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1.
Hybrid nanocomposite films of titanium dioxide (TiO2) in polyimide (PI) from 2,5-bis(4-aminophenyl)-1,3,4-oxadiazole (BAO) and 4,4′-oxydiphthalic anhydride (ODPA) have been successfully fabricated by an in situ sol-gel process. These nanocomposite films exhibit fair good optical transparency up to 40 wt% of TiO2 content. X-ray diffraction spectroscopy shows three sharp peaks in pure BAO-ODPA PI. It results from the intermolecular regularity. However, the intermolecular regularity in the hybrid film is disrupted by the introduction of TiO2 nanoparticles with no sharp peak in XRD spectra. Fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS) results confirm the formation of TiO2 particles in PI matrix. The surface Ti content is much lower than the theoretical bulk content in all hybrid films. The ratio of the former to the latter increases with the TiO2 content and levels off at TiO2 wt%≥20. Transmission electron microscope (TEM) images show that the TiO2 phase is well dispersed in the polymer matrix. The size of the TiO2 phase increases from 10 to 40 nm when the TiO2 content is 5-30 wt%, respectively.  相似文献   

2.
Hybrid polyimide (PI)/titanium dioxide (TiO2) films were prepared by in situ polymerization and sol–gel and in‐sol methods (where in‐sol method indicates that in situ polymerization and the sol–gel method were used in the same samples). The mechanical and electrical properties were found to be sensitive to the processing methods and the dispersion of nano titanium dioxide (nano‐TiO2) in the PI matrix. For the PI/TiO2 films prepared by the in situ polymerization method, their tensile strength increased with increasing TiO2‐in situ (“TiO2‐in situ” is “the TiO2 nano‐particles prepared by in situ polymerization method”) concentration. However, the optimal corona lifetime of the PI/TiO2 films was 15 min at 20 kHz and 2 kV because of poor dispersion. For the PI/TiO2 films prepared by the sol–gel method, the corona lifetime reached 113 min because of superior dispersion and a tensile strength of about 19.63 MPa. A balance of mechanical and electrical performances was achieved with the in‐sol method. The corona‐resistant life of the PI/TiO2 films was 43 min, which was about six times longer than that of the neat PI. Their tensile strength was 83.5 MPa; these films showed no decrease in this value compared with the pure PI films. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44666.  相似文献   

3.
The goal of this project is to obtain poly(vinyl alcohol) (PVA)/TiO2‐bovine serum albumin (BSA) nanocomposite (NC) films in different weight percentages of modified TiO2. For this purpose, to prevent the accumulation of nanoparticles (NPs) in the PVA matrix, the surface of the TiO2 NPs was treated with the BSA molecules. To achieve this aim, ultrasonic waves were used as an environmentally friendly and green process that decrease the time of reactions, help better spreading of TiO2 NPs and maintain dimensions of TiO2 NPs in the nanoscale range. In the end, the features of the PVA/TiO2‐BSA NC films were considered with a variety of techniques. The Fourier transform infrared spectroscopy, energy dispersive X‐ray, and X‐ray diffraction showed that the BSA was well placed on the surface of TiO2 NPs. The thermal gravimetric analysis and UV‐visible results demonstrated that all the PVA/TiO2‐BSA NC films have better thermal and optical properties than the pure PVA. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46558.  相似文献   

4.
A series of polyimide/titania (PI/TiO2) hybrid films have been successfully synthesized based on titanium tetrabutoxide (Ti(OEt)4), 3,3′,4,4′‐bezonphenone tetracarboxylic dianhydride (BTDA), 4,4′‐oxydianiline (ODA), and 1,3‐bis(aminopropyl) tetramethyldisiloxane (APrTMOS) by a sol–gel process. The atomic oxygen (AO) exposure tests were carried out using a ground‐based AO effects simulation facility. The chemical structure of PI/TiO2 films was characterized by Fourier transform‐infrared (FT‐IR) spectroscope before and after AO exposure. The glass transition temperature (Tg) and mechanical properties were examined by dynamic mechanical analysis (DMA) and universal mechanical testing machine, respectively. The tensile strength and elongation of the hybrid film decreased with the increase of TiO2 content, whereas the Tg increased with the increase of TiO2 content. The effects of TiO2 content on the morphology and structure evolvement of PI/TiO2 hybrid films were also investigated using field emission scanning electron microscopy (FE‐SEM) and X‐ray photoelectron spectroscope (XPS), respectively. The results indicated that a TiO2‐rich layer resulting from the Ti(OEt)4 formed on the PI film after AO exposure, which decreased the mass loss rate and obviously improved the AO resistance of PI films. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

5.
Polyimide/titania (PI/TiO2) nanocomposite films have been successfully fabricated through the in situ formation of TiO2 within a PI matrix via sol–gel method. Poly(amic acid) (PAA), which is the precursor of PI, was successfully synthesized by mixing pyromellitic dianhydride (PMDA), with equimolar amount of a diamine monomer having a pendent benzoxazole unit and two flexible ether linkages in N,N-dimethylformamide (DMF) solvent. Tetraethyl orthotitanate [Ti(OEt)4] and acetylacetone were then added to the resulted PAA. After imidization at high temperature, PI/TiO2 hybrid films were formed. The structure and morphology of the hybrid nanocomposites with different titania contents (0 wt%, 5 wt%, 10 wt%, and 15 wt%) were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, and transmission electron microscopy. The results indicate that the TiO2 nanoparticles were homogeneously dispersed in the hybrid films. The thermogravimetric analysis of nanocomposites confirms the improvement in the thermal stability with the increase in the percentage of titania nanoparticle. Transmission electron microscopy showed that the nanoparticles with an average diameter of 25–40 nm were dispersed in the polymer matrix.  相似文献   

6.
Thermally stable polyimide/titania (PI/TiO2) hybrid nanocomposite films have been successfully synthesized through the in situ formation of TiO2 within a PI matrix via sol‐gel process. Poly(amic acid) (PAA) solution is prepared from 3,5‐diamino benzoyl amino phenyl‐14H‐dibenzo[a,j]xanthene and 4,4′‐(hexaflouroisopropylidene)diphthalic anhydride in N‐methyl‐2‐pyrrolidinone solvent. The different amounts of tetraethyl orthotitanate and actylacetone are incorporated into PAA matrix, and then thermally imidized to form PI/TiO2. The chelating agent, acetylacetone, was applied to reduce the gelation rate of titanium alkoxide. Thermal decomposition temperatures of nanocomposites with a 10% weight loss were in excess of 500°C, and char yields higher than 63% at 800°C in nitrogen. The chemical and morphological structures of the hybrid nanocomposites were characterized by Fourier transform infrared spectroscopy, X‐ray diffraction, and transmission electron microscopy. The results show that the TiO2 particles are well dispersed in the PI matrix with particle size between 10 and 30 nm in diameter. POLYM. COMPOS., 35:1486–1493, 2014. © 2013 Society of Plastics Engineers  相似文献   

7.
In this study, a series of PI/TiO2 nanohybrid materials were prepared from polyamic acid of 3,3′,4,4′-benzophenonetetracarboxylic dianhydride/3,3′-diaminodiphenyl sulfone, and titania precursor by the sol-gel method. The titania content in the hybrid system was varied from 0 to 5 wt %. The physical and mechanical properties of the hybrids such as refractive index, optical transmission, and tensile strength were investigated. It was determined that incorporation of titania precursor into the PI matrix improved the refractive indices and tensile modulus of the hybrid films. It was observed that the optical transmittance and tensile strength of the nanohybrids were slightly decreased with the increasing titania content. It was determined that the hybrid films might have enhanced the UV shielding properties compare to the PI films. Furhermore, the hybrid materials showed better thermal stability than the PI. SEM studies demonstrated that titania particles (1 and 3 wt %) were distributed homogeneously through the PI matrix. The effect of the titania content in the PI on DC conductivity and dielectric constant were also analyzed. For the PI film containing 5 wt % titania, activation energy value increased to 1.0 eV from the value of 0.65 eV. DC conductivity value of the films depending on titania content varied between 3.0 × 10−11 and 1.4 × 10−10 S/cm at room temperature. Relative dielectric constants of the films were calculated from capacitance measurements depending on frequency (40–100 kHz) at different temperatures (303–360 K). The values increased with the increasing titania content. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

8.
A series of novel ternary polyimide/SiO2/polydiphenylsiloxane (PI/SiO2/PDPhS) composite films were prepared through co‐hydrolysis and condensation between tetramethoxysilane, diphenyldimethoxysilane (DDS) and aminopropyltriethoxysilane‐terminated polyamic acid, using an in situ sol–gel method. The composite films exhibited good optical transparency up to 30 wt% of total content of DDS and SiO2. SEM analysis showed that the PDPhS and SiO2 were well dispersed in the PI matrix without macroscopic separation of the composite films. TGA analysis indicated that the introduction of SiO2 could improve the thermal stability of the composite films. Dynamic mechanical thermal analysis showed that the composite films with low DDS content (5 wt%) had a higher glass transition temperature (Tg) than pure PI matrix. When the content of DDS was above 10 wt%, the Tg of the composite decreased slightly due to the plasticizing effect of flexible PDPhS linkages on the rigid PI chains. The composite films with high SiO2 content exhibited higher values of storage modulus. Tensile measurements also showed that the modulus and tensile strength of the composite films increased with increasing SiO2 content, and the composite films still retained a high elongation at break due the introduction of DDS. The density and water absorption of the composite films were also characterized. Copyright © 2006 Society of Chemical Industry  相似文献   

9.
To improve the properties of polyimide (PI), different mass fractions of alumina (Al2O3) nanoparticles, unmodified or modified by KH550, were incorporated into PI matrix to form PI/Al2O3 hybrid films by in situ polymerisation. The effects of Al2O3 additives on the structure, dielectric and mechanical properties of the films were studied. Fourier transform infrared spectroscopy confirmed the successful preparation of PI/Al2O3 hybrid films, and the microstructures of the samples showed a more uniform dispersion of the modified Al2O3 nanoparticles than the unmodified ones in the matrix. The dielectric constant of the films increased with increasing filler content, and the maximum electrical breakdown strength of 311 MV m?1 was obtained with a filler content of 8.0 wt-% modified Al2O3 in the matrix. Both unmodified and modified Al2O3-reinforced PI hybrids demonstrated improved mechanical properties compared with the PI matrix. Moreover, the properties of films with Al2O3 modified by KH550 were better.  相似文献   

10.
Polyimide/silica–titania (PI/SiO2–TiO2) hybrid films were prepared via an in situ sol–gel process. The PI precursor, poly(amic acid) (PAA), which contains 2,2'‐bis[4‐(4‐aminophenoxy)‐phenyl]propane (p‐BAPPP), 3,3',4,4'‐ benzophenetetracarboxylic anhydride (BTDA) and 3‐aminopropyltrimethoxysilane (APrTMOS), was first synthesized; this was followed by the addition of phenyltrimethoxysilane (PTMS) and/or tetraethyl orthotitanate (Ti(OEt)4) to fabricate PI/SiO2–TiO2 films. The relative content of SiO2 to TiO2 has remarkable effects on the crosslink structure and resultant properties of the hybrids. XPS results confirm that the amount of Si on the surface of the hybrids is higher than that in the bulk. The distribution of Ti in the hybrid films is contrary to the above trend because of the formation of three‐dimensional Si? O? Si, Si? O? Ti, and Ti? O? Ti networks. The SiO2 content of the hybrids containing only silica significantly affects their refractive index, contact angle, and dielectric constant. The films with added PTMS show higher contact angles than pure PI because nonpolar segments, ? C2H6 or benzene groups, tend to distribute on the surface. Upon the addition of (Ti(OEt)4), some hydrophilic segments on the surface of the hybrids are induced because of the formation of a crosslinked structure. The denser crosslinked molecular structure, and consequently lower CTE and higher Tg are obtained from hybrids containing more TiO2. By comparing the above properties and flexibility, the best composition of metal oxides (SiO2/TiO2) in hybrids is 20/80. That is, an optimum ratio of metal oxides in PI hybrids induces superior properties for advanced practical applications. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013  相似文献   

11.
Polyimide/titania (PI/TiO2) composite was synthesized by in situ sol–gel polymerization, and carbon/titanium carbide (TiC) composite films were prepared by carbothermal reduction of the PI/TiO2 composite at 1,600 °C under flowing argon. The structure and properties of the composites were studied by wide angle X-ray diffraction (WAXD), Fourier transform infrared spectrometer (FTIR), scanning electron microscopy, and energy dispersive X-ray spectroscopy. The carbon/TiC composite films exhibited metallic luster on the surface and compact structure in cross section with well dispersed TiC particles. WAXD intensity distribution revealed that TiC particles formed by tightly bonding between elemental carbon and titanium formed crystallites which as a filler provided tough films. The results indicated that heat treatment of PI/TiO2 under argon is a promising method for preparing tough carbon composite films.  相似文献   

12.
Dielectric and conduction properties of polyimide/silica nano‐hybrid films were investigated with the silica content and the testing frequency, using a small electrode system. The hybrid films were prepared through sol‐gel process and thermal imidization, by using pyromellitic dianhydride and 4,4′‐oxydianiline as polyimide precursors, and tetraethoxysilane and methyltriethoxysilane as silica precursors. The dielectric coefficient of PI/SiO2 films was monotonically increased with increasing silica content, and decreased with increasing testing frequency. The dielectric loss of PI/SiO2 films had no obvious changes with increasing silica content, but monotonically increased with increasing testing frequency. These can be contributed to the different quantity and migration chunnels of current carriers, which were mainly influenced by a few of complicated factors. There were remarkable differences between conduction property of PI/TEOS‐SiO2 films and PI/MTEOS‐SiO2 films because of the different size and dispersion status of silica particles in the polyimide matrix. POLYM. COMPOS., 2008. © 2008 Society of Plastics Engineers  相似文献   

13.
Novel TiO2–Ag core–shell micro‐/nanowires (TiO2 shell coating on Ag core) have been successfully prepared via a solvent–thermal method. Energy dispersive spectroscopy and X‐ray diffraction analyses revealed that the micro‐/nanowires were composed of Ag, Ti and O elements, and Ag was face‐centered cubic whereas TiO2 was mainly amorphous. Interestingly, scanning electron microscopy (SEM) and transmission electron microscopy results showed that most of the TiO2 bristles were perpendicular to and uniformly studded on the surface of the Ag cores. Subsequently, TiO2–Ag/poly(arylene ether nitrile) (PEN) composite films were prepared via a solution‐casting method in order to investigate the effect of TiO2–Ag on the PEN matrix. SEM images showed that there was good interfacial adhesion between fillers and PEN matrix owing to the special bristle‐like structure. Thermal analysis results showed that the TiO2–Ag/PEN composite films possessed excellent thermal properties endowed by the PEN matrix. The dielectric constant of the composite films increased to 9.3 at 100 Hz when the TiO2–Ag loading reached 40 wt%. Rheology measurements revealed that the network formed by TiO2–Ag was sensitive to shear stress and nearly time independent. © 2013 Society of Chemical Industry  相似文献   

14.
Polyimide/mica (PI/mica) hybrid films were prepared from pyromellitic dianhydride/4,4-bis(3-aminophenoxy)biphenyl (PMDA/4,3-BAPOBP) and mica in a solution of N,N-dimethylacetamide. The structure–property relationships of the composites were studied by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet–visible spectroscopy and differential scanning calorimetry. FTIR indicated successful preparation of PI/mica hybrid films. XRD and SEM results indicated that the mica was well dispersed in the PI matrix. The dependence of morphology, glass transition temperatures (Tg), dielectric properties and mechanical properties at room temperature of the hybrid films on the content of mica was discussed. It was observed that Tg, the breakdown strength and tensile strength of the hybrid films, could be simultaneously increased when the mica content was lower than 8?wt-%. Meanwhile, the dielectric constant and dielectric loss of PI/mica hybrid films increased with the increase in the mica content.  相似文献   

15.
Nano-titania (TiO2) incorporated into polyimide (PI) matrix can significantly enhance the adhesion strength for PI/TiO2 hybrid film and copper system. Surface modifications by various plasma treatments (Ar, Ar/N2 and Ar/O2) were also applied in this study to improve the adhesion strength. The Ar/N2 plasma treatment is regarded as the more effective way in promoting the adhesion strength. The maximum adhesion value of 9.53 N/cm was obtained for the PI/TiO2-1 wt% hybrid film with Ar/N2 plasma treatment. It is enhanced about 10 times as large as pristine PI. Furthermore, by Ar/O2 plasma treatment, a weak boundary of copper oxide was formed at the interlayer between PI/TiO2 hybrid film and copper which decreases the adhesion strength. The effects of plasma treatment and content of nanosized TiO2 on the adhesion strength between PI/TiO2 hybrid film and copper system were studied. Atomic force microscope and contact angle analyses were used to measure the changes in surface morphology and surface energy as a result of plasma treatment. Besides, the interfacial states of peeled-off polymer side and copper side were investigated by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Based on the result of XPS spectra, the peeled-off failure mode between PI/TiO2 hybrid film and copper was proposed in this study.  相似文献   

16.
The sol–gel fabrication of new well-dispersed polyimide (PI)/TiO2 nanohybrid films is reported. The PI matrixes are synthesized via the polycondensation of pyromellitic dianhydride and a diamine monomer containing several constructive functional groups which introduced some interesting features to the final nanocomposite (NC) materials. The TiO2–heteroatom interactions associated with the flexible characteristic of polymer backbone (which facilitates the stated interactions) have been led to the fabrication of well-dispersed nanoparticles with less than 100 nm in sizes, as confirmed by means of transmission electron microscopy. Thermal analysis techniques (TGA and DSC) have shown the superior thermal stability of fabricated NCs. The UV–Vis spectroscopy has illustrated a growing trend in the absorption efficiency along with the increase in TiO2 contents. The created TiO2 nanoparticles showed amorphous structures according to the X-ray diffraction patterns.  相似文献   

17.
In this study, the synthesis, morphology, and thermal properties of new poly(ether imide)/titania nanohybrid films were investigated. The novel diamine containing functional nitrile groups was prepared in two steps by the nucleophilic substitution reaction and it was fully characterized by different techniques. Reaction of this diamine with pyromellitic dianhydride and 4-aminobenzoic acid gave poly(ether imide) with carboxylic acid end groups. This acid functionalized poly(ether imide) was condense with different amount of TiO2 nanoparticles to provide organic-inorganic bonding, and the flexible films of these hybrid were prepared. The obtained materials were characterized by Fourier transform-infrared spectroscopy, thermogravimetry analysis (TGA), differential scanning calorimetry, X-ray powder diffraction, UV–Vis spectroscopy, field emission-scanning electron microscopy, and transmission electron microscopy (TEM) techniques. TEM of the nanohybrid films with 12% of TiO2 contents confirms well dispersion of nanoparticles in the polymer matrix. TGA data indicated that the thermal behavior of the hybrid materials was increased with an increasing the content of TiO2 nanoparticles. The tensile stress–strain of the hybrids was investigated and the resulting nanocomposites showed good mechanical properties. The permeability and selectivity of the PEI/TiO2 membranes as a function of the titania weight percentage were study and the results indicated that the permeabilities of CO2 and N2 increase with increasing the titania content.  相似文献   

18.
Poly(lactic acid)/titanium dioxide (TiO2) composite films were prepared by direct melt processing using three different procedures (i.e., compression molding, twin‐screw melt extrusion, and melt extrusion and thermoforming). The effect of TiO2 loading and processing procedures on the phase morphology and on the thermal, mechanical, and barrier properties of the obtained nanocomposites were analyzed respectively by field‐emission scanning electron microscopy‐energy dispersive spectrometry, differential scanning calorimetry, universal testing machine, and water vapor and oxygen permeability measurements. The incorporation of TiO2 nanoparticles into the poly(lactic acid) matrix increased the crystallinity and improved the barrier properties of the composites. The maximum tensile strength was achieved at the 2% content of TiO2 for the films produced by compression molding and twin‐screw melt extrusion, whereas the tensile strength for films produced by melt extrusion and thermoforming decreases markedly with an increasing TiO2 content. The photocatalytic activities of the obtained nanocomposites were investigated by analyzing the degradation of methyl orange. Results confirmed that the processing procedures and the distribution of TiO2 in the polymer matrix are the key parameters, which rule the photocatalytic behavior of composite films. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers  相似文献   

19.
Different weight ratios of poly(9,9-dioctylfluorene-2,7-diyl) (PFO)/poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] (MEH-PPV) hybrid thin films, with and without a SiO2/TiO2 nanocomposite (NC), were successfully prepared using a solution blending method. All samples were deposited onto glass substrates by a spin coating technique to produce homogeneous thin films. The effect of the SiO2/TiO2 NC on the enhancement of the energy transfer mechanism in the PFO/MEH-PPV hybrids was investigated. The energy transfer parameters were calculated on the basis of the absorption and emission measurements. The long-range dipole–dipole energy transfer (Förster type) between the acceptor and donor molecules was enhanced in the presence of the SiO2/TiO2 NC in the hybrid thin films. The addition of the SiO2/TiO2 NC in the PFO/MEH-PPV hybrids reduced the distance between the donor and acceptor molecules more than the individual addition of SiO2 or TiO2 nanoparticles. Moreover, the direct relationships between the acceptor contents and energy transfer parameters, such as the energy transfer radius (RDA), energy transfer efficiency (η), and energy transfer probability (PDA), were estimated using theoretical fittings. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47845.  相似文献   

20.
Composite films were successfully prepared from cellulose and two kinds of nanocrystalline TiO2 particles in a NaOH/urea aqueous solution (7.5 : 11 in wt %) by coagulation with H2SO4 solution. The structure, morphology, and properties of the films were characterized by transmission electron microscopy, scanning electron microscopy, X‐ray diffraction, TGA, tensile testing, UV–vis spectroscopy, and antibacterial test. The results indicated that TiO2 particles in a cellulose matrix maintained the original nanocrystalline structure and properties. TiO2(I) (anatase) and TiO2(II) (the mixture of anatase and rutile) particles exhibited a certain miscibility with cellulose. The tensile strength of two kinds of composite films was higher than 70 and 75 MPa, when the content of TiO2(I) and TiO2(II) was 4 and 11 wt %, respectively. The cellulose composite films containing nanocrystalline TiO2 particles displayed distinct antibacterial abilities and excellent UV absorption. This work provides a potential way for preparing functional composite materials from cellulose and inorganic nanoparticles in a NaOH/urea aqueous solution, without a destruction of the structure and properties of the particles. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 3600–3608, 2006  相似文献   

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