• Journal of the Semiconductor & Display Technology
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• v.13 no.3
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• pp.13-19
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• 2014

Phosphoric acid was used as etching agent instead of conventional peroxide - based chemicals for forming pattern of ultra definition display. Etchant was synthesized by mixing etching agent, oxidation agent, buffer solution, and additive into solvent, deionized water. Thicknesses of copper, main metal of ultra definition display, for etching, were 10,000 and $30,000{{\AA}}$. Etch stop of good low skew for proper pattern formation has been occurred at the content ratio of phosphoric acid 60 - 64%, nitric acid 4 - 5%, additive(potassium acetate) 1 - 3%. Buffer solution(acetic acid) decreased the metal contact angle $63.07^{\circ}$ to $42.49^{\circ}$ for benefiting pattern formation. Content variations on four components (phosphoric acid, nitric acid, acetic acid, potassium acetic acid) of the etchant with storage time were within 3 wt% after 24 hrs of etching work.

• Restorative Dentistry and Endodontics
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• v.6 no.1
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• pp.37-50
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• 1980

Scanning Electron Microscopic (SEM) examination on the labial surface of 91 permanent upper incisors were made after etching procedure with phosphoric acid, sulfuric acid, nitric acid, hydro chloric acid, oxalic acid, formic acid, citric acid and zinc phosphate liquid for 2 minutes. Following results were obtained. 1. In the surfaces etched by 10%. 50% phosphoric acid, 50% sulfuric acid, 10%. 30% nitric acid, 10%. 50% oxalic acid, 10%. 30%. 50% formic acid, 30%. 50% citric acid and zinc phosphate liquid, there appeared to be a preferential removal of prism cores, but in the surfaces etched by 10% phosphoric acid, 50% nitric acid, 10%. 30% hydrochloric acid and 30% oxalic acid, the prism peripheries were removed preferentially. 2. According to Silverstone classification on enamel etching pattern the surface treated by zinc phosphate liquid, 30. 50% citric acid, 10%. 30%. 50% formic acid, 10%. 50% oxalic acid, 10%. 30% nitric acid, 50% sulfuric acid and 10%. 50%. phosphoric acid showed Type 1, and etched by 30% oxalic acid, 10%. 30% hydrochloric acid, 50% nitric acid and 10% phosphoric acid showed Type II. Etching of prism cores was by far the most common occurence. The changes produced could be related to intrinsic differences in histology and / or solubility of enamel.

• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.136-149
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• 1996

The effects of various All-Etching Agents (10% phosphoric acid, 10% maleic acid and 10 % citric acid) and 32 % phosphoric acid and varied etching time were evaluated by observing the morphology of the etched enamel surfaces using Scanning electron microscopy and by measuring the shear bond strength of a composite resin to human enamel. A total of 156 extracted premolar and molar teeth free of irregularities were employed in this study. Specimens for the observation of enamel morphology were divided into 12 groups of 3 teeth each, based on the type of etchant used and application time. After exposure to the etching agent specimens were washed air-dried and then glued to aluminum stubs and coated with a layer of gold for examination in the scanning electron microscope. Specimens for the evaluation of bond strength were divided into 12 groups of 10 teeth each also based on the type of etchant used and application time. After exposure to the etching agent the specimens were washed, air-dried and a thin layer of bonding agent was applied using a brush. Z 100 composite resin was light cured to the surface and stored at $37^{\circ}C$, 100% humidity for 7 days. An Instron Universal Testing Machine was used to apply a shearing force at $90^{\circ}$ angle from the enamel surface. It is concluded from this study that commercial All-etching agents can be used with a 15-second etching without adversely affecting retention of dental resin materials. At the same time, the acid concentration is probably a suitable compromise regarding the acid's function as a dentin demineralizing all-etch conditioning agent. The following results were obtained. 1. Specimens etched with 10 % citric acid showed a random superficial etching pattern which could not be related to prism morphology. 2. Specimens etched with 10 % and 32 % phosphoric acid and 10 % maleic acid showed a type I pattern in which core material was preferentially removed leaving the prism peripheries relatively intact or a type II pattern in which prism peripheries were preferentially removed. This delineation became more distinguished as etching time was increased. 3. All-Etching Agents and 32 % phosphoric acid showed a statistically significant higher shear bond strength at 15 seconds etching time.(p<0.05) 4. 10 % maleic acid and 32 % phosphoric acid exhibited a statistically significant higher shear bond strength than 10 % phosphoric and citric acid at 15 seconds etching time.(p<0.05).

• Journal of the korean academy of Pediatric Dentistry
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• v.10 no.1
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• pp.85-93
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• 1983

In one group that tested for the effects of grinding and etching on the deciduous teeth, S.E.M. examination on the ground or unground labial surface of deciduous maxillary central incisors were made after etching procedure with 40% phosphoric acid for 60 secs., 120 secs., 180 sees. each. In another group that tested for the degree of resin penetration to the ground and etched deciduous teeth, composite resin application was done to the ground deciduous maxillary central incisors that had been acid-etched for 30 secs., 60 secs., 90 sees., 120 sees., 180 secs. each. The tooth-resin specimens were cut at the middle 1/3 of the crown by 2mm thickness, and the adjacent tooth materials were demineralized by 10% hydrochloric acid, the author observed the tags of the resin replica with S.E.M.. Following results were obtained. 1. After 40% phosphoric acid etching, the unground deciduous enamel surface showed various types of etching pattern. 2. For the formation of regular micropores on deciduous enamel surface by acid etching with 40% phosphoric acid, the time over 120 secs. should be requested. 3. After 40% phosphoric acid etching, the ground deciduous enamel surface showed the same etching pattern that has been a preferential removal of prism peripheries despite different etching time. 4. On the ground group that etched over 60 secs. to 180 secs., the length of tags was $5{\mu}m$ to $8{\mu}m$, with a mean of $7{\mu}m$.

• The korean journal of orthodontics
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• v.43 no.1
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• pp.23-28
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• 2013

Objective: The purpose of this study was to evaluate the effect of casein phosphopeptide amorphous calcium phosphate (CPP-ACP) on the shear bond strength (SBS) of brackets bonded to non-demineralized teeth with either phosphoric acid etching or self-etching primer. Methods: Sixty human premolars were randomly assigned to 1 of 4 treatment groups (n = 15 each): phosphoric acid etching (group 1); self-etching primer (group 2); CPP-ACP for 2 weeks + phosphoric acid etching (group 3), and CPP-ACP for 2 weeks + self-etching primer (group 4). After bonding of the maxillary premolar metal brackets, specimens were subjected to shear forces in a testing machine. Scanning electron microscopy was used to observe etching patterns on the enamel surfaces of all teeth. A 2-way analysis of variance was used to test for effects of CPP-ACP and etching system on SBS. Results: Significantly higher mean SBSs were observed in groups subjected to phosphoric acid etching (i.e., groups 1 and 3; p < 0.05). On the other hand, SBSs did not appear to be influenced by CPP-ACP (i.e., groups 3 and 4; p > 0.05). We observed a uniform and clear etched pattern on the enamel surface of the phosphoric acid etching groups. Conclusions: CPP-ACP does not significantly affect the SBS of orthodontic brackets bonded to non-demineralized teeth, regardless of which adhesive method is used to bond the brackets.

• Restorative Dentistry and Endodontics
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• v.28 no.5
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• pp.363-368
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• 2003

The purpose of this study is to evaluate the effect of additional enamel etching with phosphoric acid on the microleakage of the adhesion of self-etching primer system. Class V cavity($4mm{\times}3mm{\times}1.5mm$) preparations with all margins in enamel were prepared on buccal surface of 42 extracted human upper central incisor teeth. Prepared teeth were randomly divided into 3 groups. Group 1：no additional pretreatment with 37% phosphoric acid (NE). Group 2：additional pretreatment with 37% phosphoric acid for 10 seconds (E10s). Group 3：additional pretreatment with 37% phosphoric acid for 20 seconds (E20s). The adhesives(Clearfil SE $Bond^{\circledR}$, Kuraray, Osaka, Japan) and composite resins(Clearfil $AP-X^{\circledR}$, Osaka, Kuraray, Japan) were applied following the manufacturer's instructions. All the specimens were finished with the polishing disc(3M dental product, St Paul, MN, USA), thermocycled for 500 cycles between $5^{\circ}C$ and $55^{\circ}C$ and resected apical 3-mm root. 0.028 stainless steel wire was inserted apically into the pulp chamber of each tooth and sealed into position with sticky wax. Surrounding tooth surface was covered with a nail varnish 2 times except areas 1mm far from all the margins. After drying for one day, soaked the samples in the distilled water. Microleakage was assessed by electrochemical method(System 6514, $Electrometer^{\circledR}$), Keithley, USA) in the distilled water. In this study, the microleakage was the lowest in group 1 (NE) and the highest in group 3(E20s)(NE

• Restorative Dentistry and Endodontics
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• v.21 no.2
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• pp.602-618
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• 1996

The purpose of this study was to investigate the effect of acid treatment of fluoride applied dentin surface with various concentrations of phosphoric acid for various periods of time on dentin bonding. Dentin specimens prepared from freshly extracted bovine mandibular anterior teeth were divided into fluoridated and nonfluoridated groups. Specimens of nonfluoridated group were pretreated with 10% phosphoric acid for 15 seconds. Those of fluoridated groups were treated with 2% sodium fluoride or 2% stannous fluoride solution for 5 minutes and stored in $37^{\circ}C$ distilled water for 3 days, followed by phosphoric acid treatment. The concentrations of phosphoric acid were 10%, 32% or 50% and the treatment periods of time were 15, 30 or 60 seconds. All the specimens were bonded with All Bond$^{(R)}$ 2 and Bisfil$^{TM}$ composite resin. After bonded specimens were stored in $37^{\circ}C$ distilled water for 24 hours, tensile bond strengths of each specimens were measured and the pretreated dentin and the fractured dentin surfaces were examined under the scanning electron microscope. The results were as follows : The tensile bond strengths from the fluoridated groups were significantly lower than those from the nonfluoridated group when the concentrations of phosphoric acid and the treatment periods of time were equal in all the groups (p<0.05). In general, the higher the concentration of phosphoric acid and the longer the treatment period of time for acid etching on the fluoride applied dentin surface, the higher were the bond strength values. Recovery of bond strength of the dentin bonding agent was better in the NaF applied group than in the $SnF_2$ applied one. SEM findings of NaF applied and $SnF_2$ applied dentin surfaces demonstrated reaction product-covered and partially or completely obstructed dentinal tubules. SEM findings of dentin surfaces fluoridated for 5 minutes followed by etching showed wider tubular openings and more clean dentin surfaces when dentin was etched with higher concentration of phosphoric acid for longer period of time. On the SEM observations of the fractured dentin-resin interface, the etched specimens of fluoridated group showed an adhesive failure mode when the concentration of phosphoric acid and the treatment period of time were same as in the nonfluoridated group. As the concentration of phosphoric acid and the treatment period of time increase during acid etching, the cohesive failure area increased. However, excessive acid etching caused adhesive failure.

• Journal of the Korean institute of surface engineering
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• v.47 no.3
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• pp.128-136
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• 2014

In the present study, we successfully developed an eco-friendly chemical etching solution and proper condition for plating on ABS material. The mechanism of forming Ni plating layer on ABS substrate is known as following. In general, the etching solution used for the etching process is a solution of chromic acid and sulfuric acid. The etching solution is given to the surface resulting in elution of butadiene group, so-called anchor effect. Such a rough surface can easily adsorb catalyst resulting in the increase of adhesion between ABS substrate and Ni plating layer. However a use of chromic acid is harmful to environment. It is, therefore, essential to develop a new alternative solution. In the present study, we proposed an eco-friendly etching solution composed of potassium permanganate, sulfuric acid and phosphoric acid. This solution was testified to observe the surface microstructure and the pore size of electrical Ni plating layer, and the adhesive correlation between deposited layers fabricated by electro Ni plating was confirmed. The result of the present study, the newly developed, eco-friendly etching solution, which is a mixture of potassium permanganate 25 g/L, sulfuric acid 650ml/L and phosphoric acid 250ml/L, has a similar etching effect and adhesion property, compared with the commercially used chromium acid solution in the condition at $70^{\circ}C$ for 5 min.

• Bulletin of the Korean Chemical Society
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• v.24 no.11
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• pp.1613-1617
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• 2003

In the phosphoric acid based etchant, the dissolution rates of Mo films were measured by microgravimetry and the corrosion potentials of Mo and Al were estimated by Tafel plot method with various concentrations of nitric acid. Dissolution rate of Mo increased with the nitric acid concentration and reached a limiting value at high concentration of nitric acid in ambient condition. Corrosion potentials of Mo and Al shifted to positive direction and the difference between potentials of both metals was about 1,100 mV and 1,200 mV with 1% and above 4% of $HNO_3$, respectively. For a Mo/Al bilayers, the dissolution rate inversion is the main reason for good taper angle in shower etching process. Taper angles are observed by scanning electron microscope (SEM) after wet etching process for Mo/Al layered films with different concentrations of $HNO_3$. In the etch side profile, it was found that Al corroded faster than Mo below 4% of $HNO_3$ in dip etching process, however, Mo corroded faster above 4%. Trend for variation of taper angle of etched side of Mo/Al layered film can be explained by considering the effect corrosion rates of both metals with various concentrations of $HNO_3$.

• Restorative Dentistry and Endodontics
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• v.34 no.1
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• pp.38-41
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• 2009

When we use the total-etch dentin adhesive system for composite resin restorations, gel or liquid acid etchant such as 37% phosphoric acid is commonly used. Thirty seven percentage phosphoric acid is very powerful erosive agent, and can cause severe harmful effects when it contacts with an oral mucosa and facial skin. This case describes iatrogenic chemical burn on facial skin caused by phosphoric acid which was happened during composite resin restorative procedure. Chemical burn by acid etchant can be evoked by careless handling of remnant and syringe. In order to prevent these iatrogenic injuries, we should check the complete removal of the etching agent both in intra and extra-oral environments after etching and rinsing procedure and it is necessary to use of the rubber dam or isolation instruments. If accidental burn were occurred. immediate wash with copious water. And bring the patient to the dermatologist as soon as possible.