• The Journal of Advanced Prosthodontics
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• v.5 no.2
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• pp.98-103
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• 2013

PURPOSE. To evaluate the effects of hydrofluoric acid etching and Er,Cr:YSGG laser irradiation on the shear bond strength of resin cement to lithium disilicate ceramic. MATERIALS AND METHODS. Fifty-five ceramic blocks ($5mm{\times}5mm{\times}2mm$) were fabricated and embedded in acrylic resin. Their surfaces were finished with 1000-grit silicon carbide paper. The blocks were assigned to five groups: 1) 9.5% hydrofluoric-acid etching for 60 s; 2-4), 1.5-, 2.5-, and 6-W Er,Cr:YSGG laser applications for 60 seconds, respectively; and 5) no treatment (control). One specimen from each group was examined using scanning electron microscopy. Ceramic primer (Rely X ceramic primer) and adhesive (Adper Single Bond) were applied to the ceramic surfaces, followed by resin cement to bond the composite cylinders, and light curing. Bonded specimens were stored in distilled water at $37^{\circ}C$ for 24 hours. Shear bond strengths were determined by a universal testing machine at 1 mm/min crosshead speed. Data were analyzed using Kruskal-Wallis and Mann-Whitney U-tests (${\alpha}$=0.05). RESULTS. Adhesion was significantly stronger in Group 2 ($3.88{\pm}1.94$ MPa) and Group 3 ($3.65{\pm}1.87$ MPa) than in Control group ($1.95{\pm}1.06$ MPa), in which bonding values were lowest (P<.01). No significant difference was observed between Group 4 ($3.59{\pm}1.19$ MPa) and Control group. Shear bond strength was highest in Group 1 ($8.42{\pm}1.86$ MPa; P<.01). CONCLUSION. Er,Cr:YSGG laser irradiation at 1.5 and 2.5 W increased shear bond strengths between ceramic and resin cement compared with untreated ceramic surfaces. Irradiation at 6 W may not be an efficient ceramic surface treatment technique.

• Journal of the Korean Vacuum Society
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• v.18 no.2
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• pp.85-91
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• 2009

There has been a rapid progress for flexible polymer-based MEMS(Microelectromechanical Systems) technology. Polycarbonate (PC) and Poly Methyl Methacrylate (PMMA), so-called acrylic, have many advantages for optical, non-toxic and micro-device application. We studied dry etching of PC and PMMA as a function of % gas ratio in the $O_2/SF_6/CH_4$ temary plasma. A photoresist pattern was defined on the polymer samples with a mask using a conventional lithography. Plasma etching was done at 100 W RIE chuck power and 10 sccm total gas flow rate. The etch rates of PMMA were typically 2 times higher than those of PC in the whole experimental range. The result would be related to higher melting point of PC compared to that of PMMA. The highest etch rates of PMMA and PC were found in the $O_2/SF_6$ discharges among $O_2/SF_6$, $O_2/CH_4$ and $SF_6/CH_4$ and $O_2/SF_6/CH_4$ plasma composition (PC: ${\sim}350\;nm/min$ at 5 sccm $O_2/5$ sccm $SF_6$, PMMA: ${\sim}570\;nm/min$ at 2.5 sccm $O_2/7.5$ sccm $SF_6$). PC has smoother surface morphology than PMMA after etching in the $O_2/SF_6/CH_4$ discharges. The surface roughness of PC was in the range of 1.9$\sim$3.88 nm. However, that of PMMA was 17.3$\sim$26.1 nm.

• The Journal of Korean Academy of Prosthodontics
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• v.46 no.5
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• pp.535-543
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• 2008

Purpose: The objective of this study was to compare the bonding characteristics of a new self-adhesive resin cement to dentin, which does not require bonding and conditioning procedure of the tooth surface, and conventional resin cement. The effect of phosphoric acid etching prior to application of self-adhesive resin cement on the shear bond strength was also evaluated. Material and methods: Fortyfive non-carious human adult molars extracted within 6 months were embedded in chemically cured acrylic resin. The teeth were ground with a series of SiC-papers ending with 800 grit until the flat dentin surfaces of the teeth were exposed. The teeth were randomly divided into 3 experimental groups. In group 1, self-adhesive resin cement, RelyX Unicem (3M ESPE, Seefeld, Germany) was bonded without any conditioning of teeth. In group 2, RelyX Unicem was bonded to teeth after phosphoric acid etching. For group 3, Syntac Primer (Ivoclar Vivadent AG, Schaan, Liechtenstein) was applied to the teeth before Syntac adhesive (Ivoclar Vivadent AG, Schaan, Liechtenstein) and Helibond (Ivoclar Vivadent AG, Schaan, Liechtenstein) followed by conventional resin cement, Variolink II (Ivoclar Vivadent AG, Schaan, Liechtenstein). To make a shear bond strength test model, a plastic tuble (3 mm diameter, 3 mm height) was applied to the dentin surfaces at a right angle and filled it with respective resin cement, and light-polymerized for 40 seconds. All the specimens were stored in distilled water at $37^{\circ}C$ for 24 hours before test. Universal Testing Machine (Z020, Zwick, Ulm, Germany) at a cross head speed of 1 mm/min was used to evaluate the shear bond strength. The failure sites were inspected under a magnifier and Scanning Electron Microscope. The data was analyzed with One way ANOVA and Scheffe test at ${\alpha}$= 0.05. Results: (1) The shear bond strengths to dentin of RelyX Unicem was not significantly different from those of Variolink II/Syntac. (2) Phosphoric acid etching lowered the shear bond strength of RelyX Unicem significantly. (3) Most of RelyX Unicem and Variolink II showed mixed fractures, while all the specimens of RelyX Unicem with phosphoric acid etching demonstrated adhesive failure between dentin and resin cement. Conclusion: Shear bond strength to dentin of self-adhesive resin cement is not significantly different from conventional resin cement, and phosphoric acid etching decrease the shear bond strength to dentin of self-adhesive resin cement.

• Restorative Dentistry and Endodontics
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• v.12 no.2
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• pp.45-53
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• 1987

The purpose of this study was to evaluate the tensile bond strength between composite resin and the human enamel. Three composite resin systems, two chemical (Clearfil Posterior, and Clearfil Posterior-3) and one light cure (Photo Clearfil-A), used with and without an intermediate resin (clearfil bonding agent), were evaluated under different amounts of load (10g, 200g and 200g for a moment) for in vitro tensile bond strength to acid-eched human enamel. Clinically intact buccal or lingual surfaces of 144 freshly extracted human permanent molars, embedded in acrylic were flattened with No #600 carborundum discs. Samples were randomly assigned to the different materials and treatments using a table of random numbers. Eight samples were thus prepared for each group(Table 2) these surfaces were etched with an acid etchant (Kurarey Co. Japan) in a mode of etching for 30 seconds, washing for 15 seconds, and drying for 30-seconds. During the polymerization of composite resin on the acid-etched enamel surfaces with and without bonding agent 10-gram, 200 gram and temporary 200 gram of load were applied. The specimens were stored in 50% relation humidity at $37^{\circ}C$ for 24 hours before testing. An universal Testing machine (Intesco model No. 2010, Tokyo, Japan) was used to apply tensile loads in the vertical directed (fig 5), and the force required for separation was recorded with a cross head speed of 0.25 mm/min and 20 kg in full scale. The results were as follow: 1. The tensile bond strength was much greater in applying a bonding agent than in not doing that. 2. The tensile bond strength of chemical cure composite resin was higher than that of light cure composite resin with applying on bonding agent on the acid-etched enamel. 3. In case of not applying a bonding agents on the acid-etching enamel, the highest tensile bond strength under 200 gram of load was measured in light cure composite resin. 4. The tensile bond strength under 200-gram of load has no relation with applying the bonding agent. 5. Under the load of 10-gram, There was significant difference in tensile bond strength as applying the bonding agent.

• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.242-253
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• 1996

Penetration degree of several dyes into dentinal tubules in vivo was compared with in vitro, and experimental sensitivity of those dyes was investigated in 64 canines of 16 cats. Dentin 1mm below cusp tip was exposed by cross-sectioning with diamond disc. Pulp of 32 canines were extirpated through cervical cavities. In the presence of smear layer or after add-etching with 37% phosphoric acid to the exposed dentin surface, acrylic collar and resin cap was attached to keep dyes. 52 mmol/$\ell$ Evans' blue, 2% Methylene blue, 10 % Silver nitrate and 5% Fluorescene were then applicated on each 4 canines respectively for 30 minutes. After rinsing, the canines were ground-sectioned longitudinally and linear dye penetration was measured under microscope. The results obtained were as follows ; 1. Evans' blue and Methylene blue penetrated significantly(P<0.05) more in vitro than in vivo only in the cases that exposed dentin surfaces were not etched with acid. 2. Silver nitrate penetrated significantly(P<0.05) more in vitro than in vivo in both cases that exposed dentin surfaces remained intact and were etched with acid. 3. The penetration degree of Fluorescene did not show statistical significance between in vivo and in vitro or in acid-etched and in not acid-etched cases.

• Analytical Science and Technology
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• v.19 no.5
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• pp.394-399
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• 2006

The polishing performance and the relationships of electrochemistry depending upon oxidizers and additives in the tungsten CMP slurry used in semiconductor industry were investigated. Hydrogen peroxide, ferric nitrate and potassium iodate were used as oxidizers and they showed different oxidation reactions on tungsten film depending on the kind of oxidizers and pH of slurry. The differences influenced the polishing performance. Etching reaction was predominated in the hydrogen peroxide. However, passivation reaction was prevailed in ferric nitrate and potassium iodate. TMAH and KOH raised the potential energy and removal rate of tungsten, and improved a dispersion characteristic of slurry by increasing absolute value of zeta potential. Addition of 100 ppm of poly(acrylic acid) of M.W. 250,000 improved dispersion ability.

• The Journal of Korean Academy of Prosthodontics
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• v.52 no.1
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• pp.1-8
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• 2014

Purpose: The purpose of this study is to evaluate the effect of applying Silano-pen to feldspathic porcelain and zirconia on shear bond strength with composite resin. Materials and methods: Feldspathic porcelain and zirconia specimens were produced into 30 per each 2 mm thick and 12 mm in diameter and their surface was made smooth and even and then embedded in acrylic resin. The specimens were divided into each Group F (Feldspathic porcelain) and Group Z (Zirconia), (1) Hydrofluoric acid etching and silane (F1 & Z1), (2) Silano-pen and silane (F2 & Z2), (3) Hydrofluoric acid etching and Silano-pen, silane (F3 & Z3). After surface conditioning, substrate surfaces of the specimen were examined by SEM. Composite resin cylinders (2 mm high, 3 mm in diameter)were bonded to specimen and shear bond strength between ceramic and composite resin was measured by using universal testing machine. The measured values were statistically analyzed by using two way ANOVA and Tukey's multiple comparison test (${\alpha}=.05$). Results: In the scanning electron micrograph of the treated ceramic surface, Group F2 and F3 appeared the high roughness and Group Z3 appeared the highest density of silica particle. In Feldspathic porcelain, the result of measuring shear bond strength showed that Group F3 was measured to be highest and Group F1 was measured to be lowest but there was no statistical significance among Groups. In zirconia, Group Z3 was measured to be highest and Group Z1 was measured to be lowest and there was statistical significance among Groups (P<.05). Conclusion: In zirconia, applying hydrofluoric acid etching and then Silano-pen and silane is effective for composite resin adhesion.

• Restorative Dentistry and Endodontics
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• v.24 no.1
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• pp.156-165
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• 1999

The purpose of this study was to evaluate the effect of surface treatments on the shear bond strength between new and old composites. Circular cavities prepared on the center of acrylic resin mold and the prepared cavities were filled with composite resin. They randomly assigned into control group and 8 groups according to the difference in surface treatments of old composites; Control group: no surface treatment, Group 1: surface treated with #120 SiC paper & bonding agent, Group 2: surface treated with #400 SiC paper & bonding agent, Group 3: surface treated with #120 SiC paper, 32% $H_3PO_4$ & bonding agent, Group 4: surface treated with #400 SiC paper, 32% $H_3PO_4$ & bonding agent, Group 5: surface treated with #120 SiC paper, primer & bonding agent, Group 6: surface treated with #400 SiC paper, primer & bonding agent, Group 7: surface treated with #120 SiC paper, 32% $H_3PO_4$, primer & bonding agent, Group 8: surface treated with #400 SiC paper, 32% $H_3PO_4$, primer & bonding agent. New composites were applicated on the old composites of experimental groups. The shear bond strengths for the experimental specimen were measured and the results were analyzed by using one way ANOVA. The observations of surface morphology after SiC paper roughening and debonded surface morphology after shear bond strength test were done by SEM. The results were as follows; 1. Shear bond strengths for specimens roughened with #120 SiC paper matching with the particle size of coarse diamond bur were significantly higher than those for the specimens with #400 SiC paper(P<0.05). By SEM, the surface of the specimens roughened with #120 SiC paper was more irregular than the specimens with #400 SiC paper. 2. Shear bond strengths for specimens treated with 32% $H_3PO_4$ etchant, primer, bonding resin were significantly higher than those for specimens treated with 32% $H_3PO_4$ and bonding resin(P<0.05). 3. Shear bond strengths for the specimens treated with 32% $H_3PO_4$ etchant and bonding resin were significantly higher than those for specimens treated with only bonding resin(P<0.05). There was no remarkable change of surface morphology after 32% $H_3PO_4$ etching. 4. It was possible to observe mixed fracture patterns (the cohesive fracture of old composite and the adhesive fracture between old and new composite) in the specimens roughened with #120 SiC paper, but almost adhesive fracture in the specimens roughened with #400 SiC paper.

• Polymer(Korea)
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• v.37 no.3
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• pp.373-378
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• 2013

The interfacial adhesion strength is very important in $SiO_x$ deposited PC film for the barrier enhanced polycarbonate (PC) flexible substrate. In this study, PC films were treated by undercoating, UV/$O_3$ and low temperature plasma and then the effect of physical and chemical surface modifications on the interfacial adhesion strength between PC film and $SiO_x$ barrier layer were studied. It was found that untreated PC film shows significantly low interfacial adhesion strength due to the smooth surface and low surface free energy of PC. Low temperature plasma treatments resulted in the increase of both surface roughness and surface free energy due to etching and the appearance of polar molecules on the PC surface. However, UV/$O_3$ treatment only shows the increase of surface free energy by developed polar molecules on the surface. These surface modifications caused the enhancement of surface interfacial strength between PC film and $SiO_x$ barrier. In the case of undercoating, it was found that the increase of surface interfacial strength was achieved by adhesion between various acrylic acid on acrylate coated surface and $SiO_x$ without increase of polar surface energy. In addition, the barrier property is also improved by organic-inorganic hybrid multilayer structure.

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.4
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• pp.426-437
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• 2005

Statement of problem : Although zirconium oxide ceramics are more and more commonly used in restorative dentistry, for many clinical applications only limited data can be found in the literature. However it is quite clear that hydrofluoric acid etching is impossible with zirconia ceramics. Therefore, other bonding techniques are required in order to lute these materials adhesively. Purpose : The purpose or this study was to evaluate the effects of surface treatments on shear bond strengths between two resin cements and a zirconia ceramic. Materials and methods : Experimental industrially manufactured yttrium-oxide-partially-stabilized zirconia ceramic discs (Adens, Korea) were used for this study. The ceramic specimens divided into five experimental groups and a control group (as received). Five surface treatments were studied 1) sandblasting with 110$\mu$m $Al_2O_3$ at 3 bars pressure 13 seconds at a distance of 10 mm, 2) flame-treated with the Silano-Pen for 5 $s/cm^3$, 3) grinding with a diamond bur. 4) sandblasting + Silano-Pen treatment, 5) diamond bur preparation + Silano-Pen treatment. Acrylic plastic tube (5 mm in height and 3 mm in diameter) were filled with composite to fabricate composite cylinders The composite cylinders were bonded to the ceramic specimens with either Superbond C&B or Panavia F resin luting agents. All cemented specimens were tested under shear loading until fracture on universal testing machine at a crosshead speed 1mm/min; the maximum load at fracture was recorded. Sheat bond strength data were analyzed with oneway analysis of variance and Tukey HSD tests (P<.05). Treated ceramic surfaces and fracture surfaces after shear testing were examined morphologically using scanning electron microscope. Results: Ceramic surface treatment with Silano-Pen after sandblasting improved the bond strength of Superbond C&B resin cement. Supevbond C& B resin cement at Silano-Pen aiker sandblasting($27.4{\pm}3.8MPa$) showed statistically higher shear bond strength than the others. Conclusion: Within the limitation of this study, Superbond C& &B resin cement are suitable for cementation of zirconia ceramics and flame-treated with the Silano-Pen after sandblasting is required to enhance the bond strength.