Polarization effect in an epoxy resin at elevated temperatures

The elucidation of a polarization process at elevated temperatures in an epoxy-novolac resin cured by BF₃ complex is made. Measurements of permittivity and dissipation factor with various types of electrodes as well as measurements of potential distribution inside the specimen are described.     

Viscoplastic deformation of an epoxy resin at elevated temperatures

The tensile behavior under monotonic loading and stress‐relaxation testing of an epoxy resin has been studied. Experimental data at various strain rates and three temperatures from ambient up to just below T_g were performed, to study the transition from the brittle behavior to a ductile and therefore viscoplastic one. Dynamic mechanical analysis was applied to study the glass transition region of the material. Furthermore, a three‐dimensional viscoplastic model was used to simulate the experimental results. This model incorporates all features of yield, strain softening, strain hardening, and rate/temperature dependence. The multiplicative decomposition of the deformation tensor into an elastic and viscoplastic part has also been applied, following the element arrangement in the mechanical model. A stress‐dependent viscosity was controlling the stress–strain material behavior, involving model parameters, calculated from the Eyring plots. A new equation for the evolution of the activation volume with deformation was proposed, based on a probability density function. The model capability was further verified by applying the same set of parameters to predict with a good accuracy the stress‐relaxation data as well. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2027–2033, 2006     

Permeability measurement on high strength concrete without and with polypropylene fibers at elevated temperatures using a new test setup

A new test setup for permeability measurement at room and high temperature is presented. The experimental results obtained by employing the new setup are reported and validated. The experiments are performed on high performance concrete, without and with addition of polypropylene fibers under temperatures ranging from 20 °C to 300 °C as well as after cooling of previously heated specimens to the room temperature. The results show that plain concrete exhibits steady increase in permeability with increasing temperature, whereas concrete with fibers exhibit a sudden increase of permeability at temperatures between 80 °C and 130 °C. The results confirm the governing role of permeability on explosive spalling and suggest the existence of mechanisms of pressure relief other than just melting of fibers. The microstructure of concrete with fibers is investigated using SEM before and after exposure to high temperature. It is observed that the melted polypropylene flows only into the micro-cracks and does not penetrate into cement paste.     

Deformation and strength characteristics of magnesia-spinnellide refractories at elevated temperatures

Conclusions We studied the thermomechanical properties of the heat resistant chromite-periclase refractories and three types of periclase-chromite refractories. It was established that the superior deformation and high-temperature strength characteristics of the chromite-periclase products ensure a more complete stress relaxation in the products during their service and reduce the wear of the linings of the melting furnaces.Translated from Ogneupory, No. 8, pp. 17–18, August, 1991.     

Effect of the interfacial area measurement parameters on the push-out strength between fiber post and dentin

PurposeTo verify the influence of different instruments and operators on the bonding interfacial area and on the push-out bond strength values.Material and methodsFifteen anterior human teeth (n=15) were selected, cleaned and standardized to 15 mm length. Root canals were prepared in 12 mm and the fiber posts were cemented using the RelyX U-100 cement. Three slices were obtained per tooth (N=45) and submitted to the push-out bond strength test. The bonding interfacial area (mm²) of each specimen was calculated based on the disc slice dimensions: coronal and apical diameter and height. The bonding area of each specimen was used to calculate the bond strength (Mpa). The dimensions were analyzed by different operators, using two instruments: G1 – Operator A with a digital caliper; G2 – Operator A with a stereomicroscope; G3 – Operator B with a digital caliper; G4 – Operator B with a digital stereomicroscope; G5 – Operator C with a digital caliper; G6 – Operator C with a stereomicroscope. The mean area was submitted to inter-operator and intra-operator analyses, while the mean area and mean of bond strength were submitted to the 2-way ANOVA with repeated measures and the Tukey test (α=0.05).ResultsThe inter-operator kappa was 0.83 to the digital caliper and 0.91 to the stereomicroscope, while the intra-operator kappa was 0.76. The operator and the measurement instrument influenced the interfacial bonding area (p=0.000 and p=0.001) and the push-out bond strength values (p=0.000 and p=0.000, respectively) of the disc slices.ConclusionThe final push-out bond strength values are influenced by the measuring instrument and by the measurer operator.     

玻璃鳞片含量对环氧胶强度和吸水性的影响

通过测试环氧胶粘剂剪切强度、经冷热循环水浴浸泡的试块的吸水性和密度变化,研究了玻璃鳞片含量对环氧胶粘涂层界面粘接强度、吸水性能的影响。研究结果表明,玻璃鳞片增加时,胶层的密度增加;经长时间浸泡后试样的密度均明显提高,含量为30%的试样增幅最大,但其体积几乎保持不变。分析试验结果后可知,胶层经浸泡后的体积变化率也应是评定其耐水性能的重要因素。     

The relationship between zeta-potential and pull-out shear strength on modified UHMWPE fiber reinforced epoxy composites

UHMWPE fiber exhibits high performance, featuring high tensile strength and modulus, because of its extended chain structure. However, this fiber demonstrates some defects, such as low melting point, creep, and poor interfacial bonding with resin. Therefore, it is still not widely applied in composites. This research attempted to improve the performance by applying interfacial treatment to the fiber, using polypyrrole (PPy) synthesized through oxidation. The interfacial shear strength was evaluated using the results of a pull-out test and a Zeta Potential. The UHMWPE fiber was exposed to PPy treatment at various temperatures. The PPy-modified fiber was then impregnated with epoxy to generate the composites. The effects of the modification were also examined. The performance of the composites was determined by the Zeta Potentials of the fiber and resin, using an EKA electrokinetic analyzer. The interfacial shear strength was determined by the pull-out test. The morphology of fiber was observed by SEM. Results show that the shear strength of the interface between the PPy-treated UHMWPE fiber and epoxy increased 215%. The correlation between the Zeta Potential and the interfacial shear strength was also observed.     

Influence of Skydrol immersion at elevated temperatures on the thermo-mechanical properties of a high-Tg anhydride epoxy resin toughened with a hydroxy-terminated polyester

Currently, the application of composites in aerospace parts exposed to higher temperatures and in aggressive media is still severely limited. To replace metal alloys, alternative resins systems with suitable long-term heat resistance are needed. In this study, the effect of the aviation hydraulic fluid Skydrol on the thermal and mechanical properties of a high-T_g, anhydride-cured epoxy resin in the unmodified and toughened state at elevated temperature is investigated. An aliphatic polyester diol was selected as an intrinsic toughener and its impact on the thermal, mechanical, and aging properties was determined. Experimental characterization of the aging effects is carried out with dynamic-mechanical characterization, infrared spectroscopy, and electron dispersion x-ray spectroscopy. In addition, the fracture toughness and the fatigue crack propagation behavior are determined. Initially, the toughened system shows an improved fracture toughness. Since oxidation is blocked by the Skydrol fluid only thermal degradation takes place as determined by the decrease in glass transition temperature T_g and network density. The thermal degradation leads to a tougher behavior, which is observed in both systems in static and dynamic mode with toughness decreasing with aging time again.     

纳米颗粒对环氧树脂胶粘剂／钢铁附着强度的影响

采用纳米Al2O3、纳米CaCO3、纳米SiO2三种纳米颗粒,机械混合对环氧树脂胶粘剂进行改性,并对纳米颗粒改性的环氧树脂胶粘试样进行了附着强度的检测。结果发现,通过改变纳米颗粒的种类和含量,环氧胶粘剂／钢铁基体之间的附着强度得到不同程度的提高,其中添加2％纳米Al2O3颗粒的环氧胶粘剂与钢铁基体的附着强度提高了4倍左右。通过断面形貌特征和不同基体粗糙度下对添加纳米颗粒环氧胶与钢铁基体之间附着强度的检测,对此现象产生的原因进行了分析和讨论。     

The reaction between phlogopite and calcium chloride at elevated temperatures

The reaction of phlogopite mica and CaCl₂·2H₂O has been studied within the temperature range 600–1000°C. The reaction products have been studied by chemical analysis, electron microscopy combined with a micro-analyser, X-ray diffraction (XRD), thermoanalytical methods and IR spectrometry. The reaction products were milled and the elemental distribution in different particle size fractions was investigated. Potassium can be converted into a water-soluble form almost completely above the melting point of CaCl₂ in this reaction. Iron, Mg and Al do not change into a soluble form. On grinding, Fe and K concentrate in smaller particles while Al prefers larger ones. The formation of several new phases in the reaction can be confirmed by XRD. The mica dehydroxylates above 700°C, which can be detected in the IR spectra, and this may affect the reaction.     

The relationship between microstructure and flexural strength of pressureless liquid phase sintered SiC ceramics oxidized at elevated temperatures

The oxidation behavior of pressureless liquid phase sintered SiC ceramics with Al₂O₃ and Y₂O₃ as sintering additives was investigated in the temperature range from 1000 °C to 1600 °C at the interval of 100 °C for 5 h. The relationship between residual flexural strength and microstructure was analyzed in detail. It was found that the SiC specimens suffered from mild oxidation below 1300 °C. The flexural strength of SiC specimens after oxidation at 1100 °C was the highest (90% of the original strength) due to the formation of dendritic grains, which filled pores and healed cracks. And the flexural strength was almost above 80% of the original flexural strength when the oxidation temperature was below 1300 °C. Meanwhile, the weight of specimens underwent steady increase. However, when the oxidation temperature was elevated to above 1400 °C, the specimens began to suffer from severe oxidation, which resulted in a lot of through pores and cracks on the surface, bringing about the sharp decrease of flexural strength to 30% of original strength when the oxidation temperature of 1600 °C was reached. And the weight of the specimens after huge increase began to show downtrend when the oxidation temperature was elevated to 1600 °C due to the spalling of oxidation products.     

Electrostatic deposition of silica nanoparticles between E‐glass fibers and an epoxy resin

The achievement of optimum adhesion between a thermoset and an inorganic material is an important goal for the composites and coatings industries. There is a growing interest in the use of structural surface modifiers, such as nanotubes, nanoparticles, and whiskers, to improve this adhesion. Here, a method for electrostatically depositing poly(ethylene imine)‐functionalized silica nanoparticles onto E‐glass fibers was developed. The deposition of 26‐nm functionalized particles onto glycidyloxypropyltrimethoxysilane (GPS)‐functionalized E‐glass fibers and then their embedding in a resin of diglycidyl ether of bisphenol A and m‐phenylene diamine increased the interfacial shear strength (IFSS) 35% over that of bare fibers and 8% over that of GPS‐functionalized fibers. IFSS was highly dependent on the particle size; the 16‐nm functionalized particles had little effect on the IFSS. When the particles size was increased to 71 and 100 nm, this led to increasingly poor IFSS values, whereas the 26‐nm particles produced the best results. Similar results were seen with the transverse flexural strength of the unidirectional composites. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41516.     

Mechanical and thermal properties of h-BN based composite containing dual glass phases at elevated temperatures

High-temperature mechanical and thermal properties of h-BN based composite containing amorphous silica and Yb-riched silicate glass phases were systematically investigated in this work. Owing to anisotropic microstructure of h-BN matrix, the obtained composite demonstrates anisotropic mechanical and thermal properties. The composite possesses higher elastic modulus at 1673?K than that at room temperature and presents excellent high-temperature stiffness. Flexural strengths in parallel and perpendicular directions reach 496?±?22 and 258?±?21?MPa at?1073?K, respectively, and increases by 74 and 66% compared with the room-temperature strengths of 285?±?4?and 155?±?5?MPa. The composite containing dual glass phases shows lower coefficients of thermal expansion in the temperature range of 473–900?K, the values are ?1.4?×?10^?6 and 0.3?×?10^?6 ?K^?1 for the perpendicular and parallel directions, respectively. Thermal conductivities in the perpendicular and parallel directions at 373?K are 24.8 and 14.8?W?m^?1?K^?1, respectively, and then decrease to 14.9 and 9.3?W?m^?1?K^?1 at 1473?K.     

Effect of glass fiber‐reinforced polymer and epoxy injection on compressive strength of elevated temperature damaged concrete

Glass fiber‐reinforced polymer (GFRP) materials have received a great deal of interest among civil engineers during the past decade. This paper presents an overview of experimental studies carried out on GFRP‐wrapped and epoxy‐injected concrete samples exposed to elevated temperatures. For this purpose, 0.30, 0.35 and 0.40 water to binder (w/b) ratios were used. For each w/b ratio, normal aggregates were replaced by lightweight aggregates with a size fraction of 0–2 mm at three different volume fractions such as 10%, 20% and 30% of total aggregate volume. At the same time, a group of air‐entrained samples was also cast for each w/b ratios. Prepared samples were exposed to 600 °C for 3 h. The damaged samples were separately repaired by GFRP and epoxy injection. Before and after elevated temperature exposure, water absorption and compressive strength were tested. After repairing with GFRP and epoxy injection, only the compressive strength test was carried out. GFRP improved the compressive strength between 1–22% and 348–1403% for samples before and after being exposed to elevated temperatures, respectively. Epoxy injection increased the compressive strength of the samples, exposed to elevated temperature, between 1% and 123%. However, the epoxy injection process failed to recover the compressive strength of the samples before elevated temperature exposure. Copyright © 2012 John Wiley & Sons, Ltd.     

Modification of epoxy resin by polysulfone to improve the interfacial and mechanical properties in glass fibre composites. II. Adhesion of the epoxy-polysulfone matrices to glass fibres

Adhesion of epoxy-polysulfone (PSF) matrices to glass fibres of 12–30 μm in diameter was studied under both quasi-static and cyclic loadings. A pull-out technique was used for adhesion measurement. It was shown that incorporation of PSF into epoxy resin changed its adhesion to fibres. A maximum was observed in the adhesion strength vs. PSF content dependence at 10 wt% thermoplastic concentration. The results obtained were compared with the data on the epoxy-PSF matrices adhesion to thick steel wire (d = 150 μm) and Nylon-6 fibres (d = 250 μm). Similar values of the adhesion strength increase (22–25%) confirmed that all the changes at the interface were connected primarily with the matrix. A new preferably non-destructive cyclic loading technique was used to test the systems under cyclic loading at varying force amplitudes, frequencies and displacement amplitudes. In this technique the interphase behaviour is characterised by two variables: by the phase angle between the deformation applied to the matrix and the force transferred by the matrix to the fibre, and also by the amplitude of this force. Minimal force amplitudes were observed for the joints with 10 wt% polysulfone. Moreover, phase-angle values for epoxy-10% polysulfone joints were minimal among all the systems investigated. Increase in the number of loading cycles caused much more damage to unmodified epoxy matrix than that to epoxy-polysulfone matrices. Thus, modification of epoxy resin by polysulfone enhanced its adhesion to fibres under both quasistatic and cyclic loadings, especially for epoxy-10% polysulfone matrix. The possible mechanism of the phenomenon observed is discussed.     

Effect of the frequency of mechanical pulses for fatigue aging testing on push-out bond strength between glass fiber posts and root dentin

The aim of this study was to evaluate the influence of the frequency of mechanical pulses during mechanical fatigue aging on bond strength between glass fiber posts and root dentin. Fiber posts were adhesively cemented in 30 bovine roots and the core was built up with composite. All specimens were subjected to mechanical cycling (45° angle; 37 °C; 50 N; 2×10⁶ pulses) at different frequencies: 2, 4, and 8 Hz. After the fatigue, each specimen was submitted to push out test. The bond strength was calculated for data analysis (one-way ANOVA, p = 0.05). The frequency did not affect the push-out (p = 0.7). The main failure mode was between dentin and cement in all groups. The mechanical pulses were not influenced by the bond strength between root dentin and fiber posts. Thus, it is possible to decrease the time-consuming in vitro tests involving posts without damaging the reliability of the test.     

Fatigue strength of diamond coating-substrate interface assessed by inclined impact tests at ambient and elevated temperatures

The effect of two different treatments of cemented carbide substrates, prior to the deposition of a nanocrystalline diamond (NCD) coating, on the film interface fatigue strength was investigated at ambient and elevated temperatures. The first substrate treatment of the cemented carbide substrate was a selective chemical Co-etching and the second one the deposition of a Cr-adhesive layer. Inclined impact tests at 25 °C and 300 °C were performed on the NCD coated specimens. The related imprints were evaluated by confocal microscopy measurements and EDX micro-analyses. The thermal residual stresses developed in the film structure at various temperatures were estimated by Finite Element Method (FEM) calculations. A fatigue damage in the NCD coating interface region was induced by the repetitive impacts. After this damage, the compressive residual stresses in the NCD film are released leading to its lifting from the substrate (bulge formation) and subsequent coating failure. The NCD film-substrate interface fatigue behavior is significantly affected by the test temperature. Based on the attained results at diverse substrate treatments, Woehler-like diagrams were developed for monitoring the fatigue failure of NCD coating interface area at 25 °C and 300 °C. The interfacial fatigue strength worsens as the impact test temperature grows in both examined substrate treatment cases. Moreover, Co-etched substrates compared to coated ones by an adhesive Cr-interlayer possess higher interfacial strength at ambient and elevated temperatures. These phenomena were investigated and related explanations are described in the paper.     

Interaction between Ca,Zn, and porous cordierite substrate at elevated temperatures

The interactions of both Ca and Zn with cordierite substrates were studied to better understand how Ca and Zn individually contribute to physio chemical changes in the cordierite diesel particulate filters (DPF) during high temperature engine exhaust conditions. The Ca and Zn doped cordierite samples were heated to temperatures of 300, 500, 900, and 1100?°C. Thermal treatment consisted of 1, 3, and 10 h exposure, separately, to simulate the duration of heat experienced by DPFs during use. Among the temperature profiles studied, SEM, XRD and EPMA mapping results indicate that the zinc–cordierite interaction is more severe in contributions to cordierite degradation than the calcium–cordierite interaction. The corrosion pathway generally followed the cordierite honeycomb porous structures. Appraised by the EPMA mapping, the element concentration across a given cordierite cross-section tends to increase for Zn doped samples, where calcium did not. XRD analysis indicate both the Ca and Zn can chemically interact with cordierite and alter the crystalline phases present at temperatures above 300?°C.     

Comparative study by DSC and FTIR techniques of an unsaturated polyester resin cured at different temperatures

The polymerization of a commercial polyester resin was investigated by differential scanning calorimetry (DSC). The conversion profiles were obtained in the temperature range 60–80°C. The autocatalytic model satisfactorily describes the experimental data. Fourier transform infrared spectroscopy (FTIR) measurements were also made in order to obtain both the styrene and polyester unsaturations conversions, which were compared to the overall conversion obtained by DSC. Overall conversion measured by DSC lies between styrene and polyester C=C bond conversion obtained by FTIR. © 1998 SCI.