This study provides a route to prepare 4-arm star poly(methyl methacrylate) (4sPMMA)/PMMA grafted SiO2 (PMMA-g-SiO2) hybrid nanocomposites that can be used as 3D printing material and filler for dental materials. First, 4sPMMA was synthesized via atom transfer radical polymerization with low metal catalyst concentration. Modified colloidal silica nanoparticles (MCSPs) were synthesized by grafting 3-methoxypropyl trimethoxysilane (MPS) onto the surface of colloidal silica nanoparticles (CSPs) and then dispersed in the solution of methyl methacrylate monomer in dioxane. The mixture of 4sPMMA and MCSPs solutions was degassed and replaced in an oil bath at 70–75°C; the reaction was continued with α,α′-azobis(isobutyronitrile) as an initiator for 24 h to form 4sPMMA/PMMA-g-SiO2 hybrid nanocomposites. Viscosity measurement showed that viscosity of the hybrid was increased with increasing MPS loading used in modification of CSPs, which verified that PMMA had been grafted onto MCSPs. Fourier transform infrared spectra of the hybrid nanocomposites demonstrated the strong molecular interaction between MCSPs and polymer matrix, and 1H NMR spectra confirmed the formation of PMMA-g-SiO2. Field emission scanning electron microscopy and transmission electron microscopy images revealed that MCSPs were well dispersed in polymer matrix with the size of about 20–30 nm. Thermal stability of the hybrid nanocomposites was improved compared with PMMA made from free radical polymerization.
The flame‐retardant low‐density polyethylene (LDPE) composites loading aluminum hydroxide (ATH), red phosphorus (RP), and expandable graphite (EG) were successfully prepared. The flame retardancy, the thermo‐oxidative stability, and the mechanical property of the composites were investigated. The synergistic effect of ATH, RP, and EG on the flame‐retardant property and thermal behavior of LDPE were observed. The limiting oxygen index value of LDPE significantly increased from 17.1% to 25.4% upon the incorporation of 15 wt.% of the mixture of three fillers with ATH:RP:EG mass ratio of 1:1:1; and this composite achieved the V‐0 classification of the UL94 vertical burning test. The thermogravimetric analysis of this composite under air atmosphere revealed that its residue weight remained 27.89% at 900°C. Furthermore, the results of tension tests indicated that the surface modification of ATH by magnesium stearate and RP by poly(methylhydrosiloxane) noticeably improved the tensile strength and the elongation of the composite.
In this study, vinyltrimethoxysilane-treated hydroxyapatite (vHAP) and PMMA-grafted HAP (gHAP) were successfully prepared from original HAP (oHAP). Three kinds of HAP (oHAP, vHAP and g HAP) were used as additives for the preparation of three groups of HAP-modified PMMA bone cements (oHAP-BC, vHAP-BC and gHAP-BC). The setting, bending and compression properties of the bone cements were conducted according to ISO 5833:2002. The obtained results showed that the maximum temperature while curing the HAP-modified bone cements (HAP-BCs) decreased from 64.9 to 60.8 °C and the setting time increased from 8.1 to 14.0 min, respectively, with increasing HAP loading from 0 to 15 wt.%. The vHAP-BC and gHAP-BC groups exhibited higher mechanical properties than the required values in ISO 5833. Electron microscopy images showed that the vHAP and gHAP nanoparticles were dispersed better in the polymerized PMMA matrix than the oHAP nanoparticles. FTIR analysis indicated the polar interaction between the PO4 groups of the HAP nanoparticles and the ester groups of the polymerized PMMA matrix. Thermal gravimetric analysis indicated that mixtures of ZrO2/HAPs were not able to significantly improve the thermal stability of the HAP-BCs. DSC diagrams showed that the incorporation of gHAP to PMMA bone cement with loadings lower than 10 wt.% can increase Tg by about 2.4 °C.
In this article, we present a study on the properties of ethylene vinyl acetate copolymer/silica nanocomposites prepared in absence and presence of EVA-g-maleic anhydride as a compatibilizer between silica nanoparticles and ethylene vinyl acetate matrix. A series of ethylene vinyl acetate/silica nanocomposites with different contents of silica nanoparticles were prepared by solution method. EVA-g-maleic anhydride with 0.5 wt% maleic anhydride groups was added to all ethylene vinyl acetate/silica nanocomposites. Fourier transform infrared, field emission scanning electron microscopy, rheology behavior, and thermogravimetry analysis were used to characterize the structure, morphology, rheological, and thermal properties of the nanocomposites, respectively. The Fourier transform infrared spectra and field emission scanning electron microscopy micrographs showed that the hydroxyl groups on the surface of silica nanoparticles interact with maleic anhydride groups in EVA-g-maleic anhydride and lead to a finer dispersion of individual silica nanoparticles in the ethylene vinyl acetate matrix. The rheological properties and thermal stability of ethylene vinyl acetate/silica nanocomposites were significantly increased after adding EVA-g-maleic anhydride into the nanocomposites. Mechanical properties including tensile strength and elongation at break of the nanocomposites were mainly affected by the content of silica nanoparticles. For the tensile strength as well as elongation at break of the nanocomposites, a maximum value was observed at the content of 0.5 wt% of silica nanoparticles. The addition of EVA-g-maleic anhydride into ethylene vinyl acetate/silica nanocomposites resulted in a further improvement of mechanical properties of the nanocomposites.
This study presents the qualitative and quantitative analyses of Fourier Transform Infrared (FTIR) spectra of poly(methyl methacrylate)/poly(vinyl chloride) blends (PMMA/PVC), as well as PVC-g-PMMA graft copolymers. Graft copolymerizations of methyl mathacrylate (MMA) onto PVC macromolecules were carried out mixture of cyclohexanone/N,N-dimethylformamide as solvents, dibenzoyl peroxide as initiator and nitrogen medium. FTIR spectra of PMMA/PVC blends showed that there were molecular interactions between C=O groups of PMMA and C-Cl groups of PVC. Assignments of infrared absorption bands for specific groups of PMMA/PVC blends have been contributed. Using regression method, linear calibration curve between PMMA mole content and peak areas of C=O groups in FTIR spectra of the blends has been found when C=O peak areas were multiplied by an appropriate factor. PMMA grafted content and total PMMA formed content in PVC-g-PMMA graft copolymers have been evaluated. The results showed that grafted PMMA content was increased since PVC was initiatly dechlorinated by NaOH solution. The grafted PMMA content and total formed PMMA content were 5.05 wt.% and 11.25 wt.% respectively when MMA monomers were grafted onto neat PVC and modified PVC molecules.
Here we report a facile approach to enhance the dispersibility of ethylene vinyl acetate copolymer (EVA)/silica nanocomposites (for the EVA/silica nanocomposites and interaction between silica nanoparticles (nanosilica) and EVA by adding EVA-g-acrylic acid (EVAgAA) as a compatibilizer, which was formed by grafting acrylic acid onto EVA chains with the aid of dicumyl peroxide). The above nanocomposites with and without EVAgAA were prepared by melt mixing in a Haake intermixer with different contents of silica and EVAgAA. Their structure and morphology were characterized by Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FE-SEM), and the mechanical, rheological, dielectrical, and flammability properties of the nanocomposites were also investigated. The FT-IR spectra of the nanocomposites confirmed the formation of hydrogen bonds between the surface silanol groups of nanosilica and C=O groups of EVA and/or EVAgAA. The presence of EVAgAA remarkably increased the intensity of hydrogen bonding between nanosilica and EVA which not only enhanced the dispersion of nanosilica in EVA matrix but also increased the mechanical, viscosity and storage modulus of EVA/silica nanocomposites. In addition, the flammability of EVA/silica nanocomposites is also significantly reduced after the functionalization with EVAgAA. However, the mechanical properties of EVA/silica nanocomposites tended to level off when its content was above 1.5 wt.%. It has also been found that the dielectric constant value of the EVA/EVAgAA/silica nanocomposites is much lower than that of the EVA/silica nanocomposites, which is another evidence of the hydrogen bonding formation between EVAgAA and nanosilica.
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