• The Journal of Korean Academy of Prosthodontics
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• v.42 no.3
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• pp.307-326
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• 2004

Statement of problem. The long-term success of implants is the development of a stable direct connection between bone and implant surface, which must be structural and functional. To improve a direct implant fixation to the bone, various strategies have been developed focusing on the surface of materials. Among them, altering the surface properties can modify cellular responses such as cell adhesion, cell motility and bone deposition. Purpose. This study was to evaluate the cellular behaviors on the surface-modified titanium by morphological observation, cellular proliferation and differentiation. Material and methods. Specimens were divided into five groups, depending on their surface treatment: electropolishing(EP) anoclizing(AN), machining(MA), blasting with hydroxyapatite particle(RBM) and electrical discharge machining(EDM). Physicochemical properties and microstructures of the specimens were examined and the responses of osteoblast-like cells were investigated. The microtopography of specimens was observed by scanning electron microscopy(SEM). Surface roughness was measured by a three-dimensional roughness measuring system. The microstructure was analyzed by X-ray diffractometer(XRD) and scanning auger electron microscopy(AES). To evaluate cellular responses to modified titanium surfaces, osteoblasts isolated from neonatal rat were cultured. The cellular morphology and total protein amounts of osteoblast-like cell were taken as the marker for cellular proliferation, while the expression of alkaline phosphatase was used as the early differentiation marker for osteoblast. In addition, the type I collagen production was determined to be a reliable indicator of bone matrix synthesis. Results. 1. Each prepared specimen showed specific microtopography at SEM examination. The RBM group had a rough and irregular pattern with reticulated appearance. The EDM-treated surface had evident cracks and was heterogeneous consisting of broad sheet or plate with smooth edges and clusters of small grains, deep pores or craters. 2. Surface roughness values were, from the lowest to the highest, electropolished group, anodized group, machined group, RBM group and EDM group. 3. All groups showed amorphous structures. Especially anodized group was found to have increased surface oxide thickness and EDM group had titaniumcarbide(TiC) structure. 4. Cells on electropolished, anodized and machined surfaces developed flattened cell shape and cells on RBM appeared spherical and EDM showed both. After 14 days, the cells cultured from all groups were formed to be confluent and exhibited multilayer proliferation, often overlapped or stratified. 5. Total protein amounts were formed to be quite similar among all the group at 48 hours. At 14 days, the electropolished group and the anodized group induced more total protein amount than the RBM group(P<.05). 6. There was no significant difference among five groups for alkaline phosphatase(ALP) activity at 48 hours. The AN group showed significantly higher ALP activity than any other groups at 14 days(P<.05). 7. All the groups showed similar collagen synthesis except the EDM group. The amount of collagen on the electropolished and anodized surfaces were higher than that on the EDM surface(P<.05).

• Journal of Adhesion and Interface
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• v.8 no.1
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• pp.15-27
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• 2007

Polyimide (PI) surface modification was carried out by ion-beam treatment and silane-imidazole coupling agent to improve the adhesion between polyimide film and copper. Silane-imidazole coupling agent contains imidazole functional groups for the formation of a complex with copper metal through a coordination bonding and methoxy silane groups for the formation of siloxane polymers. The PI film surface was first treated by argon (Ar)/oxygen ($O_2$) ion-beam, followed by dipping it into a modified silane-imidazole coupling agent solution. The results of X-ray photoelectron spectroscopy (XPS) spectra revealed that the $Ar/O_2$ plasma treatment formed oxygen functional groups such as hydroxyl and carbonyl groups on the polyimide film surface and confirmed that the PI surface was modified by a coupling reaction with imidazole-silane coupling agent. Adhesion between copper and the treated PI film by ion-beam and coupling agent was superior to that with untreated PI film. In addition, adhesion of PI film treated by an $Ar/O_2$ plasma to copper was better than that of PI film treated by a coupling agent. The peeled-off layers from the copper-PI film joint were completely different in chemical composition each other. The layer of PI film side showed similar C1s, N1s, O1s spectra to the original Upilex-S and no Si and Cu atoms appeared. On the other hand the layer of copper side showed different C1s and N1s spectra from the original PI film and many Si and Cu atoms appeared. This indicates that the failure occurs at an interface between the imidazole-silane and PI film layers rather than within the PI layers.

• The Journal of Korean Academy of Prosthodontics
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• v.45 no.1
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• pp.85-97
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• 2007

Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

• The Journal of Advanced Prosthodontics
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• v.6 no.4
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• pp.295-301
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• 2014

PURPOSE. Numerous methods were used to etch the fiber posts to improve its bonding to root canal dentin. Our aim was to evaluate the efficacy of 37% phosphoric acid in etching fiber posts in comparison with 24% hydrogen peroxide. MATERIALS AND METHODS. Ninety human maxillary central incisors were taken and post space preparation was done. Ninety fiber posts were taken and divided into three groups (n=30) based on the surface treatment they received ($H_3PO_4$, $H_2O_2$, distilled water) and each group was further divided (n=10) based on the time period of application (15 seconds, 30 seconds, 60 seconds). All the posts were luted into canals using Rely X UniCem-2. Each tooth was then sectioned into six slices and subjected to push out test. Data obtained was subjected to statistical analysis at P<.05. The surface topography was evaluated using scanning electron microscopy. RESULTS. Highest bond strength values were noted in 15 seconds etched phosphoric acid group and 60 seconds etched hydrogen peroxide group with no significant difference between two groups. Surface topography revealed complete epoxy layer removal with no damage to its structural integrity in those groups. CONCLUSION. $H_3PO_4$ etching for a period of 15 seconds is an effective alternative in improving the adhesion of fiber post to root dentin.

• The Journal of Advanced Prosthodontics
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• v.6 no.2
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• pp.96-102
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• 2014

PURPOSE. This study was performed to characterize the effects of zirconia coated with calcium phosphate and hydroxyapatite compared to smooth zirconia after bone marrow-derived osteoblast culture. MATERIALS AND METHODS. Bone marrow-derived osteoblasts were cultured on (1) smooth zirconia, (2) zirconia coated with calcium phosphate (CaP), and (3) zirconia coated with hydroxyapatite (HA). The tetrazolium-based colorimetric assay (MTT test) was used for cell proliferation evaluation. Scanning electron microscopy (SEM) and alkaline phosphatase (ALP) activity was measured to evaluate the cellular morphology and differentiation rate. X-ray photoelectron spectroscopy (XPS) was employed for the analysis of surface chemistry. The genetic expression of the osteoblasts and dissolution behavior of the coatings were observed. Assessment of the significance level of the differences between the groups was done with analysis of variance (ANOVA). RESULTS. From the MTT assay, no significant difference between smooth and surface coated zirconia was found (P>.05). From the SEM image, cells on all three groups of discs were sporadically triangular or spread out in shape with formation of filopodia. From the ALP activity assay, the optical density of osteoblasts on smooth zirconia discs was higher than that on surface treated zirconia discs (P>.05). Most of the genes related to cell adhesion showed similar expression level between smooth and surface treated zirconia. The dissolution rate was higher with CaP than HA coating. CONCLUSION. The attachment and growth behavior of bone-marrow-derived osteoblasts cultured on smooth surface coated zirconia showed comparable results. However, the HA coating showed more time-dependent stability compared to the CaP coating.

• Tribology and Lubricants
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• v.37 no.2
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• pp.54-61
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• 2021

The effect of the sand blasting before TiAlN coating in the manufacture of WC hard metal alloy tips have been studied. For four different tips, according to the status of processing of the sand blasting and the coating, residual stress measurement by X-ray diffraction and several tests for mechanical properties have been conducted. The results suggest that there was no difference in static mechanical properties, such as hardness, surface roughness and elastic modulus, between two coatings. Furthermore, compressive residual stress was generated equally on their surfaces. Additionally, the compressive residual stress in substrate WC was found to increase greatly when subjected to sand blasting treatment. However, the compressive residual stress decrease after coating regardless of sand blasting treatment. Nevertheless, it is confirmed that the compressive residual stress generated in the coating after sand blasting is less than that in the non-sandblasting coating. This was attributed to the plastic deformation occurring in the WC substrate during coating after sand blasting. In contrast to the scratch test results, sand blasting was assumed to have a negative effect on the adhesion between the coating and substrate. This is because there is a high possibility of microcracks due to plastic deformation in the WC substrate under the coating after sand blasting.

• Journal of Korean Society for Atmospheric Environment
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• v.20 no.2
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• pp.185-193
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• 2004

A catalyst with CuO ceramic filter for simultaneous treatment of dust and HAP was prepared and characterized. Catalytic ceramic filter can not only potentially achieve the substantial savings in energy but provide with effective optimization and integration of process for simultaneous removal of SO$_2$, NO$_{x}$ and particulates from flue gases. Catalytic ceramic filters remove simultaneously particulates on exterior surface of filters and reduce NO to $N_2$ and $H_2O$ by SCR (Selective Catalytic Reduction) process. Preparation of catalyst impregnated ceramic filter with disk shape (Ψ 50) follow the processing of alumino-silicate ceramic filter, support impregnation and catalyst impregnation (copper oxide). Preparation routes of alumino-silicate catalyst carrier suitable for production of catalytic filters practically were studied and developed using the sol-gel and colloidal processing, homogeneous precipitation and impregnation method. Characterization of the catalyst, catalyst carrier catalytic filter materials have been performed the using various techniques such as BET, XRD, TGA, SEM. Combination of the sol-gel and colloidal processing and impregnation method is recommended to prepare catalyst carriers economically for catalytic filter applications.s.

• Journal of Technologic Dentistry
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• v.27 no.1
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• pp.79-88
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• 2005

This study was performed to investigate the surface properties of electrochemically oxidized pure niobium by anodic oxide and hydrothermal treatment technique. Niobium specimens of $10\times10mm$ in dimension were polished sequentially from #600, #800, #1000 emery paper. The surface pure niobium specimens were anodized in an electrolytic solution that was dissolved calcium and phosphate in water. The electrolytic voltage was set in the range of 250 V and the current density was 10 $mA/cm^2$. The specimen was hydrothermal treated in high-pressure steam at 300$^{\circ}C$ for 2 hours using an autoclave. Then, specimens were immersed in the Hanks' solution with pH 7.4 at 37$^{\circ}C$ for 30 days. The surface of specimen was characterized by scanning electron microscope(SEM), energy dispersive X-ray microanalysis(EDX), potentiostat/galvanostat test, and cytotoxicity test. The results obtained was summarized as follows; According to the result of measuring corrosion behavior at 0.9% NaCl, corrosion resistance was improved more specimens treated with anodic oxide than in hydrothermal treated ones. The multi-porous oxide layer on surface treated through anodic oxidation showed a structure that fine pores overlap one another, and the early precipitation of apatite was observed on the surface of hydrothermal treated samples. According to the result of EDX after 30 days deposition in Hanks' solution, Ca/P was 1.69 in hydrothermal treated specimens. In MTT test, specimens treated through anodic oxidation and hydrothermal treated ones showed spectrophotometer similar to that of the control group. Thus no significant difference in cytotoxicity was observed (P>0.05).

• Food Science and Preservation
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• v.12 no.6
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• pp.552-557
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• 2005

Effect of pre- and post-mild heat treatment on quality of fresh-cut potatoes was investigated with the focus on surface color, firmness, phenolics, vitamin C and sensory characteristics. As the pre-heat treatment before cutting of potatoes, dried hot air (DH) and hot water (WH) treatment were conducted at $45^{\circ}C$ for 60 min, respectively. As a post-heat (CH) treatments, potato cubes were dipped into water of $55^{\circ}C$ for 45 seconds after cutting. The potato cubes were packed in 15 cm x 20 cm LDPE pouches $30^{\mu}m$ thick and then stored at $5{\pm}1^{\circ}C$. The respiration rate of fresh-cut potatoes was decreased by mild heat treatment Especially, the rate of cubes treated with DH was decreased by $20\%$ compared to that of the non-heat treated. L value of cubes treated with DH showed higher value than that of others. Firmness and free phenolics had no significant difference between the treatments. The fresh-cut potatoes prepared with non-heat treatment showed higher vitamin C content than that of the heat treated. In sensory visual color, CH treated cubes marked the best quality. Conclusively, mild heat treatment, especially CH treatment, showed positive effect on browning inhibition and quality enhancement of fresh-cut potatoes.

• Journal of Dental Rehabilitation and Applied Science
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• v.22 no.2
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• pp.125-136
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• 2006

Statement of problem. The success of the bonding between electroforming gold and resin is dependent on the surface-conditioning technique but its effective technique has net been studied widely. Purpose. The purpose of the study was to evaluate the bond strength between the electroforming gold and resin with varying the surface-conditioning technique. Materials and methods. Sixty rectangular shaped metal specimens were made and one side of each specimen were gold hard plated. The sand-blasted specimens were divided into four experimental groups with fifteen specimens in each group and were treated as follows. Group 1: Silicoating (Rocatec, 3M ESPE)+ Sinfony (3M ESPE), Group 2: SR Link+ SR Adoro (Ivoclar Vivadent), Group 3: Tin plating (Microtin, Danville Engineering)+ SR Link+ SR Adoro, Group 4: Tin plating (Micro tin, Danville Engineering)+ Silicoating (Rocatec)+ Sinfony. Shear bond strength at metal-resin interface were measured using universal testing machine. Energy Dispersive x-ray analysis was done and scanning electron microscope images were taken and observed. Results and Conclusion. The following conclusions were drawn. 1. The mean shear bond strength values in order were 11.69MPa (Group 2), 22.35MPa (Group 3), 22.40MPa (Group 1) and 27.71MPa (Group 4). There was no significant difference in Group 1, Group 3 and Group 4(P>0.05). 2. In the EDX line analysis, the Au was detected on the surface of all specimen. $SnO_2$ showed on the surface of Group 2 and $SiO_2$ was detected on the surface of Group 1. 3. Increasing of roughness by sandblasting(Group 2), formation of micro-irregularities and tin crystals by electrolytic tin plating(Group 3) and formation of surface irregularities and $SiO_2$ layer(Group 1,4) were observed in SEM photo. 4. Tin plating(Group 3) and Rocatec treatment(Group 1) showed clinically effective shear bond strength(>20MPa), but when the two surface conditioning method were used together higher bond strength were achieved.