Donghai Zhu

Effects of different compatilizers on mechanical, crystallization and thermal properties of polypropylene/magensium oxysulfate whisker composites

Abstract Two kinds of compatilizers, maleic anhydride grafted polyolefin elastomer (POE-g-MAH) and maleic anhydride grafted polypropylene (PP-g-MAH), were incorporated into a polypropylene/magnesium oxysulfate whisker (PP/MOSw) composite. Scanning electron microscopy pictures presented a clear interface between MOSw and the PP matrix in the PP/MOSw composite, while vague interfaces appeared in the PP/iPOE-g-MAH/5MOSw and PP/iPP-g-MAH/5MOSw composites. Dynamic mechanical thermal analysis results indicated that PP-g-MAH was highly compatible with the PP matrix while POE-g-MAH was not. Impact strength results showed that POE-g-MAH had a superior toughening effect on PP/MOSw composites, since the proper interfacial interaction and appearance of β-crystal PP. However, incorporating PP-g-MAH seemed to be conducive to increasing strength and modulus (both for tensile and flexural tests), as evidenced by the greatly raised interfacial adhesion between the PP matrix and MOSw. Quantitative characterization carried out by Turcsányi equation for ternary composites also confirmed that PP-g-MAH efficiently enhanced interfacial interaction, by the proof of higher B values. Therefore, the thermal stability of PP-g-MAH treated composites was far superior to that of PP/iPOE-g-MAH/5MOSw composites. Differential scanning calorimetery and polarized light microscopy results showed that POE-g-MAH promoted PP nucleation, with effects further enhanced with the presence of PP-g-MAH.

Effects of different compatibilizing agents on the interfacial adhesion properties of polypropylene/magnesium oxysulfate whisker composites

The effects of maleic anhydride-grafted polypropylene (PP-g-MAH) and maleic anhydride-grafted polyolefin elastomer (POE-g-MAH) on interfacial adhesion properties of the polypropylene/magnesium oxysulfate whiskers (PP/MOSw) composites were investigated via mechanical, thermal, ATR-FTIR and rheological tests. Although significant increases in yield strength and Young’s modulus were observed in PP-g-MAH treated composites, a sharp decline in these properties was observed in POE-g-MAH treated composites. ATR-FTIR results indicated that esterification occurred between the hydroxyl groups of MOSw and the carbonyls of anhydrides of both compatibilizers but POE-g-MAH was still incompatible with the PP matrix, as verified by the presence of shoulder peaks in DTG curves and numerous voids in SEM micrographs. On the other hand, PP-g-MAH was highly compatible with the PP matrix, as evidenced by the peaks in DTG curves and vague interfaces with wrapped melts on the surface of MOSw. Rheological behaviors also confirmed that introducing PP-g-MAH resulted in a transition from liquid-like to solid-like, which was attributed to the stronger interfacial adhesion between MOSw and the PP matrix. POE-g-MAH treated composites, in contrast to PP-g-MAH, maintained liquid-like rheological behaviors as typical molten polymers. There is likely a MOSw network formed in the PP/15PP-g-MAH/15MOSw composite as suggested by the significant deviation of G′ versus G″ plots and the two crossover frequencies observed in plots of tanδ versus frequency.

Synthesis of Mg2B2O5 whiskers via coprecipitation and sintering process

Mg2B2O5 whiskers with high aspect ratio were synthesized by coprecipitation and sintering process using MgCl2·6H2O, H3BO3, and NaOH as raw materials and KCl as a flux. Their formation process was investigated by thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), and scanning electron microcopy (SEM). It is found that the products synthesized at 832°C are monoclinic Mg2B2O5 whiskers with a diameter of 200–400 nm and a length of 50–80 μm. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) analyses show that the whiskers obtained at 832°C are single crystalline and grow along with the [010] direction. The growth mechanism of Mg2B2O5 whiskers was also presented.

Crystallization, mechanical, thermal and rheological properties of polypropylene composites reinforced by magnesium oxysulfate whisker

Polypropylene (PP) composites containing magnesium oxysulfate whisker (MOSw) or lauric acid (LA) modified MOSw (LAMOSw) were prepared via melt mixing in a torque rheometer. The heterogeneous nucleating effect of LAMOSw was clearly observed in polarized light microscopy (PLM) pictures with the presence of an abundance of small spherulites. MOSw exhibited no nucleation effect and formed a few spherulites with large size. Compared with PP/MOSw composites, PP/LAMOSw exhibited better impact strength, tensile strength and nominal strain at break, ascribing to three possible reasons: (i) more β-crystal PP formed, (ii) better dispersity of LAMOSw in PP matrix and (iii) the plasticizing effect of LA. The results of dynamic mechanical thermal analysis (DMTA) indicated that brittleness of the PP matrix at low temperature was improved by the addition of LAMOSw, while the interfacial interactions between MOSw and PP matrix were actually weakened by LA, as evidenced by the higher tanδ values over the entire range of test temperatures. In terms of the rheological properties of the composites, both the η* and G′ at low frequencies increase with the addition of MOSw or LAMOSw, indicating that the PP matrix was transformed from liquid-like to solid-like. However, a network of whiskers did not form because no plateau was found in the G′ at low frequencies. With low filler content, LAMOSw produced a stronger solid-like behavior than MOSw mainly due to the better dispersion of the LAMOSw in PP matrix. However, for highly-filled composites, the η* of PP/LAMOSw at low frequencies was smaller than that of PP/MOSw composite, since the particle-particle contact effect played a major role.

Reinforcing polypropylene with calcium carbonate of different morphologies and polymorphs

Abstract The influence of calcium carbonate (CaCO3) with different polymorphs (calcite and aragonite) and morphologies (granular and rod-like) on mechanical and crystallization properties of polypropylene (PP) was investigated. Meanwhile, these CaCO3 fillers coated with oleic acid were added in different contents to PP. The results indicate that the tensile strength, flexural strength, modulus, and crystallization property of the filler-treated samples are improved, but the impact strength decreased. The crystallinity of the composites is higher than that of neat PP. Moreover, in the rod shape filler-treated sample, in both whisker species, the mechanical properties of composites are superior to the particles filled. Differential scanning calorimetry, X-ray diffraction, and mechanical tests display that calcite whisker-reinforced composite has higher crystallization enthalpy, melting enthalpy, degree of crystallinity, and mechanical properties than aragonite whiskers and calcite particles filled composites.

Mechanical and flame retardant properties of isotactic polypropylene/magnesium oxysulfate whisker composite:

Isotactic polypropylene (iPP) composites containing magnesium oxysulfate whisker (MOSw) or lauric acid-modified MOSw (LA-MOSw) were prepared via melt mixing in a torque rheometer. Scanning electron microscopy pictures showed that the interface between MOSw and iPP matrix was defined, whereas a vague interface was seen in the iPP–LA-MOSw composites. Mechanical properties of these two groups of composites were investigated in terms of tensile, notched impact, and flexural behavior aspects for the purposes of studying toughening effect of MOSw and LA-MOSw. Tensile results showed that yield strength of composites further reduced with the presence of LA, indicating the decrease in interfacial interaction bewteen iPP matrix and MOSw. As such, LA-MOSw performed better than MOSw in toughening of iPP matrix. Flexural strength and modulus of iPP–MOSw composites increased sharply with the increase in MOSw content, while less dependence on the LA-MOSw content indicated that MOSw was deemed beneficial to increase the stiffness. In addition, flammability properties were investigated by cone calorimetry experiment. The results showed that the peak heat release rate apparently reduced with addition of MOSw or LA-MOSw. Besides, iPP–LA-MOSw composites showed higher specific extinction area values than iPP–MOSw composites, which meant the weaker smoke suppression effect of LA-MOSw. It was chiefly because of the incomplete combustion caused by the continuous and complete charred (MgO) shield. The presence of LA was another possible reason.

Synthesis of calcium chloroborate whiskers via sedimentation and sintering process

Single crystalline calcium chloroborate (Ca2B5O9Cl) whiskers with uniform diameter have been fabricated by a two-step process. The precursor was firstly prepared by the sedimentation reaction between CaCl2, H3BO3 and NaOH aqueous solutions, and then sintered at different temperatures for 6 h with KCl as flux. The XRD indicates that the product synthesized at 600 °C is Orthorhombic Ca2B5O9Cl. SEM and TEM results show that the Ca2B5O9Cl is whisker with the diameter about 0.2–0.5 μm and the length up to 15 μm. SAED analysis shows that the whisker is single crystalline and grows along [001] direction. The possible formation process and growth mechanism were proposed.