• 한국결정성장학회지
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• 제32권5호
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• pp.205-211
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• 2022

GSV (Granule Spray in Vacuum)는 상온의 진공하에서 나노 크기의 치밀한 세라믹 코팅층을 형성하는 방법이다. 일반적으로, 단사정의 지르코니아는 1150℃에서 정방정으로 변태하며, 이때 6.5 %의 체적변화를 일으켜 치밀한 단사정의 지르코니아를 만들기 어렵다. 본 연구에서는 코팅 효율에 대한 두 가지 처리 변수의 효과를 조사하는 데 중점을 두었다. 아울러, 특별한 가열과정 없이 형성된 필름의 미세구조에 관찰하였다. 샘플 기판에 증착된 지르코니아 필름에 대한 X-ray diffractometer (XRD) 분석은 단사정 지르코니아 필름이 성공적으로 증착되었음을 보여주었다.

• The Journal of Advanced Prosthodontics
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• 제16권1호
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• pp.25-37
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• 2024

PURPOSE. To investigate the effect of sintering programs and surface treatments on surface properties, phase transformation and flexural strength of monolithic zirconia. MATERIALS AND METHODS. Zirconia specimens were sintered using three distinct sintering programs [classic (C), speed (S), and superspeed (SS)] (n = 56, each). One sample from each group underwent scanning electron microscopy (SEM) and grain size analysis following sintering. Remaining samples were divided into five subgroups (n = 11) based on the surface treatments: control (CL), polish (P), glaze (G), grind + polish (GP), and grind + glaze (GG). One sample from each subgroup underwent SEM analysis. Remaining samples were thermally aged. Monoclinic phase volume, surface roughness, and three-point flexural strength were measured. Monoclinic phase volume and surface roughness were analyzed by Kruskal-Wallis and Dunn tests. Flexural strength was analyzed by two-way ANOVA and Weibull analysis. The relationships among the groups were analyzed using Spearman's correlation analysis. RESULTS. Sintering program, surface treatment, and sintering × surface treatment (P ≤ .010) affected the monoclinic phase volume, whereas the type of surface treatment and sintering × surface treatment affected the surface roughness (P < .001). Type of sintering program or surface treatment did not affect the flexural strength. Weibull analysis revealed no significant differences between the m and σ_o values. Monoclinic phase volume was positively correlated with surface roughness in the SGG and SSP groups. CONCLUSION. After sintering monolithic zirconia in each of the three sintering programs, each of the surface treatments can be used. However, for surface quality and aging resistance, G or GG can be recommended as a surface finishing method.

• The Journal of Advanced Prosthodontics
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• 제6권6호
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• pp.462-467
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• 2014

PURPOSE. This study investigated the influence of surface conditioning procedures and repeated firings on monoclinic content and strength of zirconia before cementation. MATERIALS AND METHODS. Sintered bar-shaped zirconia specimens were subjected to no surface treatment (control), air abrasion, or grinding (n=21). Their roughness was evaluated using a profilometer, and microscope analysis was performed on one specimen of each group. Then, 2 or 10 repeated firings (n=10) were executed, the monoclinic content of specimens was analyzed by X-ray diffraction, and a three-point flexural strength test was performed. Surface roughness values were compared using one-way analysis of variance (ANOVA) and Tukey honestly significant difference (HSD) tests, the monoclinic content values were tested using Kruskal-Wallis and Mann-Whitney U tests, and the flexural strength values were tested using two-way ANOVA and Tukey HSD tests (P=.05). Spearman's correlation test was performed to define relationships among measured parameters. RESULTS. Surface-treated specimens were rougher than untreated specimens and had a higher monoclinic content (P<.005), and the relationship between roughness and monoclinic content was significant (P<.000). Neither surface treatment nor firing significantly affected the flexural strength, but Weibull analysis showed that for the air-abraded samples the characteristic strength was significantly lower after the $10^{th}$ firing than after the $2^{nd}$ firing. CONCLUSION. After firing, a negligible amount of monoclinic content remained on the zirconia surfaces, and rougher surfaces had higher monoclinic contents than untreated surfaces. Multiple firings could be performed if necessary, but the fracture probability could increase after multiple firings for rougher surfaces.

• 한국세라믹학회지
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• 제42권6호
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• pp.411-416
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• 2005

Y-TZP(Yttria-stabilized Tetragonal Zirconia Polycrystal) ceramics are of great interest as engineering and structural materials due to their excellent mechanical properties arising from transformation toughening, it is also reported that the 3Y-TZP($3 mol\%$ Yttria-stabilized Tetragonal Zirconia Polycrystal) has the best mechanical properties in Y-TZP ceramics. But to use widely for engineering and structural materials, it remains an important challenge to be able to improve its fracture toughness. In order to produce the 3Y- TZP ceramics showing much better mechanical properties, milling method adding monoclinic zirconia to 3Y-TZP was adopted and the resultant mechanical properties containing apparent density and fracture toughness were measured by using proper techniques. Experimental results showed that the 3Y-TZP specimen containing $33 wt\%$ of monoclinic zirconia, which was sintered at $1450^{\circ}C$, has the highest fracture toughness value of $11.38 MPa{\cdot}m^{1/2}$ which is three times higher than that of normal 3Y-TZP ceramics.

• Korean Chemical Engineering Research
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• 제57권1호
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• pp.133-141
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• 2019

침전법으로 환류방법 또는 수열합성법을 이용하여 산 염기점을 갖는 고비표면적 지르코니아를 합성하였다. 제조된 지르코니아는 침전제로 수산화암모늄 수용액을 사용하여 Zr 용액의 pH를 2에서 10 범위 내에서 조절하였으며 질소흡착분석, X-선 회절분석(XRD), 이소프로판올 승온탈착법(IPA-TPD), 주사전자현미경 분석, X-선 광전자분광분석, 산-염기점 분석을 통해 IPA 분해반응의 촉매활성과 연관하여 특성분석을 수행하였다. 환류방법을 사용할 시, tetragonal 상이 높은 지르코니아를 얻기 위해서는 Zr 용액의 pH가 높아야 하며, pH 9 이상에서는 순수한 tetragonal 상의 지르코니아 합성이 가능하였다. 또한, 비표면적이 큰 지르코니아를 얻기 위해서는 높은 pH가 요구되었으며, pH 10에서 합성한 경우에는 $600^{\circ}C$에서 소성 후에도 $260m^2g^{-1}$의 높은 비표면적이 얻어졌다. 하지만 같은 조건 하에서 고압이 수반되는 수열합성에는 $40m^2g^{-1}$ 이하의 매우 낮은 비표면적을 보였으며, monoclinic 상의 지르코니아가 합성되었다. 고 비표면적 tetragonal 상의 지르코니아를 얻기 위해서는 용액의 pH가 가장 큰 영향을 미쳤으며, 용액의 pH와 무관하게 높은 압력이 필요한 수열합성에서는 monoclinic 지르코니아가 생성되었으며 상대적으로 비표면적이 낮게 나타났다. 높은 비표면적과 tetragonal 상을 갖는 지르코니아는 염기점에 비해 산점이 우세하여 IPA 분해반응에서 선택적 탈수반응만 진행되는 프로필렌만 생성되었다.

• 대한치과기공학회지
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• 제32권2호
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• pp.57-63
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• 2010

Purpose : This study aimed to find out the effects of treatments on the surface of Zirconia. Methods : To this end, we selected six treatments that have been used widely: steam cleaning, 2bar & 6bar sand blasting, grinding by green stone point, grinding by diamond bur, and grinding by diamond bur with water spray. Results : The results of our study showed that monoclinic rate increased from all six treatments. Monoclinic rate varied by treatments, ranged from 0.6% (steam cleaning) to 6.5% (6bar sand blasting). These values from all six treatments were below ISO 13356 standard, which is 25%. Also, we found that two treatments (green stone point and diamond bur) increased roughness of surface of Zirconia. Conclusion : This study concluded that phase changes of Zirconia were not significant by using six treatments we employed.

• 대한치과기공학회지
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• 제33권4호
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• pp.323-329
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• 2011

Purpose: This study was conducted to examine the phase transition according to the zirconia surface treatment. Methods: The specimens were divided to four groups. The first group was sintered at $1,500^{\circ}C$ and ground; the second group was sintered at $700^{\circ}C$, ground, and sintered at $1,500^{\circ}C$; the third group was sintered at $1,500^{\circ}C$, ground, and $110{\mu}m$-sandblasted; and the fourth group was sintered at $1,500^{\circ}C$, ground, $110{\mu}m$-sandblasted, treated with 9.5% hydrofluoric acid, and ultrasonic cleaner-washed for two minutes. The monoclinic fractions were measured, and the surface was observed via SEM. Results: The monoclinic fraction was $0.13{\pm}0.19%$ in the control group Zr1, $1.91{\pm}0.15%$ in the experimental group Zr2, $7.71{\pm}0.34%$ in Zr3, and $8.39{\pm}0.25%$ in Zr4. On the surface, the phase transition hardly occurred in the control group Zr1, but it increasingly occurred in the experimental groups Zr3 and Zr4. Conclusion: The monoclinic fraction was high in the experimental groups Zr3 and Zr4. The phase transition did not occur in the control group, but increasingly occurred in the experimental groups.

• 한국재료학회지
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• 제23권10호
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• pp.543-549
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• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.

• 한국분말재료학회지
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• 제17권3호
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• pp.197-202
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• 2010

Low temperature degradation behavior in yttria stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics was microscopically observed from the phase contrast between monoclinic surface and tetragonal matrix. The degradation behavior was dependent on the surface treatment of sintered Y-TZP, even if the sintering history is same. In the mirror polished specimen, the monoclinic layer appeared in a uniform thickness from the surface. On the contrary, for the specimen with coarse scratch, the thickness of degraded surface was more than double especially from the coarse scratch. Since the scratch results in local deformation, the residual stress should be induced around the scratch. With the transformation from tetragonal to monoclinic, the volume expansion exerts a stress on a neighboring grains and promotes a successive phase transformation. Such a autocatalytic effect can be triggered from the part of coarse scratch.

• 한국표면공학회지
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• 제34권5호
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• pp.486-493
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• 2001

Partially stabilized zirconia (PSZ) is an attractive material for thermal barrier coating. Zirconia exists in three crystallographic phases: cubic, tetragonal and monoclinic. Especially, the phase transformation of tetragonal phase to monoclinic phase accompanies significant volume expansion, so this transition generally results in cracking and contributes to the failure of the TBC system. Both the plasma sprayed ZrO$_2$-8Y$_2$O$_3$ (YSZ) coat and the ZrO$_2$,-25CeO$_2$,-2.5Y$_2$O$_3$ (CYSZ) coat are isothermally heat -treated at 130$0^{\circ}C$ and 150$0^{\circ}C$ for 100hr and cooled at different cooling rates. The monoclinic phase is not discovered in all the CYSZ annealed at 130$0^{\circ}C$ and 150$0^{\circ}C$. In the 150$0^{\circ}C$ heat-treated specimens, the YSZ contains some monoclinic phase while none exists in the 130$0^{\circ}C$ heat-treated YSZ coat. For the YSZ, the different phase transformation behaviors at the two temperatures are due to the stabilizer concentration of high temperature phases and grain growth. For the YSZ with 150$0^{\circ}C$-100hr annealing, the amount of monoclinic phase increased with the slower cooling rate. The extra oxygen vacancy, thermal stress, and c to t'phase transformation might suppress the t to m martensitic phase transformation.