• 한국세라믹학회지
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• 제48권1호
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• pp.80-85
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• 2011

The crystallization behavior and microstructural change of the glass-ceramics were analyzed as a function of concentration and etching time of the HF solution in order to enhance the degree of crystallinity induced by heterogeneous nucleation of glass of bottom ash containing 15 wt% $Li_2O$. The nucleation site seemed to be generated where the Si ion was eluted. The main crystal phases in the glass-ceramics fabricated in this study were $\beta$-spodumene and $Li_2SiO_3$. The specimens etched with HF of 0.5 vol% within 0~60 seconds showed increased crystalline peak intensities in XRD pattern with etching time compared to no-etched one. Also the crystal size and crystal occupancy in the glass matrix observed by SEM were increased with etching time. For the glass-ceramics etched with 1.0 and 2.0 vol% HF solution, the etching time over 10 s was not effective to increase the crystallinity. From this study, it was found that the glass-ceramics with the higher crystallinity could be obtained by HF-etching followed by heat treatment process, even though the nucleating agent or 2-stages thermal treatment process were not used.

• 한국세라믹학회지
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• 제37권6호
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• pp.604-611
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• 2000

Glass-ceramics containing a cordierite (2MgO-2Al2O3-5SiO2) as a main crystal phase was prepared from MgO-Al2O3-SiO2 system glass through a controlled 2-step heat treatment for the application to magnetic memory disk substrate for higher storage capacity. Parent glasses prepared with addition of CeO2 as a fulx and TiO2 as a nucleating agent were crystallized by a 2-step heat treatment i.e. nucleation and crystal grwoth. Then the maximum nucleation and crystal growth rates were investigated and several properties such as bending strength, surface hardness and surface roughness were also studied for heat treated glass. As a result, only a $\alpha$-cordierite was precipitated as a main crystal phase for all heat treatment conditions and the maximum nucleation and crystal growth rates were 2.4$\times$109/㎣.hr at 80$0^{\circ}C$ and 0.3${\mu}{\textrm}{m}$/hr at 915$^{\circ}C$ respectively. After being nucleated at 80$0^{\circ}C$ for 5 hours and then crystallized at 915$^{\circ}C$ for 1 hour, the heat treated glass had a crystal volume fraction of 17.6% and crystal size fo 0.3${\mu}{\textrm}{m}$, and showed the optimum properties for the application to magnetic memory disk substrates as follows. ; Bending strength of 192 MPa, Vidkers hardness of 642.1kgf/$\textrm{mm}^2$, and surface roughness of 27$\AA$.

• 한국결정성장학회지
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• 제28권6호
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• pp.229-234
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• 2018

조핵제 역할을 하는 지르코늄의 원료로써 $ZrO_2$(지르코늄 옥사이드), $ZrSiO_4$(지르코늄 실리케이트), $ZrOCl_2$(지르코늄 옥시클로라이드), $Zr(SO_4)_2$(지르코늄 서페이트) 4종류의 원료를 사용하여 $Li_2O-Al_2O_3-SiO_2$계 결정화 유리를 제조하였다. 동일한 조성의 모든 유리에서 Avrami 상수는 3 이상으로 체적 결정화가 진행됨을 확인하였다. 또한 $ZrOCl_2$, $Zr(SO_4)_2$를 사용하여 제조한 유리는 용융 과정에서 미용융물이 발생하지 않으며 지르코늄 성분이 균일하게 분포되었음을 확인하였다. 이와 같은 결과를 성분 분석, 굽힘 강도를 연계하여 평가하였다.

• 한국재료학회지
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• 제24권11호
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• pp.578-584
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• 2014

To synthesize Sn nanoparticles (NPs) less than 30 nm in diameter, a modified polyol process was conducted at room temperature using a reducing agent, and the effects of different pH values of the initial solutions on the morphology and size of the synthesized Sn NPs were analyzed. tin(II) 2-ethylhexanoate, diethylene glycol, sodium borohydride, polyvinyl pyrrolidone (PVP), and sodium hydroxide were used as a precursor, reaction medium, reducing agent, capping agent, and pH adjusting agent, respectively. It was found by transmission electron microscopy that the morphology of the synthesized Sn NPs varied according to the pH of the initial solution. Moreover, while the size decreased to 11.32 nm with an increase up to 11.66 of the pH value, the size increased rapidly to 39.25 nm with an increase to 12.69. The pH increase up to 11.66 dominantly promoted generation of electrons and increased the amount of initial nucleation in the solution, finally inducing the reduced-size of the Sn particles. However, the additional increase of pH dominantly induced a decrease of PVP by neutralization, which resulted in acceleration of the agglomeration by collisions between particles.

• 한국세라믹학회지
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• 제29권3호
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• pp.223-231
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• 1992

CaO and ZnO were added to Al2O3-SiO2 binary system respectively as flux, then ZrO2 and TiO2 were applied as nucleating agent to these CaO-Al2O3-SiO2 and ZnO-Al2O3-SiO2 ternary system glass. The transparency could not be kept in CaO-Al2O3-SiO2 system glass, whereas the transparent glass-ceramics were prepared in ZnO-Al2O3-SiO2 system glass containing ZrO2 as the nucleating agent. At this time the optimum heating temperatures for the nucleation and the crystal growth were 78$0^{\circ}C$ and 97$0^{\circ}C$. The sizes of the precipitated crystals in the transparent glass-ceramics were below 0.1 ${\mu}{\textrm}{m}$, and their light transmissibilities were more than 80%.

• 한국세라믹학회지
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• 제30권12호
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• pp.1054-1058
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• 1993

The effects of TiO2 addition as a nucleating agent on the cordierite glass-ceramics were investigated. The glass compositiion was stoichiometric cordierite composition of 13.7MgO-34.9Al2O3-51.4SiO2(wt%), and TiO2 as a nucleating agent was added by 5, 10 and 15wt% in addition. The optimum amount of TiO2 addition and appropriate heat treatment schedule were determined by using dilatometer, DTA, XRDA and SEM. The composition containing 10wt% TiO2 was proved to be the best among the investigated compositions. And the optimum heat treatment schedule was 840℃-2h for the nucleation and 1140℃-2h for the crystallization. The properties were as follows. The crystallinity was ∼75%, thermal expansion coefficient 33×10-7/℃(25∼700℃), dielectric constant 7.6(1KHz) and Vicker's hardness 5.1GPa.

• 한국세라믹학회지
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• 제38권12호
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• pp.1137-1143
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• 2001

본 연구에서는 적외선 반사체 제조를 위하여 MAS(MgO-Al$_2$O$_3$-SiO$_2$)계 유리로부터 핵행성 및 결정성장의 2단계 열처리에 의해 cordierite(2MgO.2Al$_2$O$_3$5SiO$_2$)와 rutile(TiO$_2$)을 주결정상으로 하는 결정화유리를 제조하였다. MgO-Al$_2$O$_3$-SiO$_2$3성분계 조성에 조핵제로 TiO$_2$를 첨가하여 용융법으로 유리를 제조한 후 결정화 열처리를 하여 핵생성 및 결정화 거동과 결정화유리의 결정상, 입자 크기와 확산 반사율과의 관계를 관찰하였다. 그 결과 75$0^{\circ}C$에서 3시간동안 핵생성 시킨 후 110$0^{\circ}C$/5hr 이상의 열처리 조건에서 cordierite와 rutile이 주결정상으로 석출되었으며 570~2500nm 범위에서 90% 이상의 반사율을 갖는 결정화유리를 제조하였다.

• 한국세라믹학회지
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• 제46권1호
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• pp.41-46
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• 2009

The rheological properties of highly concentrated Ag nano sol depending on particle size were studied. The Ag nano sol was prepared by reducing the Ag ion in aqueous solution. The size of Ag nano particle was controlled by two steps of nucleation and growth, and the thickness of adsorption layer was varied by molecular weight of polyelectrolytes. The polyelectrolytes acted as not only ionic complex agent in ionic state and but also dispersant after formation of Ag nano sol. The effective volume was controlled by combination of varying the molecular weight of polyelectrolytes and the size Ag nano sol. The particle size and the viscosity of nano sol were characterized by particle size analyzer, HR-TEM and cone & plate viscometer. It was found that the 10 nm and 40 nm-sized Ag nano sols were prepared by controlling the nucleation and growth steps, respectively. Finally, we could prepare highly concentrated Ag nano sol over 50 wt%.

• Macromolecular Research
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• 제14권5호
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• pp.491-498
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• 2006

The thermal degradation of poly(hexamethylene guanidine) phosphate (PHMG) was studied by dynamic thermogravimetric analysis (TGA) and pyrolysis-GC/MS (p-GC). Thermal degradation of PHMG occurs in three different processes, such as dephosphorylation, sublimation/vaporization of amine compounds and decomposition/ recombination of hydrocarbon residues. The kinetic parameters of each stage were calculated from the Kissinger, Friedman and Flynn-Wall-Ozawa methods. The Chang method was also used for comparison study. To investigate the degradation mechanisms of the three different stages, the Coats-Redfern and the Phadnis-Deshpande methods were employed. The probable degradation mechanism for the first stage was a nucleation and growth mechanism, $A_n$ type. However, a power law and a diffusion mechanism, $D_n$ type, were operated for the second degradation stage, whereas a nucleation and growth mechanism, $A_n$ type, were operated again for the third degradation stage of PHMG. The theoretical weight loss against temperature curves, calculated by the estimated kinetic parameters, well fit the experimental data, thereby confirming the validity of the analysis method used in this work. The life-time predicted from the kinetic equation is a valuable guide for the thermal processing of PHMG.

• 한국결정성장학회지
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• 제18권3호
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• pp.115-121
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• 2008

제강분진(EAF dust, 이하 더스트) 50wt%와 핵 형성제를 함유한 규산염계 유리 시편을 열처리하여 결정화 시킨 후 미세구조를 관찰하였다. 제조된 유리의 DTA 분석결과 결정화온도($T_c$)는 $850^{\circ}C$ 부근이었으며 이로부터 열처리 조건을 $950^{\circ}C$/15 hr로 정하였다. 핵 형성제 $TiO_2$는 $Fe_2O_3$나 $Cr_2O_3$에 비해 기계적 특성 및 화학적 내구성이 willemite 결정보다 우수한 franklinite 결정상의 성장을 시키는 효과가 탁월하였다. $TiO_2$가 첨가된 일부 결정화 유리 시편에서 augite 결정상이 관찰되었으며, 첨가량이 증가할수록 willemite 결정상은 줄어들고 franklinite 결정상은 증가하였다. 특히 5wt% 첨가된 시편은 willemite 결정상이 나타나지 않았으며 $1{\sim}2\;{\mu}m$ 크기의 franklinite 결정상이 유리 모상내에 고르게 분포되어 있었다. 또한 $TiO_2$가 5wt% 첨가된 시편에 $Fe_2O_3$를 첨가하면 franklinite 결정상들이 더욱 성장하여 서로 합체됨으로서 수지상 모양의 결정상을 나타내었다.