Inline electron holography and VEELS for the measurement of strain in ternary and quaternary (In,Al,Ga)N alloyed thin films and its effect on bandgap energy

We present the use of (1) dark‐field inline electron holography for measuring the structural strain, and indirectly obtaining the composition, in a wurtzite, 4‐nm‐thick InAlGaN epilayer on a AlN/GaN/AlN/GaN multinano‐layer heterosystem, and (2) valence electron energy‐loss spectroscopy to study the bandgap value of five different, also hexagonal, 20–50‐nm‐thick InAlGaN layers. The measured strain values were almost identical to the ones obtained by other techniques for similarly grown materials. We found that the biaxial strain in the III‐N alloys lowers the bandgap energy as compared to the value calculated with different known expressions and bowing parameters for unstrained layers. By contrast, calculated and experimental values agreed in the case of lattice‐matched (almost unstrained) heterostructures.     

Characterization of Heat Treated Titanium-Based Implants by Nondestructive Eddy Current and Ultrasonic Tests

This study presents nondestructive characterization of microstructure and mechanical properties of heat treated Ti, Ti-Cu, and Ti-6Al-4V titanium-based alloys and 17-4 PH stainless steel alloy for biomedical implant applications. Ti, Ti-Cu, and 17-4 PH stainless steel based implants were produced by powder metallurgy. Ti-6Al-4V alloy was investigated as bulk wrought specimens. Effects of sintering temperature, aging, and grain size on mechanical properties were investigated by nondestructive and destructive tests comparatively. Ultrasonic velocity in specimens was measured by using pulse-echo and transmission methods. Electrical conductivity of specimens was determined by eddy current tests. Determination of Young’s modulus and strength is important in biomedical implants. Young’s modulus of specimens was calculated by using ultrasonic velocities. Calculated Young’s modulus values were compared and correlated with experimental values.     

Column Fractionation of Canola Oil Deodorizer Distillate Using Supercritical Carbon Dioxide

Semi-continuous column fractionation of canola oil deodorizer distillate using supercritical CO₂ (SCCO₂) was carried out to determine the feasibility of value-added processing of this feed material for the recovery of bioactive components such as sterols and tocopherols and to determine the effect of operating conditions [pressure (20, 25 MPa using a temperature gradient of 70–100 °C), temperature (70, 100 °C) and a linear temperature gradient (70–100 °C at 25 MPa)] on extract yield and separation efficiency. Total extract yield increased significantly (p ≤ 0.05) with pressure, whereas at isobaric conditions (25 MPa) the highest yield was obtained at the lowest temperature tested (70 °C). Fractionation efficiency was reflected in the composition of fractions and was affected by operating conditions. Residue composition was determined by extract yield in addition to selectivity. Use of the thermal gradient (70–100 °C) decreased the content of volatiles, free fatty acids and tocopherols while increasing sterol content significantly (p ≤ 0.05) to a level of 40% (GC area %) in the residue obtained at 25 MPa. The findings indicate the potential of canola oil deodorizer distillate as a source of sterols and warrant further research on the countercurrent column fractionation to improve the separation efficiency.     

Effects of different particle deposition parameters on adhesion of resin cement to zirconium dioxide and phase transformation

This study evaluated the effect of air-abrasion parameters such as particle size, distance, and time on adhesion of resin cement to zirconium dioxide (Y-TZP) and t→m phase transformation. Y-TZP blocks (N = 80) (In-Ceram YZ, Vita) (4 mm^3?×?4 mm^3?×?3 mm³) were assigned into eight groups (n = 10): air-abrasion with 30 μm (CoJet Sand, S30) and 110 μm (Rocatec-Plus, S110) silica-coated alumina particles, applied for either for 10–20 s (T = time), from a distance of 10–20 mm (D = distance), composing the following groups: S₃₀T₁₀D₁₀, S₃₀T₁₀D₂₀, S₃₀T₂₀D₁₀, S₃₀T₂₀D₂₀, S₁₁₀T₁₀D₁₀, S₁₁₀T₁₀D₂₀, S₁₁₀T₂₀D₁₀, and S₁₁₀T₂₀D₂₀. Resin composite (RelyX ARC) was bonded to Y-TZP blocks in polyethylene molds. The specimens were aged (10,000 thermal cycles and water storage for 90 days) prior to shear bond test. Failure types were analyzed under stereomicroscope and SEM, and phase transformation was calculated. Data (MPa) were analyzed using 3-way ANOVA and Tukey’s tests. Air-abrasion with 110 μm silica particles (10.96) presented significantly higher bond strength (p = 0.0149) compared to 30 μm (8.96). Time (p = 0.403) and distance (p = 0.179) parameters did not affect the results significantly. Air-abrasion with 110 μm particles (12.3) promoted higher bond strength than that of 30 μm (6.4) when applied for 10 s from a distance of 10 mm (Tukey’s). Failure types were predominantly adhesive. Phase transformation ranged between 30.3 and 35.9% for 30 μm particles and 23.8–43.7% for 110 μm particles. While the size of silica-coated alumina particles were more relevant parameter for resin cement adhesion to Y-TZP, time (up to 20 s) and distance (up to 20 mm) appear to be less pertinent.     

Long-term microleakage trends in access cavities conditioned with phosphoric acid and deproteinizing agent for root-canal-treated teeth: an investigation of fluid filtration and microscopy analysis

This study evaluated the long-term microleakage of access cavities conditioned with phosphoric acid and deproteinizing agents for root-canal-treated teeth using fluid filtration and microscopical analysis. Occlusal surfaces of extracted human mandibular premolars (N = 90) were removed leaving a 4 mm coronal length from the cemento-enamel junction. After root canal treatment, the specimens were randomly divided into four experimental groups (n = 21) and the remaining teeth were used for positive control group (n = 6): SB: 35% H₃PO₄ + Adper Single Bond 2; SSB: 35% H₃PO₄ + 5.25% NaOCl + 10% Sodium ascorbate (C₆H₇NaO₆) + Adper Single Bond 2; XP: 35% H₃PO₄₊XP Bond; SXP: 35% H₃PO₄₊5.25% NaOCl + 10% Sodium ascorbate + XP Bond. All cavities were restored with a resin composite (Filtek Z250). After removing the root filling from the apical side, teeth were subjected to fluid filtration test for 1 week, 6 and 12 months followed by ×2500 thermocycling after 1st week and 6th months each. Data were analyzed using one-way ANOVA and Dunnet T3 tests (α = 0.05). SEM analyses were carried out after each microleakage evaluation in two random teeth from all groups. Microleakage values in groups SB and XP presented no significant difference in any of the evaluated period (p > 0.05). Microleakage results of SXP (0.01665) group showed significant difference compared to XP (0.03377) and SB (0.03049) groups after 12 months. SSB group (0.00901) showed significantly less microleakage among all other groups (0.01665–0.03377) (p < 0.05). Prior to endodontic treatment, in access cavities, acid etching with 35% H₃PO₄ followed by the application of NaOCl and sodium ascorbate completely destroyed the collagen layer, reducing the microleakage and resin–dentin interface degradation up to 12 months.     

Analysis of structural,morphological alterations,wettability characteristics and adhesion to enamel after various surface conditioning methods

Minimal invasive dental reconstructions and orthodontic appliances are bonded to enamel without removing the enamel with rotating instruments but the top layer of enamel may be partially aprismatic and impair adhesion. The objectives of this study were to investigate the effect of mechanical surface conditioning methods for removing enamel on its structural, morphological alterations, wettability characteristics, and adhesion of resin-based cement to the conditioned surfaces. Maxillary human incisors (N = 40, n_quadrant = 160) were obtained and coronal sections were embedded in acrylic with their labial surfaces exposed. The teeth were randomly divided into four groups and the enamel surface of each tooth was divided into four quadrants. The surfaces were conditioned in a clockwise manner by one of the following methods: (1) Non-conditioned enamel acted as the control group (C); (2) Silicone-coated disk (Sof-Lex disc, Black, 3 M ESPE) (SD); (3) Diamond bur at slow speed (DB) and (4) Airborne particle abrasion (50 μm Al₂O₃, 2 bar, 5 s) (AA). Surface roughness was measured at each quadrant using a non-contact digital profilometer and contact angle measurements were performed using a goniometer. Enamel surfaces were then etched with 37% H₃PO₄ for 60 s and roughness and wettability measurements were repeated. The enamel surfaces in each quadrant received resin composite luting cement (Variolink II, Ivoclar Vivadent) incrementally in a polyethylene mold (diameter: 1 mm²; height: 4 mm) and photopolymerized. The specimens were stored in distilled water for 24 h at 37 °C until the testing procedures and then shear force was applied to the adhesive interface until failure occurred in a Universal Testing Machine (0.5 mm/min). Microshear bond (μSBS) was calculated by dividing the maximum load (N) by the bonding surface area of the resin cement. Representative enamel surfaces were analyzed under the scanning electron microscope (SEM) (x5000) to assess the surface morphology. Failure types were analyzed using optical microscope and SEM. Data (MPa) were analyzed using one-way ANOVA and Tukey`s test for each parameter and Linear model for group comparisons (α = 0.05). Surface conditioning method significantly affected the adhesion results (p < 0.001), surface roughness (p = 0.017), and contact angle (p < 0.001). Interaction terms were significant (p > 0.05). AA (338 ± 182) created significantly higher surface roughness compared to SD (308 ± 180) and DB (242 ± 197) (p < 0.05). After etching with 37% H₃PO₄, DB (307 ± 223) resulted in significantly lower roughness than those of SD (385 ± 173) and AA (414 ± 193) (p < 0.05). AA (40 ± 11) delivered significantly lower contact angle compared to those of SD (61 ± 9) and DB (59 ± 10). After etching with 37% H₃PO₄, AA (42 ± 10) and DB (50 ± 10) presented the lowest contact angle (p < 0.05). Mean μSBS results (MPa) showed significant difference between the experimental groups (p = 0.011) and were in descending order as follows: DB (20 ± 8)^a?a b < C (12 ± 5)^b. Failure types were predominantly mixed failure type between the enamel and the resin cement with more than half of the resin remained on the enamel surface (32 to 33 out of 40) in all groups. Cohesive failure in the enamel was not observed in any of the groups. SEM analysis showed that AA group leaves abundant particles on the enamel surface and after DB and AA, etching could not remove the particles completely and expose the enamel prisms.     

Comparison of methanol/hydrochloric,ferric chloride acid versus tribochemical silica coating for adhesion of resin cement to zirconium dioxide

This study compared air-abrasion and etching regimens on adhesion of resin luting agent to zirconium dioxide. Ceramic specimens (LAVA, 3 M ESPE) (N = 16) were embedded in acrylic resin and exposed surfaces were polished. The specimens were randomly assigned into four groups (n = 12, 3 specimens for each disc): SC: Air-borne particle abrasion (30 μm aluminum oxide particles coated with silica, CoJet, 3 M ESPE); MH: Heated chemical solution (Methanol-800 mL; 37% Hydrochloric Acid-200 mL; Ferric Chloride-2 g) at 100 °C for 30 min, MHP: Primer (Metal/Zirconia Primer, Ivoclar Vivadent) + MH, P: Primer only (Metal/Zirconia Primer). Cylindrical molds (internal diameter: 0.7 mm; height: 1.5 mm) were placed on each conditioned specimen, filled with resin cement (Multilink Automix) and photo-polymerized for 60 s. After 24 h, the molds were removed and the specimens were stored in distilled water at 37 °C for six months). Microshear test was performed in a Universal Testing Machine (1 mm/min). Failures types were classified as adhesive, mixed, or cohesive. In another set of specimens (n = 2 per group) contact angle measurements were recorded. Data were analyzed statistically using Kruskal–Wallis and Dunn’s tests (α = 0.05). The surface conditioning method significantly affected the mean bond strength (MPa) (p < 0.0001): SC(18.3 ± 0.3)^a < P(5.00 ± 0.07)^b < MHP(4.7 ± 0.08)^c < MH(0.84 ± 0.01)^c. While Group SC showed mainly adhesive (58%) and mixed (41.7%) failure types, groups MH, MHP, and P presented exclusively adhesive failures. SC, MHP, and P (29–32°) showed lower contact angle than MH (78.9°). Volume loss was the highest with MHP (9.92 μl) followed by SC (9.67 μl).     

Graphene oxide-containing isocyanate-based polyimide foams: Enhanced thermal stability and flame retardancy

Isocyanate-based graphene oxide-containing polyimide foams were synthesized by a semi-prepolymer method. In this method, while the first solution containing pre-polymer was derived from pyromellitic dianhydride and excess polymethylene polyphenylene isocyanate (PM200), the second solution contains dianhydride derivatives, water, catalysts, surfactants, and graphene oxide. PIFs were prepared with 0%, 0.25%, 0.50%, 0.75%, and 1% graphene oxide by weight, respectively. PIFs exhibited a minimum side reaction and urea generation was not seen for all PIFs instead of imide bonding. The addition of graphene oxide (GO) leads to a more close-packed structure. Therefore, crosslinking density and thermal stability of graphene oxide-containing polyimide foams increased. Upon the addition of 1% GO, almost seven times higher compression strength was obtained compared to neat PIFs. Also, LOI values supported the theory that thermally stable and flame retardant PIFs can be synthesized via the isocyanate-based process with GO.     

Synthesis of N‐polyethereal polypyrroles and their application for the preconcentration of rare earth ions

Conducting polymers containing polyether pseudocages (P I , P II , P III ) have been synthesized via chemical oxidation of 1,5‐bis(1,1‐pyrrole)‐3‐oxabutane (M I ), 1,8‐bis(1,1‐pyrrole)‐3,6‐dioxahexane (M II ), and 1,11‐bis(1,1‐pyrrole)‐3,6,9‐trioxaundecane (M III ) using anhydrous FeCl₃ in CHCl₃. Because as obtained polymer resins did not give any response toward any cations, they were reduced (undoped) using chemical reducing agents. Tetrabutylammonium hydroxide was found to be more effective in undoping to obtain more reproducible and reusable polymer resins. The undoped polymer resins were tried in the extraction of rare earth metal ions from the aqueous medium. Among them, only P III resin removes La(III), Eu(III) and Yb(III) and can be employed for the preconcentration of these metal ions. For batch extraction of La(III), Eu(III) and Yb(III) at neutral pH values, percent recoveries of 98.0 ± 1.0, 90.7 ± 1.4, 87.3 ± 4.0, respectively, has been obtained. The sorption capacity is found as 1.3 mg of La(III) per gram of P III resin. The P III resin could be reused at least five times without significant change in its sorption capacity. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008