New insights into structural alteration of enamel apatite induced by citric acid and sodium fluoride solutions.

Attenuated total reflectance infrared spectroscopy and complementary scanning electron microscopy were applied to analyze the surface structure of enamel apatite exposed to citric acid and to investigate the protective potential of fluorine-containing reagents against citric acid-induced erosion. Enamel and, for comparison, geological hydroxylapatite samples were treated with aqueous solutions of citric acid and sodium fluoride of different concentrations, ranging from 0.01 to 0.5 mol/L for citric acid solutions and from 0.5 to 2.0% for fluoride solutions. The two solutions were applied either simultaneously or consecutively. The citric acid-induced structural modification of apatite increases with the increase in the citric acid concentration and the number of treatments. The application of sodium fluoride alone does not suppress the atomic level changes in apatite exposed to acidic agents. The addition of sodium fluoride to citric acid solutions leads to formation of surface CaF2 and considerably reduces the changes in the apatite P-O-Ca framework. However, the CaF2 globules deposited on the enamel surface seem to be insufficient to prevent the alteration of the apatite structure upon further exposure to acidic agents. No evidence for fluorine-induced recovery of the apatite structure was found.

CO2 laser-induced zonation in dental enamel: a Raman and IR microspectroscopic study.

The gradient of structural alteration and molecular exchange across CO(2) laser-irradiated areas in dental enamel was analyzed by Raman and attenuated total reflectance infrared microspectroscopy. The type and the degree of structural changes in morphologically distinguishable zones within the laser spot vary depending on the laser-irradiation parameters--power (1 and 3 W), treatment time (5 and 10 s), and operational mode (super pulse and continuous wave). Using higher power, irrespective of the operation mode, the enamel tissue ablates and a crater is formed. The prevalent phase at the bottom of the crater is dehydrated O(2) (2-)-bearing apatite, that is, the fundamental framework topology is preserved. Additional nonapatite calcium phosphate phases are located mainly at the slope of the laser crater. No structural transformation of mineral component was detected aside the crater rim, only a CO(3)-CO(2) exchange, which decays with the radial distance. A lower-power laser irradiation slightly roughens the enamel surface and the structural modification of enamel apatite is considerably weaker for continuous wave than for super pulse mode. Prolonged low-power laser treatment results in recrystallization, and thus structural recovering of apatite might be of clinical relevance for enamel surface treatments.

Effect of debonding force direction on orthodontic shear bond strength.

INTRODUCTION: The aim of this study was to determine the influence of debonding force direction in shear bond strength testing of orthodontic brackets in vitro. METHODS: One hundred fifty extracted bovine permanent mandibular incisors were randomly divided into 5 groups of 30 specimens each. Before bonding with a composite adhesive, enamel surfaces were etched with 37% phosphoric acid for 30 seconds. Teeth were bonded with mesh-based stainless steel orthodontic brackets. Shear bond strength was measured with a universal testing machine. Debonding forces were directed either parallel to the bracket base (group B), toward the enamel surface (group A: 15 degrees), or away from the enamel surface (group C: 15 degrees; group D: 30 degrees; group E: 45 degrees). RESULTS: Shear bond strength measurements were as follows: 22.90 (SD, 1.72) MPa (group A), 17.90 (SD, 2.63) MPa (group B), 12.99 (SD, 1.71) MPa (group C), 7.93 (SD, 1.14) MPa (group D), and 6.65 (SD, 1.14) MPa (group E). Analysis of variance indicated that shear bond strengths were significantly different between the groups investigated. Mean adhesive remnant index scores ranged between 1.60 in group B and 2.13 in group D. CONCLUSIONS: Shear bond strength measurements were significantly influenced by the direction of the debonding force, indicating the need for control and standardization of this testing parameter in orthodontic shear bond strength testing.

Magnetic forces on orthodontic wires in high field magnetic resonance imaging (MRI) at 3 tesla.

BACKGROUND: In a previous investigation we reported on magnetic forces in the static magnetic field of a 1.5 Tesla MRI system. The aim of the present investigation was to assess forces on orthodontic wires in a high field strength MRI system at 3 Tesla. MATERIALS AND METHODS: Thirty-two different orthodontic wires (21 archwires, eight ligature wires and three retainer wires) were investigated in a 3 Tesla high field strength MRI system (Intera, Philips Medical Systems, Best, The Netherlands). Translational forces were measured by the deflection angle test (ASTM F2052-02), and rotational forces assessed on a 5-point qualitative scale. RESULTS AND CONCLUSION: Translational forces ranged between 43.5 mN and 136.1 mN for retainer wires and between 0.6 mN (Noninium) and 208.4 mN (Orthos Stainless Steel) for steel archwires. Translational forces were up to 53.8 times as high as gravitational forces for retainer wires and up to 54.5 times as high for steel archwires, associated with marked rotational forces for the most part. Archwires manufactured from nickel-titanium, titanium-molybdenum and cobalt-chromium and different ligature wires showed no or negligible forces in the magnetic field. Carefully ligated wires should not present a risk due to translational and rotational forces in the high field MRI system at 3 Tesla.

Influence of cross-head speed in orthodontic bond strength testing.

OBJECTIVE: The aim of this study was to investigate the influence of cross-head speed on debonding force of orthodontic brackets. METHODS: One hundred and twenty extracted permanent bovine mandibular incisors were randomly divided into 4 groups of 30 specimens each. Teeth were bonded with stainless steel orthodontic brackets. Enamel surfaces were etched with 37% phosphoric acid for 30 seconds and bonded with a composite adhesive. Debonding force measurements were performed with a universal testing machine Zwicki Z 2.5 (Zwick, Germany). Cross-head speeds of the four groups were: 0.1 mm s-1 (group A), 0.5 mm s-1 (group B), 1.0 mm s-1 (group C), 5.0 mm s-1 (group D). RESULTS: Mean debonding force measurements were as follows: 215.35 (39.09) N (group A), 231.79 (48.62) N (group B), 236.64 (39.26) N (group C), 224.95 (34.67) N (group D). Analysis of variance indicated that there were no significant differences in debonding forces between the groups investigated. The adhesive remnant index showed a median value of 2.0 for all groups. SIGNIFICANCE: Cross-head speed variation between 0.1 and 5 mm min-1 does not seem to influence debonding force measurements or failure mode of brackets bonded to enamel with a composite adhesive.

Influence of force location in orthodontic shear bond strength testing.

OBJECTIVE: The purpose of the present study was to analyze the influence of debonding force location in shear bond strength testing of orthodontic brackets in vitro. METHODS: Ninety extracted permanent bovine mandibular incisors were randomly divided into 3 groups of 30 specimens each. Teeth were bonded with stainless steel orthodontic brackets. Enamel surfaces were etched with 37% phosphoric acid for 30s and bonded with a composite adhesive. Debonding force measurements were performed with a universal testing machine. Location of the debonding force was: bracket base (group A), ligature groove (group B), occlusal bracket wings (group C). RESULTS: Mean shear bond strength measurements were as follows: 22.70(4.23)MPa (group A), 11.52(2.74)MPa (group B), 9.44(2.96)MPa (group C). Analysis of variance indicated that there were significant differences in shear bond strength. Post-hoc Tukey tests showed that bond strength measurements of group A were significantly different from those of groups B and C. The adhesive remnant index also showed significant differences and ranged from a mean of 1.53 in group A to a mean of 2.10 in group C. SIGNIFICANCE: Debonding force location had a significant influence on shear bond strength measurements and bond failure pattern, indicating that this parameter needs to be taken into consideration for interstudy comparison of in vitro results.

Magnetic field interactions of orthodontic wires during magnetic resonance imaging (MRI) at 1.5 Tesla.

BACKGROUND: Orthodontic appliances pose a potential risk during magnetic resonance imaging (MRI) due to forces on metallic objects within the static magnetic field of MRI systems. The aim of the present investigation was to measure forces on orthodontic wires caused by the static magnetic field of a 1.5-Tesla MRI system, and to assess the safety hazards associated with these forces. MATERIALS AND METHODS: Thirty-two different orthodontic wires (21 arch wires, eight ligature wires and three retainer wires) were investigated in a 1.5-Tesla MRI system (Magnetom Symphony, Siemens Medical Solutions, Erlangen, Germany). The translational forces were measured using the deflection angle test (ASTM F2052-02); rotational forces were assessed on a 5-point qualitative scale. RESULTS AND CONCLUSION: All retainer wires and the steel arch wires (the Noninium arch wire being the exception) were subjected to considerable rotational and translational forces within the MRI system's magnetic field. Translational forces were from 9.1- to 27.6-times as high as gravitational forces on these objects. Steel ligature wires and arch wires made of cobalt chromium, titanium molybdenum, nickel-titanium, and brass alloys showed no or negligible forces within the magnetic field. The translational and rotational forces within the MRI magnetic field should pose no risk to carefully-ligated arch wires. Steel retainer wire bonds should be checked to ensure secure attachment prior to an MRI investigation.

Custom base preaging in indirect bonding.

This in vitro evaluation analyzed the influence of custom base composite age on bond strength in indirect bonding. One hundred fifty permanent bovine mandibular incisors were randomly divided into 10 groups of 15 specimens each. Stainless steel brackets were bonded to the teeth using the Thomas indirect bonding technique using two different custom base composite-sealant combinations: (1) chemically cured Phase II composite and chemically cured Custom I.Q. sealant, and (2) light-cured Transbond XT composite and chemically cured Sondhi Rapid Set sealant. The composite custom bases were preaged for 24 hours and for seven, 15, 30, and 100 days. Shear bond strength tests for the two composite-sealant combinations showed no significant differences. Preaging of the custom base composite up to 30 days did not affect shear bond strength, and mean bond strength values exceeded 15 MPa in these groups. However, bond strength measurements for groups with a custom composite base aged for a longer interval (100 days) before sealant polymerization were significantly lower. On the basis of the results of this study, clinicians can safely use custom base composites aged up to 30 days when using the Thomas indirect bonding technique.

Effect of time on bond strength in indirect bonding.

The purpose of this in vitro investigation was to determine the influence of a reduced time interval before debonding on shear bond strength of stainless steel brackets bonded with a custom base indirect technique. A total of 135 bovine permanent mandibular incisors was randomly divided into nine groups of 15 specimens each. Three base composite-sealant combinations were investigated: (1) Phase II base composite, Custom I.Q. sealant, (2) Phase II base composite, Maximum Cure sealant, and (3) Transbond XT base composite, Sondhi Rapid Set sealant. Shear bond strength was measured for three different debonding time intervals: (1) time of transfer tray removal as recommended by the manufacturer, (2) 30 minutes after bonding of the sealant, and (3) 24 hours after bonding of the sealant. For groups bonded with Maximum Cure or Sondhi Rapid Set sealants, no influence of debonding time on shear bond strength was found. The Custom I.Q. sealant groups showed significantly lower bond strength measurements when debonded at the recommended tray removal time, and the Weibull analysis indicated a higher risk of bond failure at clinically relevant levels of stress. All base composite-sealant combinations showed acceptable bond strength at 30 minutes and 24 hours after bonding of the sealant.

In vitro investigation of indirect bonding with a hydrophilic primer.

The aim of this in vitro investigation was to evaluate bond strength for a custom base indirect bonding technique using a hydrophilic primer on moisture-contaminated tooth surfaces. Stainless steel brackets were bonded to 100 permanent bovine incisors using a light-cured custom base composite adhesive, a chemically cured sealant, and the hydrophilic primer Transbond MIP (3M-Unitek, Monrovia, Calif). Five groups (A-E) of 20 teeth each were formed according to the time of contamination (before or after application of the primer) and the type of contaminant (distilled water or saliva): A, control group with no contamination; B, contamination with saliva before application of the primer; C, contamination with water before application of the primer; D, contamination with saliva before and after application of the primer; and E, contamination with water before and after application of the primer. Mean bond strength for the group without contamination (A) was 15.07 +/- 4.14 MPa and was not significantly different from bond strengths for groups B (14.91 +/- 3.99 MPa) and C (16.12 +/- 3.67 MPa), in which contamination occurred before application of the hydrophilic primer. Average bond strength in group D was 11.92 +/- 4.76 MPa. The lowest mean bond strength was measured for group E (9.85 +/- 3.77 MPa) and was significantly lower than for groups A, B, and C. Contamination after primer application resulted in an increased risk of bond failure at clinically relevant levels of stress.

In vitro evaluation of a moisture-active adhesive for indirect bonding.

The aim of this in vitro investigation was to evaluate bond strength for a cyanoacrylate adhesive in combination with an indirect bonding technique. Eighty bovine permanent mandibular incisors were randomly divided into four groups of 20 teeth each. The influence of two factors on shear bond strength was investigated: (1) type of adhesive (Smartbond cyanoacrylate, Sondhi Rapid Set composite sealant) and (2) time of debonding (30 minutes and 24 hours after bonding). Stainless steel mesh-based brackets were used. Although, bond strength was not significantly different for the two debonding time periods, significantly lower bond strength measurements were found for the cyanoacrylate adhesive (P < .001). The mean bond strength for the cyanoacrylate adhesive group was 5.44 +/- 1.65 MPa for debonding 30 minutes and 6.92 +/- 1.48 MPa for debonding 24 hours after the bonding procedure vs 16.16 +/- 5.25 MPa and 14.98 +/- 2.85 MPa for the composite adhesive groups debonded at 30 minutes and 24 hours, respectively. The Weibull analysis indicated that there was an increased risk of bond failure at clinically relevant levels of stress for indirect bonding with the cyanoacrylate adhesive.

Bond strength with custom base indirect bonding techniques.

Different types of adhesives for indirect bonding techniques have been introduced recently. But there is limited information regarding bond strength with these new materials. In this in vitro investigation, stainless steel brackets were bonded to 100 permanent bovine incisors using the Thomas technique, the modified Thomas technique, and light-cured direct bonding for a control group. The following five groups of 20 teeth each were formed: (1) modified Thomas technique with thermally cured base composite (Therma Cure) and chemically cured sealant (Maximum Cure), (2) Thomas technique with thermally cured base composite (Therma Cure) and chemically cured sealant (Custom I Q), (3) Thomas technique with light-cured base composite (Transbond XT) and chemically cured sealant (Sondhi Rapid Set), (4) modified Thomas technique with chemically cured base adhesive (Phase II) and chemically cured sealant (Maximum Cure), and (5) control group directly bonded with light-cured adhesive (Transbond XT). Mean bond strengths in groups 3, 4, and 5 were 14.99 +/- 2.85, 15.41 +/- 3.21, and 13.88 +/- 2.33 MPa, respectively, and these groups were not significantly different from each other. Groups 1 (mean bond strength 7.28 +/- 4.88 MPa) and 2 (mean bond strength 7.07 +/- 4.11 MPa) showed significantly lower bond strengths than groups 3, 4, and 5 and a higher probability of bond failure. Both the original (group 2) and the modified (group 1) Thomas technique were able to achieve bond strengths comparable to the light-cured direct bonded control group.

Enamel conditioning for orthodontic bonding with a single-step bonding agent.

AIM: In-vitro evaluation of an alternative method to the conventional acid etch technique. MATERIAL AND METHOD: 240 human anterior and posterior teeth were divided into 16 groups of 15 teeth each. Group variables were: tooth type, enamel conditioning technique (Prompt L-Pop((R)): 3M Espe, Seefeld, Germany, or 37% phosphoric acid and bonding), adhesive (Transbond trade mark XT: 3M Unitek, Monrovia, CA, USA and ENlight((R)): Ormco, Orange, CA, USA), and testing procedure (shear and tensile bond strength). Upper lateral incisors and premolar brackets (Mini-Diamond((R)): Ormco, Orange, CA, USA) were used. Intergroup differences were analyzed by an analysis of variance. The enamel surface and the failure mode of debonded specimens were investigated with light and scanning electron microscopy. RESULTS: Despite a tendency towards a higher bond strength after phosphoric acid conditioning, no statistically significant differences were found between the enamel conditioning methods. Statistically significant differences were recorded for the different adhesives: bond strength with Transbond trade mark XT was higher than with Enlight((R)). CONCLUSION: The single-step bonding agent sems to provide an acceptable bond strength between adhesive and enamel. No enamel fractures were detected. In vivo studies will be conducted to investigate the clinical performance of the new material.

The fracture behaviour of dental enamel.

Enamel is the hardest tissue in the human body covering the crowns of teeth. Whereas the underlying dental material dentin is very well characterized in terms of mechanical and fracture properties, available data for enamel are quite limited and are apart from the most recent investigation mainly based on indentation studies. Within the current study, stable crack-growth experiments in bovine enamel have been performed, to measure fracture resistance curves for enamel. Single edge notched bending specimens (SENB) prepared out of bovine incisors were tested in 3-point bending and subsequently analysed using optical and environmental scanning electron microscopy. Cracks propagated primarily within the protein-rich rod sheaths and crack propagation occurred under an inclined angle to initial notch direction not only due to enamel rod and hydroxyapatite crystallite orientation but potentially also due to protein shearing. Determined mode I fracture resistance curves ranged from 0.8-1.5 MPa*m(1/2) at the beginning of crack propagation up to 4.4 MPa*m(1/2) at 500 microm crack extension; corresponding mode II values ranged from 0.3 to 1.5 MPa*m(1/2).

Size-dependent elastic/inelastic behavior of enamel over millimeter and nanometer length scales.

The microstructure of enamel like most biological tissues has a hierarchical structure which determines their mechanical behavior. However, current studies of the mechanical behavior of enamel lack a systematic investigation of these hierarchical length scales. In this study, we performed macroscopic uni-axial compression tests and the spherical indentation with different indenter radii to probe enamel's elastic/inelastic transition over four hierarchical length scales, namely: 'bulk enamel' (mm), 'multiple-rod' (10's microm), 'intra-rod' (100's nm with multiple crystallites) and finally 'single-crystallite' (10's nm with an area of approximately one hydroxyapatite crystallite). The enamel's elastic/inelastic transitions were observed at 0.4-17 GPa depending on the length scale and were compared with the values of synthetic hydroxyapatite crystallites. The elastic limit of a material is important as it provides insights into the deformability of the material before fracture. At the smallest investigated length scale (contact radius approximately 20 nm), elastic limit is followed by plastic deformation. At the largest investigated length scale (contact size approximately 2 mm), only elastic then micro-crack induced response was observed. A map of elastic/inelastic regions of enamel from millimeter to nanometer length scale is presented. Possible underlying mechanisms are also discussed.

Crack arrest within teeth at the dentinoenamel junction caused by elastic modulus mismatch.

Enamel and dentin compose the crowns of human teeth. They are joined at the dentinoenamel junction (DEJ) which is a very strong and well-bonded interface unlikely to fail within healthy teeth despite the formation of multiple cracks within enamel during a lifetime of exposure to masticatory forces. These cracks commonly are arrested when reaching the DEJ. The phenomenon of crack arrest at the DEJ is described in many publications but there is little consensus on the underlying cause and mechanism. Explanations range from the DEJ having a larger toughness than both enamel and dentin up to the assumption that not the DEJ itself causes crack arrest but the so-called mantle dentin, a thin material layer close to the DEJ that is somewhat softer than the bulk dentin. In this study we conducted 3-point bending experiments with bending bars consisting of the DEJ and surrounding enamel and dentin to investigate crack propagation and arrest within the DEJ region. Calculated stress intensities around crack tips were found to be highly influenced by the elastic modulus mismatch between enamel and dentin and hence, the phenomenon of crack arrest at the DEJ could be explained accordingly via this elastic modulus mismatch.

Torque stability of plastic brackets following multiple loading and artificial material aging--an in-vitro comparison.

OBJECTIVE: The objective of this study was to compare the loaddeflection behavior of plastic brackets made of various materials in response to repeated torque loads with each other and with steel brackets. Material fatigue during wire's play in the bracket slot, the brackets' elasticity and the torsional forces applied were analyzed. MATERIAL AND METHODS: Groups of ten brackets, each made of pure polycarbonate or variously reinforced polycarbonate or polyurethane, with and without a metal slot, were artificially aged and then torqued with a testing machine five times consecutively in a torque- measuring apparatus. The control group consisted of ten steel brackets. The resulting forces were recorded with the testing machine, and the wire's deflection recorded with a digital goniometer on a PC and submitted to one-way variance analysis at p < 0.05. RESULTS: There were strong fluctuations among the bracket types in both the play of the wire in the bracket slot as well as the brackets' elasticity. The slot of all the polycarbonate-based brackets was bent open after a single load, except for those with a metal slot. After a single load of up to 20 degrees torque, all the brackets exhibited a significant loss of torque stability ranging between 5% for pure polyurethane and 28.5% for ceramic-reinforced polycarbonate. The loss of torque stability was roughly 17% on average. This loss did not increase significantly when additional loads were applied. CONCLUSIONS: Each bracket material requires its own torque value to transfer identical torque values onto the tooth in clinical practice. Comparison with steel brackets revealed that only plastic brackets with a metal slot are suitable for clinical use. Adding ceramic and glass fibers to polycarbonate, or using polyurethane has no benefit in terms of torque stability. In addition, after a single application of torque, all brackets lose torque stability in response to a renewed load.

Determination of the elastic/plastic transition of human enamel by nanoindentation.

OBJECTIVES/METHODS: From a materials scientist's perspective, dental materials used for tooth repair should exhibit compatible mechanical properties. Fulfillment of this criterion is complicated by the fact that teeth have a hierarchical structure with changing mechanical behavior at different length scales. In this study, nanoindentation with an 8 microm spherical indenter was used to determine the elastic/plastic transition under contact loading for enamel. RESULTS: The indentation elastic/plastic transition of enamel at the length scale of several hundreds of hydroxyapatite crystallites, which are within one enamel rod, is revealed for the first time. The corresponding penetration depth at the determined indentation yield point of 1.6GPa and 0.6% strain is only 7 nm. As a consequence of the small depth it is decisive for the experiment to calibrate the indenter tip radius in this loading regime. The elastic modulus of 123GPa was evaluated directly by the Hertzian penetration and not by the unloading part of the indentation curve. SIGNIFICANCE: We believe these data are also a valuable contribution to understand the mechanical behavior of enamel and to develop nanoscale biomimetic materials.

Radiofrequency-induced heating near fixed orthodontic appliances in high field MRI systems at 3.0 Tesla.

OBJECTIVE: To assess radiofrequency (RF)-induced heating of fixed orthodontic appliances during acquisition of three different sequences in magnetic resonance imaging (MRI) at 3 Tesla. MATERIALS AND METHODS: Ten commonly used fixed orthodontic appliances were investigated utilizing a phantom head and simulating the in vivo intraoral situation. A 3 Tesla MRI system (Intera, Philips Medical Systems, Best, The Netherlands) was used to acquire T1w spin-echo (T1 SE), T1w turbo spin-echo (T1 TSE) and T1w gradient-echo (T1 GRE) sequences in axial orientation. Continuous temperature measurement was performed with a dedicated four channel fluoroptic thermometry system. For each orthodontic appliance temperature probes were placed at three predefined sites in order to perform temperature measurements during MR imaging. The fourth temperature probe was fixed to the neck of the phantom head and served as the reference. Mean temperature alterations were determined for all appliances. RESULTS: Temperature elevations ranged from -0.3 degrees C to 0.2 degrees C and were negligible for all orthodontic appliances investigated. There was no difference in mean temperature alteration for any of the three imaging sequences. CONCLUSION: Based on the data of our experimental study the radiofrequency-induced heating of orthodontic brackets during high field MRI at 3 Tesla can be categorized as negligibly low. Even the clinical routine examination of the head at 3 Tesla using high-energetic pulse sequences can be applied without hesitation in patients with fixed orthodontic appliances.

Side effects of a non-peroxide-based home bleaching agent on dental enamel.

Changes in the chemistry and structure of enamel due to a non-peroxide-based home bleaching product (Rapid White) were studied in vitro using attenuated total reflectance-infrared spectroscopy, Raman spectroscopy, electron probe microanalysis, flame atomic absorption spectroscopy, and total reflection X-ray fluorescence. The results revealed that the citric-acid-containing gel-like component of the bleaching system substantially impacts on the dental hard tissue. Enamel is affected on several levels: (i) the organic component is removed from superficial and deeper enamel layers and remnants of the bleaching gel are embedded in the emptied voids; (ii) cracks and chemical inhomogeneities with respect to Ca and P occur on the surface; and (iii) within a submicron layer of enamel, the Ca-O bond strength in apatite decreases, thus enhancing calcium leakage from the bleached enamel hard tissue.