Synthesis,characterization, and thermal properties of phosphorus‐containing,wholly aromatic thermotropic copolyesters

A series of phosphorus‐containing, wholly aromatic thermotropic copolyesters from acetylated 2‐(6‐oxide‐6H‐dibenz〈c,e〉〈1,2〉oxa phosphorin‐6‐yl)‐1,4‐dihydroxy phenylene, p‐acetoxybenzoic acid, terephthalic acid, and isophthalic acid were prepared by melting polycondensation. The structure and basic properties of the polymers, such as the glass‐transition temperature (T_g), melting temperature (T_m), thermal stability, crystallinity, and liquid crystallinity, were investigated with Fourier transform infrared, elemental analysis, differential scanning calorimetry (DSC), thermogravimetric analysis, wide‐angle X‐ray diffraction, and hot‐stage polarizing optical microscopy. The copolyesters had relatively high T_g values ranging from 183 to 192°C. The T_m values obtained from DSC curves for samples P‐20 and P‐25 were 290 and 287°C, respectively (where the number in the sample name indicates the molar fraction of the phosphorus‐containing monomer in the reactants). The initial flow temperatures of other samples observed with hot‐stage polarizing microscopy were 271–290°C. The 5% degradation temperatures in nitrogen ranged from 431 to 462°C, and the char yields at 640°C were 41–52%. All the copolyesters, except P‐40, were thermotropic and nematic. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 1278–1284, 2002     

Synthesis and characterization of sPS/montmorillonite nanocomposites

The present work analyzed the possibility of obtaining and producing syndiotactic polystyrene (sPS)–based nanocomposites. The work first focused on possible technology to use for intercalation from solution and melt intercalation. Using a blend of sPS with atactic polystyrene (aPS) as the matrix was also considered. Thermal analysis techniques, such as differential scanning calorimetry (DSC) and thermogravimetry (TGA), were used to study the thermal properties and stability of the nanocomposites obtained and to select the most appropriate nanocharges. The effect of the introduction of nanofillers on these properties also was evaluated. X–ray diffraction was used to investigate the degree of clay exfoliation. Finally, mechanical characterization of the nanocomposites obtained was performed and compared to that of the pure material. The tests demonstrated that nanodispersion of phyllosilicate layers improved the mechanical behavior of the polymers analyzed, especially the annealed sPS. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 4957–4963, 2006     

Thermal characterization and thermal degradation of copolyimides containing fluorine and phosphine oxide

A series of copolyimides containing different ratios of fluorine and phosphine oxide were synthesized. The copolymers were characterized with Fourier transform infrared, differential scanning calorimetry, and thermogravimetric analysis measurements. The copolymers were thermally stable up to 700 K and exhibited glass‐transition temperatures in the range of 495–562 K. The glass‐transition temperatures of the copolymers decreased with an increase in the phosphine oxide content. The thermal decomposition behavior of the copolymers was investigated. The copolymers with higher phosphine oxide contents displayed lower onset decomposition temperatures and char yields. A new method involving the multiple‐rate isotemperature was used to define the most possible mechanism [G(α)] for the reactions. The overall kinetic model function of the thermal decomposition of these copolymers obeyed the Avrami–Erofeev model equation, G(α) = [?ln(1 ? α)]^1/m, where α is the conversion degree. The apparent kinetic parameters of the degradation processes were also obtained. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2139–2143, 2005     

Processing and characterization of injection moldable polymer–particle composites applicable in brazing processes

A novel method has been developed to process highly filled polymer–particle composites to test samples as braze metal preforms. Polypropylene (PP), low‐density polyethylene (LD‐PE) and high‐density polyethylene (HD‐PE) were used as polymer matrices. Two types of nickel‐based braze metal microparticles (Ni 102 and EXP 152) were compounded to the polymer matrices at filler contents up to 65 vol %. With enhancing filler content, torque at kneading rotors, and injection molding parameter were significantly affected by increasing viscosity. Injection molded composites show well‐distributed spherical microparticles and particle–particle interactions. Polymers decompose residue‐free at temperatures above 550°C, even for their composites. Adding particles reduces polymer crystallinity, whereas defined cooling at 5°C/min significantly increases the crystallinity and melt peak temperature of polymers compared to undefined cooling prior injection molding. Storage modulus of polymers increases significantly by adding filler particles. LD‐PE + 65 vol % EXP 152 show the most suitable composite performance. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Synthesis of UV and thermal dual curing oligomer for solder resist ink using ink-jet printing

A novel solder resist ink for inkjet printing containing the ultraviolet (UV) and thermal dual curing oligomer is introduced in this work. Three kinds of acrylic monomers for the synthesis of the oligomer are successful prepared and their structures are determined by Fourier transfer infrared. Both UV curing process and thermostability are monitored under UV differential scanning calorimetry and thermogravimetric analysis. For the photoreaction process, the oligomer using Lauryl methacrylate as the material of copolymerization possesses the highest reactivity and conversion of carbon–carbon double bond. Besides, this kind of oligomer also owns excellent thermostability, just losing 5.9% of its weight at 288 °C. The solder resist inks containing the oligomers and jetting by the inkjet printer are tested with the adhesion, soldering resistance, and other performances, presenting the outstanding heat resistance and wide application prospects. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47428.     

Morphology and thermal properties of poly(L‐lactic acid)/organoclay nanocomposites

A modified clay was used to prepare poly(L ‐lactic acid)/clay nanocomposite dispersions. X‐ray diffraction and transmission electron microscopy experiments revealed that poly(L ‐lactic acid) was able to intercalate the clay galleries. IR spectra of the poly(L ‐lactic acid)/clay nanocomposites showed the presence of interactions between the exfoliated clay platelets and the poly(L ‐lactic acid). Thermogravimetric analysis and differential scanning calorimetry were performed to study the thermal behavior of the prepared composites. The properties of the poly(L ‐lactic acid)/clay nanocomposites were also examined as functions of the organoclay content. The exfoliated organoclay layers acted as nucleating agents, and as the organoclay content increased, the crystallization temperature increased. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synthesis and characterization of PLA nanocomposites containing nanosilica modified with different organosilanes II: Effect of the organosilanes on the properties of nanocomposites: Thermal characterization

Thermal behavior of polylactic acid (PLA)/nanosilica nanocomposites prepared via bulk ring opening polymerization from lactide was investigated by differential scanning calorimetry and thermogravimetric analysis (TGA). Both unmodified nanosilica and modified by surface treatments with different amounts of two distinct silanes were used. Samples containing pure silica show enhanced crystallization processes; with silane‐modified silica this effect is magnified, especially in the case of materials with high loadings of epoxy silane. Nonisothermal crystallization temperatures become higher and isothermal crystallization kinetics show a marked increase of Kinetic constant (K_c). TGA analyses show that, when pure nanosilica is present, nanocomposites have a thermal stability far greater than the one of standard PLA, starting their degradation at temperatures up to 70°C higher than the ones of pure PLA. When silanes are present, thermal stability lowers as silane content increases, but it is anyway higher than the one of the pure polymer. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Synthesis and performance of phenolic polybutadiene‐bound stabilizers

An antioxidant derivative, 6‐sulfanylhexyl 3‐(3,5‐di‐tert‐butyl‐4‐hydroxyphenyl)propanoate, was synthesized and examined. With a radical initiator, the addition of this compound to pending vinyls of OH‐telechelic, low molecular weight liquid polybutadiene (LBH) was performed to various degrees of conversion to form polymeric antioxidants (PAOs) in which the phenolic moiety was separated from the main chain by a spacer [? CH₂CH₂? S? (CH₂)₆? O? CO? ]. Pure, unstabilized LBH was mixed in several ratios with PAOs, Irganox 1520, and Irganox 1076, and the oxidation stabilities of these mixtures, determined by thermogravimetric analysis and differential scanning calorimetry, were compared. Probably because of their good compatibility with LBH, PAOs exhibited equal or better effectiveness than commercial antioxidants of the Irganox type. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 87: 885–889, 2003     

Combined effect of a plasticizer and carvacrol and thymol on the mechanical,thermal, morphological properties of poly(lactic acid)

In this study, the effects of the monotherpenic phenol concentration on the properties of biocomposites containing plasticized poly(lactic acid) (PLA) with acetyl tributyl citrate (ATBC) were investigated. The monotherpenic phenols carvacrol (C) and thymol (T) were added to PLA by a melt‐blending method. The prepared samples were characterized by means of tensile testing, Fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry, scanning electron microscopy (SEM), and antibacterial activity tests. The addition of ATBC to PLA resulted in hydrogen bonding between ATBC and PLA. We observed that ATBC, C, and T reduced the glass‐transition temperature of PLA. The presence of C and T decreased the maximum degradation temperature slightly. Because of the plasticization effect of the additives, the tensile strength and Young's modulus of PLA decreased, whereas the extent of elongation they experienced before failure increased. This effect was also observed with SEM analysis in terms of plastic deformation at break. The antibacterial activity tests showed that samples containing high concentrations of C demonstrated an improved antibacterial activity against Staphylococcus aureus, Salmonella typhimurium, and Listeria monocytogenes bacteria. We observed that C exhibited a higher inhibition against bacterial strains than T. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45895.     

Binary mixtures of polyethylene and oxidized wax: Dependency of thermal and mechanical properties upon mixing procedure

The influence of the preparation procedure on the thermal and mechanical properties of linear low‐density polyethylene (LLDPE)– and LDPE–oxidized wax blends was investigated. It was found that mechanically mixed blends show reduced thermal stability as well as ultimate mechanical properties (stress and strain at break) compared to that of extrusion mixed blends. However, the structure of the blend and consequently its thermal and mechanical behavior also depend on the initial morphology of polyethylene. DSC measurements show miscibility up to high wax contents in both blend types, but increasing the amount of wax in LDPE blends induces increasing crystallinity. As a result, the LDPE/wax blends show improved thermal stability of between 20 and 50°C at low wax concentrations. Although the elasticity modulus of the blends increases, increasing the amount of wax generally degrades the mechanical properties. The main reason for this is the reduced number of tie chains. Changes in the average concentration of tie chains with increasing wax content were calculated and a correlation was made with the ultimate properties of the blends. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 2446–2456, 2003     

Fabrication,characterization, and properties of poly(ethylene‐co‐vinyl acetate)/magnetite nanocomposites

Poly(ethylene‐co‐vinyl acetate) (EVA)/magnetite (Fe₃O₄) nanocomposite was prepared with different loading of Fe₃O₄ nanoparticles. The mixing and compounding were carried out on a two‐roll mixing mill and the sheets were prepared in a compression‐molding machine. The effect of loading of nanoparticles in EVA was investigated thoroughly by different characterization technique such as transmission electron microscopy (TEM), X‐ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), limiting oxygen index (LOI), and technological properties. TEM analysis showed the uniform dispersion of filler in the polymer matrix and the dispersion of filler decreased with increase in filler content. XRD of the nanocomposite revealed the more ordered structure of the polymer chain. An appreciable increase in glass transition temperature was observed owing to the restricted mobility of Fe₃O₄‐filled EVA nanocomposite. TGA and flame resistance studies indicated that the composites attain better thermal and flame resistance than EVA owing to the interaction of filler and polymer segments. Mechanical properties such as tensile strength, tear resistance, and modulus were increased for composites up to 7 phr of filler, which is presumably owing to aggregation of Fe₃O₄ nanoparticle at higher loading. The presence of Fe₃O₄ nanoparticles in the polymer matrix reduced the elongation at break and impact strength while improved hardness of the composite than unfilled EVA. The change in technological properties had been correlated with the variation of polymer–filler interaction estimated from the swelling behavior. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40116.     

Improvements in the thermal conductivity and mechanical properties of phase‐change microcapsules with oxygen‐plasma‐modified multiwalled carbon nanotubes

The thermal properties and mechanical properties are the key factors of phase‐change microcapsules (microPCMs) in energy‐storage applications. In this study, microPCMs based on an n‐octadecane (C18) core and a melamine–urea–formaldehyde (MUF) shell supplemented with O₂‐plasma‐modified multiwalled carbon nanotubes (CNTs) were synthesized through in situ polymerization. Meanwhile, two different addition methods, the addition of modified CNTs into the emulsion system or into the polymer system, were compared and examined. Scanning electron microscopy micrographs showed that the microPCMs were spherical and had a broadened size distribution. Fourier transform infrared testing demonstrated that the modified CNTs did not affect C18 coated by MUF resin. The results indicate that the thermal conductivity and mechanical properties of the microPCMs were remarkably improved by the addition of a moderate amount of modified CNTs, but the heat enthalpy and encapsulated efficiency decreased slightly. Moreover, the thermal conductivity and mechanical properties of microPCMs modified with CNTs directly added to the polymer system were superior to those with CNTs added to emulsion system. In particular, when 0.2 g of modified CNTs were added to the polymer system, the thermal conductivity of the microPCMs was improved by 225%, and the breakage rates of the microPCMs at 4000 rpm for 5, 10, and 20 min decreased by 74, 72, and 60%, respectively, compared with that of the microPCMs without modified CNTs. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45269.     

Charge dynamics and thermal properties of epoxy based micro and nano hybrid composites at high temperatures

This paper presents the effects of the filler type and testing temperature on the charge dynamics and thermal properties of the epoxy resin. The micro-nano hybrid composites with different content of the micro and nano aluminum nitride (AlN) fillers are fabricated. The morphology of micro-nano hybrid composites is characterized. Electrical testing and thermal analysis methods are adopted to analyze its electrical and thermal performance. The results show that the space charge accumulation is suppressed and the charge decay process is facilitated in the hybrid composites. The electrical performances of the hybrid composites are enhanced by the nano-fillers. The apparent mobility and activation energy are decreased with nano-AlN fillers in the composites at the high temperature. The glass transition temperature and thermal stability of the materials is improved with the nano-AlN. A hypothetical mechanism is proposed to explain the charge carrier injection and transport of the composites at different temperatures.     

Water states and thermal processability of boric acid modified poly(vinyl alcohol)

To further improve the processability of water plasticized poly(vinyl alcohol) (PVA), boric acid (BA), which can rapidly form reversible crosslinked structure with the hydroxyl groups of PVA, was adopted as a modifier, and the water states, thermal performance, and rheological properties of modified PVA were investigated. The results showed that ascribing to the formation of the crosslinked structure between PVA and BA, the content of nonfreezing water in system increased, indicating that the bondage of PVA matrix on water enhanced, thus retarding the tempestuous evaporation of water in system during melt process and making more water remained in system to play the role of plasticizer. Meanwhile, this crosslinked structure shielded part hydroxyl groups in PVA chains, leading to the further weakening of the self‐hydrogen bonding of PVA, and guaranteeing a lower melting point and higher decomposition temperature, thus obtaining a quite wide thermal processing window, i.e., ≥179°C. The melt viscosity of BA modified PVA slightly increased, but still satisfied the requirements for thermal processing, thus reinforcing the flow stability of the melt at high shearing rate. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43246.     

Thermal and dynamic mechanical characterization of acrylic bone cements modified with biodegradable polymers

In this work, a thermal and a dynamic mechanical study of new formulations self‐curing acrylic bone cements is reported. The basic formulation of poly(methylmethacrylate) (PMMA)‐based acrylic bone cements has been modified with biodegradable polyesters such as poly(l ‐lactic acid), poly(β‐hydroxybutyrate), and different kinds of thermoplastic starches. Differential scanning calorimetry (DSC) (dynamic and isothermal conditions), thermogravimetric analysis (TGA), dynamic mechanical thermal analysis (DMTA), and scanning electron microscopy (SEM) were used to determine the influence of the biodegradable polymer in the behavior of the biomedical formulations. DSC assay revealed a strong dependence of the polymerization enthalpy (ΔH_cur) with increasing solid : liquid ratio and a low influence of the nature of the added biodegradable polymer on glass transition. TGA analysis showed the different mechanism of PMMA‐biodegradable polymer interaction depending on the solubilization of the added polymer in methylmethacrylate monomer during curing. DMTA showed the reinforcing capacity of segregated phases of the polymer included in the cement. The solubilization of aliphatic polyesters in the resulting PMMA polymerized phase led to a drop in mechanical stiffness observed from storage modulus (E′) profiles. Moreover, tan δ shifts to higher temperatures (4–7°C) during a second scan, confirming the presence of residual monomer content. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Thermal and nondestructive analysis of high density polyethylene filled with milled salago fiber

Fillers are utilized for different purposes. In plastic industry, fillers are mainly used to extend the bulk of the compound; however, they can also improve physical properties, materials processing, and reduce cycle time of plastics. In this article, high-density polyethylene was filled with untreated and 5% alkaline-treated salago fiber, and thereafter the thermal and nondestructive properties of the composites were investigated. It was found that the chemical treatment of fiber increased the thermal stability and the mean coefficient value of linear thermal expansion of the treated composites as compared to the untreated ones. Moreover, the increase of fiber content in composites increased the crystallinity level while decreased the thermal capacity and melting temperature of the composites. The zinc, calcium, and phosphorus contents were found to be within the industry-acceptable range for elemental contents in polyolefins. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47873.     

Characterization of an alkali‐treated grass fiber by thermogravimetric and X‐ray crystallographic analysis

The thermal behavior of grass fiber was characterized by means of thermogravimetric analysis and differential scanning calorimetry analysis. The results proved that the removal of water‐soluble matter improved the thermal behavior of grass fiber over that of unleached fiber, and this was further enhanced by an alkali treatment of the grass fiber. The isothermal weight loss of the grass‐fiber specimens was analyzed at 100, 200, and 300°C for different time periods. Accelerated aging of the grass‐fiber samples was carried out to determine the effect of aging on the tensile strength. Partially delignified grass fiber showed maximum thermal stability. X‐ray diffraction analysis was also performed to verify the composition and to correlate the change in the tensile strength due to the water leaching and alkali treatment. The processing of grass fiber with NaOH and NaClO₂ reduced the amorphous fraction in the fiber sample. This may have been a result of the loss of the amorphous noncellulosic components of the fibers and the degradation of the unordered regions of the grass fiber. However, mercerization of the grass fiber revealed an increase in the amorphous fraction after a certain time exposure, confirming the decrease in the crystallinity. The morphology of the water‐leached and alkali‐treated grass fiber was studied with scanning electron microscopy © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

The effect of formaldehyde/phenol (F/P) molar ratios on function and curing kinetics of high‐solid resol phenolic resins

A series of high‐solid resol phenolic resins (HSRPRs) were synthesized with different molar ratios (1.6, 1.8, 2.0, 2.2, and 2.4) of formaldehyde to phenol using calcium oxide and sodium hydroxide as catalyst. The effects of F/P molar ratios on physical properties, free formaldehyde and phenol, activity, structure, and thermally resistant properties of HSRPRs were fully investigated by chemical assays, liquid and solid ¹³C‐NMR, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The curing kinetics of different F/P molar ratios were explored with differential scanning calorimeter at four different heating rates (5, 10, 15, 20°C/min) from 35 to 200°C. Overall, HSRPRs with F/P = 2.0 had excellent comprehensive properties. The study was significant in solving the wastewater problem during the process of industry‐scale preparation of HSRPRs. We believed that the experimental findings would provide a new avenue for further study and application of HSRPRs. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

The effect of PETA/PETTA composite system on the performance of UV curable waterborne polyurethane acrylate

UV curable waterborne polyurethane acrylate based on pentaerythritol triacrylate (PETA)/pentaerythritol tetraacrylate (PETTA) composite system was prepared by using polycaprolactone glycol (PCL), isophorone diisocyanate (IPDI), β‐cyclodextrin (β‐CD) and 2,2‐dimethylol butanoic acid (DMBA) as the main materials. Besides, PETA was used as capping agent and PETTA was used as reactive diluent. By varying the additive amount of PETA and PETTA, a series of emulsions and films were obtained. The molecular structure was characterized by infrared spectra and a series of performance tests such as particle size, contact angle, tensile properties, UV curing performance, differential scanning calorimetry and thermogravimetric analysis were conducted. The result showed that more compact network structure was formed by introducing PETTA with higher reactivity into the polyurethane molecule under UV irradiation and many performances were improved as a whole. However, there existed phase separation to a certain extent. Especially when the content of PETTA was higher than 83.33%, the effect of compatibility became more prominent. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41262.