Characterization of a rigid silicone resin

Silicone resins have been used as binders for ceramic frit coatings and can withstand temperatures of 650°C to 1260°C. Conceptually, silicone resins can potentially be used as matrices for high temperature fiber‐reinforced composites. The mechanical and thermal properties of a commercially available silicone resin, Dow Corning® 6‐2230, were characterized. Neat 6‐2230 resin was found to have inferior room temperature mechanical properties such as flexural, tensile and fracture properties when compared to epoxy. The room temperature flexural properties and short beam shear strength of the silicone/glass composites were also found to be lower than those of epoxy/glass composite with similar glass content. However, the silicone resin had better elevated temperature properties. At an elevated temperature of 316°C, the retentions of flexural modulus and strength were 80% and 40% respectively of room temperature values; these were superior to those of phenolic/glass. Unlike the carbon‐based resins, the drop in flexural properties of the silicon/glass laminates with temperature leveled off with increase in temperature beyond 250°C. The resin weight loss at 316°C in 100 cm³/min of flowing air was small compared to other carbon‐based resins such as PMR‐15 and LaRC TPI. Only Avimid‐N appeared comparable to Dow Corning® 6‐2230.     

Epoxy-based composite adhesives with improved lap shear strengths at high temperatures for steel-steel bonded joints

High-performance room temperature-cure epoxy structural adhesives utilizing simplified formulation are developed. The developed structural adhesive consists of diglycidyl ether of bisphenol A (DGEBA) and novolac epoxy blend as a base resin, micrometer-sized silica particles as a reinforcing filler, and triethylenetetramine as a curing agent. The developed ambient temperature-cure epoxy structural adhesive with optimized formulation exhibits outstanding properties including high glass transition temperature of 95°C, high thermal stability with degradation temperature at 5% weight loss of 364°C, exceptionally high rubbery plateau modulus of 320 MPa, good flame-retardant characteristics with limiting oxygen index of 40, and high single lap shear strength for single lap steel-steel bonded joint of 548 MPa at the temperature of 80°C. The silica-filled DGEBA/novolac epoxy composite adhesive is a potential candidate for applying as a structural adhesive for construction with long-term durability.     

Effects of heat accelerated aging on tensile strength of three dimensional braided/epoxy resin composites

The tensile tests of three‐dimensional (3Dim) and four‐directional (4Dir) carbon fiber braided/epoxy resin composites and carbon fiber woven plain fabric laminated/epoxy composites after heat accelerated aging at 150 and 180°C for 60, 120, and 180 h were carried out respectively. The reason of the changes of tensile property of these composites after different aging period of time at different high temperature was explained. The results of two‐way ANOVA analyzing indicate that the aging time has a significant effect on tensile strength of these composites. With the increase of accelerated aging period of time at high temperature, the tensile strengths of these composite samples decreased compared with that of composite samples without aging. However the decrease of tensile strength of 3Dim and 4Dir braided composites is less than that of laminated composites. One of the reasons is after aging for a long time at high temperature, the resin is damaged and becomes brittle which make the bonding force between fiber and resin decrease. Another reason is the structure of reinforcement of composites. After aging, the structure of 3Dim and 4Dir braided/epoxy resin composites still keeps the integrity which makes the 3Dim and 4Dir composites have less tensile performance degradation (3Dim and 4 Dir: three‐dimensional and four‐directional). POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

Synthesis and characterization of chlorinated soy oil based epoxy resin/glass fiber composites

Composites with good toughness properties were prepared from chemically modified soy epoxy resin and glass fiber without additional petroleum based toughening agent. Chlorinated soy epoxy (CSE) resin was prepared from soybean oil. The CSE was characterised by spectral, and titration method. The prepared CSE was blended with commercial epoxy resin in different ratios and cured at 85°C for 3 h, and post cured at 225°C for 2 h using m‐phenylene diamine (MPDA) as curing agent. The cure temperatures of epoxy/CSE/MPDA with different compositions were found to be in the range of (151.2–187.5°C). The composite laminates were fabricated using epoxy /CSE/MPDA‐glass fiber at different compositions. The mechanical properties such as tensile strength (248–299 MPa), tensile modulus (2.4–3.4 GPa), flexural strength (346–379 MPa), flexural modulus (6.3–7.8 GPa) and impact strength (29.7–34.2) were determined. The impact strength increased with the increase in the CSE content. The interlaminor fracture toughness (G_IC) values also increased from 0.6953 KJ/m² for neat epoxy resin to 0.9514 KJ/m² for 15%CSE epoxy‐modified system. Thermogravimetric studies reveal that the thermal stability of the neat epoxy resin was decreased by incorporation of CSE. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Synthesis and characterization of bis(4‐cyanato 3,5‐dimethylphenyl) naphthyl methane/epoxy/glass fiber composites

Bis(4‐cyanato 3,5‐dimethylphenyl) naphthylmethane was prepared by treating CNBr with bis(4‐hydroxy 3,5‐dimethylphenyl) naphthylmethane in the presence of triethylamine at −5 to 5°C. The dicyanate was characterized by FT‐IR and NMR techniques. The prepared dicyanate was blended with commercial epoxy resin in different ratios and cured at 120°C for 1 hr, 180°C for 1 hr, and post cured at 220°C for 1 hr using diamino diphenyl methane (DDM) as curing agent. Castings of neat resin and blends were prepared and characterized by FT‐IR technique. The morphology of the blends was evaluated by SEM analysis. The composite laminates were also fabricated from the same composition using glass fiber. The mechanical properties like tensile strength, flexural strength, and fracture toughness were measured as per ASTMD 3039, D 790, and D 5528, respectively. The tensile strength increased with increase in cyanate content (3, 6, and 9%) from 322 to 355 MPa. The fracture toughness values also increased from 0.7671 kJ/m² for neat epoxy resin to 0.8615 kJ/m² for 9% cyanate ester epoxy modified system. The thermal properties were also studied. The 10% weight loss temperature of pure epoxy is 358°C and it increased to 398°C with incorporation of cyanate ester resin. The incorporation of cyanate ester up to 9% loading level does not affect the T_g to a very great extent. POLYM. COMPOS., 2008. © 2008 Society of Plastics Engineers     

Accelerated-curing epoxy structural film adhesive for bonding lightweight honeycomb sandwich structures

Accelerating the curing of epoxy/aromatic amine adhesives and improving their toughness are challenges in heat-resistant epoxy structural adhesives. Herein, we report an epoxy/aromatic amine adhesive accelerated curing system with an oxo-centered trinuclear (chromium III) complex, which is toughened using a thermoplastic block copolymer (TPBC). The reaction characteristics, heat resistance, microstructure, and bonding properties of the accelerated epoxy adhesives were analyzed. The reaction peak temperature of the epoxy with 3% catalyst was 113.1°C, which was 113.6°C lower than that of epoxy without catalyst, and the modified epoxy resin demonstrated a potential for rapid curing at medium temperature. The glass transition temperature of the TPBC-toughened epoxy adhesive was 125°C after curing, indicating excellent thermal stability after medium temperature curing. The introduction of the TPBC increased the single-lap shear strength of the epoxy adhesive without reducing its heat resistance. The shear strength at room temperature and 120°C of the modified epoxy adhesive with 50 phr of TPBC was 25.2 and 10.9 MPa, respectively. Moreover, the epoxy film adhesive exhibited outstanding bonding properties when used in the bonding of lightweight honeycomb sandwich structures.     

High‐temperature tensile behavior at different crosshead speeds during loading of glass fiber‐reinforced polymer composites

The present study evaluates on the static tensile behavior of glass fiber reinforced polymer (GFRP) composites at 50% and 70% volume fractions of reinforcement tested at room (25 °C), 70 °C, 90 °C, and 110 °C temperatures with 1, 10, 100, 500, and 1000 mm/min crosshead speeds to investigate the impact of high temperature on the mechanical properties and different dominating failures modes. The experimental results reveal that with increase in crosshead speeds the tensile strength of the composite is increasing. The effect of crosshead speeds and temperature with changing fiber volume fractions affects the GFRP composite. Although both the composite systems are found to be crosshead speed sensitive. Crosshead speed sensitivity seems to be more unpredictable at high temperature and at high crosshead speed. Furthermore, it appears to be more unprecedented nature of fluctuation with high fiber volume fraction. The crucial parameters required during the materials designing in various structural components were evaluated and modelled with the help of Weibull constitutive model. The fractography analyses were done to identify the various dominating failure modes in the GFRP composite. There was no significant change found in the glass transition temperatures (T_g) of both the composite system when exposed to different temperature environments. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44715.     

Geopolymer reinforced with E‐glass leno weaves

This study explores the viability of fiberglass‐geopolymer composites as an intermediate temperature structural ceramic composite. E‐glass fibers are cheap, readily available, resistant to heat, electricity and chemical attack. Geopolymers are refractory and can be processed at room temperature. However, pure geopolymers have low tensile strength and fracture toughness, as is typical of ceramics. In this work, tensile and flexure properties of metakaolin‐based sodium and potassium geopolymers reinforced with E‐glass leno weaves were measured and the data was analyzed by Weibull statistics. The average tensile and flexural strengths for sodium geopolymer reinforced with E‐glass leno weaves were 39.3 ± 7.2 MPa and 25.6 ± 4.8 MPa, respectively. For potassium geopolymer reinforced with E‐glass leno weaves, the average tensile and flexural strengths were 40.7 ± 9.9 MPa and 15.9 ± 4.0 MPa, respectively. The composites were heat treated for one hour at two temperatures, 300°C and 550°C and their flexure properties were studied at room temperatures. The average flexural strengths for sodium geopolymer reinforced with E‐glass leno weaves were reduced to 6.6 ± 1.0 MPa after heat treatment at 300°C, and 1.2 ± 0.3 MPa after heat treatment at 550°C, respectively. For potassium geopolymer reinforced with E‐glass leno weaves, the average flexural strengths were 6.1 ± 1.5 MPa and 1.3 ± 0.3 MPa after heat treatment at 300°C and 550°C, respectively. SEM and EDS were performed to observe the fiber‐matrix interface. XRD was done to check if the geopolymer was amorphous as expected.     

Tensile properties of two-dimensional carbon fiber reinforced silicon carbide composites at temperatures up to 2300 °C

Carbon fiber reinforced silicon carbide (C/SiC) composites are of the few most promising materials for ultra-high-temperature structural applications. However, the existing studies are mainly conducted at room and moderate temperatures. In this work, the tensile properties of a two-dimensional plain-weave C/SiC composite are studied up to 2300 °C in inert atmosphere for the first time. The study shows that C/SiC composite firstly shows linear deformation behavior and then strong nonlinear characteristics at room temperature. The nonlinear deformation behavior rapidly reduces with temperature. The Young’s modulus increases up to 1000 °C and then decreases as temperature increases. The tensile strength increases up to 1000 °C firstly, followed by reduction to 1400 °C, then increases again to 1800 °C, and lastly decreases with increasing temperature. The failure mechanisms being responsible for the mechanical behavior are gained through macro and micro analysis. The results are useful for the applications of C/SiC composites in the thermal structure engineering.     

Calendar of events

Printed circuit boards are subject to increasingly hostile environment, for example, to a higher reflow temperature with the new lead-free solders. Consequently, thermal stability of copper clad laminates, a major component in printed circuit boards, is a critical issue in electronic packaging industries. In order to understand thermal degradation behavior, popcorn blister tests were performed at high temperatures for three different brands of copper clads laminated with FR-4 epoxy-saturated glass fabrics. Regardless of the brand, all the specimens became defective with blisters at about 250 °C. Detailed examination of fracture morphology with a scanning electron and an optical interferometric microscope revealed that popcorn blisters started not at the interface between copper foil and epoxy resin but at the interface between epoxy resin and glass yarns inside the FR-4 fabric. Sizing agent, an organic lubricant used for glass fibers, is suspected for the initial breakdown of the interface between glass yarns and epoxy resin. As epoxy resin degraded through decomposition of amino-alcohol portion or some other reaction, the gas products then diffused to the yarn-resin interface area. When the temperature reached about 250 °C, the pressure of such gas pockets became strong enough to rupture the laminate under both tension and shear stresses or to advance the fracture through the epoxy via cleavage fracture. Fracture patterns displayed both river and hackle markings, typical characteristics of epoxy fracture. The river markings seemed to indicate cleavage fracture of the epoxy (mode I) which was in close contact with glass yarns. The hackle markings, on the other hand, suggested rupturing of epoxy under both tension and shear stresses (modes I and II), which were most likely caused by a change in the maximum principal tensile stress direction due to interlocked copper nodules.     

Effects of Temperature and Loading Rate on the Mechanical Properties of a High Temperature Epoxy Adhesive

The variation of the mechanical properties of adhesives with temperature and strain rate is one of the most important factors to consider when designing a bonded joint due to the polymeric nature of adhesives. It is well known that adhesive strength generally shows temperature dependence. Moreover, in many structural applications, the applied loads can be dynamic and the design of the joint requires the knowledge of the high loading rate mechanical behaviour of the adhesive. In this study, the combined effect of the temperature and test speed on the tensile properties of a high temperature epoxy adhesive was investigated. Tensile tests were performed at three different test speeds and various temperatures (room temperature (RT) and high temperatures (100, 125 and 150°C)). The glass transition temperature (T _g) of the epoxy adhesive investigated is approximately 155°C. The ultimate tensile stress decreased linearly with temperature (T) while increased logarithmically with the loading rate, which is in the accord with the Airing's molecular activation model.     

Progressive Failure Analysis of Reinforced-Adhesively Single-Lap Joint

The failure behavior of reinforced-adhesively single-lap joints was investigated experimentally and numerically. The reinforced adhesive was produced by mixing waste composite particles and an epoxy-based commercial adhesive. The single-lap joint was prepared with an adhesive and unidirectional fiber glass/epoxy composite plates with a (0°/90°)₃ stacking sequence. Three types of adhesive were used: an un-reinforced adhesive (ADH), an adhesive mixed with glass fiber-reinforced epoxy resin composite plate particles (GFRC), and an adhesive mixed with carbon fiber-reinforced epoxy resin composite plate particles (CFRC). The adhesive thickness (ta) and overlap length (lap) were 0.4, 0.8, 1.2, and 1.6 mm and 10, 20, 30, and 40 mm, respectively. Progressive failure analysis was performed with the ANSYS? 11.0 finite element program using ANSYS? parametric design language (APDL) code. In the numerical study, the failure loads of the composite and the adhesive were determined with the Hashin failure criteria and the Tresca failure criteria, respectively. The difference between the experimental and numerical studies ranged from 2% to 10%. The failure load of reinforced-adhesively single-lap joints was 1.3–22.8% higher than that of the un-reinforced adhesive.     

Temperature dependence of the tensile properties of lignin/paper composites

The mechanical properties of dioxane lignin (DL)/paper and kraft lignin (KL)/paper composites were investigated as functions of temperature and strain rate. The tensile properties of the lignin/paper composites were governed by the viscoelastic properties of lignins used as a matrix. In the temperature dependence of the tensile properties, the strength of DL/paper composite decreased at 70° and 130°C at which the elongation had maxima. This behaviour was caused by the viscoelastic properties of DL having two relaxations in the primary dispersion region at 120° and 160°C. In the case of KL/paper composite, a drastic decrease in the strength and maximum of elongation were observed at the glass transition of KL (140°C). The strain rate dependence of the strength of DL/paper composite showed behaviour typical of viscoelastic materials. The strength increased with increase of the strain rate and then decreased after reaching a maximum, which showed a transition from a brittle to a ductile type of fracture.     

Creep and relaxation behavior of woven glass/epoxy substrates for multilayer circuit board applications

The creep behavior of a common woven glass/epoxy composite substrate for multilayer circuit board applications was characterized using dynamic mechanical analysis (DMA). The creep compliance was measured in both the warp and fill directions of the composite over a temperature range of 30°C to 155°C. The creep compliance of the neat FR-4 epoxy matrix was also characterized for comparison with the composite response. Master creep curves were obtained for the neat resin and the composite in the warp and fill directions assuming thermorheologically simple behavior and applying the time-temperature superposition principle. The creep data was fit to a Prony series and then converted to relaxation data in the Laplace domain. Micromechanical models were developed to predict the relaxation behavior of the woven glass/epoxy composite from the elastic properties and the geometry of the glass fabric and relaxation behavior of the neat resin. Model predictions were compared with experimental data.     

Thermal and electrical properties of epoxy composites at high alumina loadings and various temperatures

Epoxy microcomposites with high loading micro alumina (Al₂O₃, 100–400 phr) were prepared by casting method and their thermal and electrical properties were studied at temperatures from 25 to 150 °C. The electric resistance device and the dielectric electrode device were designed to measure the electrical properties of the composites. Thermogravimetric analysis (TGA) and scanning electron microscopic proves the homodispersion of Al₂O₃ microparticles in epoxy. TGA indicates that the temperature of 5 % weight loss of epoxy/Al₂O₃ (100 phr) composite is 366 °C, 34 °C higher than that of pure epoxy. Differential scanning calorimetry shows that the glass transition temperature of epoxy/Al₂O₃ composite (400 phr) increases to 114.7 °C, 9.2 °C higher than that of pure epoxy. Thermal conductivity test demonstrated that with increasing Al₂O₃ content at 25 °C, thermal conductivity of epoxy/Al₂O₃ composites increased to 1.382 W/(m K) which is 5.62 times that of pure epoxy. Electrical tests demonstrate that by increasing of Al₂O₃ content and temperature, the electric resistance and dielectric properties of the composites show great dependencies on them. Resistivities of all the specimens decreased with the increasing of temperature owing to the increasing molecular mobility in the higher temperature. Resistivity of pure epoxy at 25 °C is about 9.56 × 10¹⁶ Ω cm, about one order of magnitude higher than that of pure epoxy at 125 °C and two orders of magnitude higher than that of pure epoxy at 150 °C. These results can give some advice to design formulations for practical applications in power apparatus.     

Mechanical and thermal properties of epoxy resins with reversible crosslinks

The tensile properties: Young's modulus, ultimate tensile strength, ultimate elongation, the glass transition temperature, and the dynamic mechanical properties (dynamic shear modulus (G'), loss tangent (Tan δ)), of three epoxy resins (Epon 828, Epon 836, Epon HPT 1071) cured with the disulfide-containing crosslinking agent—4.4-dithiodianilme (DTDA) have been characterized. The results show that DTDA is a satisfactory crosslinking agent for the epoxide resins that have been studied as compared to the well-known curing agent methylene dianiline (MDA). There are no significant differences between the properties of Epon 828 cured with DTDA at stoichiometric ratio (2:1) and Epon 828 cured with DTDA at small amine excess ratio (1.75:1). The glass transition temperature of the cured tetrafunctional epoxy resin Epon HPT 1971 (235°C) is significantly higher than that of difunctional epoxy resins such as Epon 828 (T_g–175°C), but the product is too brittle to be used without plasticizer.     

Investigation of CNT modification of epoxy resin in CFRP strengthening systems

The use of carbon fiber‐reinforced polymers (CFRPs) to reinforce old structures has become popular in recent years. In this study, the chemical structure of the epoxy resin used as the bonding agent in the CFRP strengthening system was modified by dispersing multi‐walled carbon nanotubes (MWCNTs) in order to improve the performance of the strengthening system. Composites were fabricated with different mixing orders employing the solvent‐assisted dispersion method and ultrasonic mixing. Thermogravimetric analysis, dynamic mechanical analysis, and tensile tests were conducted to investigate the effect of CNT dispersion and fabrication method on the thermal and mechanical properties of epoxy composite. In addition, the temperature‐dependent tensile behavior of fabricated composites was studied by performing tensile tests at elevated temperatures. The morphology of CNT/epoxy composites was characterized using scanning electron microscopy (SEM). Fourier transform infrared (FTIR) was also used to show the influence of solvent on the molecular structure of composites. Based on the experimental results, the decomposition temperature of the epoxy resin was heightened by 15°C as a result of solvent‐assisted dispersion of nanotubes. However, the glass transition temperature (T_g) was slightly reduced due to the solvent effect. FTIR analysis revealed that the solvent negatively affects the curing process of epoxy composite. A considerable enhancement was recorded in the tensile properties as a result of CNT infusion. This was attributed to the homogeneous dispersion of nanotubes which was shown by SEM images. Using solvent to disperse nanotubes led to the reduction of tensile strength of the epoxy composite at elevated temperature due to the lower T_g. POLYM. COMPOS. 37:1021–1033, 2016. © 2014 Society of Plastics Engineers     

A novel latent initiator for cationic polymerizations of epoxides: Composite catalysts containing aluminum complexes phase‐separated in epoxides

A novel latent initiator for cationic polymerizations of epoxides heterogeneous aluminum complex/phenol initiator (HAP) is reported. Phase transitions are newly employed for realizing the latent property. The initiator consists of 4,4′‐dihydroxydiphenylsulfone and aluminum tris(alkyl acetoacetate), with the alkyl group containing more than 18 carbons. The composite initiator is phase‐separated and dispersed uniformly in epoxy resins at room temperature. When the mixture is heated to a temperature greater than 70°C, the composite initiator makes clear mixtures with epoxy resins because of the phase change in the aluminum complexes. Homogeneous epoxy resins containing these composite initiators are ready for various types of processing, including impregnation and injection. Gelation occurs rapidly at temperatures greater than 100°C. The phase change in the initiator makes it possible for the epoxy compounds to have a long storage stability at room temperature and a high curing speed at greater than 100°C. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 1046–1053, 2002     

Durability of PBI adhesive bonded joints under various environmental conditions

Structural adhesives are finding increasing use in many applications. However, their utilization at elevated temperature has always been a challenge due to their low thermal and mechanical properties. However, in recent years, the development of high performance polymers have overcome the problem of using adhesive bonding at high temperature to some extent. Polybenizimidazole (PBI) is one such recently emerged high performance polymer with excellent thermal and mechanical properties. It has a tensile strength of 160 MPa and a glass transition temperature (T_g) of 425 °C. Due to its excellent thermal and mechanical properties, it has the potential to be used as an adhesive under various environmental conditions. In the present work, efforts are devoted to explore the potential of using PBI at high temperature and in hot-wet environmental conditions. M21 and DT120 epoxy based carbon fiber composite bonded joints were prepared and tested. Both M21/carbon composite and DT120/carbon composite have exhibited a reduction in joint strength of about 16% and 25% respectively after 1000 h of conditioning in a hot-wet environment. However, a reduction in lap shear strength of 52% and 56% is observed when composite bonded joints were tested at 80 °C.     

Tensile Properties of Arenga pinnata Fiber-Reinforced Epoxy Composites

The aim of this study is to determine the tensile properties of Arenga pinnata fiber as a natural fiber and epoxy resin as a matrix. The Arenga pinnata fibers were mixed with epoxy resin at the various fiber weight percentages of 10%, 15%, and 20% Arenga pinnata fiber and with different fiber orientations such as long random, chopped random, and woven roving. Hand lay-up processes in this experiments were to produce specimen test with the curing time for the composite plates is in the room temperature (25–30°C). Results from the tensile tests of Arenga pinnata fiber reinforced epoxy composite are that the 10 wt.% woven roving Arenga pinnata fiber showed the highest value for maximum tensile properties. The tensile strength and Young's modulus values for 10 wt.% of woven roving Arenga pinnata fiber composite are 51.725 MPa and 1255.825 MPa, respectively. The results above indicate that the woven roving Arenga pinnata fiber has a better bonding between its fiber and matrix compared to long random Arenga pinnata fiber and chopped random Arenga pinnata fiber. Scanning electron microscopy (SEM) tests were carried out after tensile tests to observe the interface of fiber and matrix adhesion.