Friction and wear properties of basalt fiber reinforced/solid lubricants filled polyimide composites under different sliding conditions

Short basalt fibers (BFs)‐reinforced polyimide (PI) composites filled with MoS₂ and graphite were fabricated by means of hot‐press molding technique. The tribological properties of the resulting composites sliding against GCr15 steel ring were investigated on a model ring‐on‐block test rig. The wear mechanisms were also comparatively discussed, based on scanning electron microscopic examination of the worn surface of the PI composites and the transfer film formed on the counterpart. Experimental results revealed that MoS₂ and graphite as fillers significantly improved the wear resistance of the BFs‐reinforced polyimide (BFs/PI) composites. For the best combination of friction coefficient and wear rate, the optimal volume content of MoS₂ and graphite in the composites appears to be 40 and 35%, respectively. It was also found that the tribological properties of the filled BFs/PI composites were closely related with the sliding conditions such as sliding speed and applied load. Research results show that the BF/PI composites exhibited better tribological properties under higher PV product. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Surface modification and preparation of nanofiltration membrane from polyethersulfone/polyimide blend—Use of a new material (polyethyleneglycol‐triazine)

Blends of polyethersulfone/polyimide (PES/PI) were prepared by dissolving in dimethylformamide/dioxane (DMF/DO) to manufacture nanofiltration membranes by using polyvinylpirrolidone (PVP) as a pore former. The membrane modification was carried out by adding ethylenediamine (EDA) to open the imide group ring of PI and by using polyethyleneglycol (PEG)‐triazine, as a new modifier material, that was produced in the laboratory. This modification involves the formation of a covalence ‐C‐N‐ bound between PEG‐triazine and amine groups (according to addition‐elimination reactions) at different temperatures. After functionalizing the membranes, diethanolamine (DA) was utilized as a hydrophilic modifier to change the membranes properties. SEM, AFM, FTIR‐ATR, EDS (X‐ray analysis) and contact angle tests were carried out to characterize modified membranes. The hydrophilicity of PES/PI membranes was improved by modification. An increase in pure water flux (up to 195 kg/m² h) and a decline in NaCl rejection (from 25 to 16%) are largely influenced by diminishing the PES/PI ratio in L₁‐L₅ membranes (Category 1). In L₆, L₇, and L₈ membranes (Category 2), by introducing PEG‐triazine into the membrane recipe, salt rejection increased from 75 to 80%. Addition of DA further enhances the salt rejection up to 93%. Fluxes were approximately similar for membranes in Category 2. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Surfactant‐dispersed carbon black in polyimide nanocomposites: Spectroscopic monitoring of the dispersion state in the polymer matrix

The effects of an anionic surfactant on the dispersion of carbon black (CB) for the purpose of forming conducting composite films were examined with ultraviolet–visible (UV–vis) absorption spectroscopy. To obtain a good dispersion and size reduction of aggregated CB in a polymer matrix, sodium dodecyl sulfate (SDS), used as a surfactant, was introduced into a CB suspension. A set of concentrations with various ratios of CB to SDS (ranging from 1 : 0.4 to 1 : 10) was established before mixing with poly(amic acid) (PAA), a precursor of pyromellitic dianhydride and oxydianiline, was performed. The CB/PAA solution mixtures were submerged under an ultrasonic bath for several hours, then cast onto dry plate glasses, and finally subjected to thermal imidization to produce CB/polyimide (PI) nanocomposite films with various CB weight fractions ranging from 0.025 to 0.50 wt %. A method for evaluating the absorbance at 500 nm of the CB/PI nanocomposite films was established. The absorbance of CB/PI nanocomposite samples of various thicknesses was also normalized to get rid of the effects of the different thicknesses. UV–vis spectra showed that the minimum weight ratio of CB to SDS in the nanocomposite films that achieved well‐dispersed CB and still had transparent properties was 1 : 2.0. Transmission electron microscopy demonstrated that CB was dispersed homogeneously in the PI matrix, and the size of the aggregated CB was affected by the amount of the surfactant. The dielectric properties of the nanocomposite films without the surfactant increased by approximately 2 orders of magnitude with an increasing mass weight fraction of CB and decreased when the surfactant was added. The surfactant also reduced the tensile strength of the CB/PI nanocomposites when the CB/SDS ratio was higher than 1 : 2.0. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Synthesis and characterization of polyimide/modified mCOC composites

Two types of monomers, 4,4′‐(hexafluoroisopropylidene) diphthalic anhydride and 4,4′‐oxydianiline, were employed to synthesize poly(amic acid) (PAA) as a precursor of polyimide (PI). Through the addition of modified metallocene cyclic olefin copolymer (mCOC), PAA/mCOC composites were formed. PI/mCOC composites were obtained through a blade coating and multistep thermal curing process. The structure of the prepared PI/mCOC composites was characterized through Fourier transform infrared spectrometry. The results showed that the copolymerization of PAA and modified mCOC improved thethermal stability and hydrophobic and electrical properties of the PI/mCOC composites. The formation of a network structure between PI and modified mCOC considerably reduced the mobility of PI molecules, thereby improving the glass transition temperature and thermal properties of the composite. The thermal and hydrophobic properties were improved by increasing the mCOC grafting ratio. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44144.     

Synthesis and properties of the amino‐functionalized multiple‐walled carbon nanotubes/polyimide nanocomposites

The 1,6‐hexanediamine‐functionalized multi‐walled carbon nanotubes(a‐MWNTs)/polyimide(PI) nanocomposite films were prepared through in‐situ polymerization followed by mixture casting, evaporation, and thermal imidization. To increase the compatibility of carbon nanotubes with the matrix polyimide, a‐MWNTs was used as the filler. According to the results, a‐MWNTs were homogeneously dispersed in the nanocomposite films. With the incorporation of a‐MWNTs, the mechanical properties of the resultant films were improved due to the strong chemical bonding and interfacial interaction between a‐MWNTs and 4,4′‐oxydiphthalic anhydride(ODPA)/4,4′‐Oxydianiline(ODA) polyimide matrix. The thermal stability of the a‐MWNTs/polyimide nanocomposite was also improved by the addition of a‐MWNTs. The electrical tests showed a percolation threshold at about 0.85 vol% and the electrical properties were increased sharply. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Autophotosensitive negative polyimide

A novel autophotosensitive polyimide (APSPI) was synthesized through introducing benzophenone (BP) moiety into the backbone chain and acrylate group into side chain of PI. The BP moiety can generate active radicals, which can initiate acrylate group to form crosslinked network. The study of photosensitive properties revealed its good photolithographic properties, with a resolution about 12 μm and a sensitivity of 330 mJ/cm². © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Effect of surface treatment on the tribological performance of carbon fiber reinforced thermoplastic polyimide composites

The effect of rare earth solution (RES) surface treatment of carbon fibers (CFs) on the tensile strength and tribological properties of CF‐reinforced polyimide (CF/PI) composite was investigated. Experimental results revealed that the tensile strength of RES‐treated CFs reinforced PI composite was improved by about 19% compared with that of untreated composite, while 7% improvement was achieved by air oxidation. Compared with the untreated and air‐oxidated CF/PI composite, the RES‐treated composite had the lowest friction coefficient and specific wear rate under given applied load and reciprocating sliding frequency. RES treatment effectively improved the interfacial adhesion between CFs and PI. The strong interfacial adhesion of the composite made CFs not easy to detach from the PI matrix and prevented the rubbing‐off of PI, and accordingly improved the friction and wear properties of the composite. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Semi‐aromatic polyimide/Ag nanocomposite derived from vanillin

The development of bioprecursor polyimide/Ag nanocomposites (PI/Ag NCs) is reported in this investigation. Semiaromatic bioprecursor PI was successfully synthesized through direct polycondensation reaction between aromatic diamine containing pyridine ring and aliphatic dianhydride. Aromatic diamine as a monomer was synthesized using a renewable resource, vanillin. The main attractive aspects of this PI are the renewable origin of the diamine, presence of pyridine and high aromatic rings content, as well as aliphatic content on the polymer backbone. The structure of synthesized monomer and PI were proven by FTIR, and nuclear magnetic resonance. The PI/Ag NCs containing 3, 5, and 7 wt % of Ag nanoparticles (Ag NPs) were prepared through solution technique and the resulting NCs were characterized by Fourier transform infrared spectra, wide angle X‐ray diffraction, transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). TEM results showed that the Ag NPs were dispersed homogeneously in the PI matrix on nanoscale. TGA results indicated improving in thermal properties of PI/Ag NCs compared to the neat PI due to the interaction between the PI matrix and the Ag NPs. Antibacterial activity of PI/Ag NCs was tested by the disk diffusion method using Escherichia coli as model strain of gram‐negative bacteria. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44001.     

Pervaporative studies using polyimide‐filled PDMS membrane

The application of pervaporation (PV) to the removal of volatile organic from aqueous solutions has become very interesting in the last few years. It is caused by the increasing level of compounds, such as petrochemical solvents (benzene, toluene, and xylenes) or chlorinated solvents (trichloroethylene or tetrachloroethylene), which are polluting the natural environment. In this work, effects of polyimide (PI) (prepared by direct polycondensation of dianhydride and diamine followed by thermal cyclization of polyamic acid) filler on PV properties of poly(dimethyl siloxane) (PDMS) have been studied. PDMS membrane filled with PI was used for the separation of benzene (Bz) and toluene (Tol) from the diluted aqueous solution and the results were compared with the neat PDMS membrane of similar thickness. The PDMS‐PI membrane showed normalized flux (J′) upto 1.2 kg μm/m²h for Bz and 1.48 kg μm/m²h for Tol and selectivity of organics varies from 7.3 to 3.2 for Bz and 8.9 to 2.8 for Tol with increasing concentration of organics. Concentration of PI filler in PDMS varied 5–25% w/w. PI filler increases thermal as well as mechanical stability of filled PDMS membranes. PDMS membrane filled with 25% PI was chosen for the pervaporation studies. The membranes were characterized by FTIR, thermogravimetric analyser and scanning electron microscopy. The mechanical strength of PDMS filled with 25% w/w PI (SPI‐25) membrane was found to be 2.7 MPa. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Enhanced mechanical and thermal properties of polyimide/organically modified montmorillonite hybrid film based on stable poly(amic acid) ammonium salt

In this study, polyimide/organically modified montmorillonite (PI/OMMT) hybrid film was prepared by in situ polymerization from the stable poly(amic acid) ammonium salt/OMMT (PAAS/OMMT) precursor hybrid. PAAS was obtained by incorporating calculated triethylamine into terpolymer poly(amic acid) (PAA), which was synthesized by pyromellitic dianhydride (PMDA), 4,4′‐oxydianiline and p‐phenylenediamine in dimethylacetamide (DMAc). OMMT as a type of layered clays was prepared through surface treatment of montmorillonite (MMT) with 1‐hexadecylamine. Mechanical property measurements of PI/OMMT hybrid film indicated that the addition of 5 wt% of OMMT increased the Young's modulus of PI film up to 11.24 GPa, which is 58% higher than the pristine PI film from PAAS. Besides, the tensile strength increased to 168.36 MPa, which was higher than that of PI film derived from PAA (164.3 MPa) and PI film derived from PAAS (145.2 MPa). Moreover, the thermal stabilities of PI/OMMT hybrid film with appropriate OMMT content were also better than those of original PI films. POLYM. COMPOS., 34:2076–2081, 2013. © 2013 Society of Plastics Engineers     

Electrochemical polymerization of 2‐phenylindole and characterization of its polymer

High‐quality poly(2‐phenylindole) (PPI) films were synthesized electrochemically by direct anodic oxidation of 2‐phenylindole (PI) in boron trifluoride diethyl etherate (BFEE). The onset oxidation potential of PI in this medium was measured to be only 0.83 V versus a saturated calomel electrode (SCE), which was much lower than that determined in acetonitrile (ACN) containing 0.1 mol L^–1 tetrabutylammonium tetrafluoroborate (1.05 V vs. SCE). PPI films obtained from BFEE showed good electrochemical behavior and thermal stability with an electrical conductivity of 10^–2 S cm^–1. Structural studies showed that the polymerization of PI mainly occurred at the 3,6‐positions. As‐formed PPI films could be partly dissolved in dimethyl sulfoxide. Fluorescence spectral studies indicated that PPI was a blue‐green light emitter. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Kinetic and characterization of UV-curable silicone urethane methacrylate in semi-IPN-structured acrylic PSAs

To improve the thermal stability of general acrylic pressure-sensitive adhesives (PSAs), polydimethylsiloxane (PDMS) was used and UV curing was employed. Silicone urethane methacrylate (SiUMA) was synthesized and introduced into acrylic PSAs for a semi-interpenetrating polymer network structure. The structure of the SiUMA was investigated through C NMR, H NMR, and FT-IR. The kinetics and behaviors of SiUMA (S1) were found by adding photoinitiators (PI) of 0.5, 1.0, 5.0, and 10?phr in a binder, which were examined using the photo-DSC (pDSC). After setting PI as 5.0?phr in a binder and UV intensity as 1000?mJ/cm², the SiUMA, which was prepared by a radical polymerization, was added to acrylic PSA to 20, 40, 60, and 80% composition, and its kinetics and behaviors were analyzed by pDSC. Finally, the peel strength was checked to evaluate adhesion performance of the acrylic PSAs. The reaction rate was increased with increasing amounts of S1 and PI. Peel strength was dropped sharply with increasing crosslinking density.     

Preparation and characterization of polyimide/modified layered double hydroxide nanocomposites

Polyimide (PI)/modified layered double hydroxide (m‐LDH) nanocomposites were prepared in this study. For this work, m‐LDHs were prepared from layered double hydroxides (LDHs) through an anionic exchange reaction with pyromellitic dianhydride (PMDA), succinic acid or terephthalic acid. PMDA and 4,4′‐oxydianiline were used to make the poly(amic acid) precursor for PI. X‐ray diffraction and transmission electron microscopy measurements confirmed that the PMDA‐modified LDH (PMH) and terephthalic acid‐modified LDH (TMH) were well dispersed in the PI matrix. For the succinic acid‐modified LDH, some of the LDH was intercalated with the succinic acid molecules but most maintained its original structure. Thus, the PI/PMH and PI/TMH nanocomposites exhibited improved mechanical, thermal and electrical properties compared to pure PI. The PMH has aromatic groups and is expected to have better π–π interactions with the PI chains than the other m‐LDHs. Thus, the PI/PMH nanocomposites exhibited the best properties among the nanocomposites investigated. Copyright © 2010 Society of Chemical Industry     

Effect of the mole ratios of silane-modified polyvinylimidazoles on adhesion promotion of the polyimide/ copper system

Polyvinylimidazoles (PVIs) modified with vinyltrimethoxysilane (VTS) and y-methacryloxypropyltrimethoxysilane (γ-MPS) in different mole fractions were used as adhesion promoters (primers) for the polyimide (PI)/copper interface. The effects of the compositions of the silane-modified PVI copolymers on the lap shear strength between PI and copper were investigated at different bonding temperatures. Contact angle measurements and scanning electron microscopic (SEM) analysis were performed to characterize the interfacial phenomena between PI and the primer, and Fourier transform infrared (FTIR) spectroscopy was employed to investigate the thermo-oxidative degradation of PI at the different bonding temperatures and the locus of failure after the lap shear test. In the PI/γ-MPS-modified PVI/copper system, γ-MPS-modified PVI containing a lower γ-MPS content showed higher lap shear strengths, but the behavior was opposite in the PI/VTS-modified PVI/copper system. In particular, VTS-modified PVI with a 1: 1 silane/VI mole ratio showed the best performance for adhesion promotion of the PI/copper interface at all bonding temperatures. The interfacial adhesion strength between PI and the primer was a crucial factor for adhesion promotion of the PI/γ-MPS-modified PVI/copper system. In the PI/VTS-modified PVI/copper system, however, the primer's capability to suppress the thermal degradation of PI at the bonding temperature was the main factor in controlling the adhesion strength.     

Thermal imidization of poly(amic acid) precursors on surface-modified poly(tetrafluoroethylene) films via graft copolymerization with glycidyl methacrylate

A novel method for preparing composites of polyimides (PI) laminated to poly(tetrafluoroethylene) (PTFE) films is reported. PI/PTFE composites were developed through thermal imidization of poly(amic acid) (PAA) precursors on surface-modified PTFE films. Surface modification of PTFE films was carried out via Ar plasma pretreatment of the films, followed by UV-induced graft copolymerization with glycidyl methacrylate (GMA). The surface composition and topography of the graft copolymerized PTFE films and the delaminated PI and PTFE surfaces were characterized by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), respectively. The adhesion strengths of the PI (imidized PAA) on the GMA graft copolymerized PTFE films were evaluated as a function of various thermal imidization schedules. The adhesion reliability of the PI/PTFE composites was tested by a series of hydrothermal cycles. The development of strong Tpeel adhesion strengths of about 8 N/cm with excellent reliability for the PI/PTFE composites was attributable to the synergistic effect of coupling the curing of the epoxide functional groups of the grafted GMA chains with the imidization process of the PAA and the fact that the GMA chains were covalently tethered onto the PTFE surface. The PI/PTFE composites delaminated via cohesive failure inside the PTFE substrates. The delaminated PI film with a covalently adhered 'rough' PTFE surface layer exhibited a water contact angle as high as 140°.     

Synthesis and characterization of polyimide/multi‐walled carbon nanotube nanocomposites

Polyimide/multi‐walled carbon nanotube (PI‐MWNT) nanocomposites were fabricated by an in situ polymerization process. Chemical compatibility between the PI matrix and MWNTs is achieved by pretreatment of the carbon nanotubes in a mixture of sulfuric acid and nitric acid. The dispersion of MWNTs in the PI matrix was found to be enhanced significantly after acid modification. The glass transition (T_g) and decomposition (T_d) temperature of PI‐MWNT nanocomposites were improved as the MWNT content increased from 0.5 to 15 wt%. The storage modulus of the PI/MWNT nanocomposites is nine times higher than that of pristine PI at room temperature. The tensile strength of PI doubles when 7 wt% MWNTs is added. The dielectric constant of the PI‐MWNT nanocomposites increased from 3.5 to 80 (1 kHz) as the MWNT content increased to 15 wt%. The present study demonstrates that enhanced mechanical properties can be obtained through a simple in‐situ polymerization process. POLYM. COMPOS., 2008. © 2008 Society of Plastics Engineers     

Effect of the origin of ZnO nanoparticles dispersed in polyimide films on their photoluminescence and thermal stability

Polyimide (PI) films containing dispersed ZnO nanoparticles were prepared from both zinc nitrate hexahydrate (designated as Zn(NO₃)₂/PI) and ZnO nanoparticles, 2‐nm average primary size (ZnO/PI). This work shows how the origin of ZnO affects both the photoluminescence and thermal decomposition of the film. The presence of ZnO derived from Zn(NO₃)₂·6H₂O was confirmed by X‐ray diffraction technique. The fluorescent intensities from Zn(NO₃)₂/PI and ZnO/PI were much higher than that from pure PI films. When the ZnO concentration exceeded a certain saturation level, the emission intensity decreased due to the undesirable aggregation of ZnO. At the same concentration, ZnO/PI exhibited higher emission intensity than Zn(NO₃)₂/PI. All samples prepared under nitrogen emitted higher intensity than their counterparts prepared under argon. The ZnO/PI film was thermally more stable than the Zn(NO₃)₂/PI one. From TEM images of 117.6 mol% ZnO/PI films, the ZnO aggregates, whose average size was 17–90 nm, were well distributed throughout the film but poorly dispersed in nanometer range. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis of polyimide microparticles by dispersion polymerization

We synthesized polyimide (PI) microparticles by a reaction between benzophenone‐3,3,4,4‐tetracarboxylic dianhydride and 4,4′‐diaminodiphenyl ether using polyvinylpyrrolidone as a dispersant in four different organic solvents, at different temperatures, with different amounts of the dispersing agent, and with different concentrations of monomers. After dispersion polymerization, PI microparticles in the size range 200–800 nm were obtained. Absorptions at 1775 and 1720 cm^?1, due to the C?O group of PI, and at 1375 cm^?1, caused by the stretching vibration of the C? N group due to a lactam ring, were observed in the IR spectrum, which suggested the successful synthesis of PI particles. Scanning electron microscopy analysis of microparticle morphology showed that the PI particle sizes increased with increasing temperature, concentration of dispersant, and concentration of monomers. In addition, the thermal stability is also discussed on the basis of the results of simultaneous Differential Scanning Calorimetry Modulated TA Instruments (DSC–TA) measurement. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Colorless polyimide nanocomposite films with pristine clay: Thermal behavior,mechanical property,morphology, and optical transparency

Polyimide (PI)/clay hybrids were synthesized using the in situ solution intercalation method via poly(amic acid). The Na ion‐exchanged clays Na⁺‐saponite (SPT), Na⁺‐mica (Mica), and Na⁺‐montmorillonite (MMT) were used for the intercalation of PI polymer chains. Our dispersion results show that pristine SPT is more easily dispersed in a PI matrix than MMT or Mica. PI nanocomposites were prepared with various SPT contents to examine the variations with SPT content in the range 0–1 wt% of the thermomechanical properties, morphology, and optical transparency of the nanocomposites. The PI films have excellent optical transparencies, and are almost colorless. However, the optical transparency of the PI hybrid films decreases slightly with increases in the clay content. We also examined the relationship between the properties and clay content of the PI hybrid films using wide‐angle X‐ray diffraction (XRD) measurements, electronic microscopy (SEM and TEM), and universal tensile machine (UTM). The color intensities of the PI films were evaluated with a spectrophotometer. POLYM. ENG. SCI., 2009. © 2009 Society of Plastics Engineers     

Polyimide dielectric nanocomposites containing functional nanofillers based on multilayer structure: Design,preparation, and properties

Polyimide (PI) dielectric nanocomposites containing functional nanofillers based on layered structure (single-layer: BT@Al₂O₃@PI, double-layer: PI/BT@Al₂O₃@PI, three-layer: PI/BT@Al₂O₃@PI/PI) were designed and prepared by using PI as matrix, barium titanate (BT)@alumina (Al₂O₃) as nanofillers through in-situ polymerization compounding technology. FTIR tests indicated that PI and PI dielectric nanocomposites have been synthesized successfully. The molecular mass of BaTiO₃@Al₂O₃@PAA oligomer was higher than that of pure PAA when BT and Al₂O₃ nanofillers were incorporated simultaneously, as verified by GPC and intrinsic viscosity tests. XRD analysis showed that the addition of nanofillers destroyed the order of PI molecular structure and reduced the arrangement density of PI molecular chains. Both FESEM and HRTEM observations showed that the nanofillers were homogeneously dispersed in the PI matrix, contributing to the property improvements of PI dielectric nanocomposites. TGA results indicated that adding nanofillers improved the thermal stability and heat resistance of PI dielectric nanocomposites. The dielectric constant of PI/BT@Al₂O₃@PI double-layer nanocomposites was between the single-layer nanocomposites and pure PI. Due to the effective medium theory, the dielectric constant of three-layer PI/BT@Al₂O₃@PI/PI nanocomposites containing 5 wt% BT@Al₂O₃ reached 5.43. This work can be expected to provide an effective strategy to fabricate PI dielectric nanocomposite films for energy storage applications.