Influence of surface energy parameters of dental self-adhesive resin cements on bond strength to dentin

The purpose of this study was to determine the surface energy parameters of dental self-adhesive resin cements (SRCs) and to measure their bond strength to dentin. Six dental SRCs (RelyX Unicem Clicker, RU; Maxcem Elite, ME; BisCem, BC; Clearfil SA Luting, SA; Multilink Speed, MS; seT PP, SP) and one resin-modified glass ionomer cement (RelyX Luting 2, RL; control) were tested. Smear layer-covered bovine dentin was used as bonding substrate. Using the dynamic sessile drop method, surface energy, surface energy components, degree of hydrophobicity/hydrophilicity (expressed as ΔG _sws using thermodynamic notation), and apparent surface energies for each material were calculated. The luting cements were bonded to the dentin and stored in water at 37?°C for 24?h prior to shear bond strength test (n?=?10). Pearson correlation analysis was applied to detect possible correlations between surface energy parameters and measured shear bond strength (α?=?0.05). RU, SA, and MS produced negative ΔG _sws values (hydrophobic), whereas ME, BC, SP, and RL yielded positive ones (hydrophilic). RU had the highest value among all six SRCs tested, the value for MS being statistically equivalent (p?=?0.785). The base component, ΔG _sws, and surface energy determined with water showed significant negative linear correlations with dentin bond strength (r/p?=??0.801/0.030, ?0.900/0.006, and ?0.892/0.007, respectively). These results suggest that bonding to smear layer-covered bovine dentin was governed by the base component and the hydrophobicity/hydrophilicity of the SRCs.     

Investigation of fast-setting acrylic adhesives for bonding attachments to human tooth surfaces

Some of the problems encountered in adhesive bonding of plastic attachments to human tooth surfaces were investigated. Acrylic adhesives based on poly(methyl methacrylate)–methyl methacrylate monomer mixtures with benzoyl peroxide initiation and N,N-dimethylaniline acceleration were utilized. Both homopolymers and copolymers were investigated. Recently extracted upper central incisors were employed in the bonding experiments. Bond strengths were improved by pretreating the tooth surfaces with mineral acids such as H₃PO₄. Surface wetting by the liquid adhesive was shown to be improved by the acid treatment. The molecular weight of polymer or copolymer employed in the liquid adhesive had an important effect on bond strengths. The optimum molecular weight for obtaining maximum bond strengths was around 20,000 g./mole. Water immersion of the bonded specimens at 37°C. for periods up to 6 weeks had a deleterious effect on bond strengths. Nevertheless, it was shown that some of the adhesives formed reasonably strong bonds for periods exceeding 6 months even with water immersion.     

Effect on adhesion of new polymerization initiator systems comprising 5‐monosubstituted barbituric acids,aromatic sulfinate amides,and tert‐butyl peroxymaleic acid in dental adhesive resin

To develop a multipurpose dental adhesive resin, the effects of polymerization initiator systems comprising 5‐monosubstituted barbituric acid (5‐MSBA), aromatic sulfinate amide (ASA), and tert‐butyl peroxymaleic acid (t‐BPMA) with 4‐acryloxyethyltrimellitic acid (4‐AET) or its anhydride (4‐AETA) on adhesion and curing time were investigated. Tensile bond strength values of a Ni Cr alloy are affected by the inclusion of t‐BPMA, and the optimum concentration of t‐BPMA in a 5‐MSBA–ASA–t‐BPMA‐type initiator system was found to be 0.5–2.0 wt %, and it was noteworthy that the correlation between the tensile bond strength and curing time on the t‐BPMA‐concentration showed a highly negative correlation of a benzenesulfinate morphoride (BSMo) series adhesive: r = −0.957, and a p‐toluenesulfinate morphoride (p‐TSMo) series adhesive: r = −0.949. The combination of 1‐cyclohexyl‐5‐ethylbarbiturioc acid (CEBA) with ASA provides a high level of tensile bond strength to the Ni Cr alloy, and the optimum concentration of CEBA in a CEBA–ASA–t‐BPMA‐type initiator and the bond strength values were found to be 0.75 wt % CEBA: 52.3 MPa (with BSMo), and 1.0 wt % CEBA: 50.9 MPa (with p‐TSMo), respectively. It was suggested that 5‐MSBA, ASA, and t‐BPMA and their combinations provided the environment where 4‐AETA exhibited good bonding performance with increasing wettability to metal without interference of a charge‐transfer complex derived from a polymerization initiator system such as benzoyl peroxide (BPO)–amine. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 1655–1668, 1999     

Which is effective on bond strength of resin-based sealers: incorporation of powdered dentin to primer or adhesive?

The aim of this study was to investigate the effect of adding powdered dentin to primer or adhesive in a self-etch system on the shear bond strength of three resin-based sealers. Seventy-two premolars were sectioned buccolingually, and 144 root halves were divided into three groups according to the sealer used: epoxy resin-based sealer (AH Plus), methacrylate resin-based (RealSeal, Hybrid Root SEAL) n = 48. The surfaces were irrigated with 5% NaOCl, 17% EDTA, distilled water for 5 min. Four subgroups were created (n = 12): control group; Clearfil Liner Bond 2 V treated group; powdered dentin added to the primer of Clearfil Liner Bond 2 V (40 wt.%); and powdered dentin added to the adhesive of Clearfil Liner Bond 2 V (20 wt.%). Dentin powder was prepared. Three mm high buildups with a constant surface area of 3.45 mm² were created using the sealers and allowed to set (37 ºC, 100% humid, 72 h). The samples were tested to failure for shear bond strength (1 mm/min). The data were calculated (MPa) and analyzed using two-way ANOVA, one-way ANOVA, and Tukey HSD tests. Adhesive use decreased the bonding performance of AH Plus (p = 0.00). Mean bond strength of the other sealers was found similar to control. Primer or adhesive resin with powdered dentin did not increase the adhesive performance of the self-etch system used. The shear bond strength of RealSeal was significantly increased when powdered dentin was added to primer or adhesive (p = 0.00). The effect of adding powdered-dentine to primer or adhesive in a self-etch system on the shear bond strength was sealer-dependent .     

The effect of polymer network structure upon the bond strength of epoxy–aluminum joints

The bond strength to aluminum of Epon 828 cured with various amounts of methylene dianiline has been investigated as a function of the resin network structure. In order to meet this objective, a torsional test for bond shear strength was developed, and fully cured resins with different network structures were prepared. The effects of the rate of loading of the joint and the aluminum surface pretreatment on the bond strength were also examined. Very high bond shear strengths, in excess of 9000 psi, were found for joints which after machining had been polished, vapor degreased, and treated with dilute sulfuric acid–potassium dichromate solution. It was found for these joints that the average bond strength decreased as the molecular weight between crosslinks increased. For the joints without acid–dichromate treatment, the failures were adhesive, and the network structure did not seem to significantly affect the bond strength. There are indications that chemical bonding occurred in the case of the acid–dichromatetreated joints; the decrease in bond strength as per cent excess amine and M_c increased is possibly associated with a decreased amount of chemical bonding. The bond strength increased to a limiting value as the rate of testing increased.     

Evaluation of different desensitizing agents effect on shear bond strength of adhesive resin cement to dentin

Desensitizing agents can inhibit the bonding strength between dentin and adhesive resin cement. This study evaluated the effects of different desensitizing agents on the shear bond strength of adhesive resin cement to dentin. Sixty freshly extracted and caries free teeth were classified into five experimental groups, randomly (n?=?12). Each group was treated with a different desensitizing agent (Teethmate, Shield Force Plus, Admira Protect and Ultra-Ez) respectively, except for an untreated control group. After desensitizing agents and adhesive resin cement were applied to each dentin surface, all specimens were stored in incubator at 37?°C for 24?h. The shear bond strength was tested with a Universal testing machine at a 0.5?mm/min crosshead speed. Data were analysed by using a statistical software (SPSS 22). The results of the measurements were analysed by Kruskal Wallis test with Bonferroni correction and multiple comparisons were made by Wilcoxon test (p???.01). Specimens were examined by a scanning electron microscope, additionally. The Shield Force Plus showed significantly the highest shear bond strength compared with other groups (p?<?.01). Ultra-Ez showed the lowest shear bond strength (p?>?.01). There was no significant difference among Teethmate and Admira Protect groups (p?>?.01). Desensitizing agents containing resin monomers increased the bonding strength, however desensitizers containing calcium phosphate, potassium nitrate and fluoride did not effect the bonding strength of resin cement to dentin.     

A novel chemical aging method for evaluating degradation of resin-dentin bond: a preliminary study

Purpose: to investigate the use of NaOH solution as storage medium on dentin micro-tensile bond strengths (MTBS) and the micromorphology of resin–dentin interfaces. Materials and Methods: mid-coronal dentin was exposed for 45 human third molars. One of five dentin adhesives investigated was applied to each dentin surface, followed by placement of a resin composite from the same manufacturer (Clearfil S3 Bond + Clearfil Majesty, Clearfil SE Bond + Clearfil Majesty, Kuraray Co. Ltd; Adper Easy One + Z250, Adper Single Bond 2 + Z250, 3M ESPE; Gluma Comfort Bond + Charisma, Heraeus Kulzer). Bonded specimens were sectioned through resin–dentin interfaces into multiple beams with a cross-sectional area of about 1 mm². The beams were kept in 10 wt% NaOH solution at 37 °C for 0, 2, 4, 6, 8, 10, or 12 h respectively prior to MTBS evaluation. The MTBS data were analyzed statistically. Failure modes were determined by stereomicroscopy. Representative fractured surfaces and resin–dentin interfaces were examined by scanning electron microscopy. Resin–dentin interfaces were also analyzed by transmission electron microscopy (TEM). Results: dentin MTBS decreased significantly with increased storage time in NaOH. Micro-gaps appeared along the resin–dentin interfaces after NaOH treatment and became wider over time. An electron-dense hybrid layer was observed by TEM in the control group, while an electron-lucent band was detected at the resin–dentin interfaces of specimens treated with NaOH for 8 h. Conclusion: aging of resin–dentin bonds in NaOH solution may be used as an expedited chemical aging method for evaluating degradation of dentin bond.     

Bond strength of glass carbomer material to enamel and dentin following different surface pretreatments

Objective: Enamel and dentin bond strengths of restorative glass carbomer material were determined by shear bond strength (SBS) test after different surface treatments in this study.

Materials and methods: Flat enamel and dentin surfaces pre-treated with 37% phosphoric acid (15 s for enamel and dentin), or 20% polyacrylic acid (15 s for enamel and dentin). Glass carbomer applied to the treated and non-treated surfaces. Conventional glass ionomer without any surface treatment served as a control.

Results: Enamel and dentin SBSs of the conventional glass ionomer cement were significantly higher than those of the glass carbomer material bonded to enamel and dentin without any surface treatments. Acid-etching and polyacrylic acid pre-treatments yielded similar enamel bond strength to that of glass ionomer cement. For dentin bonding, only polyacrylic acid pre-treatment improved SBS of glass carbomer to dentin surface.

Conclusions: Clinicians may consider the use of polyacrylic acid conditioner prior to the use of glass carbomer material.     

Effect of saliva contamination on shear bond strength and microleakage of one-bottle etch-and-rinse and self-etch adhesives: scanning electron and confocal laser microscopic analyses

Purpose: To evaluate the effect of saliva contamination on shear bond strength, microleakage, and microstructure of the adhesive interface in two different adhesive systems by using scanning electron microscopy (SEM) and confocal laser microscopy (CLSM). Materials and methods: Randomly, 228 third molars were allocated to six groups for an etch-and-rinse adhesive One-Step Plus (Bisco Inc.) and a self-etch adhesive G Bond (GC Corp.): Group 1 – manufacturer’s instructions were followed; Group 2 – involved contamination and drying before adhesive application; Group 3 – involved contamination, washing, and blot drying before adhesive application; Group 4 – involved contamination, etching, washing, and blot drying before adhesive application; Group 5 – involved contamination and drying after adhesive application, followed by adhesive reapplication; Group 6 – involved contamination and washing after adhesive application, followed by adhesive reapplication. Shear bond strength was tested after specimens were stored in distilled water at 37?°C for 24?h. Specimens were evaluated under a stereomicroscope for microleakage. Dentin–resin interfaces were evaluated by SEM and CLSM. Results: Group 2 for One-Step Plus and Group 3 for G Bond showed significantly lower bond strengths than control groups. Microleakage values were significantly greater at dentin than at enamel margins for all groups. In Group 2, for both adhesive systems, the highest microleakage was observed at dentin margins. Further, dentin–adhesive interfaces were not uniform and gaps were found by SEM and CLSM. Conclusions: The SEM and CLSM images demonstrated high variability of dentin–resin interfaces among saliva-contaminated groups. Rinsing the saliva and re-applying adhesive might be the best way to reduce the effect of saliva contamination on bond strength and microleakage.     

Efficacy of multi-mode adhesive systems on dentin wettability and microtensile bond strength of resin composite

Purpose: To evaluate the wetting ability and the microtensile bond strength of adhesive systems in various depths of dentin. Materials and Method: 48 extracted human molars cut in half in buccolingual direction. Buccal and lingual surfaces were used to obtain deep (n = 48) and superficial (n = 48) dentin. Groups were divided into 4 subgroups: Self-etch (CSE), etch&rinse (SB), multi-mode self-etch (SAU) and multimode etch&rinse (EAU) adhesive systems. 3 consecutive contact-angle measurements were obtained: T0- 3 μl drop of distilled water on dentin; T1-Droplet of the adhesive; T2- Distilled water after polymerization of the adhesive. After composite build-ups, microtensile measurements were performed. Contact angle data were analysed with analysis of variance for repeated measures. Bond strength data were analyzed by repeated measures analysis of variance, comparisons were made according to the logarithmic values (p < 0.05). Results: The difference between groups was not significant regardless of dentin depth for all measurements (p < 0.05). All groups except CSE enhanced the wetting ability of the adhesive but reduced the wetting ability of distilled water after application of the adhesive (p < 0.05). Regarding adhesive systems, the groups showed no significant difference between bond strengths to various depths of dentin except SAU (p > 0.05); in SAU, bond strength to deep dentine were significantly higher than superficial dentin (p < 0.05). Regarding adhesives’ bond strength, CSE showed significantly greater values than the other groups (p < 0.05). Conclusion: The cavity depth does not affect the bonding ability for all adhesive systems; self-etch adhesive systems might be a better choice since different adhesives may influence the wetting ability and microtensile bond strength of the dentin substrates.     

Effect of irradiation source on the dentin bond strength of a one-bottle universal adhesive containing an amide monomer

One-bottle universal adhesives have been widely used because of their simplicity of bonding procedures for various dental materials. The present study evaluated the effect of the polymerization light source on the micro-tensile bond strengths of a universal adhesive (Clearfil Universal Bond Quick) to dentin in comparison with a one-bottle self-etch adhesive (Clearfil S³ Bond Plus) and two 2-step self-etch adhesives (Clearfil SE Bond and Clearfil SE Bond 2). The adhesives were applied to extracted human dentin according to the manufacturer’s instructions and irradiated using either a quartz-tungsten-halogen (QTH) or blue light-emitting diode (LED). Subsequently, a resin composite was incrementally built on each adhesive and light-cured using the QTH. The bonded specimens were sectioned and subjected to micro-tensile bond strength tests. Both the type of adhesive and the light source were found to statistically affect the bond strength, with no interactions. The LED gave greater bond strength than the QTH. The bond strengths of the two-step adhesives were significantly higher than those of the one-bottle products, irrespective of the light source. The Clearfil Universal Bond Quick exhibited significantly higher bond strength than the Clearfil S³ Bond Plus. LED curing improved the performance of Clearfil Universal Bond Quick, and this product generated bond strength superior to that of the existing one-bottle adhesive Clearfil S³ Bond Plus.     

An evaluation of plasma-sprayed coatings based on Al2O3 and Al2O3–13 wt.% TiO2 with bond coat on pure titanium substrate

In this study, the effects of bond coat on the properties of Al₂O₃ and Al₂O₃–13 wt.% TiO₂ coatings, which is plasma sprayed onto a commercial pure titanium substrate with and without Ni–5 wt.% Al (METCO 450 NS) as bond coating layer were investigated in terms of microhardness, bonding strength and surface roughness. Optical and scanning electron microscopy (SEM) examinations revealed that there is a uniform coating layer with no spalling and delamination. However, there is a little amount of porosity. The results indicated that the application of bond coat layer in the plasma spraying of Al₂O₃ and Al₂O₃–13 wt.% TiO₂ on pure titanium substrate has increased the hardness and bonding strength of coatings. While the adhesive bonding is dominant without bond coat, the cohesive bonding is dominant with the application of the bond coating layer. It has been observed that percentage of cohesion strength was about three times higher than that of adhesion strength.     

The influence of retention hole and adhesive systems on the shear bond strengths of resin composite to amalgam

The aim of the study is to evaluate the influence of surface-treatment methods with and without the use of a retention hole on the shear bond strength of a resin composite adhered to amalgam using an adhesive system. Amalgam specimens were divided into six groups. Group 1 (Bur) specimens were roughened with a diamond bur, Group 2 (Al₂O₃) specimens were sandblasted with a 50?μm aluminum oxide powder, Group 3 (CoJet^®) specimens were sandblasted with 30?μm CoJet^® Sand, Group 4 (Bur?+?Rh) specimen surfaces were prepared with a retention hole 1?mm in diameter and 1?mm deep and roughened with a diamond bur, Group 5 (Al₂O₃?+?Rh) specimens were also prepared with a retention hole and sandblasted with 50?μm aluminum oxide powder, and Group 6 (CoJet^®?+?Rh) surfaces were prepared with a retention hole and sandblasted with 30?μm CoJet^® Sand. Resin composite cylinders were bonded onto the amalgam surfaces using Xeno^® IV, Optibond? All-In-One, Clearfil? SE Bond, Adper? Single Bond Plus, and Scotchbond? Multi-Purpose adhesive systems. In addition, silane (Monobond S) was used for Groups 5 and 6. The shear bond was determined and statistically analyzed using two-way analysis of variance and post hoc Tukey’s tests (p?≤?0.05). The surface treatment significantly affected the shear bond strengths of the adhesive systems. The shear bond strengths of Optibond? All-In-One (2.661?±?0.48?MPa) in Group 1 and Scotchbond Multi-Purpose (3.818?±?0.98) in Group 4 were significantly higher than those of the other adhesive systems. Silica coating of the amalgam surface significantly improved the shear bond strength of the resin composites. The addition of a retention hole on the amalgam affects the bonding strength of the composite adhesion.     

Effects of different surface treatments on shear bond strength between ceramic systems and metal brackets

The aim of this study was to evaluate the shear bond strength of orthodontic brackets bonded to different kinds of ceramic surfaces after different surface conditioning methods. A total of 120 ceramic disks were divided into two main groups in terms of feldspathic or lithium disilicate. Each ceramic group was further subdivided into six subgroups depending on surface treatment (n = 10). The ceramic surfaces were conditioned by one of the following methods: Group C: control group; Group P: %37.5 orthophosphoric acid; Group HF: %9.6 hydrofluoric acid; Group L: Nd-YAG laser irradiation; Group SB: sandblasting with 50 µm Al₂O₃ particles; and Group DB: grinding with a diamond bur. Surface roughness value was evaluated with a digital profilometer. Surface topographies of one specimen from each group were observed by atomic force microscopy (AFM) after surface treatments. All samples were primed with silane before the bracket bonding, including the control group. Metal brackets were bonded to the specimens with a light curing composite resin. The samples were stored in distilled water for 24?h and thermocycled 2500× at 5 and 55 ºC for 30?s. Shear bond strengths between the ceramic surface and the bracket were measured with a universal testing machine at a crosshead speed of 0.5 mm/min. Failure modes were classified as adhesive, cohesive, or mixed. Data were analyzed using ANOVA and Tukey's tests (α = .05). Group SB had significantly rougher surface compared with the other groups in each ceramic system (p < .05), and Group SB demonstrated significantly higher shear bond strengths than other groups as well. Within the limitations of this study, surface conditioning methods, except for sandblasting and grinding, were associated with lower shear bond strengths; however, thermocycling may have had negative effects on bond strengths of specimens. Furthermore, in each ceramic system, there was a significant difference between surface-conditioning methods and surface roughness with regard to shear bond strength.     

Structure and properties of polybutadiene/montmorillonite nanocomposites prepared by in situ polymerization

Polybutadiene (PB)/Montmorillonite nanocomposites (NCs) were prepared by in situ polymerization through the anionic polymerization technique. The effects of treating method of organophilic MMT (OMMT), the type of OMMT, and the solvent used in polymerization were studied. The structure and properties of NCs were characterized using X‐ray Diffraction (XRD), transmission electron micrograph (TEM), H‐NMR spectrum, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and dynamic mechanical analysis (DMA). The consumption of BuLi was varied with different treating methods. The molecular weight distribution of PB added with OMMT (DK1) was wide, and the molecular weight distribution became narrow when OMMT‐DK1B and DK4 were added. OMMT did not disperse stably in cyclohexane, but could form a homogeneous solution in toluene and xylene. XRD and TEM showed that exfoliated NCs were obtained by in situ polymerization through the anionic polymerization technique. From the H‐NMR spectrum of PB and PB/OMMT NCs, it could be seen that the content of 1, 2 units of PB increased ～100%, while 1, 4 units decreased when 6.2 wt % of OMMT was added. The results of DSC and DMA indicated that T_g and T_dc were increased when compared with those of PB. Both storage modulus and loss modulus were increased with the addition of OMMT, and tan δ was decreased. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3615–3621, 2006     

Preparation,structural evolution,and performance of heat-resistant organosilicon polymer adhesives for joining SiC ceramics

There is an urgent need for heat-resistant adhesives with high bonding strength in order to able to fabricate large and complex SiC components for aeronautical and astronautical applications. In this study, heat-resistant organic adhesives prepared using an organosilicon polymer and inorganic additives (B₄C and SiO₂) were used successfully to bond SiC ceramics. The prepared adhesives were characterised through shear strength tests as well as using thermogravimetry-differential scanning calorimetry, Fourier-transform infrared spectroscopy, X-diffraction analysis, and scanning electron microscopy. The adhesives exhibited high room-temperature shear strengths (greater than 15 MPa) after being subjected to heat treatments at 200–1200°C. Further, the high-temperature shear strengths of the adhesives at 200, 400, 600, 800, and 1000°C were 10.5, 10.1, 7.7, 8.6, and 8.4 MPa, respectively. The high performance of the adhesives indicated that they should be suitable for joining SiC-based materials for use in high-temperature applications.     

Shear bond strength of bis-acryl resin provisional material repaired using a flowable composite

This study investigated the shear bond strength of a bis-acryl composite repaired with a flowable composite after different surface treatments. Sixty standardized cylindrical silicone molds were filled with bis-acryl resin provisional material and then divided into six groups (n = 10 per group) to undergo different surface treatments. After a surface treatment had been performed, the flowable composite was injected directly into the cylinder of each specimen, and the specimens were then cured over a 10-mm-thick glass slide for 20 s. The shear bond strength was determined using a universal testing machine at a crosshead speed of 1.0 mm/min by placing a knife-edged blade immediately adjacent and parallel to the adhesive interface between the repair material (flowable composite) and the bis-acryl resin provisional material. The mean shear bond strengths ranged from 8.98 to 17.14 MPa. The highest mean shear bond strength corresponded to the bonding group (17.14 MPa), whereas the air-particle abrasion group exhibited the lowest mean shear bond strength (8.98 MPa). Surface treatment of bis-acryl resins with bonding appears to be a promising approach for improving repair bond strength, and the bonding group exhibited the highest levels of bond strength.     

Preparation and properties of methyl methacrylate and fluoroacrylate copolymers for plastic optical fiber cladding

Copolymers of methyl methacrylate (MMA) and fluoroacrylate (FA), with different FA content (0–100 wt %), were prepared by bulk polymerization. The chemical structure was identified by ¹H‐NMR and other physical properties were measured by DSC, Abbé refractometer, X‐ray diffractometry, polarized optical microscopy, and DMA. The copolymers were confirmed as random copolymers by Fineman–Ross analysis and first‐order Markov statistics. Increasing the FA content from 0 to 100 wt % decreased the refractive index from 1.492 to 1.368. Copolymers with FA content higher than 70 wt % crystallized and led to low transparency and poor thermal properties. On the other hand, copolymers with FA content lower than 70 wt % was thermally stable (T_g was as high as 60°C) and transparent. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 2082–2089, 2004     

Studies on the kinetics of free-radical bulk polymerization of multifunctional acrylates by dynamic differential scanning calorimetry

The course and kinetics of nonisothermal bulk polymerization of multifunctional acrylates were studied by dynamic differential scanning calorimetry (DSC). Measurements were carried out for four straight-chain monomers, diethylene glycol diacrylate (DEGDA), triethylene glycol diacrylate (TEGDA), tetraethylene glycol diacrylate (TTGDA), and poly(ethylene glycol)diacrylate (PEGDA) (mol. wt. 600), to study the effect of the backbone chain length, atmosphere, and type of initiator on the crosslinking kinetics. 4,4′-Azobis(4-cyanovaleric acid) (1.0%, w/w) was used as a free-radical initiator. From the dynamic scanning of polymerization of DEGDA at five heating rates (2–30°C/min), the average heat of polymerization (ΔH_p) was found to be 524.2 J/g. An activation energy of 108.8 kJ/mol and preexponential factor 5.34 × 10¹² s^?1 were obtained from the Arrhenius plot, In dα/dt. The rate of polymerization was found manyfold greater at 20–60% conversion than at the initial stage (2–8% conversion). Polymerization was studied under both nitrogen and air atmosphere. The results corresponded well with the theory of oxygen inhibition. Different types of initiators, e.g., 4,4′-azobis(4-cyanovaleric acid) (ABCVA), 2,2′-azobisisobutyronitrile (AIBN), and benzoyl peroxide (BPO) were used for polymerization and ABCVA was found to be the most efficient among all. © 1995 John Wiley & Sons, Inc.     

The totally miscible in ternary hydrogen‐bonded polymer blend of poly(vinyl phenol)/phenoxy/phenolic

The individual binary polymer blends of phenolic/phenoxy, phenolic/poly(vinyl phenol) (PVPh), and phenoxy/PVPh have specific interaction through intermolecular hydrogen bonding of hydroxyl–hydroxyl group to form homogeneous miscible phase. In addition, the miscibility and hydrogen bonding behaviors of ternary hydrogen bond blends of phenolic/phenoxy/PVPh were investigated by using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy, and optical microscopy. According to the DSC analysis, every composition of the ternary blend shows single glass transition temperature (T_g), indicating that this ternary hydrogen‐bonded blend is totally miscible. The interassociation equilibrium constant between each binary blend was calculated from the appropriate model compounds. The interassociation equilibrium constant (K_A) of each individually binary blend is higher than any self‐association equilibrium constant (K_B), resulting in the hydroxyl group tending to form interassociation hydrogen bond. Photographs of optical microscopy show this ternary blend possess lower critical solution temperature (LCST) phase diagram. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009