• Journal of Technologic Dentistry
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• v.35 no.2
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• pp.137-142
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• 2013

Purpose: This study was to observe the surface and interfacial characteristic of Zirconia by surface treatment. And it was observed the roughness and contact angle according to processing, and the interfacial properties by surface treatment on zirconia. Methods: The oxide formation and ion diffusion between core and veneer ceramic were determined by the X-ray Dot Mapping of EPMA(Electron probe micro analyzer). The roughness was measured by 3D Digital microscope and the contact angle according to processing of zirconia was observed using distilled water on the surface. Results: The surface roughness of the specimens Z04, Z12, Z15 was measured $0.67({\pm}0.03){\mu}m$, $0.50({\pm}0.12){\mu}m$, $0.35({\pm}0.09){\mu}m$, respectively. As results of contact angle test, Z04, Z12, Z15 of specimen group without binder treatment was measured $46.79({\pm}3.17)^{\circ}$, $57.47({\pm}4.83)^{\circ}$, $56.19({\pm}2.66)^{\circ}$, respectively. but, L04, L12, L15 of specimen group without binder treatment was measured $63.84({\pm}2.20)^{\circ}$, $66.08({\pm}0.16)^{\circ}$, $65.10({\pm}1.01)^{\circ}$, respectively. Average contact angle of L15 was measured $65.10({\pm}1.01)^{\circ}$. In X-ray Dot Mapping results, thickness of binder including Al element was measured that each of L04, L12, L15 were $20{\mu}m$, $15{\mu}m$, $10{\mu}m$. Conclusion: The more rough surface increases the wettability, but the sintered exclusive binder decreases the wettability.

• 한국신재생에너지학회:학술대회논문집
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• 2010.06a
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• pp.135.1-135.1
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• 2010

최근 고온에서 사용 가능한 PEMFC용 고분자전해질 막 개발에 대한 연구가 활발히 진행되고 있다. PEMFC가 고온에서 작동하게 되면 높은 성능과 많은 장점을 갖게 된다. PEMFC를 $100^{\circ}C$ 이상에서 운전하게 될 경우 백금 전극 반응을 향상시켜 고가의 백금 촉매 양을 줄일 수 있게 되고, 수소연료 속에 미량 포함된 CO에 의한 촉매표면 피독현상에 대한 내구성을 높일 수 있어 저 순도 수소연료 사용이 가능해 진다. 또한 가습장치와 수소 연료 개질장치의 부피를 줄일 수 있게 되어 전체적인 PEMFC 시스템이 단순화 된다. 현재 연료전지용 고분자 전해질막으로 DuPont사의 과-불소계 고분자 전해질막인 Nafion$^{(R)}$이 가장 널리 사용되고 있다. Nafion$^{(R)}$은 유연한 분자구조 안에 소수성이 강한 주사슬과 친수성을 나타내는 술폰산이 결합된 곁사슬이 존재하여 술폰화 곁사슬의 클러스터 둘레에는 친수성 영역이 형성이 되기때문에 소수/친수 상 분리가 잘되어 이온 클러스터 형성이 용이하지만 제조비용이 높은 단점을 갖고 있다. 특히, 전해질 막내에서 Bronsted base 역할을 하는 물에 의해 이온전도가 이루어지기 때문에 고온에서는 수분증발로 인해 성능이 급격히 감소된다. 따라서, 본 연구에서는 고온 저가습 조건에서 운전이 가능하고 Nafion이 갖는 문제점을 해결하고자, 내열특성이 뛰어나며 높은 수소이온 전도도 학보가 용이한 Sulfonated Poly(aryl ether)sulfone(SPAES) 고분자 전해질에, 고온에서도 수화성이 유지될 수 있도록 지르코니아를 황산화한 sulfated zirconia(s-$ZrO_2$)를 함침하여 복합 고분자전해질막을 제조하여 고온 저가습 조건에서의 수소이온 전도 특성에 관한 연구를 수행하였다. 개발된 막의 물리/화학적 특성은 water content(Wup%), 이온교환 용량(IEC, meq $g^{-1}$), 수소이온전도도(s $cm^{-1}$) 열 중량 분석(TGA), X선 회절분석(XRD) 등을 통하여 분석 및 관찰하였다. 내화학 및 열적 특성분석 결과, 황산화 반응공정으로 $ZrO_2$에 술폰산기가 안정적으로 결합하고 있음이 관찰되었으며, 본 연구에서 개발된 유 무기 복합막이 $250^{\circ}C$이상 열적안정성을 확보하고 있는 것으로 판단되었다. $100^{\circ}C$ 이하의 저온 영역에서, 일정 비율의 s-$ZrO_2$/SPAES막에서 이온교환용량(IEC)이 순수 SPAES 막보다 낮음에도 불구하고, water uptake가 증가함과 동시에 수소이온 전도도가 향상된 것을 관찰하였다. 또한, 고온에서는 수소이온이 자유롭게 이동할 수 있는 water channel을 형성하는 free water는 증발 하지만 s-$ZrO_2$와 SPAES의 술폰산기 사이에 강력하게 결합하고 있는 bound Water는 $100^{\circ}C$ 이상의 고온 영역에서도 존재하여, 비록 무가습 조건에서도 일정 비율의 s-$ZrO_2$/SPAES50 전해질 막의 경우, 높은 전도도를 나타냄을 관찰할 수 있었다. 따라서 본 연구를 통해 저가습 고온 적용을 목적으로 개발된 s-$ZrO_2$/SPAES50막은 우수한 내열 특성을 나타냄과 동시에 저가습 고온 영역($120^{\circ}C$, $50RH{\downarrow}$)에서 높은 수소이온 전도도를 유지하여, 고온 저가습 연료전지 운전에 적합할 것으로 사료된다.

• Korean Journal of Materials Research
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• v.9 no.8
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• pp.768-774
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• 1999

Yttia-doped ceria-stabilized ziconia polycrystals(Ce-TZP) was prepared by dipping method and its microstructure was investigated. By controlling doped-yttria content and annealing condition, yttria-doped Ce-TZP showed the microstructure with irregular grain shape and undulated grain boundary. Irregularity of grain shape increased with the amount of yttria doped, and severe undulated grain boundary was observed mainly at the surface region. In the case of yttria-doped Ce-TZP annealed at 1$650^{\circ}C$ for 2h after two dipping times into yttrium nitrate solution of 0.2M, it showed irregular grain shape both at the surface and at the interior region as well as the most severe irregularity. Hot pressed specimen had mean grain size of 0.3$\mu\textrm{m}$ and undulated grain boundary. All specimens with irregular grain shape were retained the tetragonal phase. The fracture toughness of yttria-doped Ce-TZP with irregular grain shape was over the value of 17.6MPa.m(sup)1/2.

• Journal of Technologic Dentistry
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• v.37 no.3
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• pp.121-127
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• 2015

Purpose: This study was intended to investigate the effect of applying liner for chemical bonding and physical surface roughness created on zirconia by using a sandpaper before sintering on the bond strength between the two materials. Methods: Zirconia blocks were cut using a low-speed cutter. Plate-shaped specimen($6mm{\times}6mm{\times}3mm$) was fabricated by sintering after giving surface roughness according to four kinds of sandpapers. Depending on whether or not to use liner, 60 specimens were divided into two groups ZN(non-liner), ZL(liner), and the two groups were subdivided into four groups respectively in accordance with sandpaper used, totaling eight groups (n=10). The surface roughness (Ra) values and shapes before sintering were observed, and shear bond strength after pressing ceramic plasticity was measured with a universal testing machine. For a test of the significance, a one-way ANOVA was performed, and Tukey's multiple comparison test was conducted. Results: The observation of the surface roughness was SB04($2.22{\pm}1.16{\mu}m$), SB08($2.98{\pm}0.33{\mu}m$), SB12($2.44{\pm}1.32{\mu}m$), SB20($2.34{\pm}0.59{\mu}m$) and SA04($2.34{\pm}0.67{\mu}m$), SA08($1.28{\pm}0.90{\mu}m$), SA12($2.03{\pm}1.60{\mu}m$), SA20($2.19{\pm}1.73{\mu}m$). In the case of ZN Group, the shear bond strength was ZN04($23.26{\pm}3.83MPa$), ZN08($21.76{\pm}2.33MPa$), ZN12($20.49{\pm}3.01MPa$), ZN20($24.98{\pm}4.22MPa$)(p<0.05). As for ZL Group, the shear bond strength was ZL04($25.09{\pm}5.67MPa$), ZL08($22.98{\pm}2.26MPa$), ZL12($21.54{\pm}5.70MPa$), ZL20($23.98{\pm}3.23MPa$)(p<0.05). Conclusion: The research results showed that the bond strength of Zirconia core and Pressing ceramic was further improved by physical surface treatment before sintering, rather than by chemical bonding through liner surface treatment.

• Journal of Technologic Dentistry
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• v.35 no.1
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• pp.19-27
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• 2013

Purpose: The aim of this research was to evaluate the shear bond strength of different zirconia veneering ceramics with and without liner glass materials to yttria partially-stabilized tetragonal zirconia polycrystalline(Y-TZP). Methods: Five co mmercial zirconia veneering ceramics were used in this study, E-Max(EM), Creation ZI(CR), Cercon ceram kiss(CE), Triceram(TR) and Zirkonzahn ICE(ZI). All samples were prepared according to manufacturer's instructions. Experimental industrially manufactured Y-TZP ceramic blocks(diameter: 2.7 mm; height: 13.5 mm) were used in this study. Shear bond strength between zirconia ceramic coping and zirconia veneering ceramics were evaluated by the push-shear bond test. The fracture load data were analyzed using ANOVA and Scheffe's test(${\alpha}$=0.05). The fractured surfaces of zirconia core ceraimc and zirconia veneering ceramics were observed using a scanning electron microscope(SEM). Results: The mean shear bond strengths ranged from 20 MPa ($20.12{\pm}6.34$ MPa) to 66.6 MPa ($66.62{\pm}10.01$ MPa). The Triceram(TRG) showed the highest value and Creation ZI(CR) showed the lowest value. In all groups, Zirconia liner and glass material groups was significantly higher shear bond strength than without liner(P<0.05), with the exception of Cercon ceram kiss(CE)groups. Conclusion: Zirconia bonding materials may have the advantage of improved bond strength between zirconia ceramic core and veneering ceramics.

• Korean Journal of Materials Research
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• v.24 no.12
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• pp.677-681
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• 2014

To increase the mechanical property of zirconia, we have investigated the phase change and the resulting hardness of zirconia ceramics by hydroxyapatite (HA) powder bed sintering. It was observed using X-ray diffraction that the cubic zirconia phase, which has a higher hardness value than that of the tetragonal phase, was obtained at the surface of 3 mol% $Y_2O_3$ doped tetragonal zirconia polycrystal (3Y-TZP) ceramics during the sintering process; in our experimental conditions, the phase change at the surface increased as the sintering time increased. We believe that the observed crystalline phase change originated from the decomposition of HA and the diffusion of CaO, as follows. CaO, which was derived from the decomposition of HA at high temperature ($1400^{\circ}C$), diffused into the surface of 3Y-TZP and acted as a stabilizer. As a result, the Vickers hardness value of the treated specimens was higher than that of the non-treated specimen due to the formation of the cubic phase on the surface of 3Y-TZP.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.5 no.2
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• pp.165-174
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• 1995

A stable suspension with a colloidal $ZrO_2$ particle was prepared by an adsorption of PV A and investigated to the effects of PV A on the dispersion and particle growth within suspension. With a suspension added the optimum concentration of PYA (about 500 ppm in this study), it was shown the property of a stable sol due to the formation of adsorbed PV A layer on surface and the reduction of an agglomeration among the particles. Most of nucleation in colloidal $ZrO_2$ were occured in the early stage of hydrolysis reaction and the plate-like monoclinic $ZrO_2$ particle were grown with an aging time. The rate of particle growth and yield for a reaction were decreased with an addition of PV A. The compact prepared from well- dispersed suspension by an addition of PV A was contained the homogeneous particle arrangement and pore distribution.

• Journal of Technologic Dentistry
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• v.39 no.4
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• pp.243-251
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• 2017

Purpose: The purpose of this study was to investigate the effects of etching by monitoring the etched surfaces and the shear bonding strength of resin and porcelain with etched zirconia. Methods: The CAD/CAM was used to produce 24 zirconia blocks in groups of six. The zirconia specimen surfaces were sandblasted, and they were then divided into 12 specimens with surface etching and 12 specimens without etching for the control group. 12 specimens of composite resin were bonded using a curing light, and 12 specimens of porcelain underwent vita porcelain build-up sintering and the shear bonding strength was measured using a universal testing system. The SEM photographs were taken in order to observe any differences in the surfaces before and after etching, and they were magnified by a factor of 8 in order to observe fractured surface types. Results: The results of the shear bonding strength measurements are as follows: For the composite resin tests, between zirconia and resin, the shear bonding strength of the control group (NZR) without surface etching was 4.68 Mpa and the experimental group (EZC) with surface etching was 9.65 Mpa, which is significantly higher. The crystal structure of the zirconia was confirmed to be different in observations of the surfaces before and after etching. Conclusion : In comparing the shear bonding strength of zirconia and composite resin, the effects of etching were found to be significant. The effects of surface etching were also observed in fractured surfaces between zirconia and porcelain. This is expected to be applicable to various prosthetics as surface etching on zirconia is used in clinics.

• Journal of Technologic Dentistry
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• v.35 no.2
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• pp.121-126
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• 2013

Purpose: The aim of this research was to investigate difference in shear bond strengths of full-contour zirconia layered with porcelain. Methods: Disk-shaped (diameter: 12.0 mm; height: 3.0 mm) zirconia were randomly divided into six groups according to the surface conditioning method to be applied (N=90, n=15 per group): group 1-contol group(ZC); group 2-airborne particle abrasion with $50-{\mu}m\;Al_2O_3(5A)$; group $3-50-{\mu}m\;Al_2O_3$ + liner(5AL), group $4-110-{\mu}m\;Al_2O_3(1A)$; group $5-110-{\mu}m\;Al_2O_3$ + liner(1AL); group 6-liner(LC). On each block, zirconia porcelain was build up according to manufacturer's instructions. All samples were fixed with measuring jigs and shear bond strength were measured with Universal testing machine. Collected data were analyzed using SPSS(Statistical Package for Social Sciences) Win 12.0 statistics program. Results: LC showed the highest value($29.92{\pm}2.55$ MPa) and ZC showed the lowest value($13.22{\pm}1.37$ MPa). Zirconia liner and Alumina oxide groups was significantly higher shear bond strength than control(p<0.05). 5A (without liner $22.18{\pm}2.37$, with liner $22.84{\pm}1.74$ MPa) was higher shear bond strength than $110{\mu}m$ (without liner $20.18{\pm}2.38$, with $20.71{\pm}2.67$). Conclusion: Surface treatments may have advantage in bond strength improvement for full-contour zirconia layered with porcelain.

• Journal of Technologic Dentistry
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• v.42 no.3
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• pp.213-219
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• 2020

Purpose: This study aimed to identify the impact of physical surface roughing with a polishing tool onto the pre-sintering yttria-stabilized tetragonal zirconia polycrystals (TZP) core and liner treatment for chemical bonding on the bond strength of TZP core and veneering ceramic. Methods: Overall, 80 specimens were classified into two groups (non-liner, NL; and usingliner, UL ) depending on the use of liner, and these two groups were then subclassified into four groups depending on the polishing tool used. (1) Non-liner groups: NS, non-liner+stone point; NC, non-liner+carbide bur; NP, non-liner+paper cone point; NT, non-liner+silicon point. (2) Using-liner groups: US, using-liner+stone point; UC, using-liner+carbide bur; UP, usingliner+paper cone point; UT, using-liner+silicon point. The pre-sintering surface roughing values and shapes were observed, and after burning up the veneering ceramic, the shear bond strength was measured using a universal testing machine. For significance testing, a one-way analysis of variance and Tukey's multiple comparison test were conducted. An optical microscope was used to observe the fracture plane, and the following results were obtained. Results: Surface roughness NP (4.09±0.51 ㎛) represented a higher value than other groups (p<0.001). In shear bond strength, NS (35.21±1.44 MPa) of the NL group showed the highest bond strength (p<0.001). The UL group did not show a statistically significant difference between groups (p=0.612). Conclusion: Our study findings reveal that the bond strength of TZP core and veneering ceramic was improved by pre-sintering physical surface treatment than by chemical bonding with liner surface treatment.