Kinetic studies of water uptake and loss in glass-ionomer cements

The water sorption and desorption behaviour of three commercial glass-ionomer cements used in clinical dentistry have been studied in detail. Cured specimens of each material were found to show slight but variable water uptake in high humidity conditions, but steady loss in desiccating ones. This water loss was found to follow Fick’s law for the first 4–5 h. Diffusion coefficients at 22 °C were: Chemflex 1.34 × 10⁻⁶ cm² s⁻¹, Fuji IX 5.87 × 10⁻⁷ cm² s⁻¹, Aquacem 3.08 × 10⁻⁶ cm² s⁻¹. At 7 °C they were: Chemflex 8.90 × 10⁻⁷ cm² s⁻¹, Fuji IX 5.04 × 10⁻⁷ cm² s⁻¹, Aquacem 2.88 × 10⁻⁶ cm² s⁻¹. Activation energies for water loss were determined from the Arrhenius equation and were found to be Chemflex 161.8 J mol⁻¹, Fuji IX 101.3 J mol⁻¹, Aquacem 47.1 J mol⁻¹. Such low values show that water transport requires less energy in these cements than in resin-modified glass-ionomers. Fick’s law plots were found not to pass through the origin. This implies that, in each case, there is a small water loss that does not involve diffusion. This was concluded to be water at the surface of the specimens, and was termed “superficial water”. As such, it represents a fraction of the previously identified unbound (loose) water. Superficial water levels were: Chemflex 0.56%, Fuji IX 0.23%, Aquacem 0.87%. Equilibrium mass loss values were shown to be unaffected by temperature, and allowed ratios of bound:unbound water to be determined for all three cements. These showed wide variation, ranging from 1:5.26 for Chemflex to 1:1.25 for Fuji IX.     

Antibacterial activity of four glass ionomer cements used in atraumatic restorative treatment

The in vitro antibacterial activity of four glass ionomer cements (Fuji IX, Ketac Molar, Vidrion R and Vitromolar) indicated for Atraumatic Restorative Treatment (ART) was studied against strains of bacteria involved in the development of oral diseases, Streptococcus mutans, Streptococcus sobrinus, Lactobacillus acidophilus and Actinomyces viscosus. The agar plate diffusion test was used for the cultures, which included chlorhexidine as a positive control. The results demonstrated that all the cements evaluated presented antibacterial activity. Based on the results of this study, it can be concluded that Fuji IX and Ketac Molar presented the most effective antibacterial activity considering the ART approach.     

Influence of loading types on the shear strength of the dentin–resin interface bonding

Small differences in the shear bond test can make critical differences in the bonding strength values. The purpose of this study was to compare the influence of the orthodontic-looped wire, stainless steel tape and chisel systems used in shear bonding tests to verify the resistance in the dentin-resin interface. Forty-eight human teeth were used and divided in three groups. The teeth were ground until a flat smooth surface was achieved, that was delimited with an adhesive tape containing a hole of 4 mm diameter. After, the dentine surface was treated with Scotchbond Multi Purpose and the composite Z-100 was applied in layers, through a stainless steel mold. The samples were stored at 37 °C and 100% of relative humidity for 24 h and, then, submitted to 500 thermal cycles. After, they were taken to an universal test machine (Otto Wolpert) with crosshead speed of 6 mm/min. The results were statistically analyzed using a Tukey's test (p<0.05). The orthodontic-looped wire determined the highest values of shear bond (13.33 MPa), following by chisel (7.81 MPa) and stainless steel tape (4.87 MPa). The debonding values depend on a complex stress combination produced during the loading of the samples. Small variations in test methodologies give statistically different values for shear bond strength. Different shear strength methods in vitro make the comparative clinical performance of the resin filling materials difficult.     

Ion migration from fluoride-releasing dental restorative materials into dental hard tissues

This study was carried out in order to determine the extent to which ions released from fluoride-containing dental restoratives migrated through the enamel and dentine of extracted teeth. A total of 40 permanent human 3rd molars were used. They were extracted for orthodontic reasons, and employed within 1 month of extraction. A cervical (Class V) cavity was prepared in each tooth, then filled with one of: a conventional glass-ionomer, a resin-modified glass-ionomer, a polyacid-modified composite resin (“compomer”) or a fluoride-releasing resin composite. Ten samples were prepared per material. After 1 month, five specimens per material were prepared and examined under SEM/EDX. Concentrations of sodium, aluminium, strontium, fluorine, magnesium, silicon, phosphorus and calcium were determined within the tooth. After 18 months, the remaining five specimens for each material were prepared and studied in the same way. The greatest extent of ion migration into the tooth was found with the conventional glass-ionomer and least migration was found for the fluoride-releasing composite, which showed no evidence of fluoride migration at all. Levels of migrating ions were generally higher in the 18 month specimens than in the 1 month specimens, and also higher in the dentine than in the enamel. Ions released by restorative dental materials have been shown conclusively for the first time to be capable of migrating into the enamel and dentine surrounding the restoration. The conventional glass-ionomer showed the highest level of ion migration whereas the fluoridated composite resin showed little if any ion migration. This suggests that the conventional glass-ionomer has the greatest caries inhibiting effects of all the materials tested, and the fluoridated composite the least.     

A novel acrylic copolymer for a poly(alkenoate) glass-ionomer cement

The interest in the clinical use of polyalkenoate cements stems mainly from their behavior as bioactive adhesive materials with therapeutic action. Glass-ionomer cements set by an acid-base reaction between a degradable glass and a poly(alkenoic acid) and the therapeutic action is related to the release of fluoride ions which are present in the hardened cement that show a sustained release over years, responsible for caries inhibition in teeth. Conventional glass-ionomers, however, suffer from some disadvantages such as short working time, initial moisture sensitivity and prone to desiccation after setting and are generally brittle. In the present study, a poly(alkenoic acid) copolymer was synthesized based on acrylic acid and 2-hydroxyethylmethacrylate (HEMA) using azobisisobutyronitrile as the initiator and characterized. The acid–base reaction was carried out by reacting aqueous solutions of the new copolymer (40 and 60%) with a commercial aluminofluorosilicate glasses as used in conventional glass-ionomer cements. The results showed that the copolymer of HEMA and acrylic acid was a viable poly(alkenoic) acid for formation of glass-ionomer cements.     

<Emphasis Type="Italic">In vitro</Emphasis> microhardness of glass ionomer cements

This study evaluated the surface microhardness of four glass ionomer cements and a composite resin (Fuji IX, Ketac Molar, Vidrion R, Vitromolar and Z 250). Ten specimens of each glass ionomer cement with 8.0 mm diameter and 5.0 mm high dimensions were made and Vicker’s microhardness measurements were taken at 1 day and 1 week after initial setting reaction. The results were analyzed using Student’s T test and Tukey test (p < 0.05) and demonstrated that the values of microhardness increased after 1 week, with the exception of Fuji IX. Resin composite Z250 presented the greatest values for microhardness.     

Ion release by endodontic grade glass-ionomer cement

Cylindrical specimens (6 mm high × 4 mm diameter) of the endodontic grade glass-ionomer (Ketac Endo) were exposed to various media for 1 week, after which changes in their mass, pH of storage medium, and ion release were determined. In water, this cement was shown to release reasonable amounts of sodium, aluminium and silicon, together with smaller amounts of calcium and phosphorus, as well as taking up 2.41% by mass of water. A comparison with the restorative grade materials (Ketac Molar, ex 3M ESPE and Fuji IX, ex GC) showed both ion release and water uptake to be greater. All three cements shifted pH from 7 to around 6 with no significant differences between them. Other storage media were found to alter the pattern of ion release. Lactic acid caused an increase, whereas both saturated calcium hydroxide and 0.6% sodium hypochlorite, caused decreases. This suppression of ion-release may be significant clinically. Aluminium is the most potentially hazardous of the ions involved but amounts released were low compared with levels previously reported to show biological damage.     

Investigation of the post-hardening reaction in glass-ionomer cements based on poly(vinyl phosphonic acid)

In this study the behaviour of two PVPA-based glass-ionomer cements was investigated. The first cement was prepared from PVPA homopolymer and glass, together with a reaction modifier. In the second cement a modified version of the polymer was used instead of the homopolymer. The modification was achieved by the treatment of the polymer with a small quantity of zinc fluoride. The effect of ageing under different conditions on the strength, mass and volume of the cements was determined. The ZnF₂-containing system behaved in a fairly straightforward manner, showing a gradual increase in strength with time (up to 3 months) that was similar to glass-ionomer cements based on poly(acrylic acid). By contrast the unmodified material did not increase in strength with time, a feature that was attributed to extensive crosslinking of the material, causing it to become more brittle and hence more sensitive to defects in the specimens. With regard to the effect on mass and volume, both types of cement behaved like typical set glass-ionomers, displaying a sensitivity to dessication but little, if any, sensitivity to aqueous media.     

Age-related changes in cyclic voltammetry and potentiodynamic studies of normal human dentine

Impedance spectroscopy is one of the non-destructive techniques used by researchers to measure electrical resistance of biological tissues and ceramics. The purpose of this study is to investigate the voltage–current (V–I) characteristics of sound human dentine from young and old teeth, using cyclic voltammetry and potentiodynamic techniques. Dentine samples were prepared from freshly extracted sound third molars. After electrical measurements, dentine samples were characterized using scanning electron microscopy (SEM). Cyclic voltammetric measurements showed that variation of current through sample as a function of applied voltage is linear for dry samples of both age groups. However, for wet samples V–I characteristic were found to be different. The resistivity of dry young dentine is greater than that of old dentine in dry environment, whereas, it was found to be opposite for wet dentine samples. Using the same voltage sweep in potentiodynamic measurements dry samples display similar traces to controls suggesting that the dry dentine acts as an insulator. The number of dentinal tubules and their diameter has been found to decrease with increasing age. We propose that these changes determine the changes in electrical characteristics of sound human dentine. In spite of increasing use of electrical techniques to understand electrical properties of teeth, it is clear from this study that local structural variations and environment have a marked influence. Therefore, this baseline data needs to be considered in any future study or clinical application.     

Shear bond strength of adhesive systems to enamel and dentin. Thermocycling influence

Objectives: The purpose of the this study was to evaluate the influence of thermocycling on shear bond strength on bovine enamel and dentin surfaces of different adhesive systems. Methods: Thirty sound bovine incisors were sectioned in mesiodistal and inciso-cervical direction obtaining 60 incisal surfaces (enamel) and 60 cervical surfaces (dentin). Specimens were randomly assigned to 3 groups of equal size (n = 40), according to the adhesive system used: I—Single Bond; II—Prime & Bond NT/NRC; III—One Coat Bond. After 24-h storage in distilled water at 37^oC, each main group was divided into two subgroups: A- specimens tested after 24 h storage in distilled water at 37 ^∘C; B - specimens submitted to thermocycling (500 cycles). Shear bond strength tests were performed. Data were submitted to ANOVA and Tukey test. Results: Means (MPa) of different groups were: I—AE-16.96, AD-17.46; BE-21.60, BD-12.79; II—AE-17.20, AD-11.93; BE-20.67, BD-13.94; III—AE-25.66, AD-17.53; BE-24.20, BD-19.38. Significance: Thermocycling did not influence significantly the shear bond strength of the tested adhesive systems; enamel was the dental substrate that showed larger adhesive strength; One Coat Bond system showed the best adhesive strength averages regardless of substrate or thermocycling.     

Study on the potential inhibition of root dentine wear adjacent to fluoride-containing restorations

The purpose of this in vitro study was to determine whether the vicinity of root dentine that had been restored with fluoride-releasing materials was at reduced risk for erosive/abrasive wear compared to root dentine restored with a non-fluoride-containing material. According to a randomized complete block design, standardized cavities prepared on the surface of 150 bovine root dentine slabs were restored with glass-ionomer cement, resin-modified glass ionomer, polyacid-modified resin composite, fluoride-containing or conventional composite. Specimens were coated with two layers of an acid-resistant nail varnish exposing half of the dentine surface and half of the restoration. Subsequently, specimens were either eroded in an acidic drink or left uneroded, then exposed to artificial saliva and abraded in a toothbrushing machine. Wear depth in the vicinity of restorations was quantified by a stylus profilometer, based on the nonabraded areas surrounding the erosion/abrasion region. Two-way ANOVA did not demonstrate significant interaction between restoratives and eroded-uneroded dentine (p = 0.5549) nor significant difference among restorative materials (p = 0.8639). Tukey’s test ascertained that the wear depth was higher for eroded than for uneroded groups. Fluoride-releasing materials seemed to negligibly inhibit wear in the vicinity of restored root dentine subjected to erosive/abrasive challenges.     

Effect of ultrasound on the setting characteristics of glass ionomer cements studied by Fourier Transform Infrared Spectroscopy

OBJECTIVE: To investigate the effect of ultrasound (US) application, US staring time and US duration on the setting of glass ionomer cement (GIC) by using Attenuated Total Reflectance Fourier Transform Infrared (ATR/FTIR) spectrometer. METHODS: Two conventional GICs, Fuji IX Fast and Ketac Molar were studied. US application was started at 30 s or 40 s after mixing and was applied for times between 15 and 55 s on samples of two different thicknesses. The samples were analysed using ATR/FTIR. RESULTS: US accelerated the curing process in both cements, US needed to be applied for more than 15 s. Both Fuji IX and Ketac Molar showed increased setting on increasing the US application duration from 15 s to 55 s. Increased setting of the GICs was produced when US application started 40 s after mixing rather than 30 s after mixing. CONCLUSIONS: The significant findings of the study include that US application accelerated the setting processes, by accelerating the formation of the acid salts. The salt formation increased with increase time of US application. The effect of application of US to setting GICs is influenced by time of the start of application of the US. The effects appear to material specific, with Ketac Molar showing a greater effect than Fuji IX.     

Influence of air abrasion preparation on microleakage in glass ionomer cement restorations

The aim of this study was to assess microleakage in class V cavities prepared by air abrasion or high-speed dental bur and restored with different glass ionomer cements. Sixty bovine incisors were equally divided into 6 groups: I, II and III (preparation by high-speed) and IV, V and VI (preparation by air abrasion). Groups I and IV were restored with Fuji IX; groups II and V with Ketac Molar; and groups III and VI with Vitremer. After 24 h (37 °C), specimens were thermocycled, isolated with nail varnish, immersed in a 0.2% Rhodamine B solution for 24 hours, sectioned longitudinally and analyzed for microleakage using an optical microscope connected to a digital camera and a computer. The images were digitized and a software allowed the quantitative evaluation of microleakage in millimeters. Data were analyzed by Wilcoxon and Kruskal-Wallis tests. It was observed that there were significant differences (p ≤ 0.05) between incisal (enamel) and cervical (dentine/cementum) margins, mainly for Ketac Molar; there was no difference (p ≥ 0.05) between preparation methods, except for group II (high-speed/Ketac Molar) that showed higher infiltration; regarding the materials, Ketac Molar demonstrated the highest microleakage values (p ≤ 0.05), and only Vitremer sealed completely both margins of restorations. It was concluded that air abrasion preparation did not influence microleakage in class V restorations with the employed glass ionomer cements.     

Effect of kissing bond on fatigue behavior of friction stir welds on Al 5083 alloy

Fatigue properties of FS welds with a kissing bond (bonded welds) were studied by comparing the test results of bonded welds with those of sound welds. The fatigue life of bonded welds is 21∼43 times shorter than that of sound welds under the stress ratio R = 0.1, and the fatigue characteristic values of each welds have decreased from 100.24 MPa for sound welds to 65.57 MPa for bonded welds at 2 × 10⁶ cycles. At the macroscopic level there is no evidence of failure by shear. The fatigue fracture revealed cracks initiated from the root tip of kissing bond.     

The effect of storage in aqueous solutions on glass-ionomer and zinc polycarboxylate dental cements

Cylindrical specimens (dimensions 6 mm diameter×12 mm height) of glass-ionomer and of zinc polycarboxylate dental cement have been stored in aqueous solutions for periods of 24 h, 1 week and 1 month. The solutions were of varying composition and affinity for water, and storage in them resulted in fluctuations in mass of the cements, an effect which was attributed to differences in the partitioning of water between the solutions and the cement specimens. Unlike the zinc polycarboxylate, the glass-ionomer gained mass in most of the solutions examined (except Na₂SO₄), showing it to have a much greater affinity for water than the zinc polycarboxylate. Despite the fluctuations in water uptake by the glass-ionomer, and loss of water by the zinc polycarboxylate, no statistically significant differences in compressive strength were recorded in any solution at any storage time. This contrasts with results reported previously for zinc polycarboxylates using smaller specimens, showing that specimen size has an influence on the interaction of cements with storage solutions. ©2000 Kluwer Academic Publishers     

Effects of different preparation procedures during tooth whitening on enamel bonding

The objective of this study was to assess effects of some clinically related preparation procedures during tooth whitening on enamel bonding properties. Sixty-two extracted human teeth were cleaned and divided into four groups. Forty-two of the teeth were left with their natural surface intact while 20 teeth were polished to form a flat surface. Half of the tooth served as the experimental side and received one of the two whitening products: Opalescence (10% carbamide peroxide) and Crest Whitestrips (6.5% hydrogen peroxide), for 2 weeks. Post-bleaching intervals included: 1 day, 1 week, and 2 weeks. On these days, tooth (10 mm × 1.5 mm × 1.5 mm) sections were evaluated using Raman spectroscopy, scanning electron microscopy and tensile bond strength tests. T-test, ANOVA test, and mixed model regression analysis were used to assess the differences. No significant difference existed between natural surface and polished surface teeth for all groups at both Day One and Week Two (P > 0.05). On Day One, both treated groups had significant lower bond strength than the control group (P = 0.002). After 2 weeks, no significant difference existed between any group (P = 0.381). SEM indicated that resin–enamel interfaces in bleached enamel exhibited more defects in granular formations when compared to the control. Raman results indicated a lower degree of polymerization (DP) of adhesive at the interface for treated teeth surfaces. In summary, pre-bleaching surface treatments such as polish or non-polish, had no effect on bond strength. Bleaching significantly decreased bond strength initially, but after 2 weeks, bleaching had no significant effect on bond strength. Storage time had significant effect on Opalescence treated enamel, but not on control and Whitestrip treated enamel. The decrease of bond strength may be related to interfacial defects and low DP due to oxygen release after bleaching.     

Ultrasonically set novel NVC-containing glass-ionomer cements for applications in restorative dentistry

The objective of this study is to investigate the effects of application of ultrasound on the physical properties of a novel NVC (N-vinylcaprolactam)-containing conventional glass-ionomer cement (GIC). Experimental GIC (EXP) samples were made from the acrylic acid (AA)–itaconic acid (IA)–NVC synthesized terpolymer with Fuji IX powder in a 3.6:1 P/L ratio as recommended by the manufacturer. Specimens were mixed and fabricated at room temperature and were conditioned in distilled water at 37°C for 1 day up to 4 week. Ultrasound (US) was applied 20 s after mixing by placing the dental scaler tip on the top of the cement and applying light hand pressure to ensure the tip remained in contact with cement without causing any deformation. Vickers hardness was determined using a microhardness tester. The working and setting times were determined using a Gillmore needle. Water sorption was also investigated. Commercial Fuji IX was used as control for comparison (CON). The data obtained for the EXP GIC set through conventional set (CS) and ultrasonically set (US) were compared with the CON group, using one-way ANOVA and the Tukey multiple range test at α = 0.05. Not only ultrasonic (US) application accelerated the curing process of both EXP cement and CON group but also improved the surface hardness of all the specimens. US set samples showed significantly lower water sorption values (P < 0.05) due to improved acid–base reaction within the GIC matrix and accelerated maturation process. According to the statistical analysis of data, significant increase was observed in the surface hardness properties of CS and US specimens both in EXP samples and the CON groups. It was concluded that it is possible to command set GICs by the application of ultrasound, leading to GICs with enhanced physical and handling properties. US application might be a potential way to broaden the clinical applications of conventional GICs in restorative dentistry for procedures such as class V cavity restorations.     

Comparison of a SiO2–CaO–ZnO–SrO glass polyalkenoate cement to commercial dental materials: glass structure and physical properties

Glass polyalkenoate cements (GPCs) have previously been considered for orthopedic applications. A Zn–GPC (BT 101) was compared to commercial GPCs (Fuji IX and Ketac Molar) which have a setting chemistry analogous to BT 101. Handling properties (working, T _w and setting, T _s times) for BT 101 were shorter than the commercial GPCs. BT 101 also had a higher setting exotherm (S _x —34 °C) than the commercial GPCs (29 °C). The maximum strengths for BT 101, Fuji IX, and Ketac Molar were 75, 238, and 216 MPa (compressive, σ _c), and 34, 54, and 62 MPa (biaxial flexural strengths, σ _f), respectively. The strengths of BT 101 are more suitable for spinal applications than commercial GPCs.     

Variations in the compressive strength of dental cements stored in ionic or acidic solutions

The compressive strengths of various dental cements (a zinc polycarboxylate, a zinc phosphate, a glass-ionomer and two resin-modified glass ionomers, RMGICs) have been determined following storage in pure water, 0.9% sodium chloride solution or 20 mmol dm^–3 lactic acid solution for periods of time ranging from 24 h to 3 months. The glass-ionomer cement showed no differences between different storage solutions or at different storage times, whereas the zinc polycarboxylate, zinc phosphate and the resin-modified glass ionomer cements showed significant differences following storage in the solutions for 24 h compared with pure water. The zinc polycarboxylate cement was significantly weaker at 24 h in 0.9% NaCl and lactic acid than in pure water, whereas most of the other cements were significantly stronger in both 0.9% NaCl and lactic acid. One of the RMGICs (Vitremer luting, ex. 3M), however, was significantly stronger only in the NaCl solution, not in the lactic acid. In general, by 1 week, the strengths all reverted to being essentially the same as for specimens stored in pure water for most subsequent storage times, and did not change significantly on storage for up to 3 months. This effect of storage medium on the early strength has not been reported previously and since the media were chosen to model certain characteristics of natural saliva, the changes observed seem likely to occur in vivo. It is concluded that pure water is not the best medium for storing these cements if they are to behave as they do under clinical conditions. © 2001 Kluwer Academic Publishers     

Effect of welding parameters on diffusion bonding of type 304 stainless steel–copper bimetal

Abstract

Stainless steel AISI type 304 and electrolytic cold rolled copper were joined by diffusion bonding at temperatures ranging from 650 to 950°C, for times from 5 to 45 min, and at pressures from 2 to 12 MPa. After bonding the microstructure of the interface was investigated, including the grain size, and shear and tensile strengths of the bonded specimens were determined. From the results, it was seen that the bond shear strength was dependent on interface grain boundary migration and on grain growth during the bonding process. In addition, attempts were made to find a relationship between grain size and shear strength in the bonding area. Taking into account the results of shear testing and microstructural observation, for a sound bond, optimum bonding conditions were obtained at temperatures of 800–850°C for 15–20 min at 4–6.5 MPa. The fracture behaviour of the diffusion bonded joint was investigated by means of shear and tensile testing under different bonding conditions. It was found that both shear and tensile strengths of the bonds were sensitive to the bonding conditions, and the intermetallic phases did not affect these parameters. Furthermore, the value of shear strength of the bond surface determined by shear testing was higher than the shear strength of the fracture surface determined by tensile testing.