• 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.

• The Journal of Advanced Prosthodontics
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• 제6권4호
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• pp.253-258
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• 2014

PURPOSE. To compare marginal and internal gaps of zirconia substructure of single crowns with those of three-unit fixed dental prostheses. MATERIALS AND METHODS. Standardized Co-Cr alloy simulated second premolar and second molar abutments were fabricated and subsequently duplicated into type-III dental stone for working casts. After that, all zirconia substructures were made using $Lava^{TM}$ system. Marginal and internal gaps were measured in 2 planes (mesial-distal plane and buccal-palatal plane) at 5 locations: marginal opening (MO), chamfer area (CA), axial wall (AW), cusp tip (CT) and mid-occlusal (OA) using Replica technique. RESULTS. There were significant differences between gaps at all locations. The $mean{\pm}SD$ of marginal gap in premolar was $43.6{\pm}0.4{\mu}m$ and $46.5{\pm}0.5{\mu}m$ for single crown and 3-unit bridge substructure respectively. For molar substructure the $mean{\pm}SD$ of marginal gap was $48.5{\pm}0.4{\mu}m$ and $52.6{\pm}0.4{\mu}m$ for single crown and 3-unit bridge respectively. The largest gaps were found at the occlusal area, which was $150.5{\pm}0.5{\mu}m$ and $154.5{\pm}0.4{\mu}m$ for single and 3-unit bridge premolar substructures respectively and $146.5{\pm}0.4{\mu}m$ and $211.5{\pm}0.4{\mu}m$ for single and 3-unit bridge molar substructure respectively. CONCLUSION. Independent-samples t-test showed significant differences of gap in zirconia substructure between single crowns and three-unit bridge (P<.001). Therefore, the span length has the effect on the fit of zirconia substructure that is fabricated using CAD/CAM technique especially at the occlusal area.

• The Journal of Advanced Prosthodontics
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• 제5권3호
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• pp.248-255
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• 2013

PURPOSE. This study compared the effect of three intraoral repair systems on the bond strength between composite resin and zirconia core. MATERIALS AND METHODS. Thirty zirconia specimens were divided into three groups according to the repair method: Group I-CoJet$^{TM}$ Repair System (3M ESPE) [chairside silica coating with $30{\mu}m$ $SiO_2$ + silanization + adhesive]; Group II-Ceramic Repair System (Ivoclar Vivadent) [etching with 37% phosphoric acid + Zirconia primer + adhesive]; Group III-Signum Zirconia Bond (Heraus) [Signum Zirconia Bond I + Signum Zirconia Bond II]. Composite resin was polymerized on each conditioned specimen. The shear bond strength was tested using a universal testing machine, and fracture sites were examined with FE-SEM. Surface morphology and wettability after surface treatments were examined additionally. The data of bond strengths were statistically analyzed with one-way ANOVA and Tamhane post hoc test (${\alpha}$=.05). RESULTS. Increased surface roughness and the highest wettability value were observed in the CoJet sand treated specimens. The specimens treated with 37% phosphoric acid and Signum Zirconia Bond I did not show any improvement of surface irregularity, and the lowest wettability value were found in 37% phosphoric acid treated specimens. There was no significant difference in the bond strengths between Group I ($7.80{\pm}0.76$ MPa) and III ($8.98{\pm}1.39$ MPa). Group II ($3.21{\pm}0.78$ MPa) showed a significant difference from other groups (P<.05). CONCLUSION. The use of Intraoral silica coating system and the application of Signum Zirconia Bond are effective for increasing the bond strength of composite resin to zirconia.

• 대한치과보철학회지
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• 제42권5호
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• pp.489-500
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• 2004

Statement of problem: The use of zirconia prostheses fabricated with CAD/CAM system is on an increasing trend in dentistry. However, evaluation of the fit related to internal relief and marginal reproducibility of zirconia has not been reported. Purpose : This study was to evaluate the fit related to internal relief and marginal reproducibility of zirconia core fabricated with CAD/CAM system. Materials and methods: The evaluation was based on 30 zirconia cores and 5 IPS-Empress2 cores. Zirconia cores were fabricated in different conditions of internal relief(0, 10, 20, 30, 40 and $50{\mu}m$), and IPS-Empress2 cores were fabricated in accordance with the manufacturer's instructions. Before cementation, the marginal discrepancies or cores were measured on metal die. And then, each core was cemented to stone die, embedded in an acrylic resin and sectioned in two planes(mesiodistally and labiopalatally). The internal gaps were measured at the margin and axial surface. Measurements for the marginal discrepancies, the internal marginal gaps and the internal axial gaps were performed under a measuring microscope(Compact measuring microscope STM5; Olympus, Japan) at a magnification of ${\times}100$. In addition, the marginal conagurations of metal die, zirconia core and IPS-Empress2 core were examined with SEM(S-2700, Hitachi, Japan). Results : Within the limits of this study the results were as follows. 1. Compared with IPS-Empress2 cores, the marginal discrepancies of zirconia cores had no significant differences. the internal marginal gaps were statistically smaller and the internal axial gaps were statistically larger in each condition of internal relief. 2. The marginal discrepancies and the internal marginal gaps of zirconia cores had no significant differences related to the conditions of internal relief(P>0.05). 3. The internal axial gaps of zirconia cores with $0{\sim}20{\mu}$m for internal relief were significantly larger than that with $50{\mu}m$ (P<(0.0001). 4. SEM micrographs showed favorable marginal reproducibility of zirconia core and smooth texture on the milling surface. Conclusion: The marginal discrepancy and the internal gaps of zirconia core were clinically acceptable and the milling surface was showed smooth texture. For fabrication of the durable esthetic restoration, further investigations on complex design of core, milling accuracy, compatability of enamel porcelain and porcelain firing seems to be needed.

• 대한치과기공학회지
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• 제38권3호
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• pp.111-117
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• 2016

Purpose: The present study was performed to investigate the effect of abutment inclined angle on the marginal fit of zirconia all-ceramic crown. Methods: The Ti abutments with 3 different inclined angle($2^{\circ}$, $4^{\circ}$ and $6^{\circ}$) were fabricated. The zirconia copings were fabricated for each abutment by using dental CAD/CAM system. The manufactured zirconia copings were duplicated through silicone replica technique, and a replicated specimen was sectioned in the center of bucco-lingual and mesio-distal axial to measure the marginal fit by using a stereo microscope. The results were analyzed using a one-way ANOVA with SPSS 22.0 for Windows(${\alpha}=0.05$). Results: On the bucco-lingual axial, marginal fit was the RL3($41.5{\pm}3.4{\mu}m$), RL2($44.3{\pm}4.3{\mu}m$) and RL1($47.5{\pm}5.7{\mu}m$), respectively. On the mesio-distal axial, marginal fit was the RL3($41.1{\pm}3.7{\mu}m$), RL2($45.7{\pm}5.3{\mu}m$) and RL1($46.2{\pm}4.5{\mu}m$), respectively. One-way ANOVA showed statistically significant difference between groups for marginal fit(p<0.05). Conclusion: For marginal fit of the abutments inclined angle, RL3 specimen was superior. The abutment inclined angle had influence on marginal fit of the zirconia copings. The marginal fit of each group were within clinically acceptable range.

• The Journal of Advanced Prosthodontics
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• 제9권4호
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• pp.252-256
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• 2017

PURPOSE. This in vitro study aimed to analyze and compare the reproducibility of zirconia and lithium disilicate crowns manufactured by digital workflow. MATERIALS AND METHODS. A typodont model with a prepped upper first molar was set in a phantom head, and a digital impression was obtained with a video intraoral scanner (CEREC Omnicam; Sirona GmbH), from which a single crown was designed and manufactured with CAD/CAM into a zirconia crown and lithium disilicate crown (n=12). Reproducibility of each crown was quantitatively retrieved by superimposing the digitized data of the crown in 3D inspection software, and differences were graphically mapped in color. Areas with large differences were analyzed with digital microscopy. Mean quadratic deviations (RMS) quantitatively obtained from each ceramic group were statistically analyzed with Student's t-test (${\alpha}=.05$). RESULTS. The RMS value of lithium disilicate crown was $29.2\;(4.1){\mu}m$ and $17.6\;(5.5){\mu}m$ on the outer and inner surfaces, respectively, whereas these values were $18.6\;(2.0){\mu}m$ and $20.6\;(5.1){\mu}m$ for the zirconia crown. Reproducibility of zirconia and lithium disilicate crowns had a statistically significant difference only on the outer surface (P<.001). The outer surface of lithium disilicate crown showed over-contouring on the buccal surface and under-contouring on the inner occlusal surface. The outer surface of zirconia crown showed both over- and under-contouring on the buccal surface, and the inner surface showed under-contouring in the marginal areas. CONCLUSION. Restoration manufacturing by digital workflow will enhance the reproducibility of zirconia single crowns more than that of lithium disilicate single crowns.

• 한국세라믹학회지
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• 제32권7호
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• pp.846-852
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• 1995

The multiply reinforced mullite-zirconia composites were prepared with addition of Al2O3 particles, platelets, and fibers. The sinter-HIP specimens (presintered at 1$700^{\circ}C$ and hipped at 1$600^{\circ}C$) showed that the fracture toughness of Al2O3 fiber reinforcement (4.4 MPa.{{{{ SQRT {m} }}) was higher than those of platelet (4.0 MPa.{{{{ SQRT {m} }}) and of particle (3.9MPa.{{{{ SQRT {m} }}) reinforcement, whereas the fracture strength of Al2O3 particle reinforcement (304 MPa) was higher than those of platelet (293MPa) and of fiber (248MPa) reinforcement.

• 대한치과보철학회지
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• 제52권3호
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• pp.246-251
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• 2014

CAD/CAM을 이용하여 보철물을 제작할 경우 교합 접촉점의 위치, 면적, 형태를 원하는 대로 조절할 수 있으므로 보다 기능적인 교합의 부여가 가능하다. 또한 전통적인 Casting 기법을 이용한 주조금속 보철물이나, Porcelain의 축성을 통해 제작된 보철물에 비하여 제작과정 중의 오차가 감소하여 우수한 교합 정확도를 얻을 수 있을 것으로 기대되고 있다. 그리고 최근 소개되고 있는 CAD/CAM system에는 가상 교합기 기능이 추가되어 단일 수복물의 설계에서도 상악에 대한 하악의 운동을 재현함으로써 폐구 운동 뿐만 아니라 전/측방 운동시의 교합간섭을 고려할 수 있게 되었다. 그 동안 zirconia를 이용한 보철물의 변연 및 내면 적합도에 대한 연구는 많이 이루어졌으나 CAD/CAM을 이용해 설계된 zirconia crown의 교합 적합도에 대한 연구는 많이 이루어지지 않았다. 따라서 본 증례에서는 총 5명의 환자에서 CAD/CAM을 이용하여 제작된 7개의 지르코니아 크라운을 대상으로, 처음 설계된 zirconia crown의 교합 접촉점과 조정과정을 거쳐 구강 내 시적 후에 제작된 모델을 스캔하여 획득된 교합 접촉점을 비교하여 보철물의 정확도를 평가하고 교합조정의 양상을 파악해 보고자 하였다. 지르코니아 크라운에서 이루어진 교합조정은 대부분 기능교두 및 사면부위에서 이루어졌으며 15 - $60{\mu}m$의 분포를 보였다. CAD/CAM을 이용하여 제작된 지르코니아 크라운에서 어느정도의 교합조정은 불가피한 과정이며 이에 따른 물성저하를 보상하기 위한 추가적인 과정이 필요할 것이다.

• 한국세라믹학회지
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• 제32권12호
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• pp.1401-1407
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• 1995

Zirconia powder coated with alumina was prepared by hydrolysis of alumina butoxide. The coated powder was obtained by a hydrolysis reaction between the adsorbed water on the surface of zirconia particles and aluminum sec-butoxide. Amorphous aluminum hydroxide was uniformly coated on the surface of zirconia particles with the thickness of about 30 nm. The shape and distribution of aluminum hydroxide was varied with an existence of surfactant. The coated layer of aluminum hydroxide consists of the fine particle size, and the zirconia powder coated by alumina hydroxide have the large specific surface area of 120 $m^2$/g, compared with that of starting zirconia powder.

• Bulletin of the Korean Chemical Society
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• 제27권11호
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• pp.1844-1850
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• 2006

Two types of catalyst samples were prepared, one sulfated zirconia and the other silica doped sulfated zirconia. The acidity tests indicate that sulfated zirconia doped with silica has higher concentration and strength of acidic catalyst sites than undoped sulfated zirconia. The acidic surface sites have been characterized using FTIR, NMR, pyridine adsorption, TPD, XRD and nitrogen adsorption. Doping with silica increased the concentration of surface Lewis and Brfnsted acid sites and resulted in generation of proximate acid sites.The activity test indicates that doping sulfated zirconia with silica increases both the acidity and catalytic activity for liquid phase dehydration of methanol at 413-453 K. Methanol is sequentially dehydrated to dimethyl ether and ethylene over both catalysts. Significant amounts of propylene are also formed over the silica-doped catalyst, but not over the undoped catalyst.