Effect of Filler Treatment on Crystallization,Morphology and Mechanical Properties of Polypropylene/Calcium Carbonate Composites

Pimelic acid (PA) was used as a new surface modifier for CaCO₃. The effects of PA treatment on the crystallization, morphology, and mechanical properties of PP/CaCO₃ composites were investigated. Fourier transform infrared (FTIR) spectroscopy analysis revealed that PA bonded to CaCO₃ and formed a calcium pimelate surface layer after reacting with CaCO₃. The results of wide angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), and polarized light microscopy (PLM) proved that the PA treated CaCO₃ induced a large amount of β -iPP and decreased the spherulitic size of PP. The results of scanning electron microscopy (SEM) showed that the PA treatment enhanced the interfacial adhesion between the filler and the matrix, indicating the improvement of the compatibility between PP and CaCO₃. The toughness of the composites was improved by the more ductile β -form spherulites. When 1% of PA treated CaCO₃ was added, the notched impact strength reached its maximum, a value of 19.79 kJ/m², which was 3.64 times greater than that of the pure PP.     

Effect of Inorganic Fillers on Morphology and Mechanical Properties of PA66/POE-g-MAH/Filler Composites

Composites of polyamide 66 (PA66)/maleic anhydride grafted poly(ethylene-co-octene) (POE-g-MAH)/nano-calcium carbonate (nano-CaCO₃) and PA66/POE-g-MAH/talc were prepared by a one-step blending method. Morphology, crystallization, and mechanical properties of the composite materials were characterized with respect to different amounts of both inorganic fillers, nano-CaCO₃ and talc. Results showed that the tensile yield strength and tensile modulus of the composites were increased remarkably with introduction of nano-CaCO₃ or talc, but the notched impact strength was significantly lowered for both kinds of composites. Mechanical properties exhibited little difference between the PA66/POE-g-MAH/nano-CaCO₃ and PA66/POE-g-MAH/talc composites both for the different shapes and sizes of nano-CaCO₃ and the flake-like talc. Results of scanning electron microscopy exhibited agglomeration of the fillers. Differential scanning colorimetry analysis suggested that introduction of the inorganic fillers cause the crystallinity of PA66 to decrease by heterogeneous nucleation. The study provides a basic investigation on polymer/elastomer/rigid filler composites.     

Effect of an In-Situ Nucleating Agent on the Polymorphs and Mechanical Properties of Isotactic Polypropylene

The influence of glutaric acid (GA)/cadmium hydroxide [Cd(OH)₂] mixtures on the crystallization and properties of isotactic polypropylene (iPP) was investigated by means of differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), polarized light microscopy, and mechanical tests. It was found that the β-crystalline form was produced in the samples containing 0.15 wt% GA and more than 0.17 wt% Cd(OH)₂. The content of β-crystalline form was maximum, i.e. K_DSC = 65.4% and K_WAXD = 71.4%, when the sample was doped with GA (0.15 wt%)/Cd(OH)₂ (0.20 wt%) (the molar ratio of GA:Cd(OH)₂ was 1:1.2). It was also found that GA/Cd(OH)₂ mixtures not only induced the β-crystalline form but also made spherulites smaller. The results of mechanical tests showed that the toughness of iPP was greatly improved by bicomponent nucleator, while the stiffness decreased a little. Fourier transform infrared spectroscopy analysis indicated that an “in-situ” chemical reaction occurred between GA and Cd(OH)₂ during melt blending, yielding an effective β nucleator (cadmium glutarate).     

Mechanical Properties and Morphology of Polypropylene/Polypropylene-g-Maleic Anhydride/Long Glass Fiber Composites

Long glass fiber (LGF)-reinforced polypropylene (PP) was prepared using a self-designed impregnation device. The effect of dicumyl peroxide (DCP) and maleic anhydride (MA) content on the compatibilizer, PP grafted with maleic anhydride (PP-g-MA), was investigated by means of scanning electron microscopy (SEM) and mechanical properties. The experimental results demonstrated that the increase of DCP and MA could effectively improve the interfacial interaction between PP and GF. Good interfacial adhesion between PP and GF in PP/ PP-g-MA /LGF composites was observed from SEM studies for the higher contents of MA. The best mechanical properties of PP/ PP-g-MA /LGF(30%) composites were obtained when the content of DCP and MA were 0.4 and 0.8 wt%, respectively. The storage modulus of the PP/PP-g-MA/LGF composites increased and then decreased with the content of MA. When the content of MA was 0.8 wt%, tan δ had the lowest value, indicating that the corresponding composites had the best compatibility.     

Morphology,Nonisothermal Crystallization Behavior and Mechanical Properties of Polypropylene Modified by Ionomers

The morphology and nonisothermal crystallization behavior of polypropylene modified by ionomers based on ethylene copolymers (Surlyn 8920 and 9320) were investigated by using scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The crystallization rate of polypropylene was accelerated by the ionomers which initiated heterogeneous nucleation of the polypropylene. At low ionomers content (0.25 wt%), Surlyn 8920, neutralized by sodium, was more efficient to enhance the crystallization rate of polypropylene than Surlyn 9320 (neutralized by zinc). The crystallization process of polypropylene modified by the ionomers was analyzed by different kinetics models. The study showed that the Mo approach was applicable for this system, whereas the Avrami, Jeziorny, and Ozawa methods were not. Furthermore, the notched impact strength of polypropylene modified by the ionomers was increased without any reduction of tensile strength and flexural modulus.     

Steady Shear Rheological Behavior,Mechanical Properties,and Morphology of the Polypropylene/Carbon Nanotube Nanocomposites

Nanocomposites based on polypropylene (PP) and multiwall carbon nanotubes (MWNT) have been prepared through melt blending. Scanning electron microscopy (SEM) observations indicate that nanotubes were dispersed almost homogeneously throughout the matrix; however, some aggregates were also observed at high nanotubes loading. Rheological studies showed that at low shear rates, there is an increase in steady shear viscosity and shear stress of samples with increasing of nanotubes concentration. However, at high shear rates nanocomposites behave like pure PP. The activation energy of flow showed an increasing trend and has a maximum at 1wt% MWNT content. It was found that incorporation of nanotubes causes a remarkable decrease in surface and volume resistivity values of the polymeric matrix. The presence of CNTs improved the tensile and flexural properties of the polymeric matrix.     

Effect of β-Nucleating Agent on the Crystallization,Mechanical Properties,and Heat Resistance of Injection-Molded Isotactic Polypropylene

Injection-molded β-isotactic polypropylene (β-iPP) was prepared with a commercial β-nucleating agent (NT-A). The effect of NT-A on the crystallization, mechanical properties, and heat resistance of β-iPP was investigated by differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), polarized light microscopy (PLM), and mechanical and heat deflection tests. DSC and WAXD analysis showed that the content of β-crystals in the nucleated iPP was higher than that of pure iPP, and the content of β-crystals of the core was higher than that of the skin. PLM observations showed that injection-molded iPP had an obvious skin-core structure. NT-A induced abundant β-crystals and resulted in small spherulites which improved the Izod notched impact strength. When the content of NT-A was 0.075wt%, the Izod notched impact strength reached a maximum, 2.6 times more than that of pure iPP. The heat distortion temperature was also improved by NT-A.     

Influence of the Polymer/Inorganic Filler Interface on the Mechanical,Thermal, and Flame Retardant Properties of Polypropylene/Magnesium Hydroxide Composites

The relationship between the interface structure and the macroscopic properties of composites composed of isotactic polypropylene (iPP) and magnesium hydroxide (MH) was investigated with a focus on mechanical properties, thermal stability, and flame retardancy. Surface treatment of MH was carried out using dodecanoic acid (DA) and dodecylphosphate (DP), both of which interacted with MH to form submonolayer coverages. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) revealed that both organic reagents adhere to the MH surface via ionic interactions. Even low amounts of organic reagents on the MH surface were sufficient to improve the mechanical, thermal, and flame retardant properties of the composites. The incorporation of 1.8 wt% of DP in (70/30) iPP/MH-DP composite decreased the peak heat release rate (PkHRR) to 39% compared with that of neat iPP. Since the effects of DA with the same dodecyl chains were not significant, it is concluded that the phosphate groups in DP provide flame retardancy.     

Effect of Surface Structure of Nano-CaCO3 Particles on Mechanical and Rheological Properties of PVC Composites

To study the effect of different surface structures on resultant mechanical and rheological properties, nano-CaCO₃ particles were treated with isopropyl tri-stearyl titanate (H928), isopropyl tri-(dodecylbenz-enesulfonyl) titanate (JN198), and isopropyl tri-(dioctylpyrophosphato) titanate (JN114). Scanning electron microscopy (SEM) and dynamic mechanic analysis (DMA), carried out to characterize the effective interfacial interaction between the nano-CaCO₃ particles and a poly(vinyl chloride) (PVC) matrix, indicated that JN114 treated nano-CaCO₃ particles had the strongest interfacial interaction with a PVC matrix, while H928 treated nano-CaCO₃ had the weakest. The rheological and mechanical properties of PVC/nano-CaCO₃ composites were investigated as a function of surface structure and filler volume fraction. The tensile yield stress and elongation at break decreased with the increasing of calcium carbonate content while tensile modulus increased. PVC filled with JN114 treated nano-CaCO₃ had the highest tensile modulus and tensile yield stress, while those filled with H928 treated nano-CaCO₃ had the highest elongation at break at the same filler content. The impact strength of PVC/nano-CaCO₃ composites increased with the increasing of CaCO₃ content, and PVC composites filled with JN198 treated nano-CaCO₃ particle had a higher impact strength than those with JN114 or H928 treated, with the value reaching 23.9 ± 0.7 kJ/m² at 11 vol% CaCO₃, four times as high as that of pure PVC. Rheological properties indicated that a suitable interfacial interaction and a good dispersion of inorganic filler in a PVC matrix could reduce the viscosity of PVC/nano-CaCO₃ composites. The interfacial interaction was quantitatively characterized by semiempirical parameters calculated from the tensile strength of PVC/nano-CaCO₃ composites to confirm the results from the SEM and DMA experiments.     

Thermal and Flammability Properties of Polypropylene/Silica Aerogel Composites

Polypropylene (PP)/silica aerogel (SA) composites were prepared and their thermal and flammability properties were studied. The PP/SA composites with different weight percent were prepared via melt compounding method using an internal mixer. Their morphology, thermal conductivity, thermal stability and combustion behavior were characterized. The SEM images confirmed the homogenous mixing of the components. The measurement of the thermal conductivities of samples indicated that PP would be a better thermal barrier in the presence of SA. The thermal gravimetric analysis results showed that combining the silica aerogel particles into polypropylene increased the decomposition temperature. The resultant composites displayed improved flame retardancy with a significant reduction in the peak heat release rate and increase of limited oxygen index value. It can be concluded that the flame retardant mechanism of PP/SA composites is associated with two decisive factors: a coat-like char effect and a physical crosslinking effect.     

The Crystallization and Morphology of Isotactic Polypropylene Nucleated by Magnesium Sulfate Whiskers Surface Modified by Pimelic Acid

Pimelic acid (PA) was used to modify the surface of magnesium sulfate whiskers (M-HOS). The treated M-HOS and its effects as a function of concentration on the crystallization and morphology of isotactic polypropylene (iPP) were investigated. Scanning electron microscopy (SEM), wide-angle X-ray diffraction (WAXD), thermogravimetic analysis (TGA), and Fourier transform infrared spectroscopy (FTIR) revealed that PA reacted with M-HOS and formed magnesium pimelate on the surface after the reaction. The results of differential scanning calorimetry (DSC) and polarized light microscopy (PLM) showed that the treated M-HOS had the ability to induce β-spherulites, increase the crystallization temperature and decrease the size of spherulites in iPP. It was the most effective to form β-spherulites when the content of PA treated M-HOS was 5 wt%.     

Mechanical Properties and Rheological Behavior of Dynamically Vulcanized Trans-Polyisoprene/Polypropylene Blends

The degree of dynamic vulcanization, mechanical properties, rheological behavior, and the ageing-resistant performance of thermoplastic vulcanizates (TPVs) based on Trans 1,4-polyisoprene/polypropylene (TPI/PP) blends with the blend ratios of 70/30, 60/40, and 50/50 were investigated. The results showed that TPI fully dynamically vulcanized in the Haake mixer chamber when mixed with PP, and the specimen with the blend ratio 70/30, for the same sulfur content in all samples, had the lowest cross-linking degree of the TPI phase. The shear viscosity of TPI/PP-TPVs dropped as the shear rate increased and the specimen with the blend ratio 70/30 had a relatively greater shear viscosity in the region of shear rates less than 1000 s^?1. With the antiageing agent Vulkanox 4020 NA (Bayer) added, all the TPI/PP-TPVs showed good ageing characteristics, and the specimen with the blend ratio 70/30 possessed the best mechanical properties.     

Microstructural Evolution and Its Effect on Mechanical Properties of Isotactic Polypropylene by Shear Plastic Deformation at Elevated Temperatures

Isotactic polypropylene (iPP) was plastically shear deformed by equal channel angular extrusion (ECAE) at extrusion temperatures varied from 45 to 125°C (25 mm/min). The evolutions of morphology and crystal orientation were studied by reflected optical microscopy (ROM), scanning electron microscopy (SEM), and X-ray diffraction. It was found that the original spherulites were deformed into nearly ellipsoids with their long axis tilted at an angle away from the flow direction. Azimuthal scanning results revealed that two preferred crystal orientations were formed after ECAE. The crystal plasticity was activated by increasing the extrusion temperature, followed by fast rotation of crystallites toward the shear direction. The thermal mechanical analysis (TMA) indicated that low extrusion temperature was favorable to fix the molecular orientation. The iPP samples processed at the investigated temperatures displayed a significant increase in the impact strength, especially for those extruded at 45°C and 65°C. The tensile results revealed a greater elongation at break in the samples deformed at low temperatures (45°C and 65°C) but not in those deformed at high temperatures (85°C or above).     

Effect of Carbon Nanotubes on the Mechanical Properties of Polypropylene/Wood Flour Composites: Reinforcement Mechanism

Maleic anhydride grafted polypropylene (PP-g-MA) was employed as the compatibilizer and carbon nanotubes (CNTs) or hydroxylated CNTs as reinforcements for polypropylene/wood flour composites. The results showed that when the PP-g-MA loading level was 10 wt%, the bending strength, tensile strength, Izod notched impact strength, and elongation at break of PP-wood composites were enhanced by 85% (66.3 MPa), 93% (33.7 MPa), 5.8% (2.01 kJ/m²), and 64% (23%), respectively, relative to the uncompatibilized composites. The introduction of pristine CNTs only improved slightly the overall mechanical properties of the compatibilized composites due to poor interfacial compatibility. Unlike CNTs, incorporating hydroxylated CNTs (CNT-OH) could significantly improve all of the mechanical properties; for instance, at 0.5 wt% CNT-OH loading, the flexural strength and tensile strength reached 68.5 MPa, and 40.4 MPa about 6.6% higher than that for the composites with the same CNT loading. Furthermore, CNT-OH also remarkably enhanced the storage modulus. Contact angle and morphology observations indicated that the increases in mechanical properties could be attributed to the improvements of interfacial interactions and adhesions of CNTs with the matrix and fillers.     

The Morphology and Mechanical Properties of Isotactic Polypropylene Injection-Molded Samples with the Presence of β-Nucleation Agent and Periodical Shear Field

The pressure vibration injection molding (PVIM) method was used to prepare β-nucleated isotactic polypropylene samples (PVIM β-iPP samples); a relatively low, periodical shear was imposed on the polymer melt in the mold at the filling and packing stages. The crystal structures and crystal orientation of the PVIM β-iPP samples were investigated by polarizing light microscopy (PLM), scanning electron microscopy (SEM), and synchrotron two-dimensional wide-angle X-ray diffraction (2D-WAXD). The PLM observations indicated that a cylindrite layer, rather than the transition layer, was found in PVIM β-iPP samples, which is different from the conventional injection-molded (CIM) samples. In addition, the thickness of the oriented layer of the PVIM samples was obviously greater than that of the CIM samples. The SEM observations demonstrated that a large amount of shish-kebab structures appeared in the shear layer of the PVIM β-iPP samples; at the same time, numerous β-spherulites were formed in the core layer. The 2D-WAXD data indicated that orientation homogeneity, to some degree, could be obtained by the periodical shear during PVIM. As a result, the above-mentioned morphology of the PVIM β-iPP samples leads to potentially useful prominent reinforcement and toughening of the material.     

Phase Structure,Thermal, and Mechanical Properties of Polypropylene/Hollow Glass Microsphere Composites Modified with Maleated Poly(ethylene-octene)

Maleated poly(ethylene-octene) (POE-g-MAH), as a compatilizer and toughener, was incorporated in polypropylene/hollow glass microspheres (PP/HGM) binary composites, and the phase structure and thermal and mechanical properties of these composites were investigated. Scanning electron microscopy analysis indicated that the phase structure of ternary composites could be controlled by POE-g-MAH and the surface treatment of HGM. Fourier transform infrared spectroscopy revealed that there was an amidation reaction between the treated HGM and POE-g-MAH during melt compounding. Differential scanning calorimetry suggested that the crystallization and melting behaviors of ternary composites were influenced by phase structure. Evaluation of mechanical properties showed that the amide linkage between the treated HGM and POE-g-MAH was favorable for improving the properties of ternary composites.     

Structure and Properties of Glass Fiber Reinforced Polypropylene/Liquid Crystal Polymer Blends

A liquid crystal polymer (LCP) was used to improve the physical properties of glass fiber reinforced polypropylene (GFRPP). The LCP was beneficial to improve the mechanical and heat resistant properties of the GFRPP/LCP composite. Compared with the GFRPP with 30% (w%) glass fiber (GF), the yield strength and the impact strength for the GFRPP/LCP composites increased by 62.7% and 18.1%, respectively, with a 6.8°C increase in the Vicat softening temperature for a 5% LCP addition to the GFRPP composites. The crystallinity of the polypropylene (PP) matrix for the GFRPP/LCP composites increased for 5% LCP and then decreased with increasing the LCP content. The γ-phase crystals for the PP matrix occurred in the shear layer of the injection molded GFRPP/LCP samples. The improved adhesion interface between the GF and the PP matrix was beneficial to reinforce and toughen the GFRPP/LCP composites with a small addition of the LCP.     

Comparison of Mechanical Properties and Rheological Behavior of Trans-Polyisoprene/Polypropylene and Ethylene Propylene Diene Rubber/Polypropylene Thermoplastic Vulcanizates

The degree of dynamic vulcanization, mechanical properties, rheological behavior, and the ageing-resistant performance of trans 1,4-polyisoprene (TPI)/polypropylene (PP) and ethylene propylene diene rubber (EPDM)/PP thermoplastic vulcanizates with a blend ratio of 60/40 were investigated comparatively. The results showed that TPI had fully dynamically vulcanized when mixed with PP in the Hakke mixer chamber (175°C, 60 rpm) while EPDM had only partly dynamically vulcanized due to its saturated main chain backbone. With increased sulfur content, the torque at the end of the curing curves of the two thermoplastic vulcanizates (TPVs) increased in the curing characteristics measuring process as the degree of crosslinking increased. Comparing the two blends, TPI/PP-TPVs were possessed of a better mobility, a little lower tensile strength and tear strength, a little higher 100% modulus and hardness, and much lower elongation at break. EPDM/PP-TPVs had better ageing-resistant characteristics due to EPDM's saturated main chain backbone.     

Mechanical Properties and Tensile Deformation Behavior of Polyamide 6/Maleated and Unmaleated Ethylene Propylene Diene Terpolymer/Nano-CaCO3 Ternary Composites

Ternary composites composed of polyamide 6 (PA6), a mixture of maleated (EPDM-g-MA) with unmaleated ethylene propylene diene terpolymer (EPDM) rubber at weight ratio 80/20 (defined as EPDM-M), and nano-calcium carbonate (nano-CaCO₃) were prepared by a two-step compounding route. Sandbag microstructure, in which nano-CaCO₃ agglomerates were embedded EPDM-M, were observed by scanning electron microscopy (SEM). Deformation of the composites was studied by video-aided tensile tests during uniaxial tension. The microstructural morphology and interfacial interaction were investigated through SEM and dynamic mechanical analysis (DMA). Compared to PA6/EPDM-M/nano-CaCO₃ ternary composites without sandbag microstructure (E2), the microstructural morphology of PA6/EPDM-M/nano-CaCO₃ ternary composites with sandbag microstructure (E3) showed that numerous microfibrils and cavitations were formed by simultaneously stretching and debonding of nano-CaCO₃ agglomerates and EPDM-M in the sandbag microstructure, which resulted in a higher volume strain and larger quantity of energy dissipation. Additionally, better interfacial interaction between the sandbag microstructure and PA6 matrix in E3 caused a lower α-relaxation temperature and easier external energy transmission than E2 without sandbag microstructure. Consequently, the presence of the sandbag particles in PA6/EPDM-M/nano-CaCO₃ ternary composites changed the tensile yield deformation of PA6 from a more deviatoric plasticity to a more dilatational plasticity.     

Effect of Polyethylene Functionalization on Mechanical Properties and Morphology of PE/SiO2 Composites

In this study composites of high density polyethylene (HDPE) with various SiO₂ content were prepared by melt compounding using maleic anhydride grafted polyethylene (PE-g-MAH) as a compatibilizer. The composites containing 2, 4 and 6% by weight of SiO₂ particles were melt-blended in a co-rotating twin screw extruder. In all composites, polyethylene-graft-maleic anhydride copolymer (PE-g-MAH, with 0.85% maleic anhydride content) was added as a compatibilizer in the amount of 2% by weight. Morphology of inorganic silica filler precipitated from emulsion media was investigated. Mechanical properties and composite microstructure were determined by tensile tests and scanning electron microscopy technique (SEM). Tensile strength, yield stress, Young's modulus and elongation at break of PE/SiO₂ composites were mainly discussed against the properties of PE/PE-g-MAH/SiO₂ composites. The most pronounced increase in mechanical parameters was observed in Young's modulus for composites with polyethylene grafted with maleic anhydride. The increase in the E-modulus of PE/PE-g-MAH/SiO₂composites was associated with the compatibility and improvement of interfacial adhesion between the polyethylene matrix and the nanoparticles, leading to an increased degree of particle dispersion. This finding was verified on the basis of SEM micrographs for composites of PE/PE-g-MAH/4% by weight of SiO₂. The micrographs clearly documented that addition of only 2 wt% of the compatibilizer changed the composite morphology by reducing filler aggregates size as well as their number. Increased adhesion between the PE matrix and SiO₂ particles was interpreted to be a result of interactions taking place between the polar groups of maleic anhydride and silanol groups on the silica surface. These interactions are responsible for reduction of the size of silica aggregates, leading to improved mechanical properties.