Microstructural analysis of Co-Cr dental alloy at the metal-porcelain interface: a pilot study.

OBJECTIVE: The purpose of the study was to observe whether conventional porcelain firings had an effect on the underlying microstructure of cobalt-chromium alloys used in porcelain-fused-to-metal systems. METHODS: One as cast (non-veneered) and two porcelain veneered Co-Cr specimens layered with and without tungsten(W)-metal conditioner were manufactured and analysed. Electron backscatter diffraction was used to determine the crystal structures and grain size across the porcelain-fused-to-metal interface. RESULTS: No difference was found in the microstructure of the alloy in both with and without W-metal conditioner. For the porcelain fired specimens, disparately sized granular structures were observed adjacent to the metal-porcelain interfaces compared to the bulk of the metal. Ellipsoid shaped grains at the alloy surface ranged between 1-11 µm in diameter and averaged 2.70 µm (SD: 2.17 µm) for the specimen layered with W-metal conditioner and 2.86 µm (SD: 1.85 µm) for the specimen layered without W-metal conditioner. Grains located in the bulk were > 200 µm with dendritic-like features. The depth of the fine grain structure adjacent to the surface had an average depth of 15 µm. The crystal structure of the surface layer was found to be predominantly hexagonal close-packed whereas the underlying bulk was a mixture of both face-centered cubic and hexagonal close-packed phases. For the as cast specimen, similar large grains of over 200 µm was observed but exhibited no dendritic like features. In addition, no fine grains were observed at the surface region of the as cast alloy. CONCLUSION: Conventional porcelain firings altered the interfacial and bulk microstructure of the alloy while the presence of the W-metal conditioner had no influence on the underlying alloy microstructure.

X-ray microdiffraction, TEM characterization and texture analysis of human dentin and enamel.

Human tooth is a complex bioceramic composite, which consists of enamel, dentin and the interface, the dentin-enamel junction (DEJ). The crystal properties and ultrastructure of the inorganic phase through the thickness of healthy human molar teeth were investigated using X-ray microdiffraction (µXRD), electron diffraction and transmission electron microscopy (TEM) techniques. The XRD data were analysed using the Le Bail profile fitting approach. The size and the texture of the crystallites forming enamel and dentin in the crown part of teeth were measured using both techniques and then compared. Results showed that the thickness of dentin crystallites was found to decrease towards the DEJ, whereas the thickness of the enamel crystallites increased from the DEJ towards the outer layers. It was demonstrated that enamel exhibited an increase of texture in 002 lattice planes from the DEJ towards the outer layers. Texture was also detected in 102 lattice planes. The texture effect in 002 planes at the scale of less than 1 µm was also demonstrated in dentin. The variation of lattice parameters as a function of the position within the thickness of dentin and enamel was also observed. The values of the nonuniform microstrain in the dentin and enamel crystallites were from 1.40 × 10(-6) % to 4.44 × 10(-5) %. The good correlation between XRD and TEM indicated that µXRD is a useful technique to study crystallography and microstructure of heterogeneous enamel and dentin. The observed gradient characteristics of texture and crystallite size in enamel and dentin maybe an evolutionary outcome to resist wear and fracture, thereby contributing to the excellent mechanical properties of teeth.

Identifying the source of bullet wipe: a randomised blind trial.

OBJECTIVE: To assess the usefulness of scanning electron microscopy and energy dispersive x-ray spectroscopy in matching bullet wipe to the bullet. HYPOTHESIS: Bullet wipe can be used to match a bullet type to a crime scene.

Gunshot induced indirect femoral fracture: mechanism of injury and fracture morphology.

INTRODUCTION: Indirect ballistic fractures occur when a projectile passes close to, but not contacting, the bone. The mechanism of how these fractures occur is not yet proven, but recently the acoustic shockwave has been excluded as a cause. The objective of this study is to determine whether the expanding temporary cavity, the collapse of this cavity or its oscillation causes these fractures. In addition, we describe the fracture morphology and biomechanical causes of this injury. METHOD: 40 fresh deer femora were strain gauged and embedded in ballistic gelatin before being shot with four different projectiles with varying distances off the bone. Pressure recordings, chronographs and radar allowed assessment of local pressures and energy transfer. High-speed video allowed the temporal relationship between the temporary cavity and fracture formation to be analysed, while sample dissection allowed the fracture morphology to be described. RESULTS: The fractures produced were consistently wedge-shaped and caused by the expansion of the temporary cavity, flexing the bone beyond its yield point, causing tension failure on the cortex opposite the expanding temporary cavity and a compression wedge on the side of the cavity. Local pressure was not predictive of fracture formation but the energy transfer to the gelatin block was predictive. CONCLUSIONS: Indirect fractures are caused by the expansion of the temporary cavity and relate to the proximity of this cavity to the bone. Fractures occur from flexion of the bone and classically display wedge-shaped fracture patterns with the apex of the wedge pointing away from the expanding cavity.

Tooth wear and wear investigations in dentistry.

Tooth wear has been recognised as a major problem in dentistry. Epidemiological studies have reported an increasing prevalence of tooth wear and general dental practitioners see a greater number of patients seeking treatment with worn dentition. Although the dental literature contains numerous publications related to management and rehabilitation of tooth wear of varying aetiologies, our understanding of the aetiology and pathogenesis of tooth wear is still limited. The wear behaviour of dental biomaterials has also been extensively researched to improve our understanding of the underlying mechanisms and for the development of restorative materials with good wear resistance. The complex nature of tooth wear indicates challenges for conducting in vitro and in vivo wear investigations and a clear correlation between in vitro and in vivo data has not been established. The objective was to critically review the peer reviewed English-language literature pertaining to prevalence and aetiology of tooth wear and wear investigations in dentistry identified through a Medline search engine combined with hand-searching of the relevant literature, covering the period between 1960 and 2011.

Structure and compositional characteristics of caniniform dental enamel in the tuatara Sphenodon punctatus (Lepidosauria: Rhynchocephalia).

OBJECTIVE: The evolution of dental tissues in relation to tooth function is poorly understood in non-mammalian vertebrates. We studied the dentition of Sphenodon punctatus, the sole remaining member of the order Rhynchocephalia in this light. METHODS: We examined 6 anterior maxillary caniniform teeth from adult Sphenodon by scanning electron microscopy, nano-indentation and Raman spectroscopy. RESULTS: The elastic modulus (E) for tuatara enamel was 73.17 (sd, 3.25) GPa and 19.52 +/- 0.76 Gpa for dentine. Hardness (H) values for enamel and dentine were 4.00 (sd, 0.22) and 0.63 +/- 0.02 Gpa respectively. The enamel was thin (100 gm or less), prismless and consisted of grouped parallel crystallites. Incremental lines occurred at intervals of about 0.5 to 1 rm. There were tubular structures along the enamel dentine junction running from the dentine into the inner enamel, at different angles. These were widened at their base with a smooth, possibly inorganic lining. Enamel elastic modulus and hardness were lower than those for mammals. CONCLUSIONS: The presence of enamel tubules in the basal part of the enamel along the EDJ remains speculative, with possible functions being added enamel/dentinal adhesion or a role in mechanosensation.

Indentation of the cornea: A Bi-layer contact problem.

Histological observations of the cornea have identified the presence of multiple layers with differing thickness and function. The composition of the cornea consists primarily of collagen fibrils held together with proteoglycans but with an aqueous interstitial component being dominant. Indentation provides a means to quantify the spatial variation of the mechanical properties of the cornea, however the role of the different layers on the indentation response has barely been addressed. In addition, the response of the fluid content and its displacement during indentation has not been adequately considered. In this study indentation of the cornea with a relatively large spherical tipped indenter (R = 500 µm) is considered. It was observed that the initial phase of loading did not fit a classic Hertz elastic response but showed an initial steeper slope that gradually declines with increasing force and displacement. A relatively simple approach is developed that initially considers the cornea as a poro-elastic bi-layer contact problem, that is the presence of an outer thin stiffer Bowman's layer overlaying the thicker less stiff stroma.

Nano-indentation characterisation of natural carious white spot lesions.

The aim of this paper was to characterise the mechanical properties (MPs) and microstructural features of natural enamel white spot lesions (WSLs) using nano-indentation. Five natural WSLs from 4 extracted sound premolar teeth were cross-sectioned. Elastic modulus and hardness were measured systematically across the WSLs at intervals of 25 and 50 microm. The WSLs showed a large reduction in MPs compared to sound counterpart: elastic modulus was up to 83% lower (77.0 +/- 2.2 to 13.4 +/- 2.1 GPa) and hardness up to 91% lower (3.39 +/- 0.41 to 0.29 +/- 0.07 GPa). The intact surface layer above WSLs had less than 34% reduction in MPs. Detailed MP measurements were mapped as two-dimensional contour plots. Typically, WSLs displayed steep MP gradients at the lesion boundary and more uniform MPs with isolated variations in the lesion body. Despite the large reduction in MPs, the microstructure of WSLs remained intact. We postulate that loss of mineral and change of the hierarchical microstructure at the crystallite level contributed to the overall MPs of WSLs.

Elemental composition of imported porcelain-fused-to-metal crowns--a pilot study.

OBJECTIVES: To identify any potentially toxic elements in porcelain-fused-to-metal (PFM) crowns and a bridge manufactured in China. MATERIALS AND METHODS: Eight PFM crowns and part of a bridge were sourced from China for testing. They were given a typical glaze firing cycle prior to scanning electron microscope analysis. Electron dispersive spectroscopic spot and mapping analysis was carried out on the porcelain/metal collar interface areas in order to determine their elemental composition and distribution. RESULTS: No toxic elements were detected. The alloy used in the crowns was a nickel-chromium base metal, and that in the bridge was a gold-palladium noble alloy. The veneering porcelain was similar to a standard dental veneering porcelain. CONCLUSIONS: Within the limitations of the testing method and small sample size, no toxic elements were detected.

A system of calibrating microtomography for use in caries research.

Desktop microcomputed tomography (micro-CT) offers a non-invasive 3-dimensional analysis of structures and their physical properties. To date, the use of micro-CT has mostly involved qualitative observations, with the extent of quantitative analysis relying on automated internal calibration by the micro-CT control software. However, the value of such calibration is limited by machine drift. For an accurate quantitative use of micro-CT, it is recognized that external means of calibration are needed. A novel system of calibration standards, also known as 'phantoms', is presented. A range of low mineral concentration phantoms involving triethylene glycol dimethacrylate/glycerolate dimethacrylate resin mixed with commercial pure hydroxyapatite (HAP), from 0.07 to 1.05 g/cm(3), was fabricated. Sintered HAP was impregnated with the same resin, producing phantoms with medium-level mineral concentrations up to 1.90 g/cm(3). These phantoms were easy to create, proved accurate and stable with repeated use, and were found to mimic the composite nature of dental enamel and dentine structures under investigation.

Thermal induced deflection of a porcelain-zirconia bilayer: Influence of cooling rate.

OBJECTIVE: To determine the thermal expansion of a porcelain (VM9) and tetragonal zirconia (Y-TZP) as well as the deflection upon re-heating and cooling of a bilayer fabricated from these two materials after slow and rapid cooling during initial fabrication. METHODS: The coefficient of thermal expansion (CTE) of bulk porcelain and Y-TZP as well as bilayer beam deflection was measured with a novel non-contact optical dilatometer. The influence of cooling rate during initial fabrication of the porcelain-zirconia bilayer and the bulk porcelain during subsequent heating and cooling is investigated. Specimens were heated to 900°C in the dilatometer, well in excess of the glass transition temperature (Tg) and softening temperature (Ts) of the porcelain. RESULTS: The thermal expansion of the porcelain above Tg exhibits a threefold increase in CTE over that observed below Tg. Observations of the bilayer deflection reflect the difference in the CTE of the component materials and enable Tg and Ts temperatures for the porcelain to be estimated. Initial cooling rate of the porcelain and porcelain-YTZP bilayer was found to have a profound influence on the subsequent response to slow reheating and cooling as well as the resultant residual deflection. SIGNIFICANCE: The estimation of the residual stress and potential for chipping of porcelain-zirconia dental restorative systems should not be based solely on thermal expansion data measured below Tg.

Size or hierarchical dependence of the elastic modulus of three ceramic-composite CAD/CAM materials.

OBJECTIVE: To measure the elastic modulus of three ceramic-composite CAD/CAM materials at three different microstructural dimensions: macro, micro, and nano. METHODS: Three novel ceramic-composite CAD/CAM materials (Enamic, Lava Ultimate, and Cerasmart) were investigated. Rectangular cross-sections 10 × 5.7 × 1 mm3 (n = 30) were cut from standard sized milling blocks of each material prior to polishing. Specimens were macro-tested using three-point bending and with a dynamic mechanical analyzer (DMA), micro-tested using a nano-indentation system, and finally at the nano-level with an atomic force microscope (AFM). Data were analyzed with 1-way ANOVA (α = 0.05). RESULTS: At the macro level Enamic showed the highest elastic modulus, followed by Lava Ultimate and Cerasmart respectively (p < 0.001). Measurements at the micro and nano level resulted in bimodal distributions of the elastic modulus values associated with the various phases present with values higher and lower than measured at the macro level. Only at the nano-level were the various phases of Cerasmart able to be distinguished. CONCLUSIONS: The tested materials showed different elastic modulus at the different size or hierarchical levels that enabled comparison with the hierarchical values of enamel. SIGNIFICANCE: Studying the mechanical properties of these novel materials at different size or hierarchical scales can help to understand their potential clinical performance, such as structural durability and opposing tooth wear and lead to more biomimetic like dental restorative materials.

The dehydration effect on mechanical properties of tooth enamel.

Exploring the subtle mechanical property changes of tooth enamel in different conditions is important for dental research. However, some experimental results can be deceptive and may lead to misunderstanding. In particular, we show the dehydration associated with increased mechanical properties of tooth enamel as monitored by Nanomechanical System Testing (NST) can be misleading. The results indicate that the friction coefficient decreased with an increase of hardness of enamel upon dehydration, which appears to imply that dehydrated enamel has better mechanical properties than hydrated enamel. However, more critical scrutiny of the actual situation, suggests dehydrated teeth enamel are more prone to damage and greater wear. To appreciate the basis for the contrast between the experimental results and reality of natural hydrated enamel, which has better resistance to wear, and is critical for an understanding of the aetiology of enamel resistance to fracture.

Micromechanical property recovery of human carious dentin achieved with colloidal nano-beta-tricalcium phosphate.

Reconstitution of carious dentin has been recognized as difficult, because it progresses by loss of collagen polymerization and by demineralization under acidic conditions. Recently, colloidal alkaline nano-calcium phosphate, prepared by electrical discharge in a buffered physiological saline solution, has been shown to be effective in the formulation of a bone-like biocomposite by simply being mixed with acidic collagen solution. It was hypothesized that colloidal calcium phosphate was suitable for the reconstitution of carious dentin. Natural caries lesions in dentin from permanent teeth were exposed to colloidal hydroxyapatite and beta-tricalcium phosphate for 10 days. The micromechanical properties of these tissues were evaluated by nano-indentation. The elastic modulus of human carious dentin improved after samples were immersed in colloidal beta-tricalcium phosphate. The mineral density of carious dentin exposed to beta-tricalcium phosphate increased more than that immersed in hydroxyapatite. However, since it was not directly proportional to micromechanical recovery, mineral density alone was not a sufficient indicator of mechanical behavior.

Relationship between nanohardness and mineral content of artificial carious enamel lesions.

The aim of this study was to compare cross-sectional nanohardness, measured using an ultra-microindentation system, with mineral content, from transversal microradiography, of artificial enamel caries lesions. Sections (85 +/- 10 microm) from 16 bovine enamel samples with artificial caries were prepared. The mineral content and cross-sectional nanohardness at known depths from the surface were compared. Both methods showed lesion profiles with a surface layer. The determination of nanohardness seems limited to lesions with a mineral content >45 vol%. There was a moderate linear relationship between mineral content and the square root of nanohardness (R2 = 0.81). It was concluded that the conversion of cross-sectional hardness into mineral content remains questionable and cannot be recommended.

Relationship between laser fluorescence and enamel hypomineralisation.

OBJECTIVES: To study the relation between the mechanical properties of hypomineralised enamel, and its laser fluorescence (LF). METHODS: Five extracted teeth with molar-incisor hypomineralisation (MIH) were sectioned longitudinally through the defects and polished to prepare the hypomineralised enamel for testing. Hardness (H) and elastic modulus (E) of enamel were measured using nanoindentation. Measurement recording started from the cervicoenamel junction and proceeded occlusally in increments of 200 microm. Laser fluorescence readings were taken along the same line and at the same sites using a DIAGNOdent pen. RESULTS: H, E, and LF readings from cervical enamel were within the expected range for normal sound enamel. After log transformation of the H and E measurements to allow for linear correlation analysis, there was a significant and moderately strong inverse correlation between LF and H or E samples (r (between specimens)=0.59, r (between specimens)=0.39, respectively; p<0.001). CONCLUSIONS: This study shows that, in the absence of dental caries, increased DIAGNOdent readings can indicate enamel hypomineralisation. While the increased LF readings in carious enamel are thought to be related to the presence of caries bacterial metabolites, the increased readings in hypomineralised enamel may be related to proteins in the hypomineralised enamel and/or light scattering by the inhomogeneous enamel.

FTIR characterization of the setting reaction of biodentine™.

OBJECTIVE: To provide insight of the setting reactions of Biodentine™, a hydraulic calcium silicate cement, based upon observations using Fourier Transform Infra-Red (FTIR) spectroscopy. METHODS: FTIR spectra of components before and during the setting reaction were taken using the attenuated total reflectance (ATR) technique. Measurements over wavelengths 600-4000cm-1 were taken at regular intervals for two days. RESULTS: FTIR spectrum of Biodentine™ powder revealed a number of peaks from 650 to 1100cm-1 and a plateau from 1400 to 1500cm-1, indicative of SiO and CO3-bonding, while the mixing fluid exhibited water peaks. Results following mixing displayed three distinct regimes; (i) incubation phase, during the first 35min, when minimal change occurred, (ii) rapid transitory stage, between 35 and 90min, when major changes occurred, and (iii) slow sustained reaction stage for remaining 45h. Incubation appears to be associated with the presence of CO3-peaks. The transition region indicates formation of CaOH and Jennite OH-peaks, anticipated intermediate reaction phases. At 90min, the end of second stage, CaOH and Jennite are replaced by a dominant Portlandite (Ca(OH)2)-peak and minor presence of Tobermorite, another anticipated intermediate phase, and water reduction. During the following 45h Portlandite and Tobermorite decline while the water peak increases. SIGNIFICANCE: FTIR can be used to follow the chemical reactions in dental cements and provides insight into the relatively slow setting reactions of hydraulic calcium silicate cements.

Influence of ageing on glass and resin bonding of dental glass-ceramic veneer adhesion to zirconia: A fracture mechanics analysis and interpretation.

Adhesion plays a major role in the bonding of dental materials. In this study the adhesion of two glass-ceramic systems (IPS e.max and VITABLOCS) to a zirconia sintered substrate using a glass (for IPS e.max) and resin (VITABLOCS) before and after exposure to ageing for 14 days in distilled water at 37 °C are compared using two interfacial fracture mechanics tests, the 3 point bend Schwickerath (Kosyfaki and Swain, 2014; Schneider and Swain, 2015) and 4 point bend (Charalambides et al., 1989) approaches. Both tests result in stable crack extension from which the strain energy release rate (G, N/m or J/m2) can be determined. In the case of the 3 PB test the Work of Fracture was also determined. In addition, the Schwickerath test enables determination of the critical stress for the onset of cracking to occur, which forms the basis of the ISO (ISO9693-2:2016) adhesion test for porcelain ceramic adhesion to zirconia. For the aged samples there was a significant reduction in the resin-bonded strengths (Schwickerath) and strain energy release rate (both 3 and 4 PB tests), which was not evident for the glass bonded specimens. Critical examination of the force-displacement curves showed that ageing of the resin resulted in a major change in the form of the curves, which may be interpreted in terms of a reduction in the critical stress to initiate cracking and also in the development of an R-curve. The extent of the reduction in strain energy release rate following ageing was greater for the Schwickerath test than the Charalambides test. The results are discussed in terms of; the basic mechanics of these two tests, the deterioration of the resin bonding following moisture exposure and the different dimensions of the specimens. These in-vitro results raise concerns regarding resin bonding to zirconia. STATEMENT OF SIGNIFICANCE: The present study uses a novel approach to investigate the role of ageing or environmental degradation on the adhesive bonding of two dental ceramics to zirconia. This continues to be a major clinical problem but current approaches, till now, have relied upon a myriad of strength based tests to quantify the extent of environmental degradation with time. In this paper we use two fracture mechanics approaches, based upon simple 3 and 4 point bend testing procedures that enable stable debonding crack extension to occur. The paper provides a more critical approach to evaluate the role of environmental degradation of adhesion for dental materials.

Frictional coefficient during flossing of teeth.

OBJECTIVE: This in-vitro study aimed to develop a technique to measure the frictional forces and determine the frictional coefficient (µ) associated with the rubbing of dental floss against teeth. Incorrect flossing technique and the etiology of grooves at the cementoenamel junction (CEJ) of proximal area of teeth has long been a controversial topic. We hypothesized that the µ between teeth surfaces and dental floss is affected by contact angulation. MATERIALS AND METHODS: Tests were conducted using two different types of dental floss (waxed and unwaxed nylon) on different surfaces (enamel, dentine, smooth and rough glass rods) under different moisture conditions (dry and wet). The µ generated by performing C-shape flossing was measured, using the Capstan equation, at constant load (100g) over different flossing contact sliding angulations. In addition, the surface characteristics of intact and used nylon flosses were compared using a scanning electron microscope (SEM). RESULTS: The mean µ was highest with a smooth glass rod (0.42±0.11), followed by rough glass rods (0.30±0.07), dry enamel (0.27±0.08), wet enamel (0.23±0.06), then dentine (0.18±0.04). Moreover, higher µ was associated with waxed floss when used against dry enamel, smooth and rough glass rods (P<0.001). At different moisture conditions, waxed floss demonstrated greater µ with dry surfaces (P<0.03). No association was found between µ and dental floss contact angulation. Both floss types showed deterioration after usage; although waxed type exhibited markedly greater deterioration when used on dry surfaces. In conclusion, the magnitude of the µ was found to be influenced by surface roughness, moisture condition, and independent of the contact angulation area during sliding of dental floss. SIGNIFICANCE: It is important to consider the potential side effects of frictional forces on both tooth surface and dental floss during clinical application.

Modelling of fracture behaviour in biomaterials.

One of the most frequent causes of degradation and failure of quasi-brittle biomaterials is fracture. Mechanical breakdown, even when not catastrophic, is of particular importance in the area of biomaterials, as there are many clinical situations where it opens the path for biologically mediated failures. Over the past few decades the materials/biomaterials community has developed a number of numerical models, but only with limited incorporation of brittle failure phenomena. This article investigates the ability of a non-linear elastic fracture mechanics (NLEFM) model to reliably predict failure of biomaterials with a specific focus on the clinical settings of restorative dentistry. The approach enables one to predict fracture initiation and propagation in a complex biomechanical status based on the intrinsic material properties of the components. In this paper, we consider five examples illustrating the versatility of the present approach, which range from the failure of natural biomaterials, namely dentine and enamel, to a restored tooth, a three unit all ceramic bridge structure and contact-induced damage in the restorative layered materials systems. It is anticipated that this approach will have ramifications not only to model fracture events but also for the design and optimisation of the mechanical properties of biomaterials for specific clinically determined requirements.