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1.
Novel polyphenylene oxide (PPO) microcapsules filled with epoxy resins (PPOMCs) were synthesized by in situ polymerization technology with 2, 6‐dimethy phenol as shell materials and diglycidyl ether of bisphenol A epoxy resins as core materials. The structures and morphologies of PPOMCs were characterized using Fourier‐transform infrared spectroscopy, micro‐confocal Raman microscope, laser scanning confocal microscopy, scanning electron microscopy and optical microscopy, respectively. The thermal properties of PPOMCs were investigated using differential scanning calorimetry and thermogravimetric analysis. The influences of different processing parameters such as the weight ratio of shell material to core material, kind of surfactant and reaction temperature on the morphologies and sizes of PPOMCs were investigated. Preliminary investigation on application of PPOMCs to thermosetting resins 4,4′‐bismaleimidodiphenylmethane/O,O′‐diallylbisphenol A (BMI/BA) system was conducted. Results indicate that PPOMCs can be synthesized successfully. The sizes and surface morphologies of PPOMCs may be significantly affected by different processing parameters. PPOMCs can be well prepared at about 30°C, and they depend strongly on the kind of surfactant and the weight ratio of shell material to core material. PPOMCs basically exhibit high thermal stability when the temperature is below 258°C. The addition of PPOMCs can improve the mechanical properties and maintain the thermal properties of BMI/BA system. The released core materials from PPOMCs may repair the matrix cracks through the polymerization of epoxy resins initiated by curing agent. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

2.
An inorganic-organic hybrid material system consisting of (3-glycidyloxypropyl)trimethoxysilane, dimethyldimethoxysilane and zirconium(IV) n-propoxide was prepared by the sol-gel method. The influence of processing parameters including Zr content, UV irradiation and sol ageing on the thermal stability of the resultant thin films was characterised by thermogravimetry. It was demonstrated that the crosslinking of epoxy groups in the structure was the primary reason for variation in the thermal stability of the system. As Zr and/or UV irradiation may be employed to crosslink the epoxy groups in the structure, the thermal stability of the system can be tuned by the optimal combination of these two crosslinking methods.  相似文献   

3.
Polythiophene nanoparticles as a conductive filler was prepared with average diameter of 20-35 nm and its molecular structure was confirmed by the FT-IR, TEM, XRD and UV-vis analysis. A new conductive epoxy nanocomposite was synthesized by curing of diglycidyl ether of bisphenol A/4,4′-(4,4′ Isopropylidenediphenoxy) bis (Phthalic Anhydride) involving various percentages of polythiophene nanoparticles. DSC and DMTA studies revealed that low percentage of the polythiophene nanoparticles, i.e. 1%, results in improved crosslink density as evidenced by increasing in the glass transition temperature. The addition of polythiophene nanoparticles into the epoxy matrix resulted in a significant increment in the electrical conductivity, mechanical properties, thermal stability and activation energy of thermal degradation. The advanced isoconversional method is utilized to describe the curing behavior and thermal degradation process of the neat epoxy and epoxy nanocomposite. We have utilized the Coats-Redfern and Criado methods to find the solid state thermal degradation reaction mechanism. For the nanocomposite, the mechanism was recognized to be two-dimensional diffusion (D2) reaction and it changes to a nucleation and growth (A4) for pure epoxy system.  相似文献   

4.
Montmorillonite (MMT) was modified with the acidified cocamidopropyl betaine (CAB) and the resulting organo-montmorillonite (O-MMT) was dispersed in an epoxy/methyl tetrahydrophthalic anhydride system to form epoxy nanocomposites. The dispersion state of the MMT in the matrix was investigated by X-ray diffraction and scanning electronic microscopy. The thermal stability of the epoxy nanocomposites was examined by TGA. Thermal stability of the epoxy nanocomposite is dependent upon the dispersion state of the OMMT in the epoxy matrix although all the epoxy nanocomposites had enhanced thermal stability compared with the neat epoxy resin. The thermal stability of the epoxy resin nanocomposites was correlated with the dispersion state of the MMT in the epoxy resin matrix.  相似文献   

5.
Activated carbon derived from oil palm empty fruit bunch (AC-EFB), bamboo stem (AC-BS), and coconut shells (AC-CNS) were obtained by pyrolysis of agricultural wastes using two chemical reagents (H3PO4 or KOH). The AC-EFB, AC-BS and AC-CNS were used as filler in preparation of epoxy nanocomposites. Epoxy nanocomposites prepared at 1, 5 and 10 % activated carbons filler loading using KOH and H3PO4 chemical agents. Transmission electron microscopy confirms better dispersion of the nano-activated carbons in the epoxy matrix at 5 % activated carbon. The presence of 5 % AC-CNS in the epoxy matrix using H3PO4 chemical reagent resulted in an improvement of the thermal stability of epoxy matrix. KOH treated AC filled epoxy nanocomposites were slightly better in thermal stability as compared to H3PO4 treated AC filled epoxy nanocomposites, may be due to better interaction of filler with epoxy matrix. Thermal analysis results showed that thermal stability of the activated carbon filled epoxy nanocomposites improved as compared to the neat epoxy matrix. The degree of crystallinity of epoxy matrix was improved by adding the activated carbon due to interfacial interaction between AC and epoxy matrix rather than loading of AC alone. Developed nanocomposites from biomass (agricultural wastes) materials will help to reduce the overall cost of the materials for its demanding applications as insulating material.  相似文献   

6.
In this study, a previously unreported methodology is attempted to improve the inherent brittleness in diglycidyl ether of bisphenol-A based epoxy resin using hyperbranched polymers as toughening agents. Four different hyperbranched polyesters (HBPs) with increasing generations (1–4, denoted as HBP-G1 to HBP-G4) were synthesized by reacting calculated amount of dipentaerythritol (used as a core) and dimethylol propionic acid (AB2 type monomer) through pseudo one-step melt polycondensation method. The newly synthesized HBPs were characterized using spectral, thermal and physical measurements, which confirmed the formation of highly branched structure and decreasing thermal stability with increasing HBP generations. Further, toughening of the epoxy resin is carried out by reacting each generation of the HBP with epoxy using hexamethylene diisocyanate as an intermediate linkage resulting in the formation of HBP-Polyurethane/Epoxy-g-Interpenetrating Polymer Networks (HBP-PU/EP-g-IPNs). A linear polyol-PU/EP-g-IPN is also synthesized for the purpose of comparison. It is found that the HBP modified epoxy samples exhibited higher toughness in comparison to that of neat epoxy and linear polyol based epoxy samples. On the other hand, flexural properties, thermal stability and glass transition temperature of the modified samples is lower than neat epoxy sample due to the existence of flexible urethane linkages and decrease in the cross-linking density of epoxy matrix. The toughening characteristics exhibited by the HBPs are corroborated from the existence of heterogeneous morphology using SEM data.  相似文献   

7.
《中国化学会会志》2017,64(4):427-433
In this study, a carbon‐controllable hierarchical micro/mesoporous carbon–silica material derived from agricultural waste rice husk was easily synthesized and utilized as filler in an epoxy matrix for electronic packaging applications. Scanning electron microscopy, thermogravimetric analysis, and N2 adsorption/desorption isotherms were used to characterize the morphology, thermal stability, carbon content, and porous structural properties, respectively, of the as‐obtained carbon–silica material, namely rice husk char (RHC ). As a filler material, the uniformly dispersed RHC filler in the epoxy/RHC composite was easily prepared through hydrogen bonding of the silanol group of silica with the epoxy matrix. For electronic packaging applications, the thermal conductivity and thermomechanical properties (storage modulus and coefficient of thermal expansion) of the epoxy/RHC composites improved with increasing carbon content. Moreover, loading of the 40% RHC filler substantially enhanced the storage modulus of the epoxy/RHC composite (5735 MPa ) compared to the epoxy with 40% commercial silica filler (3681 MPa ). Considerable commercial potential is expected for the carbon–silica composite because of the simple synthesis process and outstanding performance of the prepared packaging material.  相似文献   

8.
A diglycidylether sulfone monomer (sulfone type epoxy monomer, SEP) was prepared from bis(4-hydroxyphenyl) sulfone (SDOL) and epichlorohydrin without any NaOH or KOH as basic catalyst. FT-IR, 1H NMR, 13C NMR and mass spectroscopic instruments were utilized to determine the structure of the SEP monomer. The cured SEP epoxy material exhibited not only a higher Tg (163.81 °C) but also a higher Tg than pristine DGEBA (from 111.25 °C to 139.17 °C) when the SEP monomer moiety had been introduced into the DGEBA system. The thermal stability of cured epoxy herein was investigated by thermogravimetric analysis (TGA). The results demonstrated that the sulfone group of the cured SEP material decomposed at lower temperatures and formed thermally stable sulfate compounds, improving char yield and enhancing resistance against thermal oxidation. Additionally, the IPDT and char yield of the cured SEP epoxy (IPDT = 1455.75, char yield = 39.67%) exceeded those of conventional DGEBA epoxy (IPDT = 667.27, char yield = 16.25%).  相似文献   

9.
Microcapsules containing phase change materials (microPCMs) have many potential applications because of their thermoregulation or thermosaving abilities. At the same time, it is still essential to understand the interface stability of microPCMs/polymer composites during a thermal transmission. The aim of this work was to fabricate novel microPCMs containing dodecanol by an in situ polymerization using methanol-modified melamine–formaldehyde (MMF) prepolymer as shell material and investigate the interface morphologies of microPCMs/epoxy composites treated by a simulant thermal process with a ten times repeated temperature variation. A series of microPCMs were fabricated by 1,000–3,000 r·min−1 emulsion speed with the PCM contents of 40–70%. The average diameter, melting temperature, and encapsulation efficiency of microPCMs were 1–16 μm, 19.5 °C, and 97.4%, respectively. Tests results indicated that the properties of the microPCMs were greatly affected by core/shell ratios and emulsification stirring rates of preparation conditions. With the increasing of stirring rates, the average diameters of microPCMs were sharply decreased. The encapsulation efficiency (E e) values of microPCMs increased with the increasing of stirring rates. The contents of PCM in microcapsules (C t) and the average diameter of microPCMs both affected the interface morphologies of microPCMs/epoxy composites after the repeated thermal treatments. Microcracks and gaps occurred after a thermal treatment in the interface of microPCMs and epoxy matrix obviously. The internal stress generated by the expansion or shrinking of the microPCMs was the main factor leading to the interface morphology changes and damaged of composites.  相似文献   

10.
The paper concerns thermal properties of epoxy/nanotubes composites for aircraft application. In this work, influence of carbon nanotubes on thermal stability, thermal conductivity, and crosslinking density of epoxy matrix was determined. Three kinds of nanotubes were used: non-modified with 1- and 1.5-μm length, and 1-μm length modified with amino groups. Scanning electron microscopy observations were done for examining dispersion of nanotubes in the epoxy matrix. Glass transition temperature (T g) was readout from differential scanning calorimetry. From dynamic mechanical analysis, crosslinking density was calculated for epoxy and its composites. Also, thermogravimetric analysis was done to determine influence of nanotubes addition on thermal stability and decomposition process of composites. Activation energy was calculated from TGA curves by Flynn–Wall–Ozawa method. Thermal diffusivity was also measured. SEM images proved the uniform dispersion of carbon nanotubes without any agglomerates. It was found that nanotubes modified with amino groups lead to the increase of epoxy matrix crosslinking density. The significant increase in T g was also observed. On the other hand, addition of carbon nanotubes leads to the decrease of thermal stability of polymer due to the increase of thermal diffusivity.  相似文献   

11.
Epoxy/clay nanocomposites with a high degree of exfoliation were achieved by intercalating liquid crystalline epoxy into clay intragallery as well as using a so-called ‘solution compounding’ process. In this process, clay modified was first treated with trichloromethane to form organoclay-trichloromethane suspension followed by liquid crystalline epoxy modification. The liquid crystalline epoxy grafted clay was then mixed extensively with epoxy to form epoxy/nanoclay composites. The mechanism of exfoliation was explored by monitoring the change of morphology of organoclay during each stage of processing with X-ray diffraction (XRD). The liquid crystalline epoxy grafted clay synthesised was characterised by fourier transform infrared spectroscopy (FT-IR) and polarising optical microscopy (POM). The clay platelets uniformly dispersed and highly exfoliated in the whole epoxy matrix were observed using transmission electron microscopy (TEM) and FT-IR imaging system. The epoxy nanocomposites were fabricated by incorporating different liquid crystalline epoxy grafted clay loading. The results revealed that the incorporation of liquid crystalline epoxy grafted clay resulted in a significant improvement in glass transition temperature (Tg) derived from dynamic mechanical analysis (DMA) and thermal stability measured by thermogravimetric analysis (TGA).  相似文献   

12.
In this study, the potential of recycled poly(ethylene terepthalate) (rPET) as a well‐defined reinforcing material for the in situ microfibrillar‐reinforced composite (iMFC) was investigated in comparison with that of liquid crystalline polymer (LCP). Each dispersed phase (LCP or rPET) was melt blended with high density polyethylene (PE) by using extrusion process. The rheological behavior, morphology, and the thermal stability of LCP/PE and rPET/PE blends containing various dispersed phase contents were investigated. All blends and LCP exhibited shear thinning behavior, whereas Newtonian fluid behavior was observed for rPET. The incorporation of LCP or rPET into PE significantly improved the processability. A potential of rPET as a processing lubricant by bringing down the melt viscosity of the blend system was as good as LCP. The elongated LCP domains were clearly observed in as‐extruded strand. Although the viscosity ratio of the rPET/PE system was lower than that of the LCP/PE blend system, most rPET domains appeared as small droplets. An addition of LCP and rPET into the PE matrix improved the thermal resistance significantly in air but not in nitrogen. The obtained results suggested the high potential of rPET as a processing aid and good thermally resistant material similar to LCP. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

13.
The unique polymeric silsesquioxane/4,4′-diglycidyether bisphenol A (DGEBA) epoxy nanocomposites have been prepared by sol-gel method. The structure of nanocomposites was characterized by attenuated total reflectance (ATR) and solid state 29Si NMR. The characteristic intensity of trisubstituted (T) structure was higher than that of tetrasubstituted (Q) structure from solid state 29Si NMR spectra of 3-isocyanatopropyltriethoxysilane (IPTS) modified epoxy. The activation energies of curing reaction of epoxy system and IPTS modified epoxy system are 28-66 kJ/mol and 57-75 kJ/mol, respectively, by Ozawa’s and Kissinger’s methods. The triethyoxysilane side chain of IPTS modified epoxy might interfere the curing reaction of epoxy/amine and increase the activation energy of curing. The thermal degradation of nanocomposites was investigated by Thermogravimetric analysis (TGA). The char yield of nanocomposites was proportional to the 2-(diphenylphosphino)ethyltriethoxysilane (DPPETES) moiety content at high temperature. A higher char content could inhibit thermal decomposition dramatically and enhance the thermal stability. Moreover, the nanocomposites possess high optical transparency.  相似文献   

14.
Two different multi-porous epoxy thermosets (MPETs), bi-functionality of DGEBA and tri-functionality of TGTPM, were prepared foremost for the interaction of template concentration and epoxy functionality under several physical properties. By performing an automated mercury porosimeter test, we found out template concentration was critical to the amount of voids/pores. Meanwhile, epoxy functionality decided the formation of porous structure through SEM. Comparing with TGTPM MPETs system, the DGEBA MPETs system with 20 wt% template displayed appreciable Tg and tan δ properties while the phenomenon exhibited higher thermal stability property. Additionally, thermal conductivity patterns show the DGEBA MPETs system is a remarkable material of thermal resistance. However, it reduces optical clarity, dielectric permittivity and mechanical strength according to the UV-visible spectroscopy, LCR meter, and DMA, normally. Therefore, we can understand that template concentration and epoxy functionality are key factors of physical degradation and stability in porous epoxy materials.  相似文献   

15.
The curing characteristics of carboxylic functionalized glucose resin (glucose maleic acid ester vinyl resin: GMAEV) and epoxy resin have been studied using DSC and FTIR methods. Exothermic reactions attributed to esterification and etherification reactions of the hydroxyl and carboxyl functionalities of GMAEV with the epoxy groups were identified. Exothermic reactions showed very different patterns according to the degree of carboxyl group substituent of GMAEV. The results showed that esterification reaction occurs in the early stage of cure and then etherification followed after completion of the esterification. A cured matrix containing epoxy resin and 50 wt.% of GMAEV was prepared and characterized. The cured matrix showed thermal stability up to 300 °C. The average glass transition temperature and storage modulus of the matrix were as high as 95 °C and 2700 MPa, respectively. The cured matrix of epoxy resin and GMAEV with higher degree of carboxyl group was found to have a lower density due to the formation of bulky groups in the crosslinks.  相似文献   

16.
Composites based on conductive organic/inorganic fillers dispersed in insulating matrix have been widely investigated because of their widespread applications such as electromagnetic shielding, electrostatic discharge, and sensors. In this context, novel composite materials based on epoxy resin matrix charged with polyaniline (PANI)‐doped para‐toluene sulfonic acid were elaborated. Fourier transform infrared spectroscopy, X‐ray diffraction and scanning electron microscopy were used to check the structure and the morphology of the samples. Viscoelastic behavior and thermal stability of the composites were explored by dynamic mechanical thermal analysis and thermogravimetric analysis. It was shown that the PANI particles exhibited a partial crystalline structure and were homogeneously dispersed in epoxy matrix. Consequently, this structure affected the thermal stability and viscoelastic properties of the composites. Furthermore, the dielectric and electrical properties were investigated up to 1 MHz. Measurements of dielectric properties revealed that with loading fillers in matrix, the dielectric parameters increased to high values at low frequency then decreased at values around 40 and 32 of real and imaginary parts, respectively, at 1 MHz with 15% of PANI content. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

17.
Uniform dispersion of graphene nanosheets (GNS) in a polymer matrix with strong filler–matrix interfacial interaction, preserving intrinsic material properties of GNS, is the critical factor for application of GNS in polymer composites. In this work, a novel reactive copolymer VCz–GMA containing carbazole and epoxide group was designed, synthesized and employed to noncovalently functionalize GNS for preparing epoxy nanocomposites with enhanced mechanical properties. The presence of carbazole groups in VCz–GMA enables the tight absorption of copolymer on to graphene surface via π–π stacking interaction, as evidenced by Raman and fluorescence spectroscopy, whereas the epoxide segments chemically reacts with the epoxy matrix, improving the compatibility and interaction of graphene with epoxy matrix. As a result, the VCz–GMA–GNS/epoxy composite showed a remarkable enhancement in both mechanical and thermal property than either the pure epoxy or the graphene/epoxy composites. The incorporation of 0.35 wt % VCz–GMA–GNS yields a tensile strength of 55.72 MPa and elongation at break of 3.45, which are 42 and 191% higher than the value of pure epoxy, respectively. Increased glass transition temperature and thermal stability of the epoxy composites were also observed. In addition, a significant enhancement in thermal conductivity was achieved with only 1 wt % VCz–GMA–GNS loading. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015 , 53, 2776–2785  相似文献   

18.
Novel microcapsules (MCs) with organic/inorganic hybrid shell were successfully fabricated using epoxy resin as core material and nano boron nitride (BN) and mesoporous silica (SBA‐15) as inorganic shell materials in aqueous solution containing a water‐compatible epoxy resin curing agent. The morphologies, thermal properties and Young's moduli of MCs were investigated. The results indicated that epoxy resins were encapsulated by BN/SBA‐15/epoxy polymer hybrid layer, the resulting MCs were spherical in shape and the introduction of inorganic particles made MCs had rough surface morphology. The mean modulus value of MCs was from 2.8 to 3.1 GPa. The initial decomposition temperature (Tdi) of MCs at 5 wt% weight loss was from 309 to 312°C. MCs showed excellent thermal stability below 260°C. The structures and properties of MCs could be tailored by controlling the weight ratio of inorganic particle. When the weight ratio of BN to SBA‐15 was 0.15:0.10, MCs had the highest Tdi and modulus. The resulting MCs were applied to high performance 4,4′‐bismaleimidodiphenylmethane/O,O′‐diallylbisphenol A (BMI/DBA) system to design high performance BMI/DBA/MC systems. Appropriate content of MCs could improve the fracture toughness and maintain the glass transition temperature (Tg) of BMI/DBA system. The core materials released from fractured MCs could bond the fracture surfaces of the BMI/DBA matrix through the polymerization of epoxy resins. When the healing temperature schedule of 100°C/2h+150°C/1h was applied, 15 wt% MCs recovered 98% of the virgin fracture toughness of BMI/DBA. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

19.
Siliconized epoxy matrix resin was developed by reacting diglycidyl ethers of bisphenol A (DGEBA) type epoxy resin with hydroxyl terminated polydimethylsiloxane (silicone) modifier, using γ-aminopropyltriethoxysilane crosslinker and dibutyltindilaurate catalyst. The siliconized epoxy resin was cured with 4, 4-diaminodiphenylmethane (DDM), 1,6-hexanediamine (HDA), and bis (4-aminophenyl) phenylphosphate (BAPP). The BAPP cured epoxy and siliconized epoxy resins exhibit better flame-retardant behaviour than DDM and HDA cured resins. The thermal stability and flame-retardant property of the cured epoxy resins were studied by thermal gravimetric analysis (TGA) and limiting oxygen index (LOI). The glass transition temperatures (Tg) were measured by differential scanning calorimetry (DSC) and the surface morphology was studied by scanning electron microscopy (SEM). The heat deflection temperature (HDT) and moisture absorption studies were carried out as per standard testing procedure. The thermal stability and flame-retardant properties of the cured epoxy resins were improved by the incorporation of both silicone and phosphorus moieties. The synergistic effect of silicone and phosphorus enhanced the limiting oxygen index values, which was observed for siliconized epoxy resins cured with phosphorus containing diamine compound.  相似文献   

20.
Hybrids containing silicon, phosphorous and nitrogen were prepared by the sol-gel method and compared with pure epoxy. The silicon, phosphorous and nitrogen components were successfully incorporated into the networks of polymer. Thermogravimetric analysis (TGA) was used for rapid evaluation of the thermal stability of different materials. The integral procedure decomposition temperature (IPDT) has been correlated the volatile parts of polymeric materials and used for estimating the inherent thermal stability of polymeric materials. The IPDT of pure epoxy was 464 °C and the IPDTs of hybrids were higher than that of pure epoxy. The thermal stability of hybrids increased with the contents of inorganic components. The inorganic components can improve the thermal stability of pure epoxy.Two methods have been used to study the degradation of hybrids containing silicon, phosphorous and nitrogen hybrid during thermal analysis. These investigated methods are Kissenger, Ozawa's methods. The activation energies (Ea) were obtained from these methods and compared. It is found that the values of Ea for modified epoxy hybrids are higher than that of pure epoxy. The hybrids of high activation energy possess high thermal stability.  相似文献   

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