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1.
Abstract

Chemically functionalized graphene oxide [multi-amino functionalized graphene oxide (MAGO)] was achieved by building covalent bonds between graphene oxide (GO) and a small molecule containing benzene structure and multi-amino groups. Fourier transform infrared, X-ray diffraction, X-ray photo electron spectroscopy and TEM-EDX results certified that the molecule was successfully grafted onto GO nanosheets. Subsequently, functionalized GO was incorporated into waterborne epoxy (EP) coating through ball-milling method. This molecular design can significantly improve the dispersion of MAGO in EP matrix, as well as the compatibility and interaction between MAGO and EP. Compared with GO/EP, the water absorption of MAGO/EP decreased from 4.38 to 2.59%, the adhesion strength of MAGO/EP increased from 4.72 to 6.32?MPa after immersion of 40?days in 3.5% NaCl solution. Incorporation of 1?wt% of MAGO into EP matrix prominently improved the long-term corrosion resistance. The impedance modulus of GO/EP coating decreased by four orders after 40 days immersion, while that of MAGO/EP coating only decreased by one order. The impedance modulus was still 1.47?×?108 Ω cm2, and two-time constant wasn’t detected for MAGO/EP coating. This research developed a novel green anticorrosion coating with enhanced durability for metal protection.  相似文献   

2.
Herein we report an easy and efficient approach to prepare lightweight porous polyimide (PI)/reduced graphene oxide (RGO) composite films. First, porous poly (amic acid) (PAA)/graphene oxide (GO) composite films were prepared via non‐solvent induced phase separation (NIPS) process. Afterwards PAA was converted into PI through thermal imidization and simultaneously GO dispersed in PAA matrix was in situ thermally reduced to RGO. The GO undergoing the same thermal treatment process as thermal imidization was characterized with thermogravimetric analysis, Raman spectra, X‐ray photoelectron spectroscopy and X‐ray diffraction to demonstrate that GO was in situ reduced during thermal imidization process. The resultant porous PI/RGO composite film (500‐µm thickness), which was prepared from pristine PAA/GO composite with 8 wt% GO, exhibited effective electrical conductivity of 0.015 S m?1 and excellent specific shielding efficiency value of 693 dB cm2 g?1. In addition, the thermal stability of the porous PI/RGO composite films was also dramatically enhanced. Compared with that of porous PI film, the 5% weight loss temperature of the composite film mentioned above was improved from 525°C to 538°C. Moreover, tensile test showed that the composite film mentioned above possessed a tensile strength of 6.97 MPa and Young's modulus of 545 MPa, respectively. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

3.
Copper foils are the vital elements used in microelectronic devices. Adequate adhesion between copper foils to various substrates, such as Si, SiO2 and polyimide, is crucial to functional electronic devices. Liquid‐crystalline polymers (LCPs) can be used as substrates for these modules as well as the adhesive to copper foils. The adhesion between aromatic thermosetting copolyester (ATSP)/fiberglass fabric (GF) laminates and copper foils was characterized by peel strength tests. It was found that ATSP/GF laminates with copper foil using ATSP oligomers as adhesive showed a highest average peel strength of 711 N · m?1. Scanning electron microscope (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) showed an excellent bond between the composite and the copper foil interface. Failure occurred between the backside of the copper foil and the ATSP/GF laminates in the peeling test and the mechanism is discussed. Thermogravimetic analyzer (TGA) indicated a thermal stability up to 371°C for ATSP/GF composite substrate and a glass transition temperature of over 400°C as determined by peak in tan δ during Dynamic Mechanical Analysis (DMA). Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

4.
Fire safety and thermal dissipation performance of epoxy resins thermosets were critical for its application in key fields such as electronic devices. The simultaneous improvement of flame retardant and thermal conductivity properties were still a challenge. Herein, ammonium polyphosphate (APP) was firstly encapsulated with 5‐wt% epoxy resins based on APP and then surface grafted with polyurethane polymer chain, and the resulting APP with core‐shell‐brush structure was constructed. Finally, the multiwalled carbon nanotube (MWCNT) was assembled in the intervals of polymer brush on APP surface, and the prepared filler was defined as MF‐APP. Its chemical structure and morphologies were characterized and confirmed. The wettability of MF‐APP was evaluated by water contact angles tests (WCA) and MF‐APP exhibited hydrophobic property with the WCA of 138°. When 9‐wt% MF‐APP was incorporated into EP thermosets, the thermal conductive value of EP/MF‐APP achieved 1.02 Wm?1 K?1, and the MWCNTs concentration was only 1.8 wt% in thermosets. Compared with the previous work, the prepared EP/MF‐APP thermosets exhibited outstanding thermal conductive efficiency because of the homogeneously distribution of MWCNTs. Moreover, the samples fulfilled UL‐94 V‐0 grade during vertical burning tests with the limiting oxygen index of 30.8%. As a result, the thermal conductivity and flame retardancy of EP thermosets were simultaneously enhanced with a relatively low addition amount of MF‐APP, which would bring more chance for wider application of EP thermosets in key fields.  相似文献   

5.
Conferring the flame retardant performance and thermal conductivity simultaneously for epoxy resin (EP) thermosets was significant for fire safety and thermal management applications of electrical and electronic devices. Herein, the graphitic carbon nitride (g‐C3N4) with desired amount was assembled on the surface of ammonium polyphosphate (APP), and the obtained APP/g‐C3N4 (CN‐APP) was characterized and confirmed by X‐ray diffraction, Fourier transform infrared spectroscopy tests, scanning electron microscopy, and transmission electron microscopy. CN‐APP was incorporated into EP and then cured with m‐phenylenediamine. The thermal conductive value of EP/CN‐APP thermosets achieved 1.09 W·mK?1, and the samples achieved UL‐94 V‐0 grade during vertical burning tests with the limiting oxygen index of 30.1% when 7 wt% CN‐APP with the mass fraction of APP/g‐C3N4 of 9/1 was incorporated. For comparative investigation, equal amount of individual g‐C3N4 was introduced into EP thermosets, and the thermal conductivity was only 0.4 W·mK?1. Compared with pure EP, the addition of CN‐APP enhanced the glass transition temperature of EP/CN‐APP thermosets and promoted the generation of more expanded, coherent, and compact char layer during combustion. Consequently, the heat release and smoke production of EP/CN‐APP thermosets were greatly suppressed and led to the improvement of fire safety of materials. It was an alternative and promising approach for preparing high‐performance polymeric materials especially used in integrated electronic devices.  相似文献   

6.
Although graphene oxide (GO) has large interlayer spacing, it is still inappropriate to use it as an anode for sodium‐ion batteries (SIBs) because of the existence of H‐bonding between the layers and ultralow electrical conductivity which impedes the Na+ and e? transformation. To solve these issues, chemical, thermal, and electrochemical procedures are traditionally employed to reduce GO nanosheets. However, these strategies are still unscalable, consume high amounts of energy, and are expensive for practical application. Here, for the first time, we describe the superior Na storage of unreduced GO by a simple and scalable alkali‐metal‐ion (Li+, Na+, K+)‐functionalized process. The various alkali metals ions, connecting with the oxygen on GO, have played different effects on morphology, porosity, degree of disorder, and electrical conductivity, which are crucial for Na‐storage capabilities. Electrochemical tests demonstrated that sodium‐ion‐functionalized GO (GNa) has shown outstanding Na‐storage performance in terms of excellent rate capability and long‐term cycle life (110 mAh g?1 after 600 cycles at 1 A g?1) owing to its high BET area, appropriate mesopore, high degree of disorder, and improved electrical conductivity. Theoretical calculations were performed using the generalized gradient approximation (GGA) to further study the Na‐storage capabilities of functionalized GO. These calculations have indicated that the Na?O bond has the lowest binding energy, which is beneficial to insertion/extraction of the sodium ion, hence the GNa has shown the best Na‐storage properties among all comparatives functionalized by other alkali metal ions.  相似文献   

7.
In this study, the hyperbranched polyester were successfully grafted onto graphene oxide (GO). The mechanical performance and curing kinetics of epoxy resin (EP), EP/ graphene oxide (EP/GO), and EP/ hyperbranched polyester grafted GO (EP/GO‐B) were investigated by means of mechanical tests and differential scanning calorimetry (DSC). Results revealed that the presence of GO lowered the cure temperature and accelerated the curing of EP, and the addition of GO‐B exhibited a stronger effect in accelerating the cure of EP compared with GO. Activation energies were calculated using Kissinger approach, and Ozawa approach, respectively. Results revealed lowered activation energy after the addition of GO or GO‐B at low degrees of cure, indicating that GO had a large effect on the curing reaction. The presence of GO facilitated the curing reaction, especially the initial epoxy‐amine reaction. Moreover, GO‐B exhibited better performance. Related mechanism was proposed.  相似文献   

8.
First, attapulgite‐Fe3O4 magnetic filler (ATP‐Fe3O4) was prepared by using a chemical precipitation method. Subsequently, graphite oxide (GO) was prepared through Hummer method, and then reduced GO (RGO) was prepared through GO reduced by chitosan (CS). Finally, a series of WPU‐RGO/ATP‐Fe3O4/CS composites were prepared by introduced RGO/ATP‐Fe3O4/CS to waterborne polyurethane. The structure and properties were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR), X‐ray diffraction (XRD), vibrating sample magnetometry (VSM), thermogravimetric analysis TGA, conductivity test, and tensile test. The experimental results indicated that thermal stability and tensile strength of nanocomposites were improved with the increase of the content of RGO/ATP‐Fe3O4/CS. Meanwhile, with the increase of the RGO/ATP‐Fe3O4/CS content, the electrical and magnetic properties of WPU‐RGO/ATP‐Fe3O4/CS composites were improved. When the content of RGO/ATP‐Fe3O4/CS was 8 wt%, the electrical conductivity and the saturation magnetic strength of WPU‐RGO/ATP‐Fe3O4/CS composites were 3.1 × 10?7 S·cm?1 and 1.38 emu/g, respectively. WPU‐RGO/ATP‐Fe3O4/CS composites have excellent electrical and magnetic properties.  相似文献   

9.
This work demonstrates a feasible route to synthesize the layered polypyrrole/graphite oxide (PPy/GO) composite by in situ emulsion polymerization in the presence of cationic surfactant cetyltrimethylammonium bromide (CTAB) as emulsifier. AFM and XRD results reveal that the GO can be delaminated into nanosheets and well dispersed in aqueous solution in the presence of CTAB. The PPy nanowires are formed due to the presence of the lamellar mesostructured (CTA)2S2O8 as a template. The results of the PPy/GO composite indicate the PPy insert successfully into GO interlayers, and the nanofiber‐like PPy are deposited onto the GO surface. Owing to π–π electron stacking effect between the pyrrole ring of PPy and the unoxided domain of GO sheets, the electrical conductivity of PPy/GO composite (5 S/cm) significantly improves in comparison with pure PPy nanowires (0.94 S/cm) and pristine GO (1 × 10?6 S/cm). © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 1329–1335, 2010  相似文献   

10.
In this work, graphene oxide (GO) was directly reduced by copper to reduced graphene oxide (RGO) and formed a highly uniform RGO film on copper foil or copper-modified titanium (Ti) substrate. The characterization of as-prepared RGO film by FTIR and XRD indicated that GO was partially reduced by copper while some oxygen-containing groups still remained. The conductivity of the RGO film was improved from 3.76?×?103 to 2.98?×?104 S/m after it was further electrochemically reduced due to the removal of additional oxygen groups. The graphene supercapacitor prepared with this method exhibited better performances in a neutral aqueous electrolyte compared with that reported for graphene electrodes prepared by other fabrication methods.  相似文献   

11.
A simple method was adopted to prepare poly(l-lactide)-grafted graphite oxide (PLLA-g-GO) by ring opening polymerization of l-lactide in the presence of graphite oxide (GO) with hydroxyl groups. GO was firstly treated with tolylene-2,4-diisocyanate (TDI) to create an anchor site on GO, and then reacted with 1,4-butanediol (BD) to afford functional hydroxyl groups grafted onto the surface of GO. So that, the dispersity of GO in the organic solution was enhanced. According to the thermogravimetric analysis (TGA), the organic composition of GO treated with TDI and BD (GO-TDI-OH) was estimated to be about 13 wt%. Also, using TGA, the composition of GO in the PLLA-g-GOs could be estimated. The hydroxyl groups on the GO surface acted as initiators for the ROP of l-lactide. Further, they also played as a vital role in controlling the molecular weight of the PLLA. The synthesized PLLA-g-GOs were characterized by the FTIR, 1HNMR and UV/Vis spectroscopies. The dispersion states of GO in the PLLA-g-GOs were investigated by wide angle x-ray diffraction patterns. According to differential scanning calorimeter study, it was found that GO platelets have nucleating effect on the crystallization of PLLA in the PLLA-g-GO. Additionally, the incorporation of GO improved the electrical conductivity of PLLA, indicating that GOs is a good conducting-modifiers for polymers.  相似文献   

12.
The present investigation was directed towards the synthesis of a copolymer of 2‐ethylhexyl acrylate and acrylic acid to be exploited as a pressure sensitive adhesive (PSA) matrix in transdermal drug delivery systems. The polymer synthesis involved free radical solution polymerization using 2, 2′‐azobisisobutyronitrile as the free radical initiator. The experimental methodology involved the optimization of reaction conditions for the polymer synthesis. The optimized copolymer was then characterized by IR, 1H‐NMR, DSC, GPC and XRD. The PSA was also evaluated for percent free monomer content, intrinsic viscosity, refractive index, moisture uptake potential and film forming properties. To assess it suitability in the development of transdermal systems, peel strength values with respect to release liner as well as human skin and skin irritation potential were also determined. In addition, wear performance test was conducted to evaluate adhesion and adhesive transfer. The synthesized adhesive was found to have good peel strength; exhibited excellent adhesion and adhesive transfer on removal. It was found suitable for use in transdermals and could be further exploited either as an adhesive matrix or as a system component in the area of transdermal drug delivery. Copyright © 2002 John Wiley & Sons, Ltd.  相似文献   

13.
Novel epoxy‐based semi‐interpenetrating polymer networks (semi‐IPNs) of aromatic polyimide, derived from 2,2‐benzidinedisulfonic acid (BDSA), were prepared through a thermal imidization reaction. Dynamic scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) were utilized to verify the synchronization of the imidization of sulfonated poly(amic acid) (SPAA) and the crosslinking reactions of epoxy. The semi‐IPNs of epoxy/sulfonated polyimides (SPI‐EPX) exhibit excellent film‐forming characteristics and mechanical integrity at room temperature. Conductivities at 100 °C of 0.0243 S cm?1 (SPI‐EP30) and 0.0141 S cm?1 (SPI‐EP50) were obtained, which are similar to that of the Nafion 117 (0.0287 S cm?1). The increase in the conductivity of SPI‐EP(30,40) with temperature is more rapid than that of Nafion 117. The SPI‐EPX exhibited lower methanol permeability than did Nafion117. The hydrolytic stability of the SPI‐EPX was followed by FTIR spectroscopy at regular intervals. SPI‐EPX prepared using epoxy‐based semi‐IPNs of sulfonated polyimide, SPI‐EP(40,50), exhibited higher hydrolytic stability than the phthalic polyimides (five‐membered ring polyimides).The microstructure was analyzed using atomic force microscopy (AFM) in the tapping mode, which demonstrated that SPI‐EP50 exhibited a nanophase that was separated into an essentially reticulated and venous hydrophobic and hydrophilic domains. Transmission electron microscopy (TEM) confirmed widespread and well‐connected hydrophilic domains, proving the higher hydrolytic stability and strong proton‐transporting properties of the SPI‐EPX membrane. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 2262–2276, 2008  相似文献   

14.
A highly stable proton conductor has been developed from carbon sphere oxide (CSO). Carbon sphere (CS) generated from sucrose was oxidized successfully to CSO using Hummers’ graphite oxidation technique. At room temperature and 90 % relative humidity, the proton conductivity of thin layer CSO on microsized comb electrode was found to be 8.7×10?3 S cm?1, which is higher than that for a similar graphene oxide (GO) sample (3.4×10?3 S cm?1). The activation energy (Ea) of 0.258 eV suggests that the proton is conducted through the Grotthuss mechanism. The carboxyl functional groups on the CSO surface are primarily responsible for transporting protons. In contrast to conventional carbon‐based proton conductors, in which the functional groups decompose around 80 °C, CSO has a stable morphology and functional groups with reproducible proton conductivity up to 400 °C. Even once annealed at different temperatures at high relative humidity, the proton conductivity of CSO remains almost unchanged, whereas significant change is seen with a similar GO sample. After annealing at 100 and 200 °C, the respective proton conductivity of CSO was almost the same, and was about ~50 % of the proton conductivity at room temperature. Carbon‐based solid electrolyte with such high thermal stability and reproducible proton conductivity is desired for practical applications. We expect that a CSO‐based proton conductor would be applicable for fuel cells and sensing devices operating under high temperatures.  相似文献   

15.
Polymer composites with carbon‐based nano‐fillers have generated significant interest in industry and science because of their multifunctional and valuable properties. An APA‐functionalized GO nanofiller (GO–APA) was prepared through the reaction between graphene oxide (GO) and 3‐aminophenyl acetylene (APA) in dimethylformide (DMF) with ammonia hydroxide. Furthermore the PDSEPE/GO–APA composites were made from Poly(dimethysilyleneethynylenephenylene ethynylene) (PDSEPE) and GO–APA. FT‐IR, XRD, XPS, SEM, DSC and TGA techniques were used to characterize the chemical compositions and physical and chemical properties of GO–APA and PDSEPE/GO–APA composites. As a result, the prepared PDSEPE/GO–APA composites show high thermal stabilities, excellent electrical conductivity and good flexural strength. When the weight percentage of GO–APA reaches 0.5%, the PDSEPE/GO–APA composite electrical conductivity increases by 6 orders of magnitude and the flexural strength improves by nearly 33% compared with that of cured PDSEPE resin. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

16.
In the present study, the synergistic effect of hybrid boron nitride (BN) with graphene on the thermal conductivity of epoxy adhesives has been reported. Graphene was prepared by chemical reduction of graphite oxide (GO) in a mixture of concentrated H2SO4/H3PO4 acid. The particle size distribution of GO was found to be ~10 μm and a low contact angle of 54° with water indicated a hydrophilic surface. The structure of prepared graphene was characterized by Fourier transform infrared (FTIR), X‐ray diffraction (XRD), Raman spectroscopy and atomic force microscopy (AFM). The thermal conductivity of adhesives was measured using guarded hot plate technique. Test results indicated an improvement in the thermal conductivity up to 1.65 W/mK, which was about ninefold increase over pristine epoxy. Mechanical properties of different epoxy formulations were also measured employing lap shear test. The surface characterization of different epoxy adhesive systems was characterized through XRD, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies. Fourier transform infrared also served to determine the nature of interactions between filler particles and epoxy resin. Non‐isothermal differential scanning calorimetric (DSC) technique was used to investigate the effects of graphene and BN particles on the cure kinetics and cross‐linking reaction of epoxy cured with amine curing agent. The Kissinger equation, the model‐free isoconversional Flynn–Wall–Ozawa method and the Ozawa model were used to analyze the kinetic parameter. Copyright © 2017 John Wiley & Sons, Ltd.  相似文献   

17.
Proton conductivities of layered solid electrolytes can be improved by minimizing strain along the conduction path. It is shown that the conductivities (σ) of multilayer graphene oxide (GO) films (assembled by the drop‐cast method) are larger than those of single‐layer GO (prepared by either the drop‐cast or the Langmuir‐Blodgett (LB) method). At 60 % relative humidity (RH), the σ value increases from 1×10?6 S cm?1 in single‐layer GO to 1×10?4 and 4×10?4 S cm?1 for 60 and 200 nm thick multilayer films, respectively. A sudden decrease in conductivity was observed for with ethylenediamine (EDA) modified GO (enGO), which is due to the blocking of epoxy groups. This experiment confirmed that the epoxide groups are the major contributor to the efficient proton transport. Because of a gradual improvement of the conduction path and an increase in the water content, σ values increase with the thickness of the multilayer films. The reported methods might be applicable to the optimization of the proton conductivity in other layered solid electrolytes.  相似文献   

18.
Copper foils have been widely used in microelectronic devices. Adequate adhesion between copper foils to various substrates, such as Si, SiO2, polyimide, is crucial to high performance of these devices. The adhesion between a new high temperature adhesive, aromatic thermosetting copolyester (ATSP), and various copper foils, namely, zinc(Zn)‐coated copper foil, copper foil and nickel (Ni)‐coated copper foil was characterized by a 90° peel strength test. It was found that the peel strength of Zn‐coated copper foil to ATSP was 1050 N/m, which was more than three times higher than copper foil and five times that of Ni‐coated copper foil. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and X‐ray photoelectron spectroscopy (XPS) studies indicated that this higher adhesion results from the stronger mechanical interlocking due to the rougher surface of Zn‐coated copper foil, and from chemical reactions at the interface which occur during the curing process of ATSP on the Zn‐coated copper surface. In contract to the adhesive failure at the ATSP/Cu and ATSP/Ni interfaces, the failure mechanism of ATSP/Zn is both cohesive and adhesive. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

19.
《先进技术聚合物》2018,29(10):2665-2673
A phosphazene derivative flame retardant with a highly cross‐linked microsphere structure, named poly(cyclotriphosphazene‐c‐sulfonyldiphenol) (PCPS) microspheres, were synthesized by 1‐pot reaction and then applied on flame retarded epoxy (EP) resin. The microstructure and chemical composition of PCPS microspheres were characterized using scanning electron microscopy, transmission electron microscopy, and element mapping. The thermal stability of PCPS microspheres and PCPS/EP composites was explored through thermogravimetric analysis. Thermogravimetric data showed that the PCPS microspheres have excellent thermal stability, and the char yield is about 43% at the end of 800°C. The incorporation of PCPS microspheres significantly increased the char yield of PCPS/EP composites. The flammability was investigated by limited oxygen index tests and cone calorimeter. The limited oxygen index value of PCPS/EP composite was increased to 29.8 from 26.6 when 3 wt% of PCPS microspheres was added. Compared with neat EP, the flame retardancy was greatly improved. The peak heat release rate and smoke production rate of PCPS/EP composites were reduced by 45.0% and 43.6%, respectively. The mechanical properties including tensile strength and modulus were both improved due to the enhancement of PCPS microspheres. The PCPS microspheres act as a dual function for improving both the flame resistance and mechanical strength of PCPS/EP system.  相似文献   

20.
Controlling thermomechanical anisotropy is important for emerging heat management applications such as thermal interface and electronic packaging materials. Whereas many studies report on thermal transport in anisotropic nanocomposite materials, a fundamental understanding of the interplay between mechanical and thermal properties is missing, due to the lack of measurements of direction‐dependent mechanical properties. In this work, exceptionally coherent and transparent hybrid Bragg stacks made of strictly alternating mica‐type nanosheets (synthetic hectorite) and polymer layers (polyvinylpyrrolidone) were fabricated at large scale. Distinct from ordinary nanocomposites, these stacks display long‐range periodicity, which is tunable down to angstrom precision. A large thermal transport anisotropy (up to 38) is consequently observed, with the high in‐plane thermal conductivity (up to 5.7 W m?1 K?1) exhibiting an effective medium behavior. The unique hybrid material combined with advanced characterization techniques allows correlating the full elastic tensors to the direction‐dependent thermal conductivities. We, therefore, provide a first analysis on how the direction‐dependent Young's and shear moduli influence the flow of heat.  相似文献   

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