Letteratura scientifica selezionata sul tema "Enamel, Nanoindentation, Mechanical properties, dental materials"

In the last decade, most publications on the mechanical properties of dental calcified tissues were based on nanoindentation investigation. This technique has allowed a better understanding of the mechanical behavior of enamel, dentin, and cementum at a nanoscale. The indentations are normally carried out using pointed or spherical indenters. Hardness and elastic modulus are measured as a function of indenter penetration depth and from the elastic recovery upon unloading. The unique microstructure of each calcified tissue significantly contributes to the variations in the mechanical properties measured. As complex hydrated biological composites, the relative proportions of the composite components, namely, inorganic material (hydroxyapatite), organic material, and water, determines the mechanical properties of the dental hard tissues. Many pathological conditions affecting dental hard tissues cause changes in mineral levels, crystalline structures, and mechanical properties that may be probed by nanoindentation. This review focuses on relevant nanoindentation techniques and their applications to enamel, dentin, and cementum investigations.

The presented paper is mainly focused on nanoindentation of damaged human teeth, which have been treated with amalgam filling and describing the micromechanical properties (reduced elastic modulus Er and hardness H). The analysis was carried out on two samples of tooth no. 37, the first from a woman (48 years old) and the second from a man (26 years old). For both teeth was the main cause of the extraction an advanced stage of periodontitis chronica. The provided treatment of the tooth decay has been realized using amalgam filling with a different depth of cavity drilling. Within the analysis, we have made a series of indentation experiments in the transversal sections of the teeth. In these sections, we have measured the mechanical properties in individual dental materials for the sake of determining the influence of the degradation of dentin damaged by tooth decay. The differences of micomechanical parameters occur in the dentin area (Er ≈ 7.6 GPa in the dentin-amalgam interface and Er ≈ 30.2 GPa in the center of the dentin wall). Lesser variance of values is present in the enamel area, where the difference is less than 11 % in the enamel-amalgam interface.

In this study, the mechanical properties of human dental structures have been investigated by using instrumented nanoindentation. Immersion in solutions containingStreptococcus mutans, which is the principal cause of dental caries, was applied to tooth specimens to clarify its effect on the microstructure and mechanical properties of the dental structures. With an extended time of up to 16 h, the pH value of theS. mutanssolutions dropped from 7.3 to 5.8. Therefore, after immersion in theS. mutanssolutions for 16 h, slight erosions of the dental structures began; after 64 h, severe tooth decay occurred with obviously etched dental features. After 128 h, the elastic modulus of enamel and dentine dropped to 85 and 67%, respectively, of the original values of untreated specimens, and the hardness dropped to 88 and 55%, respectively.

In this paper, an overview on nanoindentation and its combination with AFM is presented with regard to current instrument technology and applications on dental and bony tissues. Nanoindentation has been a widely used technique to determine the mechanical properties such as nanohardness and Young’s modulus for nanostructured materials. Especially, atomic force microscopy (AFM) combined with nanoindentation, with the pit positions controlled accurately, become a powerful technique used to measure mechanical properties of materials on the nanoscale, and has been applied to the study of biological hard tissues, such as bone and tooth. Examples will be shown that significantly different nanohardness and modulus in the isolated domains within single enamel, the prisms, interprisms, the surrounding sheaths and the different parts of skeletal bone, could been distinguished, while such information was unable to be obtained by traditional methods of mechanical measurements.

Enamel formation and quality are dependent on environmental conditions, including exposure to fluoride, which is a widespread natural element. Fluoride is routinely used to prevent caries. However, when absorbed in excess, fluoride may also lead to altered enamel structural properties associated with enamel gene expression modulations. As iron plays a determinant role in enamel quality, the aim of our study was to evaluate the iron metabolism in dental epithelial cells and forming enamel of mice exposed to fluoride, as well as its putative relation with enamel mechanical properties. Iron storage was investigated in dental epithelial cells with Perl’s blue staining and secondary ion mass spectrometry imaging. Iron was mainly stored by maturation-stage ameloblasts involved in terminal enamel mineralization. Iron storage was drastically reduced by fluoride. Among the proteins involved in iron metabolism, ferritin heavy chain (Fth), in charge of iron storage, appeared as the preferential target of fluoride according to quantitative real-time polymerase chain reaction, Western blotting, and immunohistochemistry analyses. Fluorotic enamel presented a decreased quantity of iron oxides attested by electron spin resonance technique, altered mechanical properties measured by nanoindentation, and ultrastructural defects analyzed by scanning electron microscopy and energy dispersive x-ray spectroscopy. The in vivo functional role of Fth was illustrated with Fth+/-mice, which incorporated less iron into their dental epithelium and exhibited poor enamel quality. These data demonstrate that exposure to excessive fluoride decreases ameloblast iron storage, which contributes to the defective structural and mechanical properties in rodent fluorotic enamel. They raise the question of fluoride’s effects on iron storage in other cells and organs that may contribute to its effects on population health.

Human teeth are exposed to various chemical and mechanical factors. From mechanical point of view it includes attrition, abrasion or their combination. Teeth and dental restorative materials are subjected to normal and shear loads. Therefore the contact-based stresses during mastication and teeth wear are of considerable importance. In order to study wear behavior of enamel, dentine and two dental restorative composite materials scratch test at various contact conditions was employed. Hardness and elastic modulus were measured using nanoindentation with spherical and pyramidal indenters. Residual wear tracks were observed using laser scanning confocal microscopy.

Mechanical properties of dental materials are increasingly studied via nanoindentation testing. Due to the excellent mechanical properties, 3-mol%-Yttria-Stabilized Tetragonal Zirconia (3Y-TZP) has become an attractive high-toughness core material for fixed dental restorations. In this paper, the mechanical properties of 3Y-TZP were studied by nanoindentation. The continuous stiffness measurement (CSM) and the single load/unload cycle test controlled by displacement and load respectively were performed with a Berkovich indenter.

In order to repair the etched human dental enamel, 45S5 bioactive glass with different particle size was used to remineralization enamel in vitro. 45S5 bioactive glass powder was sieved, and divided into the three groups. Freshly sound human second molar teeth from patients were extracted and specimens of dentine-enamel junction were prepared under water-cooled diamond saw, then the enamel surface was polished and finally rinsed. The enamel samples were soaked in simulated oral fluid (SOF) for 5 days. Particle size distribution, topological images and mechanical properties such as hardness and reduced modulus of enamel surface were evaluated by the laser particle size analyzer, atomic force microscope (AFM) and nanoindentation technology. The results indicated that the adhered particle size onto the enamel surface was concentrated on the 1-10 μm. With the decreasing particle size, adhesive capacity onto the enamel surface increased, but the mechanical properties decreased gradually after soaking in SOF for 5 days. In a short period time, Group 2 particles are suitable of repair the etched enamel, and further improve its mechanical properties. This study suggests that proper size 45S5 bioactive glass may be used to repair the acid etched teeth as a toothpaste additive.

Doctor of Philosophy(PhD)
Objectives As the outer cover of teeth structure, enamel is the hardest, stiffest and one of the most durable load-bearing tissues of the human body. Also, enamel is an elegantly designed natural biocomposite. From a material science point of view, scientists are interested in the structure and function of the nature material. How does nature design the material to meet its functional needs? From a dental clinic point of view, dental practitioners are keen to know the properties of enamel and compare it with different dental materials. What kind of dental materials can best simulate enamel as a restoration in the oral cavity? The research presented in this thesis on the mechanical behaviour of enamel in respect of its structural and compositional characteristics will attempt to provide answers or indications to the above questions. Theoretical analysis, as well as experimental investigations of both man-made and natural composites materials, has shown that hierarchical microstructure and organic matrix glues the inorganic particles together and plays an important role in regulating the mechanical properties of the composite. Bearing this finding in mind, in the current investigations, we assume the hierarchical microstructure and trace protein remnants in enamel regulate the mechanical behaviour of the natural biocomposite to meet its functional needs as a load bearing tissue with superb anti-fatigue and wear resistant properties. One of the important reasons that dental hard tissues haven’t been thoroughly investigated is due to the limited sample volume. Fortunately, with the development of nanoindentation technique and equipment, it is now possible to explore the mechanical properties of small volume samples. The application of nanoindentation on dental hard tissues has been documented. However, most investigations have concentrated on only reporting the basic mechanical properties such as elastic modulus and hardness. Very few of them have taken the role of microstructure and composition of these natural biocomposites into their considerations. The main aim of this investigation is to interpret how microstructural and compositional features of enamel regulate its mechanical behaviour. To achieve this goal, the analytical methods considering nanoindentation data need to be expanded so that more information not only elastic modulus and hardness but also stress-strain relationship, energy absorption ability, and creep behaviour may be evaluated with this technique. These new methods will also be of benefit to dental material evaluation and selection. Materials and methods Based on the Oliver-Pharr method1 for the analysis of nanoindentation data, Hertzian contact theory2 and Tabor’s theory3, a spherical nanoindentation method for measuring the stress-strain relationship was developed. Furthermore, nanoindentation energy absorption analysis method and nanoindentation creep test were developed to measure the inelastic property of enamel. With the above methods, sound enamel samples were investigated and compared with various dental materials, including dental ceramics and dental alloys. • Firstly, using a Berkovich indenter and three spherical indenters with 5, 10 and 20 µm nominal radius, the elastic modulus, hardness and stress-strain relationship of different samples were investigated and compared. • Secondly, mechanical properties of enamel in respect to its microstructure were investigated intensively using different indenters by sectioning teeth at different angles. • Thirdly, inelastic behaviour of enamel such as energy absorption and creep deformation were observed and compared with a fully sintered dense hydroxyapatite (HAP) disk to illustrate the roles of protein remnants in regulating the mechanical behaviour of enamel. • Fourthly, to confirm the functions of protein remnants in controlling mechanical behaviour of enamel, enamel samples were treated under different environments such as burning (300°C exposure for 5 min), alcohol dehydration and rehydration to change the properties of proteins before the nanoindentation tests. • Lastly, micro-Raman spectroscopy was employed to measure and compare the indentation residual stresses in enamel and HAP disk to evaluate the role of both hierarchical microstructure and protein remnants in redistributing the stresses and reinforcing the mechanical response of enamel to deformation. Results and significance Nanoindentation is an attractive method for measuring the mechanical behaviour of small specimen volumes. Using this technique, the mechanical properties of enamel were investigated at different orientations and compared with dental restorative materials. From the present study, the following results were found and conclusions were drawn.  Although some newly developed dental ceramics have similar elastic modulus to enamel, the hardness of these ceramic products is still much higher than enamel; in contrast, despite the higher elastic modulus, dental metallic alloys have very similar hardness as enamel. Furthermore, enamel has similar stress-strain relationships and creep behaviour to that of dental metallic alloys. SEM also showed enamel has an inelastic deformation pattern around indentation impressions. All of these responses indicated that enamel behaves more like a metallic material rather than a ceramic.  Elastic modulus of enamel is influenced by highly oriented rod units and HAP crystallites. As a result, it was found to be a function of contact area. This provides a basis to understand the different results reported in the literature from macro-scale and micro-scale tests. Anisotropic properties of enamel, which arise from the rod units, are well reflected in the stress-strain curves. The top surface (perpendicular to the rod axis) is stiffer and has higher stress-strain response than an adjacent cross section surface because of the greater influence of the prism sheaths in the latter behaviour.  Enamel showed much higher energy absorption capacity and considerably more creep deformation behaviour than HAP, a ceramic material with similar mineral composition. This is argued to be due to the existence of minor protein remnants in enamel. Possible mechanisms include fluid flow within the sheath structure, protein “sacrificial bond” theory, and nano-scale friction within sheaths associated with the degustation of enamel rods.  A simple model with respect of hierarchical microstructure of enamel was developed to illustrate the structural related contact deformation mechanisms of human enamel. Within the contact indentation area, thin protein layers between HAP crystallites bear most of the deformation in the form of shear strain, which is approximately 16 times bigger than contact strain in the case of a Vickers indenter. By replotting energy absorption against mean strain value of a protein layer, data from different indenters on enamel superimposed, validating the model. This model partially explained the non-linear indentation stress-strain relationship, inelastic contact response and large energy absorption ability of enamel and indicated the inelastic characteristics of enamel were related to the thin protein layers between crystallites.  Following different treatments, mechanical properties of enamel changed significantly. By denaturing or destroying the protein remnants, mechanical behaviour, especially inelastic abilities of enamel decreased dramatically, which indicates matrix proteins endow enamel better performance as a load bearing calcified tissue.  Comparison of Raman derived residual maps about indentations in enamel and a sintered homogeneous HAP showed the hierarchical structure influenced the residual stress distribution within enamel. Moreover, less residual stresses were found in enamel and were a consequence of the protein remnants. These are evidence as to how the microstructure meets the functional needs of the enamel tissue. In general, evidence from different approaches indicated that the hierarchical microstructure and small protein remnants regulated the mechanical behaviour of enamel significantly at various hierarchical levels utilising different mechanisms. This investigation has provided some basis for understanding natural biocomposites and assisting with dental clinic materials selection and treatment evaluation procedures. References 1. Oliver WC, Pharr GM. An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J Mater Res. 1992;7(6):1564-83. 2. Hertz H. Miscellaneous Papers. London: Jones and Schott, Macmillan; 1863. 3. Tabor D. Hardness of Metals. Oxford: Clarendon Press; 1951.

Doctor of Philosophy(PhD)
Objectives As the outer cover of teeth structure, enamel is the hardest, stiffest and one of the most durable load-bearing tissues of the human body. Also, enamel is an elegantly designed natural biocomposite. From a material science point of view, scientists are interested in the structure and function of the nature material. How does nature design the material to meet its functional needs? From a dental clinic point of view, dental practitioners are keen to know the properties of enamel and compare it with different dental materials. What kind of dental materials can best simulate enamel as a restoration in the oral cavity? The research presented in this thesis on the mechanical behaviour of enamel in respect of its structural and compositional characteristics will attempt to provide answers or indications to the above questions. Theoretical analysis, as well as experimental investigations of both man-made and natural composites materials, has shown that hierarchical microstructure and organic matrix glues the inorganic particles together and plays an important role in regulating the mechanical properties of the composite. Bearing this finding in mind, in the current investigations, we assume the hierarchical microstructure and trace protein remnants in enamel regulate the mechanical behaviour of the natural biocomposite to meet its functional needs as a load bearing tissue with superb anti-fatigue and wear resistant properties. One of the important reasons that dental hard tissues haven’t been thoroughly investigated is due to the limited sample volume. Fortunately, with the development of nanoindentation technique and equipment, it is now possible to explore the mechanical properties of small volume samples. The application of nanoindentation on dental hard tissues has been documented. However, most investigations have concentrated on only reporting the basic mechanical properties such as elastic modulus and hardness. Very few of them have taken the role of microstructure and composition of these natural biocomposites into their considerations. The main aim of this investigation is to interpret how microstructural and compositional features of enamel regulate its mechanical behaviour. To achieve this goal, the analytical methods considering nanoindentation data need to be expanded so that more information not only elastic modulus and hardness but also stress-strain relationship, energy absorption ability, and creep behaviour may be evaluated with this technique. These new methods will also be of benefit to dental material evaluation and selection. Materials and methods Based on the Oliver-Pharr method1 for the analysis of nanoindentation data, Hertzian contact theory2 and Tabor’s theory3, a spherical nanoindentation method for measuring the stress-strain relationship was developed. Furthermore, nanoindentation energy absorption analysis method and nanoindentation creep test were developed to measure the inelastic property of enamel. With the above methods, sound enamel samples were investigated and compared with various dental materials, including dental ceramics and dental alloys. • Firstly, using a Berkovich indenter and three spherical indenters with 5, 10 and 20 µm nominal radius, the elastic modulus, hardness and stress-strain relationship of different samples were investigated and compared. • Secondly, mechanical properties of enamel in respect to its microstructure were investigated intensively using different indenters by sectioning teeth at different angles. • Thirdly, inelastic behaviour of enamel such as energy absorption and creep deformation were observed and compared with a fully sintered dense hydroxyapatite (HAP) disk to illustrate the roles of protein remnants in regulating the mechanical behaviour of enamel. • Fourthly, to confirm the functions of protein remnants in controlling mechanical behaviour of enamel, enamel samples were treated under different environments such as burning (300°C exposure for 5 min), alcohol dehydration and rehydration to change the properties of proteins before the nanoindentation tests. • Lastly, micro-Raman spectroscopy was employed to measure and compare the indentation residual stresses in enamel and HAP disk to evaluate the role of both hierarchical microstructure and protein remnants in redistributing the stresses and reinforcing the mechanical response of enamel to deformation. Results and significance Nanoindentation is an attractive method for measuring the mechanical behaviour of small specimen volumes. Using this technique, the mechanical properties of enamel were investigated at different orientations and compared with dental restorative materials. From the present study, the following results were found and conclusions were drawn.  Although some newly developed dental ceramics have similar elastic modulus to enamel, the hardness of these ceramic products is still much higher than enamel; in contrast, despite the higher elastic modulus, dental metallic alloys have very similar hardness as enamel. Furthermore, enamel has similar stress-strain relationships and creep behaviour to that of dental metallic alloys. SEM also showed enamel has an inelastic deformation pattern around indentation impressions. All of these responses indicated that enamel behaves more like a metallic material rather than a ceramic.  Elastic modulus of enamel is influenced by highly oriented rod units and HAP crystallites. As a result, it was found to be a function of contact area. This provides a basis to understand the different results reported in the literature from macro-scale and micro-scale tests. Anisotropic properties of enamel, which arise from the rod units, are well reflected in the stress-strain curves. The top surface (perpendicular to the rod axis) is stiffer and has higher stress-strain response than an adjacent cross section surface because of the greater influence of the prism sheaths in the latter behaviour.  Enamel showed much higher energy absorption capacity and considerably more creep deformation behaviour than HAP, a ceramic material with similar mineral composition. This is argued to be due to the existence of minor protein remnants in enamel. Possible mechanisms include fluid flow within the sheath structure, protein “sacrificial bond” theory, and nano-scale friction within sheaths associated with the degustation of enamel rods.  A simple model with respect of hierarchical microstructure of enamel was developed to illustrate the structural related contact deformation mechanisms of human enamel. Within the contact indentation area, thin protein layers between HAP crystallites bear most of the deformation in the form of shear strain, which is approximately 16 times bigger than contact strain in the case of a Vickers indenter. By replotting energy absorption against mean strain value of a protein layer, data from different indenters on enamel superimposed, validating the model. This model partially explained the non-linear indentation stress-strain relationship, inelastic contact response and large energy absorption ability of enamel and indicated the inelastic characteristics of enamel were related to the thin protein layers between crystallites.  Following different treatments, mechanical properties of enamel changed significantly. By denaturing or destroying the protein remnants, mechanical behaviour, especially inelastic abilities of enamel decreased dramatically, which indicates matrix proteins endow enamel better performance as a load bearing calcified tissue.  Comparison of Raman derived residual maps about indentations in enamel and a sintered homogeneous HAP showed the hierarchical structure influenced the residual stress distribution within enamel. Moreover, less residual stresses were found in enamel and were a consequence of the protein remnants. These are evidence as to how the microstructure meets the functional needs of the enamel tissue. In general, evidence from different approaches indicated that the hierarchical microstructure and small protein remnants regulated the mechanical behaviour of enamel significantly at various hierarchical levels utilising different mechanisms. This investigation has provided some basis for understanding natural biocomposites and assisting with dental clinic materials selection and treatment evaluation procedures. References 1. Oliver WC, Pharr GM. An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J Mater Res. 1992;7(6):1564-83. 2. Hertz H. Miscellaneous Papers. London: Jones and Schott, Macmillan; 1863. 3. Tabor D. Hardness of Metals. Oxford: Clarendon Press; 1951.

Objectives As the outer cover of teeth structure, enamel is the hardest, stiffest and one of the most durable load-bearing tissues of the human body. Also, enamel is an elegantly designed natural biocomposite. From a material science point of view, scientists are interested in the structure and function of the nature material. How does nature design the material to meet its functional needs? From a dental clinic point of view, dental practitioners are keen to know the properties of enamel and compare it with different dental materials. What kind of dental materials can best simulate enamel as a restoration in the oral cavity? The research presented in this thesis on the mechanical behaviour of enamel in respect of its structural and compositional characteristics will attempt to provide answers or indications to the above questions. Theoretical analysis, as well as experimental investigations of both man-made and natural composites materials, has shown that hierarchical microstructure and organic matrix glues the inorganic particles together and plays an important role in regulating the mechanical properties of the composite. Bearing this finding in mind, in the current investigations, we assume the hierarchical microstructure and trace protein remnants in enamel regulate the mechanical behaviour of the natural biocomposite to meet its functional needs as a load bearing tissue with superb anti-fatigue and wear resistant properties. One of the important reasons that dental hard tissues haven’t been thoroughly investigated is due to the limited sample volume. Fortunately, with the development of nanoindentation technique and equipment, it is now possible to explore the mechanical properties of small volume samples. The application of nanoindentation on dental hard tissues has been documented. However, most investigations have concentrated on only reporting the basic mechanical properties such as elastic modulus and hardness. Very few of them have taken the role of microstructure and composition of these natural biocomposites into their considerations. The main aim of this investigation is to interpret how microstructural and compositional features of enamel regulate its mechanical behaviour. To achieve this goal, the analytical methods considering nanoindentation data need to be expanded so that more information not only elastic modulus and hardness but also stress-strain relationship, energy absorption ability, and creep behaviour may be evaluated with this technique. These new methods will also be of benefit to dental material evaluation and selection. Materials and methods Based on the Oliver-Pharr method1 for the analysis of nanoindentation data, Hertzian contact theory2 and Tabor’s theory3, a spherical nanoindentation method for measuring the stress-strain relationship was developed. Furthermore, nanoindentation energy absorption analysis method and nanoindentation creep test were developed to measure the inelastic property of enamel. With the above methods, sound enamel samples were investigated and compared with various dental materials, including dental ceramics and dental alloys. • Firstly, using a Berkovich indenter and three spherical indenters with 5, 10 and 20 µm nominal radius, the elastic modulus, hardness and stress-strain relationship of different samples were investigated and compared. • Secondly, mechanical properties of enamel in respect to its microstructure were investigated intensively using different indenters by sectioning teeth at different angles. • Thirdly, inelastic behaviour of enamel such as energy absorption and creep deformation were observed and compared with a fully sintered dense hydroxyapatite (HAP) disk to illustrate the roles of protein remnants in regulating the mechanical behaviour of enamel. • Fourthly, to confirm the functions of protein remnants in controlling mechanical behaviour of enamel, enamel samples were treated under different environments such as burning (300°C exposure for 5 min), alcohol dehydration and rehydration to change the properties of proteins before the nanoindentation tests. • Lastly, micro-Raman spectroscopy was employed to measure and compare the indentation residual stresses in enamel and HAP disk to evaluate the role of both hierarchical microstructure and protein remnants in redistributing the stresses and reinforcing the mechanical response of enamel to deformation. Results and significance Nanoindentation is an attractive method for measuring the mechanical behaviour of small specimen volumes. Using this technique, the mechanical properties of enamel were investigated at different orientations and compared with dental restorative materials. From the present study, the following results were found and conclusions were drawn.  Although some newly developed dental ceramics have similar elastic modulus to enamel, the hardness of these ceramic products is still much higher than enamel; in contrast, despite the higher elastic modulus, dental metallic alloys have very similar hardness as enamel. Furthermore, enamel has similar stress-strain relationships and creep behaviour to that of dental metallic alloys. SEM also showed enamel has an inelastic deformation pattern around indentation impressions. All of these responses indicated that enamel behaves more like a metallic material rather than a ceramic.  Elastic modulus of enamel is influenced by highly oriented rod units and HAP crystallites. As a result, it was found to be a function of contact area. This provides a basis to understand the different results reported in the literature from macro-scale and micro-scale tests. Anisotropic properties of enamel, which arise from the rod units, are well reflected in the stress-strain curves. The top surface (perpendicular to the rod axis) is stiffer and has higher stress-strain response than an adjacent cross section surface because of the greater influence of the prism sheaths in the latter behaviour.  Enamel showed much higher energy absorption capacity and considerably more creep deformation behaviour than HAP, a ceramic material with similar mineral composition. This is argued to be due to the existence of minor protein remnants in enamel. Possible mechanisms include fluid flow within the sheath structure, protein “sacrificial bond” theory, and nano-scale friction within sheaths associated with the degustation of enamel rods.  A simple model with respect of hierarchical microstructure of enamel was developed to illustrate the structural related contact deformation mechanisms of human enamel. Within the contact indentation area, thin protein layers between HAP crystallites bear most of the deformation in the form of shear strain, which is approximately 16 times bigger than contact strain in the case of a Vickers indenter. By replotting energy absorption against mean strain value of a protein layer, data from different indenters on enamel superimposed, validating the model. This model partially explained the non-linear indentation stress-strain relationship, inelastic contact response and large energy absorption ability of enamel and indicated the inelastic characteristics of enamel were related to the thin protein layers between crystallites.  Following different treatments, mechanical properties of enamel changed significantly. By denaturing or destroying the protein remnants, mechanical behaviour, especially inelastic abilities of enamel decreased dramatically, which indicates matrix proteins endow enamel better performance as a load bearing calcified tissue.  Comparison of Raman derived residual maps about indentations in enamel and a sintered homogeneous HAP showed the hierarchical structure influenced the residual stress distribution within enamel. Moreover, less residual stresses were found in enamel and were a consequence of the protein remnants. These are evidence as to how the microstructure meets the functional needs of the enamel tissue. In general, evidence from different approaches indicated that the hierarchical microstructure and small protein remnants regulated the mechanical behaviour of enamel significantly at various hierarchical levels utilising different mechanisms. This investigation has provided some basis for understanding natural biocomposites and assisting with dental clinic materials selection and treatment evaluation procedures. References 1. Oliver WC, Pharr GM. An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J Mater Res. 1992;7(6):1564-83. 2. Hertz H. Miscellaneous Papers. London: Jones and Schott, Macmillan; 1863. 3. Tabor D. Hardness of Metals. Oxford: Clarendon Press; 1951.

Enamel plays an important role in tooth function. Optimal combinations of composition and structure endow enamel with unique mechanical properties that remain largely unexplored. Specifically, more detailed understanding of the loadbearing ability of enamel is needed to mimic it synthetically and to design next generation biocomposite materials. This research investigates the variables that influence deformation behaviour of tooth enamel in relation to its hierarchical structure. Initially, a new method was developed for preparing flat, finely polished tooth samples that were maintained in their normal hydrated state for nanoindentation testing. In contrast to conventional methods, which commonly utilise either inappropriate or excessive drying and/or chemically based embedding media (i.e., resins, glues), a novel embedding process was developed using an aqueous putty compound. Additionally, a custom-designed holder was manufactured for mounting wet tooth specimens on the nanoindentation stage that eliminated the need for hot wax or glue during testing. Considering that enamel is a functionally graded material that has different values of Young’s modulus (E) and hardness (H) over the enamel thickness, a new approach of data analysis was developed for interpreting the mechanical properties of enamel at a range of fixed constant indentation depths. Resultant functions were used for predictive purposes. The values of E and H obtained from the nanoindentation instrument demonstrated a well-known decreasing gradient from the enamel occlusal surface towards the enamel-dentine junction (EDJ). In contrast to studies using conventional methods, this research showed that both properties also decreased with increasing depths at fixed locations. Furthermore, experimental results showed that resin embedding had detrimental effects on the E and H of enamel (i.e., both properties decreased with increasing depth), but had positive effects on both mild and severe wear resistance parameters (i.e., both parameters increased with increasing depth). When contrasted against the mechanical properties of enamel samples prepared using conventional protocols, this study postulates that the new hydrated method has, for the first time, revealed the genuine E and H properties of this tissue. The effects of sample preparation methods on tooth microstructure, especially along the EDJ, were investigated with optical microscopy and scanning electron microscopy (SEM). The new method of sample preparation combined with a careful dehydration process maintained the integrity of the EDJ interface even after applying multiple Berkovich indents up to maximum load of 400 mN. In contrast, the EDJ and the enamel surface were commonly separated and fractured in teeth that had been resin-embedded. Accordingly, the new method of sample preparation proved to be reliable for investigating the genuine microstructural characteristics of teeth. The behaviour of the elastic region in tooth enamel was investigated with analytical and finite element models. The models were fitted into experimental values of E obtained from nanoindentation tests with a Berkovich indenter to identify a relationship between the mechanical responses of enamel under different loading conditions and microstructure. The decrease in E for enamel with increasing indentation depth was related to its enhanced load-bearing ability. The change of E was directly linked to the microstructural evolution (i.e., the rotation of mineral crystals) of enamel. The effective crystal orientation angle was found to be between 44o and 48o for indentation depths from 0.8 and 2.4 μm below according to the analytical model. The range of angles facilitated the shear sliding of mineral crystals and reduced the stress level as well as the volume of material under higher loads. The behaviour of the plastic region in healthy enamel was investigated with finite element models fitted to nanoindentation data obtained with a Berkovich indenter to determine deformation mechanisms that result in excellent mechanical responses for tooth enamel during loading. When nanoindentation was conducted with increasingly applied loads but at a fixed location, the values of H decreased with increasing indentation depth. The decreasing trend in H was simulated by finite element models and showed a reduction in stress level and yield strength with increasing load. This key mechanism of the loading dependence of mechanical properties resulted in remarkable enamel resilience and was related to the change of effective crystal orientation angle within the enamel microstructure. The mechanical behaviour of enamel with respect to its microstructure was also investigated on teeth exposed to commercially available whitening treatments (tooth bleaching). Enamels exposed to a 6% bleaching treatment exhibited degraded mechanical properties (E and H) compared to unbleached controls. Furthermore, the creep and recovery responses of bleached enamel were also significantly reduced compared to controls. To determine the variables regulating tooth enamel deformation mechanisms during whitening treatments, analytical models were fitted to stress-strain curves. The effective crystal orientation angle of healthy enamel and the protein shear stress, τc, were identified as 50o and 2.5 % of the transverse stiffness of a staggered composite (E2), respectively. After the bleaching treatment, the effective crystal orientation angle of enamel increased to 54o for τc = 1.5 % of E2. Notably, bleaching reduced shear (τc) by 40 % compared to normal readings for unbleached controls. The changes in mechanical responses of bleached enamel were linked to the decrease of the shear bearing ability of protein components in the enamel microstructure. It is envisaged that these findings will provide new perspectives on applications of bleaching treatments and lead to the development of bleaching agents with less damaging effects to healthy enamel. This work should stimulate new interest in understanding the deformation behaviour of tooth enamel at small scales, and offer new methods for the collection and analysis of data from samples prepared close to their native state, upon which novel and biologically relevant high-performance biocomposite materials can be engineered.

Orientadores: Alan Roger dos Santos Silva, Mario Fernando de Goes
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Odontologia de Piracicaba
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Resumo: Este estudo avaliou o comportamento mecânico de tecidos dentários de pacientes com câncer de cabeça e pescoço submetidos à radioterapia. No capítulo I, o ensaio mecânico da nanoindentação foi utilizado para determinar a dureza e módulo de elasticidade do esmalte, dentina e da região de união restauradora em dentina (adesivo, camada híbrida e dentina subjacente). Foram utilizados seis dentes incisivos inferiores irradiados in vivo e não irradiados (grupos controle). A dureza e o módulo de elasticidade e foram obtidos após a realização da nanoindentação com pico de força de 1000 µN em dentina intertubular e região de união restauradora e 1500 µN em esmalte (centro do prisma) usando o microscópio de força atômica equipado com nanoidentador com tempo 5-2-5 seg para carregamento, aplicação e descarregamento da carga. A análise de variância a um fator foi aplicada com nível de significância de 0.05%. O valor da nanodureza e módulo de elasticidade não foram estatisticamente diferentes entre os tecidos avaliados em ambos os grupos irradiados e controle. Desta foma, pode-se concluir que tanto a dureza como o módulo de elasticidade de dentes submetidos à radioterapia in vivo não apresentam alterações das propriedades mecânicas no esmalte, dentina e região de união adesivo/dentina devido á ação direta da radioterapia. No capítulo II, foram avaliadas as propriedades viscoelásticas (storage e loss modulus) de três regiões diferentes: esmalte, junção amelo-dentinária (JAD) e dentina de dentes irradiados in vivo. Cinco dentes não irradiados (grupo de controle, n = 5) e cinco dentes irradiados in vivo (grupo irradiado, n = 5) foram utilizados para produzir cinco fatias de cada para avaliar a três áreas distintas: o esmalte, o JAD , e a dentina. A análise por mapeamento (Modulus Mapping Analysis) foi escolhida para avaliar a perda e armazenamento de energia mediante uma carga aplicada. Três regiões de dados foram coletados de cada área de tecido de cada fatia, totalizando quinze mapeamentos por tecido por grupo. Os valores do módulo foram calculados pelo software Hysitron® e a análise da variância (ANOVA Plot Split) e teste de Tukey a 5% de significância foram utilizados para comparar os grupos e tecidos. As três áreas avaliadas de ambos os grupos controle e irradiado revelaram diferença estatística no módulo de perda e armazenamento. Ambos os valores de perda e de armazenamento apresentaram-se maiores no grupo irradiado para esmalte (164,44 ± 36,60 GPa; 177,59 ± 58,84 GPa), JAD (50,85 ± 35,78 GPa; 83,33 ± 38,59 GPa) e dentina (21,18 ± 18,61 GPa; 52,44 ± 26,56 GPa) do que no grupo controle para o esmalte (127,15 ± 74,45 GPa; 162,85 ± 74,63 GPa), JAD (25,72 ± 9,64 GPa; 21,93 ± 52,78 GPa) e dentina (10,39 ± 8,65 GPa; 32,10 ± 20,39 GPa), respectivamente. Foi possível concluir neste estudo, que as propriedades viscoelásticas dos dentes irradiados in vivo apresentam-se diferentes das do grupo controle. Estes resultados sugerem que, após a radioterapia, os tecidos dentais estariam mais suscetíveis a fraturas
Abstract: This study evaluated the mechanic properties of enamel, dentin, and dentin bond interface of patients who undergone head and neck cancer treatment. On I chapter, the nanoindentation technique was used to determine the hardness (H) and reduced modulus of elasticity (Er) of the control group on enamel, dentin, and dentin bond interface (adhesive layer, hybrid layer and underlyer dentin). The Er and H were obtained after completion of nanoindentation with peak force of 1000 µN on intertubular dentin and restorative dentin interfaces and 1500 µN on enamel (prism center) using the atomic force microscope with nanoindenter accopled with test time 5-2-5 seconds for loading, holding and unloading. The one-way analysis of variance (p'< ou ='0.05) was applied and the valus for H and Er for both groups and tissues were no statistical different. As conclusion, the nanohardeness and elastic modulus behavior of the enamel, dentin and dentin bond interface was not impacted by the radiotherapy treatment of head and neck cancer. On II chapter, the viscoelastic properties were assessed (storage and loss modulus) of three different regions: enamel, dentin-enamel junction (DEJ) and dentin irradiated teeth in vivo. Five non irradiated teeth (control group, n=5) and five in vivo irradiated teeth (irradiated group, n=5) were used to produce five beams that were used to evaluate three different areas: the enamel, the DEJ, and the dentin. Perpendicular sections to the long axis of the teeth were made at middle region of the crown to produce the beams. The Modulus Mapping Analysis was chosen to evaluate the loss and storage moduli of each area. Three data regions were collected of each tissue area of each beam, summing a total of fifteen data per tissue per group. The modulus values were calculated by the Hysitron® software and an Analysis of Variance (ANOVA Split Plot) and Tukey test at 5% of significance was used to compare groups and tissues. All the three areas evaluated of control and irradiated group revealed statistical difference on the Loss and Storage Moduli. Both the loss and storage values are higer on the irradiated group for enamel (164.44±36.60 GPa; 177.59±58.84 GPa), DEJ (50.85±35.78 GPa; 83,33±38,59 GPa) and dentin (21.18±18.61 GPa; 52.44±26.56 GPa) than control group values for enamel (127.15±74.45 GPa; 162.85±74.63 GPa), DEJ (25.72±9.64 GPa; 21.93±52.78 GPa) and dentin (10.39±8.65 GPa;32,10±20,39 GPa), respectivally. The viscoelastic properties of in vivo irradiated teeth are different from control group. The enamel, DEJ and dentin presented the higer values on the in vivo irradiated group. These finds suggest that after radiotherapy, the dental tissues are more susceptible to fractures
Doutorado
Materiais Dentarios
Doutora em Materiais Dentários

El texto completo de este trabajo no está disponible en el Repositorio Académico UPC por restricciones de la casa editorial donde ha sido publicado.
PURPOSE: To assess the influence of simulated oral erosive/abrasive challenges on the bond strength of an etch-and-rinse two-step bonding system to enamel using an in situ/ex vivo protocol. METHODS: Bovine enamel blocks were prepared and randomly assigned to four groups: CONT - control (no challenge), ABR - 3x/day-1 minute toothbrushing; ERO - 3x/day - 5 minutes extraoral immersion into regular Coca Cola; and ERO+ABR - erosive protocol followed by a 1-minute toothbrushing. Eight blocks were placed into an acrylic palatal appliance for each volunteer (n = 13), who wore the appliance for 5 days. Two blocks were subjected to each of the four challenges. Subsequently, all the blocks were washed with tap water and Adper Single Bond 2/Filtek Z350 were placed. After 24 hours, 1 mm2 beams were obtained from each block to be tested with the microtensile bond strength test (50 N load at 0.5 mm/minute). The data were statistically analyzed by one-way RM-ANOVA and Tukey's tests (alpha = 0.05). RESULTS: No difference was detected among the ABR, ERO, and CONT groups (P > 0.05). ERO+ABR group yielded lower bond strengths than either the ABR and ERO groups (P < 0.0113).
Revisión por pares

Ceramics are increasingly used as structural materials with biomedical applications due to their mechanical properties, biocompatibility, esthetic characteristics and durability. Specifically, zirconia-based compounds are commonly used to develop metal-free restorations and dental implants. The consolidation of ceramics is usually carried out through powders by means of processes that require a lot of energy, as long as processing times and high temperatures (over 1400°C) are required. In the recent years, new research is being developed in this field to reduce both energy consumption and processing time of ceramic powders. One of the most promising techniques for sintering ceramics is microwave heating technology. The main objective of this chapter is to obtain highly densified zirconia-alumina compounds by microwave technology. After sintering, the materials are characterized to determine whether the final properties meet the mechanical requirements for their final applications as dental material. Finally, the characterization of specimens treated by low-temperature degradation (LTD) is carried out after each 20 h of LTD exposure up to 200 h. In addition, the quantification of monoclinic phase by micro-Raman spectroscopy, analysis by AFM and Nomarski optical microscopy and assessment of the roughness and mechanical properties (hardness and Young’s modulus) by nanoindentation technique have been studied.

This study utilizes novel characterization techniques nanoindentation and nanoscratch for testing both the human enamel and dentine together with two biocompatible dental filling materials; epoxy nanocomposite and silver amalgam. Nanoindentation tests were performed to obtain accurate hardness and reduced modulus values for the enamel, dentin and two different fillers. We utilized Nano-scratch tests to obtain critical load in scratch test and resistance to sliding wear. Testing showed the silver amalgam filling has a higher modulus of elasticity, hardness and wear resistance compared to the nanocomposite. The novel mechanical characterization techniques utilized might assist in better understanding the mechanical behavior of the dental fillers and thus facilitate the design of robust fillers with excellent mechanical properties.

Nanoindentation (NI) has been used with increasing frequency to characterize the mechanical properties of biological tissues. However, the majority of prior studies in this area have focused on hard tissues such as bone, enamel, and dentin [1]. For soft, hydrated tissues and biomaterials, methods of analyzing the force-displacement curves to obtain meaningful information on viscoelastic material properties are still under development. In particular, methods for using NI to quantify the biphasic material properties (aggregate modulus HA, permeability k, Poisson’s ratio ν) of tissues such as articular cartilage have not been established. Such methods could be applied in studies using small animal models to investigate biological and biomechanical mechanisms of articular cartilage degeneration and repair. The overall goal of this study was to develop the use of NI for characterization of the mechanical properties of soft, hydrated materials.

Tooth reconstruction materials are used to reconstruct damaged teeth as well as to recover their functions. In this study, the mechanical properties of various tooth reconstruction materials were determined using test specimens of identical shape and dimension under the same compressive test condition; the hardness values of them were obtained from previous studies and compared with those of enamel and dentin. Amalgam, dental ceramic, dental gold alloy, dental resin, zirconia and titanium were processed as tooth reconstruction material specimens. For each material, 10 specimens having a of 3.0 × 1.2 × 1.2 mm (length × width × height) were used. The stresses, strains, and elastic moduli of amalgam, dental ceramic, gold alloy, dental resin, zirconia, and titanium alloy were obtained from the compressive test. The hardness values of amalgam, dental ceramic, gold alloy, dental resin, zirconia, and titanium alloy were obtained from the references [14–19]. And, the stresses, strains, elastic moduli, and the hardness values of enamel and dentin were obtained from the reference [13]. The mechanical role of enamel is to crush food and protect dentin because of its higher wear resistance, and that of dentin is to absorb bite forces because of its higher force resistance. Therefore, the hardness value should be prioritized for enamel replacement materials, and mechanical properties should be prioritized for dentin replacement materials. Therefore, zirconia and titanium alloy were considered suitable tooth reconstruction materials for replacing enamel, and gold alloy, zirconia, and titanium alloy were considered suitable tooth reconstruction materials for replacing dentin. However, owing to the excessive mechanical properties and hardness values of zirconia and titanium alloy, these may show poor biocompatibility with natural teeth. Thus far, no tooth reconstruction material satisfies the requirements of having both a hardness value similar to that of enamel and mechanical properties similar to those of dentin.

Dental restorative materials including amalgam, dental ceramic, gold alloy, dental resin, zirconia, and titanium alloy are used to reconstruct damaged teeth, as well as to recover their function. In this study, the mechanical properties of various dental restorative materials were determined using test specimens of identical shape and dimension under the same three-point bending test condition, and the test results were compared to enamel and dentin. The maximum bending force of enamel and dentin was 6.9 ± 2.1 N and 39.7 ± 8.3 N, and the maximum bending deflection was 0.12 ± 0.02 mm and 0.25 ± 0.03 mm, respectively. The maximum bending force of amalgam, dental ceramic, gold alloy, dental resin, zirconia, and titanium alloy were 1.9 ± 0.4 N, 2.7 ± 0.6 N, 66.9 ± 4.1 N, 2.7 ± 0.3 N, 19.0 ± 2.0 N, and 121.3 ± 6.8 N, respectively, and the maximum bending deflection was 0.20 ± 0.08 mm, 0.28 ± 0.07 mm, 2.53 ± 0.12 mm, 0.37 ± 0.05 mm, 0.39 ± 0.05 m, and 2.80 ± 0.08 mm, respectively. The dental restorative materials that possessed greater maximum bending force than that of enamel were gold alloy, zirconia, and titanium alloy. Gold alloy and titanium alloy had greater maximum bending force than dentin. The dental restorative materials that possessed greater maximum bending deflection than that of enamel were all of the dental restorative materials, and the dental restorative materials that possessed greater maximum bending deflection than that of dentin were all of the dental restorative materials except amalgam. The appropriate dental restorative materials for enamel are gold alloy and zirconia and for dentin is gold alloy concerning the maximum bending force and the maximum bending deflection. These results are expected to aid dentists in their choice of better clinical treatment and to contribute to the development of dental restorative materials that possess properties that are most similar to the mechanical properties of dental hard tissue.