Can Heat Treatment Procedures of Pre-hydrolyzed Silane Replace Hydrofluoric Acid in the Adhesion of Resin Cement to Feldspathic Ceramic?

Purpose: To evaluate the influence of heat treatment (HT) procedures of a pre-hydrolyzed silane on bond strength of resin cement to a feldspathic ceramic.Materials and Methods: Ceramic and composite blocks (N = 30) were divided into six groups (n = 5) and subjected to the following conditioning procedures: G1: 9.6% hydrofluoric acid (HF) for 20 s + silane (RelyX Ceramic Primer, 3M ESPE) + resin cement (Panavia F2.0, Kuraray) (control); G2: HF (20 s) + silane + heat treatment in furnace (HTF) (100 degrees C, 2 min) + resin cement; G3: silane + HTF + resin cement; G4-HF (20 s) + silane + heat treatment with hot air (HTA) (50 +/- 5 degrees C for 1 min) + resin cement; G5: silane + HTA + resin cement; G6: silane + resin cement. The microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using a stereomicroscope and SEM to categorize the failure types. The data were statistically evaluated using one-way ANOVA and Tukey's test (5%).Results: The control group (G1) showed no pre-test failures and presented significantly higher mean MTBS (16.01 +/- 1.12 MPa) than did other groups (2.63 +/- 1.05 to 12.55 +/- 1.52 MPa) (p = 0.0001). In the groups where HF was not used, HTF (G3: 12.55 +/- 1.52 MPa) showed significantly higher MTBS than did HTA (G5: 2.63 +/- 1.05 MPa) (p < 0.05). All failure types were mixed, ie, adhesive between the resin cement and ceramic accompanied by cohesive failure in the cement.Conclusion: Heat treatment procedures for the pre-hydrolyzed silane either in a furnace or with the application of hot air cannot replace the use of HF gel for the adhesion of resin cement to feldspathic ceramic. Yet when mean bond strengths and incidence of pre-test failures are considered, furnace heat treatment delivered the second best results after the control group, being considerably better than hot air application.

The Influence of the Heat Treatment Temperatures in Calcium Phosphate Synthesis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Parameters optimization of heat treatment for obtaining luminescent PZT powders

Low crystalline PZT powder samples were successfully synthesized using polymeric precursor method and slow decomposition steps. The polymeric resin precursor was thermal treated in a muffle type oven varying the temperature from 250 °C to 700 °C and the time from 3 to 24 hours in order to investigate the order/disorder mechanism toward the amorphous powders. Powder samples with low crystalline phases were obtained at lower temperatures and long time of thermal treatment, demonstrating a kinetic dependence for organic removal and a thermodynamic barrier for crystallization processes. Through XRD and FTIR spectroscopy characterizations the long time thermal treated samples showed to be composed of the solid solution of metal oxides in absent of organic matter, originating broad XRD peaks profiles and no carbonaceous bands in FTIR spectra. A Photoluminescence characterization showed that the peak emission is higher for disordered and homogeneous phases, which only can be reached through the long time of thermal treatment.

Influence of heat treatment and mechanical cycling on hardness and fracture analysis of Ti35Nb5Zr casting alloy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of post-polymerization heat treatment on a denture base acrylic resin: histopathological analysis in rats

This work examined the histological effects, on the rat palatal mucosa, of a denture base acrylic resin, submitted or not to a post-polymerization heat-treatment. Methods: Fifteen adult female Wistar rats, with sixty days old, weighting 150 g – 250 g were divided in G1: animals being maintained under the same conditions as the experimental groups following described, but without the use acrylic palatal plates (control group); G2: use of heat-polymerized acrylic resin palatal plates made of Lucitone 550; G3: use of palatal plates identical to G2, but subjected to a post-polymerization treatment in a water bath at 55°C for 60 min. The plates covered all the palate and were fixed in the molar region with light-cured resin, thus being kept there for 14 days. After the sacrifice, the palate was removed, fixed in formaldehyde 10% and decalcified with EDTA. Sections were stained using haematoxylin and eosin. Images in duplicate were made from the central region of the cuts, to measure the thickness (μm) of the keratin layers (TKC), epithelium total (TET) and connective tissue (TCC). Statistical analyses were carried out by one-way ANOVA and Tukey post-tests (α=0.05). Results: According to the results there was significant difference in the thickness of keratin between G2 and G3, with G1 having the intermediate value and similar to the other groups. There was a significant difference in the connective tissue with G3 treatment it was found to be effective, from the viewpoint of biocompatibility, for the acrylic resin denture base investigated.

Heat treatment of pre-hydrolyzed silane increases adhesion of phosphate monomer-based resin cement to glass ceramic

This study evaluated the influence of different forms of heat treatment on a pre-hydrolyzed silane to improve the adhesion of phosphate monomer-based (MDP) resin cement to glass ceramic. Resin and feldspathic ceramic blocks (n=48, n=6 for bond test, n=2 for microscopy) were randomly divided into 6 groups and subject to surface treatments: G1: Hydrofluoric acid (HF) 9.6% for 20 s + Silane + MDP resin cement (Panavia F); G2: HF 9.6% for 20 s + Silane + Heat Treatment (oven) + Panavia F; G3: Silane + Heat Treatment (oven) + Panavia F; G4: HF 9.6% for 20 s + Silane + Heat Treatment (hot air) + Panavia F; G5: Silane + Heat Treatment (hot air) + Panavia F; G6: Silane + Panavia F. Microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using stereomicroscope and scanning electron microscope (SEM) to categorize the failure types. Data were analyzed statistically using two-way test ANOVA and Tukey's test (=0.05). Heat treatment of the silane containing MDP, with prior etching with HF (G2: 13.15 ± 0.89a; G4: 12.58 ± 1.03a) presented significantly higher bond strength values than the control group (G1: 9.16 ± 0.64b). The groups without prior etching (G3: 10.47 ± 0.70b; G5: 9.47 ± 0.32b) showed statistically similar bond strength values between them and the control group (G1). The silane application without prior etching and heat treatment resulted in the lowest mean bond strength (G6: 8.05 ± 0.37c). SEM analysis showed predominantly adhesive failures and EDS analysis showed common elements of spectra (Si, Na, Al, K, O, C) characterizing the microstructure of the glass-ceramic studied. Heat treatment of the pre-hydrolyzed silane containing MDP in an oven at 100 °C for 2 min or with hot air application at 50 ± 5 ºC for 1 min, was effective in increasing the bond strength values between the ceramic and resin cement containing MDP.

Effect of pressure-assisted heat treatment on photoluminescence emission of α-Bi2O3 needles

Materials with high photoluminescence (PL) intensity can potentially be used in optical and electronic devices. Although the PL properties of bismuth(III) oxide with a monoclinic crystal structure (α-Bi2O3) have been explored in the past few years, methods of increasing PL emission intensity and information relating PL emission to structural defects are scarce. This research evaluated the effect of a pressure-assisted heat treatment (PAHT) on the PL properties of α-Bi2O3 with a needlelike morphology, which was synthesized via a microwave-assisted hydrothermal (MAH) method. PAHT caused an angular increase between the [BiO6]-[BiO6] clusters of α-Bi2O3, resulting in a significant increase in the PL emission intensity. The Raman and XPS spectra also showed that the α-Bi2O3 PL emissions in the low-energy region (below ∼2.1 eV) are attributed to oxygen vacancies that form defect donor states. The experimental results are in good agreement with first-principles total-energy calculations that were carried out within periodic density functional theory (DFT).

Effect of heat treatment on microstructure and mechanical properties of Ti-5wt-%Ni alloys for use as biomaterial

Titanium alloys are among the most important and frequently used class of biomaterials. In addition to biocompatibility, it is important that an implant material present satisfactory mechanical properties that allow long term use in the body. To improve such properties, different heat treatments are used, as well as doping with oxygen. The presence of interstitial oxygen in the crystal lattice causes deformation, increases the hardness, and causes modifications in anelasticity, thereby decreasing the elastic modulus. In this study, an alloy was prepared by arc melting precursor metals, heat and mechanically treated, and doped with oxygen, resulting in samples with different processing conditions. In each condition, the alloy was characterised in terms of amount of oxygen, X-ray diffraction, and optical microscopy. In addition, properties of the alloy, such as hardness and elastic modulus, were analysed.

The influence of heat treatment on the structure and microstructure of Ti-15Mo-xNb system alloys for biomedical applications

The Ti-15Mo-xNb system integrates a new class of titanium alloys without the presence of aluminum and vanadium, which exhibit cytotoxicity, and that have low elasticity modulus values (below 100 GPa). This occurs because these alloys have a beta structure, which is very attractive for use as biomaterials. In addition, Brazil has about 90% of the world’s resources of niobium, which is very important economically. It strategically invests in research on the development and processing of alloys containing this element. In this paper, a study of the influence of heat treatments on the structure and microstructure of the alloys of a Ti-15Mo-xNb system is presented. The results showed grain grown with heat treatment and elongated and irregular grains after lamination due to this processing. After quenching, there were no changes in the microstructure in relation to heat-treated and laminated conditions. These results corroborate the x-ray diffraction results, which showed the predominance of the β phase.

Ceramic Primer Heat-Treatment Effect on Resin Cement/Y-TZP Bond Strength

The purpose of this study was to evaluate the effect of different heat-treatment strategies for a ceramic primer on the shear bond strength of a 10-methacryloyloxydecyl-dihydrogen-phosphate (MDP)-based resin cement to a yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Specimens measuring 4.5 x 3.5 x 4.5 mm(3) were produced from Y-TZP presintered cubes and embedded in polymethyl methacrylate (PMMA). Following finishing, the specimens were cleaned using an ultrasound device and distilled water and randomly divided into 10 experimental groups (n=14) according to the heat treatment of the ceramic primer and aging condition. The strategies used for the experimental groups were: GC (control), without primer; G20, primer application at ambient temperature (20 degrees C); G45, primer application + heat treatment at 45 degrees C; G79, primer application + heat treatment at 79 degrees C; and G100, primer application + heat treatment at 100 degrees C. The specimens from the aging groups were submitted to thermal cycling (6000 cycles, 5 degrees C/55 degrees C, 30 seconds per bath) after 24 hours. A cylinder of MDP-based resin cement (2.4 mm in diameter) was constructed on the ceramic surface of the specimens of each experimental group and stored for 24 hours at 37 degrees C. The specimens were submitted to a shear bond strength test (n=14). Thermal gravimetric analysis was performed on the ceramic primer. The data obtained were statistically analyzed by two-way analysis of variance and the Tukey test (alpha=0.05). The experimental group G79 without aging (7.23 +/- 2.87 MPa) presented a significantly higher mean than the other experimental groups without aging (GC: 2.81 +/- 1.5 MPa; G20: 3.38 +/- 2.21 MPa; G100: 3.96 +/- 1.57 MPa), showing no difference from G45 only (G45: 6 +/- 3.63 MPa). All specimens of the aging groups debonded during thermocycling and were considered to present zero bond strength for the statistical analyses. In conclusion, heat treatment of the metal/zirconia primer improved bond strength under the initial condition but did not promote stable bonding under the aging condition.

Inactivation of Alicyclobacillus acidoterrestris in orange juice by saponin extracts combined with heat-treatment

Alicyclobacillus acidoterrestris is a spoilage-causing bacterium in fruit juices. The inactivation of this bacterium by commercial saponin and saponin purified extract from Sapindus saponaria fruits combined with heat-treatment is described. We investigated heat treatment (87, 90, 95, and 99 degrees C) with incubation time ranging from 0 to 50 min, in both concentrated and reconstituted juice. juices were inoculated with 1.0 x 10(4) CFU/mL of A. acidoterrestris spores for the evaluation of the best temperature for inactivation. For the temperatures of 87, 90, and 95 degrees C counts of cell viability decreased rapidly within the first 10 to 20 min of incubation in both concentrated and reconstituted juices; inactivation at 99 degrees C ensued within 1 and 2 min. Combination of commercial saponin (100 mg/L) with a very short incubation time (1 min) at 99 degrees C showed a reduction of 234 log cycle for concentrated juice A. acidoterrestris spores (1.0 x 10(4) CFU/mL) in the first 24 h of incubation after treatments. The most efficient treatment was reached with 300, 400 or 500 mg/L of purified extract of saponins from S. saponaria after 5 days of incubation in concentrated juice, and after 5 days with 300 and 400 mg/L or 72 h with 500 mg/L in reconstituted juice. Commercial saponin and purified extracts from S. saponaria had similar inactivation power on A. acidoterrestris spores, without significant differences (P>0.05). Therefore, purified extract of saponins can be an alternative for the control of A acidoterrestris in fruit juices. (C) 2012 Elsevier B.V. All rights reserved.

The influence of heat treatment on the phase relations in mineral growth systems

ABSTRACT Corundum is one of the most famous gems materials. Different heat treatment methods for enhancement purposes are commonly applied and accepted in the gem market. With this reason, the identification of the natural, unheated corundum is intensively investigated. In this study, aluminium hydroxide minerals and zircon are focused to observe the crystallization and phase change of these minerals during heat treatment procedures. Aluminium hydroxide minerals can be transformed to alumina with the corundum structure by heating. The reaction history of aluminium hydroxide minerals containing corundum was investigated comparing it with diaspore, boehmite, gibbsite and bayerite by TG and DTA methods. These hydroxide minerals were entirely transformed to corundum after heating at 600°C. Zircon inclusions in corundums from Ilakaka, Madagascar, were investigated for the influence of different heat-treatment temperatures on the recovery of their crystalline structure and on possible reactions within and with the host crystals. The host corundum was heated at 500, 800, 1000, 1200, 1400, 1600 and 1800°C. The crystallinity, the trapped pressure, and the decomposition of the zircon inclusions within the host corundum have been investigated by Raman spectroscopy. Radiation-damaged zircon inclusions may be used as an indicator for unheated Ilakaka corundum crystals. They are fully recrystallized after heating at 1000°C influencing the lowering of the 3 Raman band shift, the decreasing of FWHM of the 3 Raman band and the decreasing of the trapped pressure between the inclusion and the host corundum. Under microscopic observation, surface alterations of the inclusions can be firstly seen from transparent into frosted-like appearance at 1400°C. Then, between 1600°C and 1800 °C, the inclusion becomes partly or even completely molten. The decomposition of the zircon inclusion to m-ZrO2 and SiO2-glass phases begins at the rim of the inclusion after heating from 1200°C to 1600°C which can be detected by the surface change, the increase of the 3 Raman band position and the trapped pressure. At 1800°C, the zircon inclusions entirely melt transforming to solid phases during cooling like m-ZrO2 and SiO2-glass accompanied by an increase of pressure between the transformed inclusion and its host.

The Effect of Heat Treatment of Forages on Degradation Kinetics and Escape Protein Concentration

An in situ study was conducted to evaluate the effects of heat treatments on the degradation kinetics and escape protein concentrations of forages (alfalfa and berseem clover). Alfalfa collected at 4 and 7 weeks post-harvest and berseem clover collected at 5 and 7 weeks postharvest were freeze-dried and then heated to 100, 125, and 150o C for 2 hours. Heat treatment effects were determined by placing two bags of sample (for each treatment, maturity, and forage species for a given incubation times) into the rumen of one fistulated steer fed alfalfa hay. Bags were incubated for periods of 0 to 48 hours. Increasing levels of heat treatments of forages increased concentrations of neutral detergent fiber (NDF), acid detergent fiber (ADF), and acid detergent insoluble nitrogen (ADIN) and non-degradable protein (NDP), potentially degradable protein proportion (PDP), and protein escaping rumen degradation (PEP) while decreasing water soluble protein (WSP) and the rates of crude protein (CP), except immature berseem clover and cell wall (CW) degradation. PEP was greater and rate of CP degradation was lower at 100 and 150o C compared to 125o C in immature berseem clover.