Influence of preoxidation cycle on the bond strength of CoCrMoSi–porcelain dental composites

The purpose of this study was to evaluate the effect of preoxidation cycle on the shear bond strength (SBS) of CoCrMoSi alloy–porcelain dental composites. The porcelain was fired onto three types of metal surfaces: non-preoxidized, preoxidized and, preoxidized followed by grinding. The bond strength of metal–porcelain composites was investigated by the means of a shear test. The metal–ceramic interfaces and the fractured surfaces were analyzed using Optical Microscopy, Stereomicroscopy and SEM/EDS. Data was analyzed with Shapiro–Wilk test to test the assumption of normality. The t-test was used to compare shear bond strength results (p < 0.05). The analysis of the three types of surfaces was performed prior to porcelain firing. It was also performed a complementary analysis of an alumina-blasted preoxidized CoCrMoSi surface. The greater metal–porcelain adhesion was obtained for non-preoxidized specimens.Non-preoxidized specimens showed significantly (p < 0.05) higher shear bond strength than preoxidized/ground specimens, 115.5 ± 7.5 MPa and 74.8 ± 8.5 MPa, respectively. Porcelain showed no adhesion to preoxidized specimens. All preoxidized specimens exhibited adhesive failure type while non-preoxidized presented both adhesive and mixed failure types. Preoxidation heat treatment revealed a detrimental effect on the adhesion of CoCrMoSi–porcelain composites for dental restorations. Hence, in order to enhance CoCrMoSi–porcelain adhesion, the preoxidation heat treatment conditions, as performed in this study, should not be performed.     

Surface modifications to improve Ti–porcelain bonding

Investigations of surface modifications on cast titanium surfaces and titanium-ceramic adhesion were performed. Cast pure titanium was subjected to surface modification by preoxidation and introduction of an intermediate layer of SnO _x by sol–gel process. Surfaces only sandblasted with alumina were used as controls. Specimen surfaces were characterized by XRD and SEM/EDS. The adhesion between the titanium and porcelain was evaluated by three-point flexure bond test. Failure of the titanium–porcelain with preoxidation treatment predominantly occurred at the titanium-oxide interface. Preoxidation treatment did not affect the fracture mode of the titanium–ceramic system and did not increase the bonding strength of Ti–porcelain. However, a thin and coherent SnO _x film with small spherical pores obtained at 300 °C served as an effective oxygen diffusion barrier and improved titanium–ceramic adhesion. The SnO _x film changed the fracture mode of the titanium–ceramic system and improved the mechanical and chemical bonding between porcelain and titanium, resulting in the increased bonding strength of titanium–porcelain.     

Effect of ZrN coating by magnetron sputtering and sol–gel processed silica coating on titanium/porcelain interface bond strength

In this study, a coating technique was applied to improve the bond strength of titanium (Ti) porcelain. ZrN coating was prepared by magnetron sputtering, and silica coating was processed by a sol–gel method. The treated surfaces of the specimens were analyzed by X-ray diffraction, and the Ti/porcelain interface was investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy. The coated specimens appeared fully coherent to the Ti substrate. The fractured bonding surface was also investigated by SEM. The residual porcelain on the metal surface could be observed in the ZrN group and silica group, but there was no obvious porcelain remaining in the control group. A three-point-bending test showed that the bonding strength of the ZrN group (45.99 ± 0.65 MPa) was higher than the silica group (37.77 ± 0.78 MPa) (P < 0.001) and control group (29.48 ± 1.01 MPa) (P < 0.001), while that of the silica group was significantly higher than the control group (P < 0.001). In conclusion, conditioning the ceramic surface with ZrN and silica coatings resulted in a stronger Ti/porcelain bond. ZrN coating by magnetron sputtering was a more effective way to improve the bond strength between Ti and porcelain compared with sol–gel processed silica coating in this study.     

Estimation of the strength of adhesion between a thermoresponsive polymer coating and nitinol wire

As polymer coatings become more widely used in the biomedical device industry, both to improve biocompatibility and as coatings for localised drug delivery, quantitative methods to measure the adhesive strength between coatings and substrates become a very important consideration. The aim of this study was to take a method for estimating the interfacial fracture toughness of a film to a flat substrate and apply it to Nitinol wires used in the production of medical devices. An investigation into the affect of surface roughness on the fracture toughness was also conducted. For the present study, a thermoresponsive based Poly (N-isopropylacrylamide) polymer was coated onto nitinol wire substrates and the adhesion strength between the polymer and wire was measured using a nanoindentation technique. Different surface treated nitinol wires, with different surface topography and roughness were used, and the affect of these surface properties on adhesion strength was investigated. Results showed that it was possible to apply the delamination technique to wire samples and obtain fracture toughness values. Results also showed that the surface roughness is an important parameter that can affect the adhesion between a coating and the substrate. It was found that, as the average surface roughness increased so also did the adhesive strength between the coating and wire sample.     

A fracture mechanics approach to ceramo-metal bond evaluation

The incidence of mechanical failure of cast metal/porcelain dental restorations has promoted a study to develop reliable methods of characterizing and improving bond strengths when produced under standard dental laboratory conditions. Single-edge notch beam specimens were prepared by firing porcelain from a single blended frit to either side of a central metal coupon and subjecting these to four-point bending at 20 ± 2° C and 0.5 mm min^–1 crosshead speed. Specimens of three representative dental alloys and an experimental alloy were prepared in two specimen sizes and three notch widths. The fracture toughness (K _Ic) values were independent of notch width and specimen size over the range of these variables examined and good discrimination was obtained. The fracture toughness of all bonds was improved by a commercial hot isostatic pressure cycle. SEM examination of the fractured surfaces suggested that this improvement was due to the reduction in microporosity at the interface.     

Optimization of bond strength between gold alloy and porcelain through a composite interlayer obtained by powder metallurgy

The purpose of this study was to evaluate the influence of a composite interlayer (at the metal-ceramic interface) on the shear bond strength of a metal-ceramic composite when compared with a conventional porcelain fused to metal (PFM).Several metal-ceramic composites specimens were produced by hot pressing. To identify which was the best composition for the interlayer several composites, with different relations of metal/ceramic volume fraction, were bonded to metal and to ceramic substrates. The bond strength of the composites to substrates was assessed by the means of a shear test performed in a universal test machine (crosshead speed: 0.5 mm/min) until fracture. Some interfaces of fractured specimens as well as undestroyed interface specimens were examined with optical microscope and scanning electron microscope (SEM/EDS).The shear bond strength results for all composites bonded to metal and to ceramic substrates were significantly higher (>150 MPa) than those registered in the upper range of conventional porcelain fused to metal (PFM) techniques (∼80 MPa). The use of a composite interlayer proved to enhance metal/ceramic adhesion in 160%.     

Evaluation of subsurface damage in CAD/CAM machined dental ceramics

Commercial ceramics for dental computer aided design/computer aided manufacture (CAD/CAM) restorations suffer from surface chipping defects and microcracking. The influence of CAD/CAM machining of dental materials on the mechanical strength and extension of the damage zone was studied. Two different commercial dental ceramics, a feldspathic porcelain and a glass–ceramic, were CAD/CAM machined according to dental practice. The extension of the damage zone was analysed by a stepwise erosion of the surface, and the biaxial flexural strength was measured. To simulate the adhesive fixing of ceramic inlays, the specimens were sealed using a light-curing monomer. The different machining behaviour is dominated by the microstructure of the investigated materials. Owing to the high amount of glassy phase, the feldspathic porcelain shows extensive microcracking and chipping defects. The extent of the damage zone can be determined as 40–60 m. Sealing of the surface did not affect the flexural strength of the machined samples. The dominating response to machining of the glass–ceramic is crushing and crumbling with a major contribution of plastic deformation on a microscopic scale. The extent of the damage zone is less than 20 m. These cracks can be bridged by sealing of the surface, resulting in a substantial increase in strength. © 1998 Chapman & Hall     

Interfacial fracture characteristic and crack propagation of thermal barrier coatings under tensile conditions at elevated temperatures

Thermal barrier coatings (TBCs) have been extensively used in aircraft engines for improved durability and performance for more than fifteen years. In this paper, thermal barrier coating system with plasma sprayed zirconia bonded by a MCrAlY layer to SUS304 stainless steel substrate was performed under tensile tests at 1000°C. The crack nucleation, propagation behavior of the ceramic coatings in as received and oxidized conditions were observed by high-performance camera and discussed in detail. The relationship of the transverse crack numbers in the ceramic coating and tensile strain was recorded and used to describe crack propagation mechanism of thermal barrier coatings. It was found that the fracture/spallation locations of air plasma sprayed (APS) thermal barrier coating system mainly located within the ceramic coating close to the bond coat interface by scanning electron microscope (SEM) and energy dispersive X-Ray (EDX). The energy release rate and interface fracture toughness of APS TBCs system were evaluated by the aid of Suo–Hutchinson model. The calculations revealed that the energy release rate and fracture toughness ranged, respectively, from 22.15 J m⁻² to 37.8 J m⁻² and from 0.9 MPa m^1/2 to 1.5 MPa m^1/2. The results agree well with other experimental results.     

Influence of artificial ageing on surface properties and <Emphasis Type="Italic">Streptococcus mutans</Emphasis> adhesion to dental composite materials

The aim of this in vitro study was to investigate the influence of artificial ageing on the surface properties and early Streptococcus mutans adhesion to current dental composites for the direct restoration of class II defects. Three hundred and thirty specimens each were prepared from five dental composites, and were randomly allotted to various artificial ageing protocols (storage in distilled water/ethanol/artificial saliva for 7/90/365 days; thermal cycling, 6,000 cycles 5/55°C). Prior and after each treatment, surface roughness (R_a) and hydrophobicity were determined, and S. mutans adhesion (ATCC 25175; 2.5 h, 37°C) was simulated with and without prior exposition to human whole saliva (2 h, 37°C). Adherence of S. mutans was determined fluorometrically. Means and standard deviations were calculated, and analyzed using three-way ANOVA and post-hoc analysis (α = 0.05). For both R_a and S. mutans adherence to uncoated and saliva-coated specimens, significant influences of the composite material, the ageing medium and the ageing duration have been observed; for surface hydrophobicity, significant influences of the composite material and the ageing duration were found. For uncoated specimens, significant increases in S. mutans adhesion were observed with prolonged artificial ageing, whereas significant decreases in S. mutans adhesion were found for the saliva-coated specimens. The data indicate influences of the artificial ageing method on surface parameters such as R_a and hydrophobicity as well as microbial adhesion. The results underline the relevance of saliva coating on the outcome of studies simulating microbial adhesion, and highlight differences in the susceptibility of dental composites for the adhesion of oral bacteria.     

Characterization and comparison between APS coatings prepared from ball milled and plasma processed nickel–aluminium powders

Plasma spraying has wide range of applications which include corrosion, thermal and abrasion resistance coatings. In the present work, nickel and aluminium powders were ball milled and the same were thermal plasma processed to produce spherical nickel alumindes particles. Both ball milled and plasma processed powders were spray deposited on stainless steel (SS 304) substrate using atmospheric plasma spray technique (APS). The experiments were carried out for different plasma input power levels, torch to base distances and coating thicknesses. Microstructure, micro hardness, adhesive strength, and porosity of the coatings are reported and discussed. Effect of plasma processing parameters and plasma spheroidization of powders on coating properties has been evaluated and reported. High plasma power, low torch to base distance lead to high temperature supplied to in-flight particles which correspond to high hardness, low porosity and high adhesion. Spherical morphology and formation of nickel aluminide intermetallic were achieved by plasma spheroidization. Coatings prepared from plasma processed powders enhance the coating properties positively.     

Shear bond strength and characterization of interfaces between electroformed gold substrates and porcelain

This study aimed to determine the effects of two different sandblasting conditions on the shear bond strength between electroformed Au substrates and porcelain, and characterize the interface between the Au substrate and porcelain. Electroformed Au specimens, 0.3 mm thick with a cap-like shape were prepared. The prepared specimens were then divided into two different groups and each group was sandblasted with a different size of alumina grains (100 or 250 μm) prior to dental porcelain application. Bonded specimens from each group were subjected to shear testing. After debonding, the fracture mode was analyzed by optical microscopy and SEM-EDX. One intact bonded specimen from each group was metallographically prepared to characterize the interfacial bonding by SEM-EDX and area scan analysis. The shear bond strength values (MPa) and standard deviations were 8.2 ± 1.8 and 9.1 ± 2.7 for the samples blasted with 100 and 250 μm alumina particles, respectively. No statistically significant difference was found between the two groups. In addition, no differences in fracture mode were found between the two groups. Qualitative analysis showed that, surprisingly, the Au substrate contained O, N, and P which might be related to the Au–sulfite electrolyte used in electroforming. As expected, the retained porcelain comprised Si, O, Al, Ca, Na and K. Mutual diffusion of Au, P, Si, Na, K and O without concentration gradients was found at the interface. Mutual ionic diffusion at the interface between ceramics and electroformed Au substrates (as opposed to mechanical interlocking) seems to be the most possible factor contributing to Au–ceramic bonding.     

Thermo-mechanical performance of an ablative/ceramic composite hybrid thermal protection structure for re-entry applications

Hybrid thermal protection systems for aerospace applications based on ablative material (ASTERM™) and ceramic matrix composite (SICARBON™) have been investigated. The ablative material and the ceramic matrix composite were joined using graphite and zirconia–zirconium silicate based commercial high temperature adhesives. The thermo-mechanical performance of the structures was assessed from room temperature up to 900 °C. In all the joints there is a decrease of shear strength with the increase of temperature. Analysis of the fractured surfaces showed that above 150 °C the predominant mode of fracture is cohesive failure in the bonding layer. The joints fabricated with the zirconia–zirconium silicate based adhesive present the best performance and they have the potential to be used as hybrid thermal protection systems for aerospace applications in the temperature range 700–900 °C.     

等离子喷涂制备钢质涂布刮刀陶瓷涂层

以涂层平面度为评价标准,通过正交试验优化等离子喷涂工艺参数,在普通蓝钢刮刀上制备Al2O3-20%TiO2涂层,并对涂层的显微形貌、结合强度和耐磨性进行了研究.结果表明:弧电流550 A,喷涂距离100 mm,走枪速度0.8 m/s时等离子喷涂制备的Al2O3-20%TiO2涂层平面度最优;涂层具有良好的结合强度和耐磨性,结合强度大于30 MPa;磨粒磨损机理为切削和脆性断裂或脱落磨损.     

Evaluation of the bond strength of a low-fusing porcelain to cast Ti–24Nb–4Zr–7.9Sn alloy

The purpose of this study was to compare the bonding characteristics of titanium porcelain Duceratin bonded to Ti–24Nb–4Zr–7.9Sn (TNZS) alloy and commercial pure titanium (cp Ti). The bond strengths between porcelain and TNZS were tested by a three-point flexural device. The same tests for the cp Ti were used as for the control. Coefficient of thermal expansion (CTE) of TNZS was evaluated with a push-rod dilatometer. Interfacial characterization was carried out by X-ray energy-dispersive spectrometry (EDS) analysis operating in line scan mode. Additionally, microstructure characterizations of TNZS and cp Ti after debonding fracture were analyzed by scanning electron microscope (SEM) and EDS. The porcelain bond strength of TNZS alloy was 31.51 MPa, showing a significant increase relatively to that of cp Ti (23.89 MPa) (P < 0.05). Mean CTE values of TNZS alloy was 9.51 × 10^? 6/°C exceeding the porcelain by 0.81 × 10^? 6/°C, attesting to a better mechanical performance. Interfacial characterization showed the mutual diffusion of Ti, Si, O and Sn along the TNZS–ceramic interface. Both SEM and EDS results revealed that fracture modes of TNZS specimens exhibited a mixed mode of cohesive and adhesive failures. The results demonstrated that TNZS could be a good alternative for the metal–ceramic restoration in the future.     

Synthesis and characterization of composite membrane by deposition of acrylic acid plasma polymer onto pre-treated polyethersulfone support

The plasma techniques were explored to deposit a layer of hydrophilic polymer on asymmetric porous membranes used as support material. Microporous membranes were synthesized by the phase inversion technique from polyethersulfone (PES) and submitted to a surface treatment with RF-plasma of non-polymerizable gas. Carbon dioxide (CO₂) was selected to generate this plasma and to increase the surface energy. Further plasma treatment proceeded with acrylic acid (AA) in vapor phase as source for the permanent surface hydrophilic functionalization. The infrared spectra with horizontal attenuated total reflectance (HATR) show that the deposited plasma polymer provides a high concentration of carbonyl and hydroxyl groups. The hydrophilic polymer layer was evenly deposited, with good adhesion to the support, as was observed by electronic microscopy (SEM). The surface free energy (γ_S) was increased through plasma treatments and confirmed by the decrease of contact angle (θ) measurements and increase of adhesion work (W _a). The nitrogen permeability decreased 650 times; after that a dense thin film was deposited by plasma treatment during 40 min (at 5 W and 8 Pa). Final composite membranes show stability, high surface hydrophilicity, and a surface chemical nature very stable with time.     

The effect of surface treatments on the adhesion of electrochemically deposited hydroxyapatite coating to titanium and on its interaction with cells and bacteria

The effect of different mechanical and chemical pre-treatments on the adhesion strength of hydroxyapatite (HAp) coating on a commercially pure titanium (CP-Ti) substrate was studied by means of a standard tensile test followed by microscopic and chemical analysis to determine the locus of fracture. In addition, the effects of either these pre-treatments or post-treatment by low-energy electron irradiation, which allowed tuning the wettability of the surface, on both osteoblast progenitor attachment and S. aureus bacteria attachment were investigated. A dedicated program was developed for unambiguous identification and count of stained cells. A single-phase HAp coating was formed by electrodeposition. A series of surface pre-treatments consisted of grinding down to P1000, etching in HNO₃/HF solution, grit blast, soaking in NaOH and subsequent heat treatment provided the highest adhesion strength to the HAp coating. Osteoblast progenitors derived from rats may be attached preferentially to a hydrophilic surface (post-treatment to θ = 30°), while the bacteria seemed to be less attached to hydrophobic surfaces (post-treatment to θ = 105°). However, the results were not statistically different. The bacteria seemed to be less attached to the smoother, uncoated surfaces.     

基于表面能理论研究盐冻循环对沥青-矿料界面粘附性的影响

根据表面能理论,采用接触角测量法测定盐冻循环前后苯乙烯-丁二烯-苯乙烯（SBS）、废胎胶粉（CR）和复合胶粉（CCR）3种聚合物改性沥青、石灰岩、玄武岩和花岗岩的表面自由能参数,分别计算出盐冻循环前后沥青-矿料系统的粘附功和剥落功,从而确定盐冻循环对沥青-矿料系统粘附和剥落特性的影响。结果表明:盐冻循环前后,沥青与矿料的粘附过程以及水侵入沥青-矿料界面的剥落过程的比表面自由能变化均为负值,说明沥青与矿料的粘附过程和剥落过程均自发进行;随着盐冻循环次数和盐浓度的增加,沥青-矿料系统粘附功逐渐减小,剥落功逐渐增大,粘附性和抗水损害能力逐渐减弱;当沥青种类相同时,沥青与石灰岩的粘附功最大,剥落功最小,沥青与花岗岩的粘附功最小,剥落功最大;当矿料种类相同时,CCR改性沥青与矿料的粘附功最大,剥落功最小,SBS改性沥青与矿料的粘附功最小,剥落功最大。      

Novel wear resistant and low toxicity dental obturation materials

Preparation of new polymer (polyurethane) + ceramic nanohybrids for filling dental cavities is reported. Short curing times (below 10 min) are achieved. Some tribological properties are determined and compared with those of commercial dental materials. The new materials provide scratch resistance as well as good adhesion to dentin and enamel, low toxicity and high chemical resistance; additionally, they can be easily pigmented to match the teeth color. Microscratch testing which provides the instantaneous penetration depth, the residual depth after scratch healing and the percentage recovery turns out to be a useful tool for differentiation of quality between dental obturation materials.     

Effect of ion exchange on <Emphasis Type="Italic">R</Emphasis>-curve behavior of a dental porcelain

The objective of this study was to evaluate the effect of the ion exchange treatment on the R-curve behavior of a leucite-reinforced dental porcelain, testing the hypothesis that the ion exchange is able to improve the R-curve behavior of the porcelain studied. Porcelain disks were sintered, finely polished, and submitted to an ion exchange treatment with a KNO₃ paste. The R-curve behavior was assessed by fracturing the specimens in a biaxial flexure design after making Vickers indentations in the center of the polished surface with loads of 1.8, 3.1, 4.9, 9.8, 31.4, and 49.0 N. The results showed that the ion exchange process resulted in significant improvements in terms of fracture toughness and flexural strength as compared to the untreated material. Nevertheless, the rising R-curve behavior previously observed in the control group disappeared after the ion exchange treatment, i.e., fracture toughness did not increase with the increase in crack size for the treated group.     

Influence of grain size on wear behavior of SiC coating for carbon/carbon composites at elevated temperatures

To improve the wear performance of SiC coating for C/C composites at elevated temperatures, the grain was refined by adding small amounts of titanium, in the raw powders for preparing this coating. The related microstructure and mechanical characteristics were investigated by scanning electron microscopy, X-ray diffraction, energy dispersive spectroscopy and nano-indention. The results show that the grain size of SiC coating decreased from ∼30 μm to ∼5 μm due to the addition of grain refiner. TiC formed by reacting titanium with graphite, can act as perfect heterogeneous nucleus for the nucleation and growth of β-SiC. The wear resistance and fracture toughness of SiC coating was improved by grain refinement. However, the increasing interfaces increased the friction resistance and resulted in the high friction coefficient of fine-grained coating at room temperature. As the temperature rose, oxides layer formed on the surface of fine-grained coating, which can reduce the adhesive wear and decrease the friction coefficient. The fine-grained coating exhibited relative low friction coefficient of ∼0.41 owing to a compact silica film formed on the worn surface at 600 °C, and the wear was dominated by plastic deformation and shear of silica film. The wear of coarse-grained coating was controlled by the fracture of SiC at high temperature.