• Korean Chemical Engineering Research
• /
• v.50 no.2
• /
• pp.229-237
• /
• 2012

Phosphorus was incorporated into Co/$Al_2O_3$ catalyst for FTS by impregnating an acidic precursor, phosphoric acid, in ${\gamma}-Al_2O_3$ support to improve the mechanical strength, the hydrothermal stability of the catalyst particle, and the catalytic performance as well. Surface characterization techniques such as FT-IR revealed that $AlPO_4$ phase was generated on the surface of the P-modified catalyst. The addition of phosphorus was found to alleviate the interaction between cobalt and alumina surface, and to increase reducibility of catalyst. The catalytic activity such as $C_{5+}$ productivity and turnover frequency (TOF) was calculated to evaluate catalytic performance. The influence of calcination temperature of the $Al_2O_3$ containing 2 wt.% P on the catalytic performance was also investigated. Through hydrothermal stability test and XRD analysis, the P-modified catalyst had strong resistant to the pressurized and hot $H_2O$. The mechanical strength of the P-modified catalyst was also examined through an in-house fluidized-bed vessel, and it was found that the catalyst fragmentation could be successfully suppressed with P. Taken as a whole, the best performance was shown to be at 1~2 wt.% P in alumina and at the calcination temperature of $500^{\circ}C$.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06b
• /
• pp.219-222
• /
• 1996

수열법은 밀폐용기중에서 10$0^{\circ}C$이상의 가열, 가압된 수용액이 반응에 관여하는 것으로써, 수정, CaCO3, AlPO4, GaPO4 등과 같은 단결정의 육성 뿐만 아니라 균일분산계로부터 균일한 결정성의 미립자 합성에도 폭넓게 이용되고 있다. 세라믹분말의 합성에 있어서, 이 방법은 특히 형상, 입자크기의 제어가 용이할 뿐만 아니라 고상법, 졸-겔법, 공침법에서와 같은 열처리, 분쇄과정이 필요없기 때문에 고순도의 초미립자를 얻을 수 있는 장점이 있다. 근년 미국, 일본에서는 수열법을 이용한 유전, 압전체 등 세라믹분말의 일부가 공업적인 규모로 대량 생산되고 있다. 그러나 이에 대한 국내 기술은 아직 초기단계에 이르고 있는 실정이다. 따라서 본 연구실에서는 수열법에 의한 단결정 육성 (예; 자수정, CaCO3, AlPO4, GaPO4, KTP, Emerald 등), 박막제조 (예; GaP, PbTiO3, BaTiO3 등), 정제 (고령토, 장석, 도석 등), 원석처리 (진주, 인공 emerald, 비취 등) 그리고 각종 세라믹분말의 합성 등과 같은 다양한 기반기술의 축적과 동시에 공업화에 대응한 수열장치를 위하여 반응용기의 대형화, 엄밀한 밀폐방식, 실용적인 수열조건 등을 개발해 오고 있다. 본 발표에서는 현재까지의 연구개발 내용 중에서 결정성 미립자에 관련한 세라믹분말의 합성에 대한 일부의 결과들을 보고한다. 일반적으로 수열장치는 전기로, 반응용기, 온도 및 압력제어계 등을 기본으로 하고 있으며 시판용의 대부분이 교반기가 부착된 수직형 (vertical type)이다. 이와 같은 방식에 있어서는 엄밀한 밀폐가 곤란, 반응온도의 한계성 (25$0^{\circ}C$ 이하), 증진율의 한계성 (소량생산) 등과 같은 점이 있기 때문에 본 연구실에서는 개폐식 전기로내에 엄밀한 밀폐가 가능한 수평식(horizontal type)의 반응용기를 채택한 뒤 이를 회전 또는 시이소(seesaw)식으로 움직일 수 있도록 하여 연속공정화, 온도구배의 자율조절 그리고 보다 저온에서도 인위적인 이온의 확산을 효율적으로 유도할 수 있도록 하였다. 이와 같은 방식은 기존의 방식과 비교하여 반응용기 내에 응집현상과 미반응물이 존재하지 않으며 또한 단분산으로 결정성 미립자를 대량적으로 얻을 수 있는 장점이 있었다. 다음은 이상과 같이 본 연구실에서 자체 개발한 수열장치를 이용하여 PbTiO3, (Pb,La)TiO3Mn, BaTiO3, ZnSiO4:Mn, CaWO4 등과 같은 세라믹분말에 대한 합성 실험의 결과이다. 압전성, 초전성이 우수한 PbTiO3 및 (Pb,La)TiO3:Mn 분말의 수열합성은 PbO, TiO2, La2O3 등의 분말을 출발원료로 하여 합성도도 25$0^{\circ}C$부근의 알카리성 용액중에서 결정성 PbTiO3 및 (Pb,La)TiO3:Mn 미립자를 단상으로 얻었으며 입자의 형상 및 크기는 합성온도와 수열용매의 종류에 의존하였다. 유전체로서 폭넓게 응용되고 있는 BaTiO3 분말은 Ba(OH)2.8H2O, TiO2와 같은 최적의 출발원료를 선택함으로써 15$0^{\circ}C$ 부근의 저온영역에서도 용이하게 합성할 수 있었다. 특히 본 연구에서는 수용성인 Ba(OH)2.8H2O를 사용함으로써 host-guest적인 반응을 유도시키는데 있어 물의 가장 실용적이고 효과적인 수열용매임도 알았다. ZnSiO4:Mn, CaWO4, MgWO4와 같은 형광체 분말은 공업적으로 고상반응 또는 습식법에 의해 얻어지고 있으나 이들 방법에 있어서는 분쇄공정으로 인한 형광특성의 저하와 같은 문제점이 있다. 따라서 본 연구에서는 수열법을 이용하여 이들 화합물의 합성을 시도하였으며 그 결과 합성온도 30$0^{\circ}C$ 부근의 알칼리성 용액중에서 수열적으로 얻어짐을 알았다. 여기서의 합성분말을 이용하여 실제 조명램프로 제조한 결과 녹색, 청색 발광용 형광체로서 우수한 형광특성을 나타내었다. 천연에서 소량 산출되고 있는 고가의 (Li,Al)MnO2(OH)2:Co 분말은 도자기의 전사지용 청색안료로써 이용되고 있다. 본 연구실에서는 LiOH.H2O, Al(OH)3, MnO2 등의 분말을 출발원료로 하고 24$0^{\circ}C$ 온도 부근 그리고 물을 수열용매로 하여 천연산에 필적하는 (Li,Al)MnO2(OH)2:Co 분말을 인공적으로 합성하였다.

• The Journal of Korean Academy of Prosthodontics
• /
• v.47 no.2
• /
• pp.191-198
• /
• 2009

Statement of problem: Ceramics have been important materials for the restoration of teeth. The demands of patients for tooth-colored restorations and the availability of various dental ceramics has driven the increased use of new types of dental ceramic materials. Improved physical properties of theses materials have expanded its use even in posterior crowns and fixed partial dentures. However, ceramic still has limitation such as low loading capability. This is critical for long-span bridge, because bridge is more subject to tensile force. Purpose: The wire reinforced ceramic was designed to increase the fracture resistance of ceramic restoration. The purpose of this study was to evaluate the fracture resistance of wire reinforced ceramic. Material and methods: Heat pressed ceramic(ingot No.200 : IPS Empress 2, Ivoclar Vivadent, Liechtenstein) and Ni-Cr wire(Alfa Aesar, Johnson Matthey Company, USA) of 0.41 mm diameter were used in this study. Five groups of twelve uniform sized ceramic specimens(width 4 mm, thickness 2 mm, length 15 mm) were fabricated. Each group had different wire arrangement. Wireless ceramic was used as control group. The experimental groups were divided according to wire number and position. One, two and three strands of wires were positioned on the longitudinal axis of specimen. In another experimental group, three strands of wires positioned on the longitudinal axis and five strands of wires positioned on the transverse axis. Three-point bending test was done with universal testing machine(Z020, Zwick, Germany) to compare the flexural modulus, flexural strength, strain at fracture and fracture toughness of each group. Fractured ceramic specimens were cross-sectioned with caborundum disc and grinded with sandpaper to observe interface between ceramic and Ni-Cr wire. The interface between ceramic and Ni-Cr wire was analyzed with scanning electron microscope(JSM-6360, JEOL, Japan) under platinum coating. Results: The results obtained were as follows: 1. The average and standard deviation in flexural modulus, flexural strength and fracture toughness showed no statistical differences between control and experimental groups. However, strain was significantly increased in wire inserted ceramics(P<.001). 2. Control group showed wedge fracture aspects across specimen, while experimental groups showed cracks across specimen. 3. Scanning electron microscopic image of cross-sectioned and longitudinally-sectioned specimens showed no gap at the interface between ceramic and Ni-Cr wire. Conclusion: The results of this study showed that wire inserted ceramics have a high strain characteristic. However, wire inserted ceramics was not enough to use at posterior area of mouth in relation to flexural modulus and flexural strength. Therefore, we need further studies.

• Journal of Dental Rehabilitation and Applied Science
• /
• v.27 no.2
• /
• pp.197-207
• /
• 2011

The study aimed at examining how different reline resins affect flexural strength and flexural modulus of denture base. A total of 80 specimens ($64{\times}10{\times}3.3$ mm, according to ISO 1567:1999) of heat-polymerized resin, 40 specimens for (Lucitone199(Dentsply Int., NewYork, USA), SR Ivocap(Ivoclar AG, Schaan, Liechtenstein)) respectively, were polymerized according to the manufacturer's instructions and divided into eight groups(n = 10). Control group specimens remained intact. Specimens in the other groups were abraded on both sides to 2 mm thickness, and were relined in 1.3 mm thickness with 3 types of resins (Lucitone199(Dentsply), SR Ivocap(Ivoclar), and Rebase II(Tokuyama Co., Ltd, Tokyo, Japan)). All specimens were preserved in distilled water at $37^{\circ}C$ for 50 hours, and then were subjected to flexural strength testing in a universal testing machine using 3-point loading. A crosshead speed of 5 mm/min was used, and the distance between the supports was 50 mm. Data analyses included one-way analysis of variance(ANOVA) and the Tukey Honestly Significant Difference test (p=.05). Both heat-polymerized resin groups and auto-polymerized resin groups showed statistically low flexural strength and flexural modulus than control groups. Specimens relined with Lucitone 199 showed significantly higher flexural strength and flexural modulus than those relined with SR-Ivocap. Specimens relined with auto-polymerized resin showed significantly lower flexural strength and flexural modulus than those relined with heat-polymerized resin. Relining with heat-polymerized resins showed superior mechanical properties to relining with an auto-polymerized resin. Relining with the same heat-polymerized resin as the denture base does not affect mechanical properties of a denture. Lucitone199 using a compression-mould technique resulted in the highest flexural strength.

• Restorative Dentistry and Endodontics
• /
• v.34 no.2
• /
• pp.130-136
• /
• 2009

The aim of this study was to develop a method for measuring the slumping resistance of flowable resin composites and to evaluate the efficacy using rheological methodology. Five commercial flowable composites (Aelitefil flow:AF, Filtek flow:FF, DenFil flow:DF, Tetric flow:TF and Revolution:RV) were used. Same volume of composites in a syringe was extruded on a glass slide using a custom-made loading device. The resin composites were allowed to slump for 10 seconds at $25^{\circ}C$ and light cured. The aspect ratio (height/diameter) of cone or dome shaped specimen was measured for estimating the slumping tendency of composites. The complex viscosity of each composite was measured by a dynamic oscillatory shear test as a function of angular frequency using a rheometer. To compare the slumping tendency of composites, one way-ANOVA and Turkey's post hoc test was performed for the aspect ratio at 95% confidence level. Regression analysis was performed to investigate the relationship between the complex viscosity and the aspect ratio. The results were as follows. 1. Slumping tendency based on the aspect ratio varied among the five materials (AF

• Korean Journal of Soil Science and Fertilizer
• /
• v.45 no.2
• /
• pp.293-300
• /
• 2012

This study was to investigate the unsuitable rate of the storage facilities, the changes in corrosion process over time after installation according to the status, the time to install the facilities, years elapsed after facilities installation, inspection of methods and motivation, and so on, based on the results of the inspection at the petroleum storage facilities conducted by domestic soil-relate specialized agency to derive optimal management plans which meet the status of soil contamination facilities. The results showed that the facilities more than 5 years after the initial leak test at the time of the installation need to be inspected periodically by considering costs of leak test and remediation of polluted soil. The inspection period can be decided by cost and leak test methods showing discrepancies for the results obtained from individual test whether it was direct or indirect. To compensate these matters, we suggested that the direct inspection method on regular schedule is recommended. On the other hand, the inspection can be voluntarily completed to ease burden of the results by inspection or equivalent level to this inspection method. Also, it may need improved construction supervision and performance test system to minimize the occurrence of the nature defects in installing the facilities as well as the upgrade program for the facilities during intervals of inspection period.

• Restorative Dentistry and Endodontics
• /
• v.24 no.1
• /
• pp.166-179
• /
• 1999

Apical sealing is essential for the success of surgical endodontic treatment. Root-end cavity is apt to be contaminated with moisture or blood, and is not always easy to be dried completely. The purpose of this study was to evaluate the influence of dry methods of retrocavity on the apical seal in endodontic surgery. Apical seal was investigated through the evaluation of apical leakage and adaptation of filling material over the cavity wall. To investigate the influence of various dry methods on the apical leakage, 125 palatal roots of extracted human maxillary molar teeth were used. The clinical crown of each tooth was removed at 10 mm from the root apex using a slow-speed diamond saw and water spray. Root canals of the all the specimens were prepared with step-back technique and filled with gutta-percha by lateral condensation method. After removing of the coronal 2 mm of filling material, the access cavities were closed with Cavit$^{(R)}$. Two coats of nail polish were applied to the external surface of each root. Apical three millimeters of each root was resected perpendicular to the long axis of the root with a diamond saw. Class I retrograde cavities were prepared with ultrasonic instruments. Retrocavities were washed with physiologic saline solution and dried with various methods or contaminated with human blood. Retrocavities were filled either with IRM, Super EBA or composite resin. All the specimens were immersed in 2% methylene blue solution for 7 days in an incubator at $37^{\circ}C$. The teeth were dissolved in 14 ml of 35% nitric acid solution and the dye present within the root canal system was returned to solution. The leakage of dye was quantitatively measured via spectrophotometric method. The obtained data were analysed statistically using one-way ANOVA and Duncan's Multiple Range Test. To evaluate the influence of various dry methods on the adaptation of filling material over the cavity wall, 12 palatal roots of extracted human maxillary molar teeth were used. After all the roots were prepared and filled, and retrograde cavities were made and filled as above, roots were sectioned longitudinally. Filling-dentin interface of cut surfaces were examined by scanning electron microscope. The results were as follows: 1. Cavities dried with paper point or compressed air showed less leakage than those dried with cotton pellet in Super EBA filled cavity (p<0.05). However, there was no difference between paper point- and compressed air-dried cavities. 2. When cavities were dried with compressed air, dentin-bonded composite resin-filled cavities showed less apical leakage than IRM- or Super EBA-filled ones (p<0.05). 3. Regardless of the filling material, cavities contaminated with human blood showed significantly more apical leakage than those dried with compressed air after saline irrigation (p<0.05). 4. Outer half of the cavity showed larger dentin-filling interface gap than inner half did when cavities were filled with IRM or Super EBA. 5. In all the filling material groups, cavities contaminated with blood or dried with cotton pellets only showed larger defects at the base of the cavity than ones dried with paper points or compressed air.