Preparation and characterization of double‐MF shell microPCMs used in building materials

A kind of double‐shell heat energy storage microcapsule was prepared used melamine formaldehyde (MF) resin as shell material, and the properties of the microcapsules were investigated. A phase change material, with melt point of 24°C and phase transition heat of 225.5J/g, was used as core. The microcapsules would be used in indoor walls to regulate the temperature and save energy. The surface morphological structure was examined by means of scanning electron microscopy. The strength of the shell was evaluated through observing the surface change after pressure by means of scanning electron microscopy. The average diameter of the microcapsules was 5 μm ～ 10 μm. Diameter of 1 μm ～ 5 μm could also be obtained by using different stirring speeds. The globular surface was smooth and compact. The thickness was 0.5 μm ～ 1 μm. Also, the melting point of the microcapsules was 24.7°C, nearly equal to the pure phase change material. The DSC results make clear that the polymer shell of the microcapsules does not influence the properties of the phase change material. It was also found that the avoiding penetration property of the double‐shell microcapsules was better than that of single shell, and the average diameter of 5 μm was better than 1 μm. With the increase of ratio of the core material, the compactability decreased, and the shell thickness decreased. The mass ratio of core and shell was 3 : 1 to ensure that the microcapsules had good heat storage function. The measuring test showed that the microcapsules did not rupture at a pressure of 1.96 × 10⁵ Pa. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 1755–1762, 2005     

Expansion space and thermal stability of microencapsulated n‐octadecane

5.0–50.0 vt% of cyclohexane was mixed with 95.0–50.0 vt% of n‐octadecane as the oil‐phase during the emulsion process in the in situ polymerization of melamine‐formaldehyde. By heat‐treating the microcapsules in an oven at 100°C, the cyclohexane was removed and expansion space was formed inside the microcapsules. The microcapsules were characterized by using FTIR, SEM, DSC, TGA, and gas chromatography. When the microcapsules are heat‐treated at temperatures higher than 180°C, Tm, ΔHm, Tc, and ΔHc of the microcapsules decrease. The attenuation of enthalpy of the microcapsules containing expansion space is obviously lower than that of the control sample, however. The permeability of the microcapsule shell decreases with the increase of cyclohexane content. There is a maximum between the thermal stabilities of the microcapsules and the cyclohexane contents. The microcapsules synthesized with 30.0–40.0 vt% of cyclohexane have the highest thermal stabilities, with 230°C and 289°C in air and nitrogen atmosphere, respectively. The thermal stable temperatures are approximately 67°C and 102°C higher than that of the control sample, respectively. The expansion space inside the microcapsules allows the n‐octadecane to expand in the temperature rising process and exert lower pressure to the shell, therefore keeping the shell intact and increasing the thermal stabilities of the microcapsules. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 390–396, 2005     

Heat‐resistant sustained‐release fragrance microcapsules

In this study, fragrance microcapsules were prepared by a spray‐drying method, in which the osmanthus flower fragrance acted as the core material and gum arabic and maltodextrin acted as shell materials. Scanning electron microscopy images showed that the microcapsules were approximately spherical in shape with a concave surface. Fourier transform infrared spectroscopy was used to prove the formations of the microcapsules. The fragrance retention rate at high temperatures (80–120°C) after a short heating time (30 min) reached 85.20 ± 2.72% and the retention rate after a long heating time (a week) at 60°C reached 95.40 ± 2.88%. The retention rate after 100 days exceeded 90%, and the transdermal release experiments showed that on the surface of the skin, the fragrance in the microcapsules stayed longer than in the pure fragrance oil. These results indicate that the fragrance microcapsules had an excellent aroma‐reserving ability. The results of the release test proved that the transport mechanism of the fragrance microcapsules conformed to the Weibull equation. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40053.     

Structures and properties of thermoregulated acrylonitrile–methyl acrylate sheet containing microphase change materials

A series of melt processable poly(acrylonitrile–methyl acrylate) copolymers with a feeding ratio of 85/15 mol% (abbreviated as 85/15 AN/MA below) containing 0–25 wt% of microencapsulated phase change materials (micro‐PCMs) were synthesized by aqueous precipitation polymerization. The number average sequence lengths (NASLs) and tacticity of 85/15 AN/MA were determined using ¹³C‐NMR. The results showed that the NASL of contiguous AN sequences is 10.00 and the tacticity is atactic with approximately 51% m and 49% r diads (the relative orientation of two adjacent cyanogroup). 85/15 AN/MA containing various contents of micro‐PCMs were processed into sheets in melt condition at 210°C and 20 MPa. The structures and properties of the copolymers and sheets containing micro‐PCMs were studied by using Fourier transform infrared spectroscopy, nuclear magnetic resonance (¹H‐NMR), scanning electron microscopy, differential scanning calorimetry, gel permeation chromatography, X‐ray diffraction, and dynamic mechanical analysis. The composition of AN/MA copolymer agreed well with its monomer feed ratio. The melting enthalpy of the sheets containing 25 wt% of micro‐PCMs was approximately 25 J/g, which increased steadily as the micro‐PCMs content increased. The modulus of the sheets decreased with the micro‐PCMs content increased. The glass transition temperature (T_g) of the sheets was in the range of 79.7–81.7°C, which also increased with the micro‐PCMs content increasing. POLYM. COMPOS., 2013. © 2013 Society of Plastics Engineers     

Storage stability and solubility of poly(urea‐formaldehyde) microcapsules containing A‐olefin drag reducing polymer

Microcapsules containing α‐olefin drag reducing polymer were prepared by in situ and interfacial polymerization with urea, formaldehyde, and styrene as shell materials, respectively. IR spectrums of prepared shells indicated the formations of poly(urea‐formaldehyde) and polystyrene in the microencapsulating process. The morphologies of uncoated particles and microcapsules were observed by scanning electron microscopy (SEM) which proved that the α‐olefin drag reducing polymer particles were effectively coated. For the purpose of determining the stability of microcapsules in transportation and storage, the static pressure experiment was carried out and lasted for 6 months. In this process, microcapsules with polystyrene as shell material stuck together after 3 months; however, those with poly(urea‐formaldehyde) kept the state of particles. The thermal characteristics of uncoated particles (core), poly(urea‐formaldehyde) (shell), and microcapsules with that as shell material were characterized by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) which proved that thermal stable temperature of microcapsules containing α‐olefin drag reducing polymer with poly(urea‐formaldehyde) as shell material was below 225°C, and the mean heat absorbed by microcapsules in the temperature increasing process was 1.5–2.0 W/g higher than that by cores. The evaluation of drag reducing rate of microcapsules showed that the microencapsulating process had no influence on the drag reduction of α‐olefin drag reducing polymer. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Preparation and characterization of flame retardant phase change materials by microencapsulated paraffin and diethyl ethylphosphonate with poly(methacrylic acid‐co‐ethyl methacrylate) shell

Microcapsules containing paraffin and diethyl ethylphosphonate (DEEP) flame retardant with uncrosslinked and crosslinked poly (methacrylic acid‐co‐ethyl methacrylate) (P(MAA‐co‐EMA)) shell were fabricated by suspension‐like polymerization. The surface morphologies of the microencapsulated phase change materials (microPCMs) were studied by scanning electron microscopy. The thermal properties and thermal stabilities of the microPCMs were investigated by differential scanning calorimetry (DSC), and thermal gravimetric analysis (TGA). The flame retarding performances of the microcapsule‐treated foams were calculated by using an oxygen index instrument. The DSC results showed that the crosslinking of the polymer shell led to an increase in the melting enthalpies of the microcapsule by more than 15%. The crosslinked P(MAA‐co‐EMA) microcapsules with DEEP and without DEEP have melting enthalpies of 67.2 and 102.9 J/g, respectively. The TGA results indicated that the thermal resistant temperature of the crosslinked microcapsules with DEEP was up to 171°C, which was higher than that of its uncrosslinked counterpart by ～20°C. The incorporation of DEEP into the microPCM increased the limiting oxygen index value of the microcapsule‐treated foams by over 5%. Thermal images showed that both microcapsule‐treated foams with and without DEEP possessed favorably temperature‐regulated properties. As a result, the microPCMs with paraffin and DEEP as core and P(MAA‐co‐EMA) as shell have good thermal energy storage and thermal regulation potentials, such as thermal‐regulated foams heat insulation materials. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41880.     

Preparation of coated thermo‐regulating textiles using Rubitherm‐RT31 microcapsules

Spherical microcapsules with a 49 wt % of Rubitherm^® RT31 were successfully synthesized by means of suspension‐like polymerization to be used for textile applications in summer conditions. Microcapsules were fixed into seven fabric substrates for different textile applications by a coating technique without deteriorating original functionalities of the textiles. Thermal performance of different coated textiles with 35 wt % of microcapsules was evaluated by differential scanning calorimetry (DSC) and infrared thermography (IR) techniques and the physical characteristics of textiles with thermo‐regulating properties were examined by environmental scanning electron microscopy (ESEM). It was observed that all treated textile substrates allow to obtain thermo‐regulating properties with acceptable latent heat storage capacities. Results also indicated that the presence of microcapsules containing Rubitherm^® RT31 produces a significant thermal insulation effect during a cold to warm transition (20–45°C). Thus, this kind of microcapsules can be used to obtain textiles with thermal comfort‐related properties. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Further study on double‐melting endotherms of isotactic polypropylene

The origins of the single‐ and double‐melting endotherms of isotactic polypropylene crystallized at different temperatures were studied carefully by differential scanning calorimetry, wide‐angle X‐ray diffraction, and small‐angle X‐ray scattering. The experimental data show that spontaneous crystallization occurs when the crystallization temperature is lower than 117°C; thus the lamellae formed are imperfect. At a lower heating rate, the recrystallization or reorganization of these imperfect lamellae leads to double endotherms. On the other hand, when the crystallization temperature is higher than 136°C, two major kinds of lamellae with different thickness are developed during the isothermal process, which also results in the double‐melting endotherms. In the intermediate temperature range the lamellae formed are perfect, and there is only a single peak in the distribution of lamellar thickness. This explains the origin of the single‐melting endotherm. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 163–170, 2000     

Thermal and morphological stability of polystyrene microcapsules containing phase‐change materials

Polystyrene microcapsules with paraffin wax as the active agent [phase‐change material (PCM)] were produced by a Shirasu porous glass emulsification technique and a subsequent suspension‐like polymerization process. The suitability of the obtained microcapsules for textile applications was studied. The thermal properties, surface morphology, and structural stability of the PCM microcapsules were investigated with differential scanning calorimetry, thermogravimetric analysis, and environmental scanning electron microscopy. The microcapsules could be used without any appreciable damage or irreversible changes in their integrity until 135°C. Furthermore, these microcapsules were heat‐resistant and could endure the curing conditions of textile coating up to 140°C for 30 min. In addition, the stability of the microcapsules under common laundering conditions was tested. It was confirmed that the microcapsules were durable enough and maintained their stability during stirring in hot water and alkaline solutions. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Preparation,characterization, and prominent thermal stability of phase‐change microcapsules with phenolic resin shell and n‐hexadecane core

Microcapsules with phenolic resin (PFR) shell and n‐hexadecane (HD) core were prepared by controlled precipitation of the polymer from droplets of oil‐in‐water emulsion, followed by a heat‐curing process. The droplets of the oil phase are composed of a polymer (PFR), a good solvent (ethyl acetate), and a poor solvent (HD) for the polymer. Removal of the good solvent from the droplets leads to the formation of microcapsules with the poor solvent encapsulated by the polymer. The microstructure, morphology, and phase‐change property as well as thermal stability of the microcapsules were systematically characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimety (DSC), and thermogravimetric analysis (TGA). The phase‐change microcapsules exhibit smooth and perfect structure, and the shell thickness is a constant fraction of the capsule radius. The initial weight loss temperature of the microcapsules was determined to be 330°C in N₂ and 255°C in air, respectively, while that of the bulk HD is only about 120°C both in air and N₂ atmospheres. The weight loss mechanism of the microcapsules in different atmosphere is not the same, changing from the pyrolysis temperature of the core material in N₂ to the evaporation of core material caused by the fracture of shell material in air. The melting point of HD in microcapsules is slightly lower than that of bulk HD, and a supercooling was observed upon crystallization. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Preparation and properties of phase‐change heat‐storage UV curable polyurethane acrylate coating

Phase‐change heat‐storage UV curable polyurethane acrylate (PUA) coating was prepared by applying microencapsulated phase change materials (microPCMs) to PUA coating. MicroPCMs containing paraffin core with melamine‐formaldehyde shell were synthesized by in situ polymerization. The effect of stirring speed, emulsification time, emulsifier amount, and core/shell mass ratio on particle size, morphology, and phase change properties of the microPCMs was studied by using laser particle size analyzer, Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopic analysis, scanning electron microscopy, and differential scanning calorimetry. The results showed that the diameter of the microcapsules decreased with the increase of stirring speed, emulsification time, and emulsifier amount. When the mass ratio of emulsifier to paraffin is 6%, microcapsules fabricated with a core/shell ratio of 75/25 have a compact surface and a mean particle size of 30 μm. The sample made under the above conditions has a higher efficiency of microencapsulation than other samples and was applied to PUA coating. The dispersion of microPCMs in coating and heat‐storage properties of the coating were investigated. The results illustrated that the phase‐change heat‐storage UV curable PUA coating can store energy and insulate heat. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41266.     

Synthesis and characterization of melt‐processable polyimides derived from 1,4‐bis(4‐amino‐2‐trifluoromethylphenoxy)benzene

A series of molecular‐weight‐controlled imide resins end‐capped with phenylethynyl groups were prepared through the polycondensation of a mixture of 1,4‐bis(4‐amino‐2‐trifluoromethylphenoxy)benzene and 1,3‐bis(4‐aminophenoxy)benzene with 4,4′‐oxydiphthalic anhydride in the presence of 4‐phenylethynylphthalic anhydride as an end‐capping agent. The effects of the resin chemical structures and molecular weights on their melt processability and thermal properties were systematically investigated. The experimental results demonstrated that the molecular‐weight‐controlled imide resins exhibited not only meltability and melt stability but also low melt viscosity and high fluidability at temperatures lower than 280°C. The molecular‐weight‐controlled imide resins could be thermally cured at 371°C to yield thermoset polyimides by polymer chain extension and crosslinking. The neat thermoset polyimides showed excellent thermal stability, with an initial thermal decomposition temperature of more than 500°C and high glass‐transition temperatures greater than 290°C, and good mechanical properties, with flexural strengths in the range of 140.1–163.6 MPa, flexural moduli of 3.0–3.6 GPa, tensile strengths of 60.7–93.8 MPa, and elongations at break as high as 14.7%. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Synthesis and characterization of organosoluble polyfluorinated polyimides derived from 3,3′,5,5′‐tetrafluoro‐4,4′‐diaminodiphenylmethane and various aromatic dianhydrides

A polyfluorinated aromatic diamine, 3,3′, 5,5′‐tetrafluoro‐4,4′‐diaminodiphenylmethane (TFDAM), was synthesized and characterized. A series of polyimides, PI‐1–PI‐4, were prepared by reacting the diamine with four aromatic dianhydrides via a one‐step high‐temperature polycondensation procedure. The obtained polyimide resin had moderate inherent viscosity (0.56–0.68 dL/g) and excellent solubility in common organic solvents. The polyimide films exhibited good thermal stability, with an initial thermal decomposition temperature of 555°C–621°C, a 10% weight loss temperature of 560°C–636°C, and a glass‐transition temperature of 280°C–326°C. Flexible and tough polyimide films showed good tensile properties, with tensile strength of 121–138 MPa, elongation at break of 9%–12%, and tensile modulus of 2.2–2.9 GPa. The polyimide films were good dielectric materials, and surface and volume resistance were on the order of a magnitude of 10¹⁴ and 10¹⁵ Ω cm, respectively. The dielectric constant of the films was below 3.0 at 1 MHz. The polyfluorinated films showed good transparency in the visible‐light region, with a cutoff wavelength as low as 302 nm and transmittance higher than 70% at 450 nm. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1442–1449, 2007     

Fabrication and thermal properties of microPCMs: Used melamine‐formaldehyde resin as shell material

An in‐situ polymerization process prepared a series of melamine formaldehyde (MF) microcapsules containing phase change material (PCM) as core material. The phase change temperature of this PCM was 24°C and its phase transition heat was 225.5 J/g. The microencapsulated phase change materials (MicroPCMs) were bedded in indoor‐wall materials to store and release heat energy, which would economize heat energy and make the in‐door condition comfortable. We investigated the structural formation mechanism by microscope and scanning electron microscopy (SEM). The superficial morphology measurements indicated the optimal shell material dropping rate 0.5 mL min^?1, double‐shell, and temperature elevating speed 2°C/10 min. The results obtained in the present investigation were reasonably understood on the basis of getting determinate rigidity and compacted shell. Also, the observed results were used to control the mass of shell material to get desired thickness of shell. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 2006     

Microencapsulation of sulfur in poly(urea–formaldehyde)

Poly(urea–formaldehyde) (PUF) microcapsules loaded with sulfur were prepared by in situ polymerization. Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry and thermogravimetric (TG) analysis were used for the characterization of the obtained microcapsules. The chemical structure of the microcapsules was determined by FTIR. SEM analysis showed that the microcapsules were spherical and that the mean diameter of microcapsules was 42 ± 1 μm. Thermal analysis showed that the microcapsules were thermally stable below 247°C. The release properties of sulfur from the PUF microcapsules during the vulcanization of acrylonitrile–butadiene rubber (NBR) were studied by analysis of the vulcanization properties. The results show that at a vulcanizing temperature of 160°C, all of the sulfur entrapped in PUF was released out through the microcracks and pores of the shell, and the curing time of the microcapsule curing system compared with that of the sulfur curing system was longer. The mechanical properties of the NBR vulcanized by sulfur microcapsules were better than those of the NBR vulcanized by sulfur. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Organosoluble and light‐colored fluorinated polyimides based on 1,1‐bis[4‐(4‐amino‐2‐trifluoromethylphenoxy)phenyl]‐1‐phenylethane and various aromatic dianhydrides

To investigate the CF₃ group affecting the coloration and solubility of polyimides (PI), a novel fluorinated diamine 1,1‐bis[4‐(4‐amino‐2‐ trifluoromethylphenoxy)phenyl]‐1‐phenylethane (2) was prepared from 1,1‐ bis(4‐hydrophenyl)‐1‐phenylethan and 2‐chloro‐5‐nitrobenzotrifluoride. A series of light‐colored and soluble PI 5 were synthesized from 2 and various aromatic dianhydrides 3a–f using a standard two‐stage process with thermal 5a– f(H) and chemical 5a–f(C) imidization of poly(amic acid). The 5 series had inherent viscosities ranging from 0.55 to 0.98 dL/g. Most of 5a–f(H) were soluble in amide‐type solvents, such as N‐methyl‐2‐pyrrolidone (NMP), N,N‐ dimethylacetamide (DMAc), and N,N‐dimethylformamide (DMF), and even soluble in less polar solvents, such as m‐Cresol, Py, Dioxane, THF, and CH₂Cl₂, and the 5(C) series was soluble in all solvents. The GPC data of the 5a–f(C) indicated that the Mn and Mw values were in the range of 5.5–8.7 × 10⁴ and 8.5–10.6 × 10⁴, respectively, and the polydispersity index (PDI) Mw /Mn values were 1.2–1.5. The PI 5 series had excellent mechanical properties. The glass transition temperatures of the 5 series were in the range of 232–276°C, and the 10% weight loss temperatures were at 505–548 °C in nitrogen and 508–532 °C in air, respectively. They left more than 56% char yield at 800°C in nitrogen. These films had cutoff wavelengths between 356.5–411.5 nm, the b* values ranged from 5.0–71.1, the dielectric constants, were 3.11–3.43 (1MHz) and the moisture absorptions were in the range of 011–0.40%. Comparing 5 containing the analogous PI 6 series based on 1,1‐bis[4‐(4‐aminophenoxy)phenyl]‐1‐ phenylethane (BAPPE), the 5 series with the CF₃ group showed lower color intensity, dielectric constants, and better solubility. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 2399–2412, 2005     

Fast pH‐thermo‐responsive copolymer hydrogels with micro‐porous structures

Micro‐porous copolymer hydrogels were prepared by γ‐ray irradiation of mixed solutions of N‐isopropylacrylamide (NIPAAm) and acrylic acid (AAc) above the lower critical solution temperature (LCST). From Cryo‐SEM observations, the gels were found to consist of three‐dimensional fibrous micro‐gels and micro‐pores. The copolymer gels swelled at temperatures below the LCST and shrunk at temperatures above it, and they showed rapid volume transitions on a time scale on the order of a minute when experiencing temperature changes between 10 and 40°C. The transition times for thermal shrinking were almost the same regardless of AAc composition, but the transition times for thermal swelling were increased with increasing AAc contents. The copolymer gels also showed rapid volume transitions with time constants on the order of an hour on experiencing pH changes between 2 and 12. The transition times for pH volume change at 10°C were within one hour, except for the gels containing only small amounts of AAc. On the other hand, the transition times for pH‐dependent volume change at 40°C were increased with increasing AAc content. The lower responsiveness of the transition results from an increase in hydrophobicity arising from the formation of inter‐ and intra‐molecular hydrogen bonds between the non‐ionized carboxylic acid groups and the amide groups. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 75–84, 2003     

Synthesis and characterization of readily soluble polyarylates derived from either 1,1‐bis(4‐hydroxyphenyl)‐1‐phenylethane or tetramethylbisphenol A and aromatic diacid chlorides

A series easily soluble polyarylates were synthesized from either 1,1‐bis(4‐hydroxyphenyl)‐1‐phenylethane or tetramethylbisphenol A with various aromatic diacid chlorides by the two‐phase interfacial polycondensation. These polyarylates have the inherent viscositiesin the range of 0.36–0.97 dL/g, and their number‐average and weight‐average molecular weights determined by gel permeation chromatography are 14,200–43,200 and 31,900–102,500, respectively. All these polyarylates are readily soluble in a wide range of organic solvents, thus these polymers can be convenient to process into heat resistance films by cast, spin‐ or dip‐coating. The polyarylates have the glass transition temperatures in the range of 165.0–201.6°C. The pendent phenyl‐containing polyarylates reveal excellent thermal stability, and their initial degradation temperatures are all above 480°C and char yields at 700°C are 37.97–40.53% in nitrogen atmosphere. However, the polymers prepared from tetramethylbisphenol A have a large decrease in thermal stability, and their initial degradation temperatures in nitrogen are only about 440°C. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Epoxy–imide resins from N‐(4‐ and 3‐carboxyphenyl)trimellitimides. I. Adhesive and thermal properties

Epoxy–imide resins were obtained by curing Araldite GY 250 (diglycidyl ether of bisphenol‐A and epichlorohydrin; difunctional) and Araldite EPN 1138 (Novolac–epoxy resin; polyfunctional) with N‐(4‐ and 3‐carboxyphenyl)trimellitimides derived from 4‐ and 3‐aminobenzoic acids and trimellitic anhydride. The adhesive lap shear strength of epoxy–imide systems at room temperature and at 100, 125, and 150°C was determined on stainless‐steel substrates. Araldite GY 250‐based systems give a room‐temperature adhesive lap shear strength of about 23 MPa and 49–56% of the room‐temperature adhesive strength is retained at 150°C. Araldite EPN 1138‐based systems give a room‐temperature adhesive lap shear strength of 16–19 MPa and 100% retention of room‐temperature adhesive strength is observed at 150°C. Glass transition temperatures of the Araldite GY 250‐based systems are in the range of 132–139°C and those of the Araldite EPN 1138‐based systems are in the range of 158–170°C. All these systems are thermally stable up to 360°C. The char residues of Araldite GY 250‐ and Araldite EPN 1138‐based systems are in the range of 22–26% and 41–42% at 900°C, respectively. Araldite EPN 1138‐based systems show a higher retention of adhesive strength at 150°C and have higher thermal stability and T_g when compared to Araldite GY 250‐based systems. This has been attributed to the high crosslinking possible with Araldite EPN 1138‐based systems arising due to the polyfunctional nature of Araldite EPN 1138. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 1729–1736, 2000     

Low dielectric thermoset. I. Synthesis and properties of novel 2,6‐dimethyl phenol‐dicyclopentadiene epoxy

A 2,6‐dimethyl phenol‐dicyclopentadiene novolac was synthesized from dicyclopentadiene and 2,6‐dimethyl phenol, and the resultant 2,6‐dimethyl phenol‐dicyclopentadiene novolac was epoxidized to 2,6‐dimethyl phenol‐dicyclopentadiene epoxy. The structures of novolac and epoxy were confirmed by Fourier transform infrared spectroscopy (FTIR), elemental analysis, mass spectroscopy (MS), nuclear magnetic resonance spectroscopy (NMR), and epoxy equivalent weight titration. The synthesized 2,6‐dimethyl phenol‐dicyclopentadiene epoxy was then cured with 4,4‐diaminodiphenyl methane (DDM), phenol novolac (PN), 4,4‐diaminodiphenyl sulfone (DDS), and 4,4‐diaminodiphenyl ether (DDE). Thermal properties of cured epoxy resins were studied by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), dielectric analysis (DEA), and thermal gravimetric analysis (TGA). These data were compared with those of the commercial bisphenol A epoxy system. Compared with the bisphenol A epoxy system, the cured 2,6‐dimethyl phenol‐ dicyclopentadiene epoxy resins exhibited lower dielectric constants (～3.0 at 1 MHz and 2.8 at 1 GHz), dissipation factors (～0.007 at 1 MHz and 0.004 at 1 GHz), glass transition temperatures (140–188°C), thermal stability (5% degradation temperature at 382–404°C), thermal expansion coefficients [50–60 ppm/°C before glass‐transition temperature (T_g)], and moisture absorption (0.9–1.1%), but higher modulus (～2 Gpa at 60°C). © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 2607–2613, 2003