Alteration of the intaglio surface of lithium disilicate glass-ceramic.

STATEMENT OF PROBLEM: Clinical adjustment of a lithium disilicate glass-ceramic (LDGC) restoration may necessitate its return to the laboratory for additional firing. Evidence of how the intaglio surface should be re-etched after internal adjustment, or after refiring, is lacking. PURPOSE: The purpose of this in vitro study was to investigate the effects of different sequences of etching, refiring, diamond rotary instrument adjustment, airborne-particle abrasion, and re-etching on the microstructure and surface roughness of the intaglio surface of heat-pressed LDGCs. MATERIAL AND METHODS: Heat-pressed LDGC specimens were ground with abrasive paper to produce a uniformly flat surface. The groups (n=3) were subjected to different combinations of etching, refiring, diamond rotary instrument adjustment, airborne-particle abrasion, and re-etching. X-ray diffraction was used to characterize the crystalline phases. Scanning electron microscopy and surface profilometry were used to characterize the microstructure and surface roughness. RESULTS: Qualitative differences were observed in the surface texture of specimens etched for different periods. Excessive etching revealed more of the underlying lithium disilicate crystallites and caused surface pitting for the longest etching period studied. Refiring altered the surface condition but did not completely remove the texture created by the original etching. Diamond rotary instrument adjustment resulted in appreciable surface damage and a higher mean value of measured surface roughness (with or without re-etching) than the other groups. Airborne-particle abrasion caused embedding of particles in the specimen surface, likely corresponding to the abrasion media, although this process resulted in qualitatively less surface damage than diamond rotary instrument adjustment. CONCLUSIONS: Excessive etching, refiring, and adjustment by airborne-particle abrasion or diamond rotary instrument result in qualitative changes in surface condition. Adjustment by diamond rotary instrument results in appreciable surface damage.

An investigation into the factors that influence toolmark identifications on ammunition discharged from semi-automatic pistols recovered from car fires.

Following a shooting incident where a vehicle is used to convey the culprits to and from the scene, both the getaway car and the firearm are often deliberately burned in an attempt to destroy any forensic evidence which may be subsequently recovered. Here we investigate the factors that influence the ability to make toolmark identifications on ammunition discharged from pistols recovered from such car fires. This work was carried out by conducting a number of controlled furnace tests in conjunction with real car fire tests in which three 9mm semi-automatic pistols were burned. Comparisons between pre-burn and post burn test fired ammunition discharged from these pistols were then performed to establish if identifications were still possible. The surfaces of the furnace heated samples and car fire samples were examined following heating/burning to establish what factors had influenced their surface morphology. The primary influence on the surfaces of the furnace heated and car fire samples was the formation of oxide layers. The car fire samples were altered to a greater extent than the furnace heated samples. Identifications were still possible between pre- and post-burn discharged cartridge cases, but this was not the case for the discharged bullets. It is suggested that the reason for this is a difference between the types of firearms discharge-generated toolmarks impressed onto the base of cartridge cases compared to those striated along the surfaces of bullets. It was also found that the temperatures recorded in the front foot wells were considerably less than those recorded on top of the rear seats during the car fires. These factors should be assessed by forensic firearms examiners when performing casework involving pistols recovered from car fires.

Hydroxyapatite and fluorapatite coatings on dental screws: effects of blast coating process and biological response.

This paper describes the deposition of hydroxyapatite (HA) and fluorapatite (FA) onto titanium dental screws using a novel ambient temperature coating technique named CoBlast. The process utilises a coating medium and a blast medium sprayed simultaneously at the substrate surface. The blast medium was a sintered apatite (sHA) and two particles sizes (<106 and <180 µm) were used to assess their influence on the coating process. The influence of the coating process on the coating composition, coating adhesion, screw morphology and screw microstructure was examined. XRD analysis revealed the coating crystallinity was the same as the original HA and FA feedstock powders. Examining the screw's morphology, the threads of the CoBlasted screws exhibited rounding compared to the unmodified screw. This is due to the abrasive nature of the CoBlast process. The degree of rounding was more significant for the screws blasted with the 180 µm sHA than the 106 µm sHA. The blast media particle size significantly influences the surface roughness of both the substrate and coating and the microstructure of the substrate. The screws did not exhibit any loss of coating after insertion into a model bone material, indicating that the coating was strongly adhered to the substrate. There was no statistically significant difference in cell attachment and cell morphology on the unmodified substrates compared to the coated substrates. In conclusion, the CoBlast process can be used to deposit HA and FA onto complex geometries such as dental screws. The choice of blast medium particle size influences the screws morphology. The coating process does not negatively impact on the cell attachment and morphology in vitro.

Effects of repeated processing on the strength and microstructure of a heat-pressed dental ceramic.

STATEMENT OF PROBLEM: The excess material produced after heat pressing a lithium disilicate glass ceramic restoration can be either discarded or reused. The reuse of this material requires that any degradation of the material quality be investigated. PURPOSE: The purpose of this study was to investigate the number of times that leftover lithium disilicate material can be re-pressed and to determine the effect that repeated use has on material properties. MATERIAL AND METHODS: A large (6.1 g) lithium disilicate ingot (A3.5) was heat pressed to yield a ceramic disk (15 × 1.5 mm) for testing. The leftover material was reused to produce a further 3 disks, with the number of pressings increasing for each specimen. An additional unpressed group was included to investigate the properties before pressing so that, in total, 5 groups were established. Specimens were tested for biaxial flexural strength, Vickers hardness, and fracture toughness. X-ray diffraction was used to characterize the crystalline phase, scanning electron microscopy for the microstructure, and differential scanning calorimetry for the thermal properties. RESULTS: No significant difference was found in the biaxial flexural strength of the groups. The hardness of the material decreased, and no significant difference was seen in fracture toughness with repeated pressings. An increase in grain size was observed with increased pressings. By using x-ray diffraction analysis, lithium disilicate was identified as the main crystal phase, and no difference in crystalline composition was found with repeated processing. CONCLUSION: This material can be reused while maintaining good mechanical properties and without significantly altering the chemical or crystalline composition in an adverse manner.

Optimisation of the enamelling of an apatite-mullite glass-ceramic coating on Ti6Al4V.

Apatite-mullite glass-ceramics (AMGCs) are under investigation as a potential alternative to hydroxyapatite (HA) as a coating for cementless fixation of orthopaedic implants. These materials have tailorable mechanical and chemical properties that make them attractive for use as bioactive coatings. Here, AMGC coatings on Ti(6)Al(4)V were investigated to determine an improved heat treatment regime using a systematic examination of the different inputs: composition of glass, nucleation hold and crystallisation hold. An upper limit to the heat treatment temperature was determined by the α + ß --> ß of Ti(6)Al(4)V at 970°C. The glass composition was modified to produce different crystallisation temperatures and sintering characteristics. A glass was found that is fully crystalline below 970°C and has good sinterability. The effects of different heat treatment time and temperature combinations on the coating and substrate morphologies were examined and the most suitable combination determined. This sample was further investigated and was found to have qualitatively good adhesion and evidence of an interfacial reaction region between the coating and substrate indicating that a chemical reaction had occurred. Oxygen infiltration into the substrate was quantified and the new route was shown to result in a 63% reduction in penetration depth.

Microwave-assisted rapid discharge sintering of a bioactive glass-ceramic.

Bioactive glass-ceramics have been developed as successful bone graft materials. Although conventional sintering in an electrically-heated furnace is most commonly used, an alternative microwave plasma batch processing technique, known as rapid discharge sintering (RDS), is examined to crystallise the metastable base glass to form one or more ceramic phases. Apatite-mullite glass-ceramics (AMGC) were examined to elucidate the effects of RDS on the crystallization of a bioactive glass-ceramic. By increasing the fluorine content of the glass, the fluorapatite (FAp) and mullite crystallization onset temperatures can be reduced. Samples were sintered in a hydrogen and hydrogen/nitrogen discharge at temperatures of ≈800 and 1000 °C respectively with the higher sintering temperature required to form mullite. Results show that the material can be densified and crystallised using RDS in a considerably shorter time than conventional sintering due to heating and cooling rates of ≈400 °C/min.

Comparison of shear bond strength and ARI of four different adhesive systems used to bond molar tubes: An in vitro study.

OBJECTIVE: The purpose of this in vitro study was to determine and compare the shear bond strength and ARI score of one traditional etch-and-rinse adhesive system serving as control, with those of two other all-in-one adhesives but with enamel acid etching preceding their application, and of one new 8th generation all-in-one bonding agent combined with a traditional adhesive used to bond stainless steel buccal tubes to molar teeth. MATERIAL AND METHODS: Four groups of teeth were formulated according to the adhesive system used to bond the tubes on the molars. Shear bond strength was measured using a universal testing machine (Hounsfield, UK). After debonding, each enamel surface was imaged using Inspex HD l080p Vesa camera (Ash Technologies Ltd., Ireland) to determine the ARI score. RESULTS: The mean SBSs in MPa for the four groups were respectively: A: 9.640 (±3.69), B: 10.261 (±3.03), C: 9.689 (±2.48), D: 8.412 (±3.02). No statistically significant differences were neither found through one-way ANOVA to exist between the group means (P: 0.715), nor for the ARI score frequence through Chi2 (P: 0.534). Maxcem Elite showed four and G-Premio Bond zero instances of enamel fracture. CONCLUSIONS: 1. SBSs of all adhesives and ARI score distributions did not present any significant differences when used to bond stainless steel molar tubes. 2. All adhesives presented with acceptable shear bond strengths for clinical use. 3. Maxcem Elite under the tested conditions presented the greatest and G-Premio the least number of enamel fractures.

Development and characterisation of a collagen nano-hydroxyapatite composite scaffold for bone tissue engineering.

Bone regeneration requires scaffolds that possess suitable mechanical and biological properties. This study sought to develop a novel collagen-nHA biocomposite scaffold via two new methods. Firstly a stable nHA suspension was produced and added to a collagen slurry (suspension method), and secondly, porous collagen scaffolds were immersed in nHA suspension after freeze-drying (immersion method). Significantly stronger constructs were produced using both methods compared to collagen only scaffolds, with a high porosity maintained (>98.9%). It was found that Coll-nHA composite scaffolds produced by the suspension method were up to 18 times stiffer than the collagen control (5.50 +/- 1.70 kPa vs. 0.30 +/- 0.09 kPa). The suspension method was also more reproducible, and the quantity of nHA incorporated could be varied with greater ease than with the immersion technique. In addition, Coll-nHA composites display excellent biological activity, demonstrating their potential as bone graft substitutes in orthopaedic regenerative medicine.

Study of the interfacial reactions between a bioactive apatite-mullite glass-ceramic coating and titanium substrates using high angle annular dark field transmission electron microscopy.

Glass of generic composition SiO(2) . Al(2)O(3) . P(2)O(5) . CaO . CaF(2) will crystallise predominantly to apatite and mullite upon heat-treatment. Such ceramics are bioactive, osseoconductive, and have a high resistance to fracture. As a result, they are under investigation for use as biomedical device coatings, and in particular for orthopaedic implants. Previous work has shown that the material can be successfully enamelled to titanium with an interfacial reaction zone produced during heat treatment. The present study uses high angle annular dark field transmission electron microscopy (HAADF-TEM) to conduct a detailed examination of this region. Results show evidence of complex interfacial reactions following the diffusion of titanium into an intermediate layer and the production of titanium silicides and titanium phosphides. These results confirm previously hypothesised mechanisms for the bonding of silicate bioceramics with titanium alloys.

Improved consistency of bond-line thickness when conducting single lap-shear joint tests.

This article details a method for improving the consistency of bond-line thickness during lap-shear sample preparation. This includes the schematic for a lap-shear sample test rig and consideration for controlled variation of the bond-line thickness for up to ten pairs of samples at a time. Concerns regarding the curing of the samples when held on a large heat reservoir are addressed through direct measurement of the bond-rig temperature in combination with the cure chamber temperature. Additionally, the application of a release coating to the bond-rig has been demonstrated to improve ease of sample removal for the bond-rig, minimizing potential damage to the lap-shear sample set before testing. The release coating provides a clean surface for subsequent sets of samples, ensuring an even surface and reducing cleaning and degradation of the machined geometries of the rig. Overall, the proposed bond-rig provides: •Increased bond-line uniformity•Up to ten samples prepared in a batch•Option to apply a release coating to improve usability and minimize cleaning.

Preparation of morselised bone for impaction grafting using a blender method.

Impaction bone grafting is a method of restoring bone stock to patients suffering significant bone loss due to revision total hip surgery. The procedure requires morselised bone (MB) to be impacted into the site of bone loss in order to stabilise the prosthesis with the aim of the long term resorption and reintegration of the impacted bone graft. Currently, the method for producing MB requires the use of expensive surgical bone mills or manually-intensive rongeurs that can produce a limited variety of particle sizes and may have a low throughput. This study examines the potential to produce suitable MB using a domestic blender. The method produces a wide range of particle sizes without the need for an adjustment of the system. It was found through packing modelling that this particle distribution resulted in reduced initial graft porosity and thus a theoretical potential to increase the graft stiffness and ability of the graft to stabilise a prosthesis in comparison to a manually prepared roughly cut morselised bone samples. Mechanical testing confirmed the increased mechanical performance of the graft through both impaction testing and subsidence testing. The blended MB was found to exhibit greater graft stiffness under the same impaction conditions. The graft was also found to have subsided less in comparison to the rough cut, less well graded MB. Scanning electron imaging also confirmed the retention of the trabecular structure necessary for revascularisation and host bone ingrowth. In conclusion, the blender method offers a rapid and cheap way of obtaining morselised bone with favourable particle size distribution, particle morphology and mechanical properties with preservation of the bone trabecular structure.

The use of hardened bone cement as an impaction grafting extender for revision hip arthroplasty.

Impaction bone grafting is a method of restoring bone stock to patients who have suffered significant bone loss due to revision total hip surgery. The procedure requires morsellised cancellous bone (MCB) to be impacted into the site of bone loss in order to stabilise the prosthesis with the aim of long term resorption and reintegration of the impacted bone graft. Due to financial cost and the potential to transmit disease, the use of supplementary material, known as an extender, is frequently used to increase the graft material volume. This study investigates the use of hardened Hydroset (Stryker Corp, MA, USA), an injectable bone cement (IBC), as an extender material and compares the performance of the IBC in different weight percent inclusions to a commercially available bone graft extender (GCP, BoneSave, Stryker Corp, MA, USA). The surgical impaction procedure was standardised and samples were evaluated in terms of graft stiffness and height. It was observed that 30wt% IBC extended samples had significantly improved graft stiffness (p = 0.02) and no significant different in height (p = 0.067) over a 100% MCB control sample. Cyclic loading, representative of gait, found that the IBC subsided similarly to the commercial bone substitute in wt% above 10%. Shear testing of the impacted grafts showed no significant differences between GCP and IBC with impaction forces determining the shear parameters of impacted grafts. The effects of the impaction and cyclical loading procedures on extender particle sizes was assessed via particle size analysis. It was found that the IBC extended samples demonstrated reduced friability, evident in the better retention of particle size as a result of both impaction and gait representative loading compared to that of the GCP samples. This indicates a potential reduction in issues arising from small particle migration to joint surfaces. Scanning electron microscopy of the MCB particles with both GCP and IBC as extenders showed retention of the porous trabecular structure post-testing which is essential for revascularisation and bone growth into the graft.

The effect of hyperbranched poly(acrylic acid)s on the morphology and size of precipitated nanoscale (fluor)hydroxyapatite.

Hydroxyapatite and fluorhydroxyapatite (F)HA nanoparticles were synthesised in the presence of branched poly(acrylic acid)s (PAA) synthesised via reversible addition-fragmentation chain transfer polymerisation and compared to those synthesised in the presence of linear PAA. Analysis of the resulting nanoparticles using Fourier transform infrared spectroscopy, powder X-ray diffraction and transition electron microscopy found that the polymer was included within the nanoparticle samples and affected their morphology with nanoparticles synthesised in the presence of branched PAA being more acicular and smaller overall.

Human plasma protein adsorption onto alumina nanoparticles relevant to orthopedic wear.

PURPOSE: Wear of ceramic orthopedic devices generates nanoparticles in vivo that may present a different biological character from the monolithic ceramic from which they are formed. The current work investigated protein adsorption from human plasma on alumina nanoparticles and monolithic samples representative of both wear particles and the ceramic components as implanted. MATERIALS AND METHODS: A physicochemical characterization of the particles and their dispersion state was carried out, and the protein adsorption profiles were analyzed using 1D SDS-PAGE and mass spectrometry. RESULTS: Significant differences in protein-binding profiles were identified where the nanoparticles selectively bound known transporter proteins rather than the more highly abundant serum proteins that were observed on the monoliths. CONCLUSIONS: Proteins associated with opsonization of particles were seen to be present in the protein corona of the nanoparticles, which raises questions regarding the role of wear particles in periprosthetic tissue inflammation and aseptic loosening.

Co-blasting of titanium surfaces with an abrasive and hydroxyapatite to produce bioactive coatings: substrate and coating characterisation.

The aim of this work is to assess the influence of two blast media on the deposition of hydroxyapatite onto a titanium substrate using a novel ambient temperature coating technique named CoBlast. CoBlast was developed to address the problems with high temperature coating techniques. The blasting media used in this study were Al2O3 and a sintered apatite powder. The prepared and coated surfaces were compared to plasma sprayed hydroxyapatite on the same substrates using the same hydroxyapatite feedstock powder. X-ray diffraction analysis revealed the coating crystallinity was the same as the original hydroxyapatite feedstock powder for the CoBlast samples while evidence of amorphous hydroxyapatite phases and ß-TCP was observed in the plasma sprayed samples. The blast media type significantly influences the adhesive strength of the coating, surface roughness of both the substrate and coating and the microstructure of the substrate. The coating adhesion increased for the CoBlasted samples from 50 MPa to 60 MPa for sintered apatite powder and alumina, respectively, while plasma spray samples were significantly lower (5 MPa) when tested using a modified pull-test. In conclusion, the choice of blast medium is shown to be a key parameter in the CoBlast process. This study indicates that sintered apatite powder is the most suitable candidate for use as a blast medium in the coating of medical devices.

The synthesis and characterization of nanophase hydroxyapatite using a novel dispersant-aided precipitation method.

The synthesis of nanophase hydroxyapatite (nHA) is of importance in the field of biomaterials and bone tissue engineering. The bioactive and osteoconductive properties of nHA are of much benefit to a wide range of biomedical applications such as producing bone tissue engineered constructs, coating medical implants, or as a carrier for plasmid DNA in gene delivery. This study aimed to develop a novel low-temperature dispersant-aided precipitation reaction to produce nHA particles (<100 nm), which are regarded as being preferable to micron-sized agglomerates of nHA. The variables investigated and optimized include the reaction pH, the rate of reactant mixing, use of sonication, order of addition, and concentration of the primary reactants, in addition, the effect of using poly(vinyl alcohol) (PVA) surfactant and Darvan 821A® dispersing agent during the reaction was also examined. It was found that by fine-tuning the synthesis parameters and incorporating the dispersing agent, monodisperse, phase-pure nano-sized particles under 100 nm were attained, suitable for clinical applications in bone regeneration.