• Title/Summary/Keyword: SURFACE CRYSTALLIZATION

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Mineralogical Characteristic Changes of Noerok Occurred from Noeseong Mountain, a Raw Material for Pigment, Depending on its Firing Process (안료 원료인 뇌성산 산출 뇌록의 소성에 따른 광물학적 특성 변화)

  • Lee, Jang Jon;Kim, Jae Hwan;Han, Min Su
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.1
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    • pp.23-32
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    • 2018
  • Noerok ia a green pigment used in Joseon dynasty, and its main usage was for forming foundation layers of Dancheong, the ornamental paintings on the surface of traditional buildings in Korea, such as the Daeung-jeon(main hall) of Bulguk-sa temple. In this research, we investigated the mineralogical characteristic changes of Noerok, a traditional Korean pigment, depending on its firing temperature. The Noerok that we experimented on was mined from Noeseong Mountain, Pohang where it is locally reserved. The major composition mineral is Celadonite, and the main constituent elements are Fe, Si, K and Mg, that refers to the existence of Fe-rich mica. As a result of phased firing experiment from $105^{\circ}C$ to $1000^{\circ}C$, the color was changed from green to pale green, then to brown, and finally to red in order. In the thermal analysis, endothermic reaction induced by the dehydration of crystalline water was confirmed at around $616^{\circ}C$. In the mineralogical change, the crystal surface [($11{\bar{1}}$) and ($02{\bar{1}}$)] of the mineral collapsed at temperatures above $600^{\circ}C$, and iron oxide was formed at $1000^{\circ}C$ or higher. Therefore, it is estimated that the crystallization temperature of Noerok is below $600^{\circ}C$, and it is also considered that it has undergone the alteration phase up to stage I, based on the presence of only a celadonite.

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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Low Temperature Preparation of Transparent Glass-Ceramic Using Metal-Alkoxides (1) Synthesis and Properties of Porous Monolithic Gel in Li2O·1.7Al2O3·8.6SiO2 (금속 알콕시드를 이용한 투명 결정화유리의 저온 합성 (1) Li2O·1.7Al2O3·8.6SiO2 다공성 겔체의 합성)

  • Chun, Kyung-Soo;Tak, Joong-Jae
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.568-574
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    • 2007
  • Crack-free dried gel monoliths of the composition $Li_2O1{\cdot}7Al_2O_3{\cdot}8.6SiO_2$ have been prepared as a precursor of transparent glass-ceramic by the hydrolysis and polycondensation of mixed metal alkoxides in solutions containing N,N-dimethylformamide as the drying control chemical additive, alcohols, and water. It was investigated that activation energy for gelation according to the variation of water concentration ranged from 13 to 14 kcal/mol. Only when the amount of water for gelation was 3 times higher than the stoichiometric amount, monolithic dry gels were successfully prepared after drying at $70{\sim}75^{\circ}C$ and at a rate of 0.1~0.3%/h. The specific surface area, the pore volume, the average pore diameters of dried gel at $180^{\circ}C$ were about $239.40m^2/g$, 0.001~0.03 mL/g, and $145.62{\AA}$, respectively. It showed that the dried monolithic gel had a porous body. The DTA curve had the first exothermic peak around $800^{\circ}C$ and the 2nd peak around $980^{\circ}C$, which may correspond to crystallization of the gel.

High crystallization of ultra-thin indium tin oxide films prepared by reactive sputtering with post-annealing (반응성 스퍼터링으로 제조한 ITO 초박막의 후 열처리에 따른 고 결정화)

  • Lee, Ho-Yun;Kim, Seo-Han;Song, Pung-Geun
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.128-128
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    • 2018
  • 최근 디스플레이 기술은 보다 가볍고, 얇고, 선명한 스마트 형태로 발전되고 있다. 특히 스마트산업의 성장으로 터치스크린패널(Touch Screen Panel, TSP)을 사용하는 기술이 다양해짐에 따라 더 높은 감도와 해상도를 달성하기 위한 핵심기술이 필요한 실정이다. TSP는 저항막 방식, 정전용량 방식, 적외선 방식, 초음파 방식 등 다양한 방식이 있다. 그 중 정전용량방식 터치 패널 (Capacitive type touch panel, CTTP)은 다른 유형에 비해 빠른 반응속도 및 멀티 터치 기능 등의 이점을 가지고 있기 때문에 연구의 초점이 되고 있다. 이를 실현하기 위해서 CTTP은 가시광영역의 높은 투과율과 낮은 비저항을 필요로 하기 때문에 박막의 초 슬림화 및 고 결정화도가 선행되어야만 한다. CTTP에 사용되는 투명전극 소재 중에서 40%의 비중을 차지하고 있는 ITO박막은 내구성과 시인성이 좋으나 생산 비용이 비싸다는 단점이 있다. 한편, 반응성 스퍼터링은 기존에 단일 소결체를 사용한 DC마그네트론 스퍼터링법보다 높은 증착률과 낮은 생산 비용으로 초박막을 만들 수 있다는 장점을 가진다. 본 실험에서는 In/Sn (2wt%) 금속 합금 타깃을 사용한 반응성 스퍼터링법을 이용하여 기판 온도 (RT 및 $140^{\circ}C$)에서 두께 30 nm의 In-Sn-O (ITO)박막을 증착하고, 대기 중 $140^{\circ}C$ 온도에서 시간에 따라 열처리한 후 박막의 물성을 관찰하였다. 증착 중 기판 가열을 하지 않은 ITO 박막의 경우, 열처리 시간이 증가함에 따라 비저항은 감소하였고, 홀 이동도는 현저하게 증가하였으며 캐리어 밀도에서는 별다른 차이가 없었다. 이를 통해 비저항의 감소는 캐리어 농도보다는 결정화를 통한 이동도의 증가와 관련 있다는 것을 확인할 수 있었다. 열처리 시간에 따른 박막의 핵 생성 및 결정 성장은 투과 전자 현미경(TEM)으로 명확하게 확인하였으며, 완전 결정화 된 박막의 grain size는 300~500 nm로 확인되었다. 기판온도 $140^{\circ}C$에서 증착한 박막의 경우, 후 열처리를 하지 않은 상태에서도 이미 결정화 된 것을 확인할 수 있었으며, 후 열처리 시에도 grain size에는 큰 변화가 없었다. 이는 증착 중에 박막의 결정화가 이미 완결된 것으로 판단된다. 또한, RT에서 증착한 박막의 경우에는 후 열처리 초기에는 산소공공등과 같은 결함들의 농도가 감소하여 투과율이 증가하였으나 완전한 결정화가 일어난 후에는 투과율이 약간 감소한 것을 확인할 수 있었다. 이는 결정화 시 박막의 표면 조도가 증가하였고 이로 인해 빛의 산란이 증가하여 투과율이 감소한 것으로 판단된다. 이러한 결과로 반응성 스퍼터링 공정으로 제조한 ITO 초박막은 후열처리에 의한 완전한 결정화를 이룰 수 있으며, 이를 통해 얻은 낮은 비저항과 높은 투과율은 고품질 TSP에 적용될 가능성을 가진다고 판단된다.

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Relationship Between Annealing Temperature and Structural Properties of BaTiO3 Thin Films Grown on p-Si Substrates (p-Si 기판에 성장한 BaTiO3 박막의 어닐링온도와 구조적 특성과의 관계)

  • Min, Ki-Deuk;Kim, Dong-Jin;Lee, Jong-Won;Park, In-Yong;Kim, Kyu-Jin
    • Korean Journal of Materials Research
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    • v.18 no.4
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    • pp.222-227
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    • 2008
  • In this study, $BaTiO_3$ thin films were grown by RF-magnetron sputtering, and the effects of a post-annealing process on the structural characteristics of the $BaTiO_3$ thin films were investigated. For the crystallization of the grown thin films, post-annealing was carried out in air at an annealing temperature that varied from $500-1000^{\circ}C$. XRD results showed that the highest crystal quality was obtained from the samples annealed at $600-700^{\circ}C$. From the SEM analysis, no crystal grains were observed after annealing at temperatures ranging from 500 to $600^{\circ}C$; and 80 nm grains were obtained at $700^{\circ}C$. The surface roughness of the $BaTiO_3$ thin films from AFM measurements and the crystal quality from Raman analysis also showed that the optimum annealing temperature was $700^{\circ}C$. XPS results demonstrated that the binding energy of each element of the thin-film-type $BaTiO_3$ in this study shifted with the annealing temperature. Additionally, a Ti-rich phenomenon was observed for samples annealed at $1000^{\circ}C$. Depth-profiling analysis through a GDS (glow discharge spectrometer) showed that a stoichiometric composition could be obtained when the annealing temperature was in the range of 500 to $700^{\circ}C$. All of the results obtained in this study clearly demonstrate that an annealing temperature of $700^{\circ}C$ results in optimal structural properties of $BaTiO_3$ thin films in terms of their crystal quality, surface roughness, and composition.

A Study on the Modification of NH4+Y-zeolite for Improving Adsorption/Desorption Performance of Benzene (NH4+Y-zeolite의 개질을 통한 벤젠 흡·탈착 성능 증진 연구)

  • Jang, Young Hee;Noh, Young Il;Lee, Sang Moon;Kim, Sung Su
    • Clean Technology
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    • v.25 no.1
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    • pp.33-39
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    • 2019
  • A.C (activated carbon) is mainly used to remove VOCs (volatile organic compounds), however, it has many problems such as fire risk due to increasing of adsorbent surface temperature during VOCs ad/desorption, increased cost by frequent replacement cycles requirement and performance degradation when containing moisture. In order to solve these problems, many researches, hydrophobic zeolite adsorbents, have been reported. In this study, $NH_4{^+}Y$-zeolite was synthesized with Y-zeolite through steam treatment and acid treatment, which is one of the hydrophobic modification methods, to secure high surface area, thermal stability and humidity resistance. The Y, Y-550-HN, Y-600-HN and Y-650-HN had adsorption capacities of $23mg\;g^{-1}$, $38mg\;g^{-1}$, $77mg\;g^{-1}$, $61mg\;g^{-1}$. The change of Si/Al ratio, which is an index to confirm the degree of modification, was confirmed by XRF (X-ray fluorescence spectrometer) analysis. As a result, the adsorbtion performance was improved when Y-zeolite modified, and the Si/Al ratio of Y, Y-550-HN, Y-600-HN, Y-650-HN were increased to 3.1765, 6.6706, 7.3079, and 7.4635, respectively. Whereas it was confirmed that structural crystallization due to high heat treatment temperature affected performance degradation. Therefore, there is an optimal heat treatment temperature of Y-zeolite, optimum modification condition study could be a substitute for activated carbon as a condition for producing an adsorbent having high durability and stability.

Highly Doped Nano-crystal Embedded Polymorphous Silicon Thin Film Deposited by Using Neutral Beam Assisted CVD at Room Temperature

  • Jang, Jin-Nyeong;Lee, Dong-Hyeok;So, Hyeon-Uk;Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.154-155
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    • 2012
  • The promise of nano-crystalites (nc) as a technological material, for applications including display backplane, and solar cells, may ultimately depend on tailoring their behavior through doping and crystallinity. Impurities can strongly modify electronic and optical properties of bulk and nc semiconductors. Highly doped dopant also effect structural properties (both grain size, crystal fraction) of nc-Si thin film. As discussed in several literatures, P atoms or radicals have the tendency to reside on the surface of nc. The P-radical segregation on the nano-grain surfaces that called self-purification may reduce the possibility of new nucleation because of the five-coordination of P. In addition, the P doping levels of ${\sim}2{\times}10^{21}\;at/cm^3$ is the solubility limitation of P in Si; the solubility of nc thin film should be smaller. Therefore, the non-activated P tends to segregate on the grain boundaries and the surface of nc. These mechanisms could prevent new nucleation on the existing grain surface. Therefore, most researches shown that highly doped nc-thin film by using conventional PECVD deposition system tended to have low crystallinity, where the formation energy of nucleation should be higher than the nc surface in the intrinsic materials. If the deposition technology that can make highly doped and simultaneously highly crystallized nc at low temperature, it can lead processes of next generation flexible devices. Recently, we are developing a novel CVD technology with a neutral particle beam (NPB) source, named as neutral beam assisted CVD (NBaCVD), which controls the energy of incident neutral particles in the range of 1~300eV in order to enhance the atomic activation and crystalline of thin films at low temperatures. During the formation of the nc-/pm-Si thin films by the NBaCVD with various process conditions, NPB energy directly controlled by the reflector bias and effectively increased crystal fraction (~80%) by uniformly distributed nc grains with 3~10 nm size. In the case of phosphorous doped Si thin films, the doping efficiency also increased as increasing the reflector bias (i.e. increasing NPB energy). At 330V of reflector bias, activation energy of the doped nc-Si thin film reduced as low as 0.001 eV. This means dopants are fully occupied as substitutional site, even though the Si thin film has nano-sized grain structure. And activated dopant concentration is recorded as high as up to 1020 #/$cm^3$ at very low process temperature (< $80^{\circ}C$) process without any post annealing. Theoretical solubility for the higher dopant concentration in Si thin film for order of 1020 #/$cm^3$ can be done only high temperature process or post annealing over $650^{\circ}C$. In general, as decreasing the grain size, the dopant binding energy increases as ratio of 1 of diameter of grain and the dopant hardly be activated. The highly doped nc-Si thin film by low-temperature NBaCVD process had smaller average grain size under 10 nm (measured by GIWAXS, GISAXS and TEM analysis), but achieved very higher activation of phosphorous dopant; NB energy sufficiently transports its energy to doping and crystallization even though without supplying additional thermal energy. TEM image shows that incubation layer does not formed between nc-Si film and SiO2 under later and highly crystallized nc-Si film is constructed with uniformly distributed nano-grains in polymorphous tissues. The nucleation should be start at the first layer on the SiO2 later, but it hardly growth to be cone-shaped micro-size grains. The nc-grain evenly embedded pm-Si thin film can be formatted by competition of the nucleation and the crystal growing, which depend on the NPB energies. In the evaluation of the light soaking degradation of photoconductivity, while conventional intrinsic and n-type doped a-Si thin films appeared typical degradation of photoconductivity, all of the nc-Si thin films processed by the NBaCVD show only a few % of degradation of it. From FTIR and RAMAN spectra, the energetic hydrogen NB atoms passivate nano-grain boundaries during the NBaCVD process because of the high diffusivity and chemical potential of hydrogen atoms.

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Deterioration Diagnosis and Source Area of Rock Properties at the West Stone Pagoda, Gameunsaji Temple Site, Korea (감은사지 서탑의 풍화훼손도 진단 및 석재의 산지추정)

  • Lee Chan Hee;Lee Myeong Seong;Suh Mancheol;Choi Seok-Won;Kim Man Gap
    • Economic and Environmental Geology
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    • v.37 no.5
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    • pp.569-583
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    • 2004
  • The rock properties of the West pagoda in the Gameunsaji temple site are composed mainly of dark grey porphyritic granodiorite with medium grained equigranular texture and developed with small numerous dioritic xenoliths. These xenoliths occurred with small holes due to different weathering processes. As a weathering results, the rock properties of this pagoda occur wholly softened to physical hardness because of a complex result of petrological, meteorological and biological causes. Southeastern part of the pagoda deteriorated seriously that the surface of rock blocks showed partially exfoliations, fractures, open cavities in course of granular decomposition of minerals, sea water spray and crystallization of salt from the eastern coast. The Joint between blocks has small or large fracture cross each other, contaminated and corrupted for inserting with concrete, cement mortar, rock fragments and iron plates, and partially accelerated coloration and fractures. There are serious contamination materials of algae, fungus, lichen and bryophytes on the margin and the surface on the roof stone of the pagoda, so it'll require conservation treatment biochemically for releasing vegetation inhabiting on the surface and the discontinuous plane of the blocks because of adding the weathering activity of stones and growing weeds naturally by soil processing on the fissure zone. Consisting rock for the conservation and restoration of the pagoda would be careful choice of new rock properties and epoxy to reinforce for the deterioration surfaces. For the attenuation of secondary contamination and surface humidity, the possible conservation treatments are needed.

The effect of different crystallization temperature of the hydroxyapatite coating produced by ion beam-assisted deposition on anodizing-treated titanium disks on human osteosarcoma cells (양극산화처리된 티타늄 표면에 이온빔보조증착방식을 이용한 수산화인회석 코팅시 소결온도의 차이가 조골세포에 미치는 영향)

  • Pae, Ah-Ran;Won, Hyun-Du;Lee, Richard Sung-Bok;Kim, Hyeong-Seob;Woo, Yi-Hyung
    • The Journal of Korean Academy of Prosthodontics
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    • v.49 no.4
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    • pp.333-340
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    • 2011
  • Purpose: The aim of this study was to study the effect of hydroxyapatite (HA) coating crystallinity on the proliferation and differentiation of human osteosarcoma cells. Materials and methods: Surface roughness of the titanium disks increased by anodizing treatment and then HA was coated using ion beam-assisted deposition (IBAD). HA coating was crystallized by heat-treated at different temperature ($100^{\circ}C$, $300^{\circ}C$, $500^{\circ}C$, $800^{\circ}C$). According to the temperature, disks were divided into four groups (HA100, HA300, HA500, HA800). With the temperature, crystallinity of the HA coating was different. Anodized disks were used as control group. The physical properties of the disk surface were evaluated by surface roughness tests, XRD tests and SEM. The effect of the crystallinity of HA coating on HOS cells was studied in proliferation and differentiation. HOS cells were cultured on the disks and evaluated after 1, 3, 5, and 7 days. Growth and differentiation kinetics were subsequently investigated by evaluating cell proliferation and alkaline phosphatase activity. Results: Regardless of the heat-treated temperature, there is no difference on the surface roughness. Crystallinity of the HA was appeared in the groups of HA500, HA800. HOS cells proliferation, ALP activity were higher in HA500 and HA800 group than HA100 and HA300. Conclusion: Within the results of this limited study, heat treatment at $500^{\circ}C$ of HA coating produced by IBAD has shown greater effect on proliferation and differentiation of HOS cells. It is considered that further in vivo study will be necessary.

Thermal and Mechanical Properties of Rapidly Solidified Zr-Ni-Cu-Al-Ti Alloy (급냉응고법으로 제조한 Zr-Ni-Cu-Al-Ti 합금의 열적, 기계적 성질)

  • Choe, Ik-Seok;Han, Tae-Gyo;Ji, Yong-Gwon;Im, Byeong-Mun;Kim, Yeong-Hwan;Kim, In-Bae
    • Korean Journal of Materials Research
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    • v.11 no.3
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    • pp.171-177
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    • 2001
  • The thermal and mechanical properties of amorphous Z $r_{62-x}$N $i_{10}$C $u_{20}$A $l_{8}$ $Ti_{x}$ (x=3, 6, 9at%) alloys were investigated. The crystallization process was confirmed as amorphous longrightarrow amorphous + Z $r_2$A $l_3$+ Zr + (Ni,Ti) longrightarrow Z $r_2$Cu + Al + (Ni,Ti) for 3at%Ti, amorphous longrightarrow amorphous + Al longrightarrow $Al_2$Ti + NiZr + CuTi for 6at%Ti and amorphous longrightarrow amorphous + Zr + Al longrightarrow Zr + $Al_2$Zr + Al $Ti_3$+ CuTi for 9at%Ti. lickers hardness ( $H_{v}$ ) increased with increasing volume fraction( $V_{f}$ ) of pricipitates for all concerned compositions. Tensile fracture strength ($\sigma_{f}$ ) showed a maximum value 1219MPa at $V_{f}$ = 38% for 3at%Ti, 1203MPa at $V_{f}$ = 2% for 6at%Ti and 1350MPa at $V_{f}$ = 5% for 9at%Ti. The $\sigma_{f}$ was rapidly decreased after showing the maximum value. The $V_{f}$ corresponding to rapidly decreased $\sigma_{f}$ coincided with the $V_{f}$ transited from ductile to brittle fracture surface.ace.

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