• Restorative Dentistry and Endodontics
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• 제6권1호
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• pp.115-122
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• 1980

The corrosion of silver amalgam is regarded as one of major causes in the failures of dental amalgam restorations. To evaluate the corrosion resistance of dental amalgam alloys, electrochemical tests such as potential and polarization measurement were used widely. But these commonly used methods have not provided the sufficient informations on relative resistance of amalgam to corrosion. In this experiment, the corrosion currents were measured using electronic potentiostat to compare some commercial dental amalgam alloys. All alloys were triturated in a amalgamator and condensed into a mold described in A.D.A. Specification No. 1 to produce cylinder form specimens of 4mm diameter by 5mm long. After specimen kept for 1 week at $37^{\circ}C$, each specimen was embedded in epoxy resin. The surfaces of specimens were then polished with a emery paper, diamond dust, and $Al_2O_3$. These specimens were immersed in artifical saliva kept at $37^{\circ}C$, and currents of each specimen were measured for 24 hours at 0.0volt (SCE). The author obtained conclusions as follows: 1. High copper amalgam showed superior resistance against corrosion to conventional amalgam, but a pellet form of high copper amalgam seemed to be susceptible to corrosion. 2. In lathe-cut alloys, fine-cut had superior resistance against corrosion to regular-cut. 3. Non-zinc conventional amalgam alloys were more resistant to corrosion than that of zinc containing conventional amalgam alloys. 4. In both of high copper and conventional amalgams, predispensed forms tended to have better resisitance to corrosion than that of pellet forms.

• Restorative Dentistry and Endodontics
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• 제16권2호
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• pp.1-17
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• 1991

The purpose of this study was to analyze the in vivo amalgam corrosion products qualitatively. 30 molars with large, intact amalgam restorations were selected. All the restorations were more than 5 years old. Twenty of the removed amalgams were embedded in acrylic resin block. The exposed surfaces of fifteen embedded amalgams were polished by amalgam polishing kit, and the rest were observed without polishing. The remaining 10 amalgams were fractured centrally and perpendiculary to the occlusal surface with a wire-cutter. After all specimens were cleaned ultrasonically in distilled water, each surface was examined under S.E.M. and E.D.A.X. (Energy Dispersive Micro X-ray Analyzer) to determine the morphology and chemical nature of the corrosion products. The following results were obtained: 1. The surfaces of the unpolished amalgam restorations were covered with thin amorphous layer of Sn-Ca-P-S complex with numerous cracks. 2. In the conventional amalgams, the major corrosion products were Sn-Cl phases however, tin oxide phases were also observed. 3. Only tin oxide phase was identified in the high copper amalgam, but it was less frequently observed than in the conventional amalgam. 4. It was easier to observe the corrosion product morphology in the fractured surfaces than in the polished ones. The morphologies of the corrosion product crystals looked like a stack of slightly bended plates in the Sn-Cl phases and polyhedra or polygonal prisms in the tin oxide phases.

• Restorative Dentistry and Endodontics
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• 제19권1호
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• pp.1-26
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• 1994

The purpose of this study was to investigate the dissolution components during corrosion of amalgams and to identify surface corrosion products in the modified Fusayama artificial saliva. Four type of amalgam alloys were used: low copper lathe cut amalgam alloy (Cavex 68), low copper spherical amalgam alloy (Caulk Spherical Alloy), high copper admixed amalgam alloy (Dispersalloy) and high copper single composition amalgam alloy (Tytin). Each amalgam alloy and Hg were triturated according to the manufacturer's direction by means of mechanical amalgamator (Capmaster, S.S.White), and then the triturated mass was inserted into the cylindrical metal mold which was 10mm in diameter and 2.0mm in height and condensed with compression of 150kg/$cm^2$ using oil pressor. The specimens were removed from the mold and stored at room temperature for 7 days and cleansed with distiled water for 30 minutes in an ultrasonic cleaner. The specimens were immersed in the modified Fusayama artificial saliva for the periods of 1 month, 3 months and 6 months. The amounts of Hg, Cu, Sn and Zn dissolved from each amalgam specimen immersed in the artificial saliva for the periods of 1 month, 3 months and 6 months were measured using Inductivity Coupled Plasma Atomic Emission Spectrometry (ICPQ-1000, Shimadzu, Japan) and amount of Ag dissolved from amalgam specimen was measured using Atomic Absorption Spectrophotometry (Atomic Absorption/Flame emission spectrophotometer M-670, Shimadzu, Japan). A surface corrosion products of specimens were analysed using Electron Spectroscopy Chemical Analyser (ESCA PHI-558, PERKIN ELMER, U.S.A.). The secondary image and back scattered image of corroded surface of specimens was observed under the SEM, and the corroded surface of specimens was analysed with the EDX. The following results were obtained. 1. The dissolution amount of Cu was the most in high copper admixed amalgam(Dispersalloy) and the least in high copper single composition amalgam(Tytin). 2. Sn and Zn were dissolved during all the experiment periods, and dissolution amounts were decreased as the time elapsed. 3. Initial surface corrosion products were ZnO and SnO. 4. Corrosion of ${\gamma}$ and ${\gamma}_2$ phase in low copper amalgams was observed and Ag-Cu eutectic alloy phase was corroded in low copper spherical amalgam(Caulk Sperical Alloy). 5. Corrosion of ${\gamma}$ and $\eta$' phase in high copper amalgams was observed and Ag-Cu eutectic alloy phase was corroded in high copper admixed amalgam(Dispersalloy). 6. Sn-Cl was produced in the subsurface of low copper amalgams and high copper admixed amalgam.

• Restorative Dentistry and Endodontics
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• 제13권2호
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• pp.221-235
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• 1988

The purpose of this study was to observe characteristic properties through the polarization curves and EMPA images from 4 different types of amalgam obtained by using the potentiostats (EG & G PARC) & EPMA (Jeol JSM-35), to investigate the degree of corrosion of each phase of amalgam on the oxidation peak, and to identify corrosion products from the corroded amalgam by use of X-ray diffractometer(Rigaku). After each amlgam alloy and Hg were triturated as the direction of the manufacturer by means of the mechanical amalgamator(Shofu), the triturated mass was inserted into the cylindrical metal mold which was 12mm in diameter and 10mm in height and was condensed by means of routine manner. The specimen was removed from the mold and stored at room temperature for about 7 days. The standard surface preparation was routinely carried out. Anodic polarization measurement was employed to compare the corrosion behaviours of the amalgams in 0.9% saline solution(pH6.8~7.0) and artificial saliva (pH6.8~7.0) at $37^{\circ}C$. The open circuit potential was determined after 30 minutes' immersion of specimen in electrolyte and the potential scan was begun at the potential of 100mV cathodic from the corrosion potential. The scan rate was 1mV/sec and the surface area of amalgam exposed to the solution was 0.64$cm^2$ for each specimen. All the potentials reported are with respect to a saturated calomel electrode (SCE). EPMA images on the determined oxidation peaks of each amalgam in artificial saliva were observed. X-ray diffraction patterns of each sample were recorded before and after polarization in artificial saliva (Aristaloy, Caulk Spherical, Dispersalloy and Tytin: at +770mV, +585mV, +8.10m V and +680m V respectively) by use of a recording diffractometer. Nickel filtered Cu $K_{{\alpha}_1}$ radiation was used and sample was scanned at $4^{\circ}(2{\theta})/min.$ from $25^{\circ}$ to $80^{\circ}$. The following results were obtained. 1. Oxidation peak potential in artificial saliva shifted to more anodic direction than that in saline solution. 2. The corrosion potential of high copper amalgam was more anodic than the potential of low copper amalgam. 3. The current density was lower in artificial saliva than in saline solution. 4. One of the corrosion products, AgCl was identified by X-ray diffraction analysis. 5. ${\gamma}_2$ phase was the most susceptible to corrosion and e phase was stable in low copper amalgam and ${\eta}$' phase and Ag-Cu eutectic were susceptible to corrosion in high copper amalgam.

• Restorative Dentistry and Endodontics
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• 제22권1호
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• pp.1-33
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• 1997

The objective of this study was to analyze the in vitro and in vivo corrosion products of low and high copper amalgams. The four different types of amalgam alloy used in this study were Fine cut, Caulk spherical, Dispersalloy, and Tytin. After each amalgam alloy and Hg were triturated according to the directions of the manufacturer by means of the mechanical amalgamator(Amalgam mixer. Shinhung Co. Korea), the triturated mass was inserted into a cylindrical metal mold which was 12mm in diameter and 10mm in height. The mass was condensed by 150Kg/cm compressive force. The specimen was removed from the mold and aged at room temperature for about seven days. The standard surface preparation was routinely carried out by emery paper polishing under running water. In vitro amalgam specimens were potentiostatically polarized ten times in a normal saline solution at $37^{\circ}C$(potentiostat : HA-301. Hukuto Denko Corp. Japan). Each specimen was subjected to anodic polarization scan within the potential range -1700mV to+400mV(SCE). After corrosion tests, anodic polarization curves and corrosion potentials were obtained. The amount of component elements dissolved from amalgams into solution was measured three times by ICP AES(Inductive Coupled Plasma Atomic Emission Spectrometry: Plasma 40. Perkim Elmer Co. U.S.A.). The four different types of amalgam were filled in occlusal and buccal class I cavities of four human 3rd molars. After about five years the restorations were carefully removed after tooth extraction to preserve the structural details including the deteriorated margins. The occlusal surface, amalgam-tooth interface and the fractured surface of in vivo amalgam corrosion products were analyzed. In vivo and in vitro amalgam specimens were examined and analyzed metallographically by SEM(Scanning Electron Microscope: JSM 840. Jeol Co. Japan) and EDAX(Energy Dispersive Micro X-ray Analyser: JSM 840. Jeol Co. Japan). 1. The following results are obtained from in vitro corrosion tests. 1) Corrosion potentials of all amalgams became more noble after ten times passing through the in vitro corrosion test compared to first time. 2) After times through the test, released Cu concentration in saline solution was almost equal but highest in Fine cut. Ag and Hg ion concentration was highest in Caulk spherical and Sn was highest in Dispersalloy. 3) Analyses of surface corrosion products in vitro reveal the following results. a)The corroded surface of Caulk spherical has Na-Sn-Cl containing clusters of $5{\mu}m$ needle-like crystals and oval shapes of Sn-Cl phase, polyhedral Sn oxide phase. b)In Fine cut, there appeared to be a large Sn containing phase, surrounded by many Cu-Sn phases of $1{\mu}m$ granular shapes. c)Dispersalloy was covered by a thick reticular layer which contained Zn-Cl phase. d)In Tytin, a very thin, corroded layer had formed with irregularly growing Sn-Cl phases that looked like a stack of plates. 2. The following results are obtained by an analysis of in vivo amalgam corrosion products. 1) Occlusal surfaces of all amalgams were covered by thick amorphous layers containing Ca-P elements which were abraded by occlusal force. 2) In tooth-amalgam interface, Ca-P containing products were examined in all amalgams but were most clearly seen in low copper amalgams. 3) Sn oxide appeared as a polyhedral shape in internal space in Caulk spherical and Fine cut. 4) Apical pyramidal shaped Sn oxide and curved plate-like Sn-Cl phases resulted in Dispersalloy. 5) In Tytin, Sn oxide and Sn hydroxide were not seen but polyhedral Ag-Hg phase crystal appeared in internal space which assumed a ${\beta}_l$ phase.

• Restorative Dentistry and Endodontics
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• 제16권2호
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• pp.18-32
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• 1991

The purpose of this study was to observe characteristic properties of amalgam through the polarization curves and SEM images from 4 type amalgams (Amalcap, Shofu spherical. Dispersalloy and Tytin) with 3 different surface finish procedures (polishing, burnishing and carving) by using the potentiostats (EG & GPARC) and SEM (Jeol JSM-35). After each amalgam alloy and Hg was triturated as the direction of the manufacturer by means of mechanical amalgamator (Samki), the triturated mass was inserted into the cylndrical metal mold which was 12 mm in diameter and 10 mm in height and was pressed with $100kg/cm^2$. 4 specimens of each type amalgam were burnished with egg burnisher and another 4 specimens of each type amalgam were carved with Hollenback carver. Above 8 specimens and remaining untreated 4 specimens were stored at room temperature for about 7 days. Untreated 4 specimens of each type amalgam were polished with abrasive papers (Deer) from #400 to #1200 and finally on the polishing cloth with $0.5{\mu}m$ and $0.06{\mu}m$ $Al_2O_3 $ powder suspended water. Anodic polarization measurements was employed to compare the corrosion behaviours of the amalgams in 0.9% saline solution at $37^{\circ}C$. The open circuit potential was determined after 30 minutes immersion of specimen in electrolyte. The scan rate was 1 mV/sec and the surface area of amalgam exposed to the solution was $0.64cm^2$ for each specimen. All the potentials reported are with respect to a saturated calomel electrode (SCE). SEM images of each specimen were taken after + 800 mV (SCE) polarization. The results were as follows: 1. The corrosion potential of high copper amalgam was more anodic than that of low copper amalgam. 2. The polished amalgam were more resistant to corrosion than any other burnished and carved amalgam. 3. In the case of polishing, current density of high copper amalgam was lower than that of low copper amalgam.

• Restorative Dentistry and Endodontics
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• 제12권1호
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• pp.39-49
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• 1986

The purpose of this study was to observe characteristic properties through the polarization curves and SEM images from 4 different types of amalgam obtained by using the potentiostats (Princeton EG & G) & SEM (Jeol/35), and to investigate the degree of corrosion on the oxidation peak of the each phase of amalgam. After each amalgam alloy and Hg was triturated as the direction of the manufacturer by means of the mechanical amalgamator (Shofu Co.), the triturated mass was inserted into the cylindrical metal mold which was 12mm in diameter and 10.0mm in height and was condensed by using routine manner. The specimen was removed from the mold and stored at room temperature for about 24 hours. The standard surface preparation was routinely carried out. Anodic polarization measurement was employed to confirm the corrosion behaviour of the amalgams in a 0.9% saline solution (P.H: 6.8-7.0) at $37^{\circ}C$. The initial rest potential (corrosion potential) was determined after 30 minutes of immersion of specimen in electrolyte, and the potential scan was begun at the point of 100mV cathodic from the corrosion potential. The scan rate was 0.17mV/sec. in the study to observe the degree of corrosion of each phase. SEI and EPMA images on the determined oxidation peaks of each amalgam were observed. The results were as follows: 1. In the four anodic polarization curves, low copper amalgams have three oxidation peaks and high copper amalgams have two oxidation peaks, -270mV, +26mV and +179mV(SEC) in the low copper lathe cut, and -300mV, +39mV and +163mV(SEC) in the low copper spherical. -4mV and +154mV(SEC) in the Dispersalloy, and +17mV and +180mV(SEC) in the Tytin as high copper amalgams. 2. ${\gamma}_2$ phase in the low copper amalgam and ${\eta}$ phase in the high copper amalgam were the most corrodible phases and Ag-Cu eutectic in high copper amalgam was the most slowly corroded phase. 3. Low copper amalgam was more susceptible in corrosion than high copper amalgam.

• Restorative Dentistry and Endodontics
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• 제18권2호
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• pp.431-445
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• 1993

The purpose of this study was to observe corrosion characteristics of six dental amalgams and was to analyse corrosion products electrochemically. After each amalgam alloy and Hg was triturated as the direction of the manufacturer by using mechanical amalgamator, the triturated mass was inserted into the cylinderical metal mold ($12{\times}10mm$) and was condensed with 160kg/$cm^2$ by using the hydrolic press. The specimen was removed from the mold and was stored at room temperature for 1 week, and was polished with amalgam polishing kit. The anodic and cathodic polarization curve was obtained by using cyclic voltammetric method with 3-electrode potentiostat in saline for each amalgam and Ag, Sn, Cu plate specimen at $37{\pm}0.5^{\circ}C$. The potential sweep range was -1.7V~0. 4V(vs SCE) in working electrode and scan rate was 50mV/s and the exposed surface area of each specimen to the electrolytic solution was $0.79cm^2$. The results were as follows. 1. In anodic-cathodic polarization curve of amalgam specimens, two anodic current rising areas and two cathodic current peaks were obtained at the low Cu amalgam(CF, CS) specimen and three anodic current rising areas and three cathodic current peaks were obtained at the high Cu amalgam (TY, DS, HV) specimen. 2. As this compared with the anodic and cathodic current peak potentials of Sn, Cu and Ag specimen, the first cathodic current peak I c was caused by the reduction of divalent tin salt, second cathodic current peak IIIc results from the reduction of quadravalent tin salt, and third cathodic current peak me results from the reduction of copper salt. 3. As reverse potential sweeping was done repeatedly, anodic current was decreased slightly in all amalgam specimens.

• Restorative Dentistry and Endodontics
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• 제16권1호
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• pp.6-15
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• 1991

The purpose of this study was to observe in vitro chloride corrosion behavior from 5 kinds of amalgam (Caulk spheracal, Amalcap, Dispersalloy, Tytin, Sybralloy) as a function of time after tritruration by using potentiostat. After each amalgam alloy and Hg was triturated as the direction of the manufacturer by the mechanical amalgamator, the triturated mass was inserted the cyrindrical matal mold ($12{\times}10mm$) and was condensed by using routine manner. The specimen was removed from the mold and was stored at room temperature for 1 week, 1 month and 3 months, and standard surface preparation was routine carried out. The 0.9% saline solution was used as electrolyte in pH 6.8~7.0 at $30{\pm}0.5.^{\circ}C$. The open circuit potential was determined after 30 minutes' immersion of 1 week, 1 month and 3 month old specimens. The scan rate was 1 mV/sec and the surface area of amalgam exposed to the solution was $0.65\;Cm^2$ for each specimen. All potentials reported are with respect to a silver / silver chloride electrode (SSE). The following result was obtained. 1. All amalgam specimens became more noble corrosion potentials which represent the improved corrosion resistance as the time elapsed. 2. Three kinds of high copper amalgam always exhibited more noble potential than low copper amalgam at 1 week, 1 month and 3 months. 3. Two kinds of low copper amalgam had the similar polarization curve pattern with 3 current peaks at each time period and current densities associated with these peaks were decreased as aging especially in caulk spherical amalgam. 4. All kinds of high copper amalgam had the similar polarization curve pattern with absence of prominent current peak at each time period, but the polarization curve of D amalgam had one apparent current peak at 1 week.

• Restorative Dentistry and Endodontics
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• 제23권1호
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• pp.502-514
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• 1998

The purpose of this study is to observe the corrosion characteristcs of four dental amalgams(CAULK FINE CUT, CAULK SPHERICAL, DISPERSALLOY, TYTIN) and to determine a function of chloride concentration through the anodic polarization curve obtained by using a potentiostat. After each amalgam alloy and Hg being triturated, the triturated mass was inserted into the cylinderical metal mold, and condensed by hydrolic pressure. Each specimen was removed from the metal mold. 24 hours after condensation, specimens were polished with the emery paper and stored at room temperature for 6 months. The anodic polarization curves were employed to compare the corrosion behaviours of the amalgam m KCl and KCl-NaCl solution, which had chlonde concentration of 0.4 g/l, 0.8 g/l, 1.2 gil, and 1.6 gil at $37^{\circ}C$ with 3-electrode potentiostat. After the immersion of specimen in electrolyte for 1 hour, the potential scan was begun. The potential scan range was - 1500mV ~+800mV(vs. S.C.E.) in the working electrode and the scan rate was 50mV/sec. The results were as follows, 1. The corrosion potential. the potential of anodic current peak, and transpassive potential in the solution of high chloride concentration shifted to more cathodic direction than those in the solution of low concentration, and the current density in the solution of high chloride concentration was higher than that in the solution of low concentration. 2. The corrosion potential, the potential of anodic current peak, and transpassive potential for CAULK FINE CUT amalgam were the most cathodic among the others, and the current density were the highest among the others. 3. In the solution of low chloride concentration, the corrosion potential, the potential of anodic current peak, and transpassive potential for DISPERSALLOY were the most anodic among the others, however in the solution of high chloride concentration, those for TYTIN were the most anodic among the others. 4. The anodic polarization curve for CAULK SPHERICAL was similar to that for high copper amalgams.