lower than $1400^{\circ}C$ by using nano-sized $\alpha-alumina$, the particle size of dispersed $ZrO_2$ could be sustained below 0.1 ${\mu}m$. But the coalescence of dispersed $ZrO_2$ between $Al_2O_3$ particles could not be avoided so that the mechanical properties were not enhanced contrary to the expectations. So Zr-polyester precursors were precipitated and coated to the surface of ultrafine $\alpha-alumina$ powders by the polymerization of Ethylene Glycol with Citric Acid and Zirconium Nitrate. By this dispersion much more uniform dispersion of $ZrO_2$ was achieved at $1450\~1600^{\circ}C$ of sintering temperature ranges. And due to especially discrete dispersion of $ZrO_2$ between $Al_2O_3$ particles, their mechanical strength was more enhanced than mechanical mixing or hydroxide precipitation methods.

Preparation of Zirconia Nanocrystalline Powder by the Hydrothemal Treatment at low Temperature (수열법에 의한 저온 결정형 지르코니아 나노 분말의 제조)

  • Noh, Hee-Jin;Lee, Jong-Kook;Seo, Dong-Seok;Hwang, Kyu-Hong
    • Journal of the Korean Ceramic Society
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    • v.39 no.3
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    • pp.308-314
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    • 2002
  • The nanocrystalline zirconia powder was synthesized from the zirconium hydroxide precipitate by hydrothermal process with the reaction temperature range 100∼250$^{\circ}$C, reaction time 1∼48 hours and additive concentration 1, 5 N NaOH solutions. The lower hydrothermal treatment temperature, the inner spherical tetragonal zirconia was synthesized. The fraction of monoclinic phase zirconia with rod shape increased with increasing the hydrothermal treatment temperature. As the concentration of the NaOH solution increases, the synthesized particle in breadth and length increased; breadth and length ratio decreased. In the case of the low concentration of NaOH solution, however, the particle length became relatively larger than its breadth resulting in the rod-shaped particles with bigger aspect ratio.

Synthesis and crystallization of nanosized zirconia powder using hydrothermal process (수열반응에 의한 나노 지르코니아 분말의 합성 및 결정화)

  • 노희진;이종국;서동석;황규홍
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.12 no.3
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    • pp.126-132
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    • 2002
  • The nanocrystalline zirconia powder with anisotropic shapes was synthesized by hydrothermal treatment of the tetragonal zirconia prepared by aging the zirconium hydroxide precipitate, which was obtained from the reaction between $ZrOCl_2{\cdot}8H_2O$ and KOH solutions under the fixed pH of 13.5, at $100^{\circ}C$ for 24 h. With increasing the hydrothermal reaction temperature and time, the fraction of tetragonal phase with spherical zirconia decreased, whereas, relatively the fraction of monoclinic phase with spindle-like and rod shape zirconia increased. As increased concentration of the NaOH solution it promoted the particle size to become larger and the crystalline phase to transform tetragonal to monoclinic. However, the specific surface area at the early stage of the reaction increased and subsequently decreased because of grain growth in powder with longer reaction time.

Surface Analysis Study on ZIRLO Cladding Hulls Oxidized at Low Temperatures (저온 산화된 ZIRLO 피복관의 표면분석 연구)

  • Jeon, Min Ku;Choi, Yong Taek;Lee, Chang Hwa;Kang, Kweon Ho;Park, Geun Il
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.12 no.3
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    • pp.235-243
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    • 2014
  • Surface oxidation behavior of ZIRLO (ZIRconium Low Oxidation) hulls was investigated using an X-ray photoelectron spectroscopy (XPS) technique. The effects of oxidation time (10-336 h at $500^{\circ}C$) and temperature ($400-700^{\circ}C$ for 10 h) were studied. Deconvolution results of the hulls oxidized at $500^{\circ}C$ revealed that a $ZrO_2$ phase appeared after 24 h (11.86%), and an increase in the $ZrO_2$ ratio was observed when the hulls were oxidized for 336 h (17.93%). On the other hand, the ZrO phase which employed 5.68% in the 10 h oxidized sample disappeared when the oxidation time increased to 24 h. The XPS results also showed that an increase in the oxidation temperature resulted in an increase in the ratio of ZrO, which increased from 0 to 5.68, 8.31, and 9.16% when the oxidation temperature increased from 400 to 500, 600, and $700^{\circ}C$, respectively. $ZrO_2$ phase was observed only in the sample that was oxidized at $700^{\circ}C$. The mechanism of ZrO formation was not conclusive, but it was suggested that a formation of hydroxide might have been accelerated at elevated temperatures leading to a formation of a $Zr(OH)_4$ phase. The relationship between the surface oxidation status of the hulls oxidized at $500^{\circ}C$ and their chlorination reaction feasibility was discussed, and it was suggested that the thickness of the oxide layer is an important parameter that determines the chlorination reaction feasibility.