The study and measurement of the shielding effectiveness (SE) of planar materials is required to predict the suitability of a certain material to form an enclosed electromagnetic shield. One of the most widely used standards for measuring the SE of planar materials is ASMT D4935-18. It is based on a coaxial sample holder (CSH) that operates up to 1.5 GHz. Due to this standard's frequency limitations, new variants with higher frequency limits have been developed by decreasing the size of the CSH conductors and the samples. However, this method and its high-frequency variants require two types of samples with very specific geometries and sizes. This method is unsuitable for certain types of nanomaterials due to their complex mechanization at such undersized scales. This contribution proposes an alternative SE measurement method based on an absorber box that mitigates the problems presented by the ASTM D4935-18 standard. The SE of rigid nanomaterial samples based on several concentrations of multi-walled carbon nanotubes (MWCNT) and two different fiber reinforcements have been obtained.
Innovative dendrimer-modified graphene oxide (GO) aerogels are reported by employing generation 3.0 poly(amidoamine) (PAMAM) dendrimer and a combined synthesis approach based on the hydrothermal method and freeze-casting followed by lyophilization. The properties of modified aerogels were investigated with the dendrimer concentration and the addition of carbon nanotubes (CNTs) in varying ratios. Aerogel properties were evaluated via scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). The obtained results indicated a strong correlation of the N content with the PAMAM/CNT ratio, where optimum values were revealed. The CO2 adsorption performance on the modified aerogels increased with the concentration of the dendrimer at an appropriate PAMAM/CNT ratio, reaching the value of 2.23 mmol g(-1) at PAMAM/CNT ratio of 0.6/0.12 (mg mL(-1)). The reported results confirm that CNTs could be exploited to improve the functionalization/reduction degree in PAMAM-modified GO aerogels for CO2 capture.
This article presents novel poly(amidoamine) (PAMAM) dendrimer-modified with partially-reduced graphene oxide (rGO) aerogels, obtained using the combined solvothermal synthesis-freeze-casting approach. The properties of modified aerogels are investigated with varying synthesis conditions, such as dendrimer generation (G), GO:PAMAM wt. ratio, solvothermal temperature, and freeze-casting rate. Scanning electron microscopy, Fourier Transform Infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy are employed to characterize the aerogels. The results indicate a strong correlation of the synthesis conditions with N content, N/C ratio, and nitrogen contributions in the modified aerogels. Our results show that the best CO2 adsorption performance was exhibited by the aerogels modified with higher generation (G7) dendrimer at low GO:PAMAM ratio as 2:0.1 mg mL−1 and obtained at higher solvothermal temperature and freeze-casting in liquid nitrogen. The enclosed results are indicative of a viable approach to modify graphene aerogels towards improving the CO2 capture.
The present paper describes a greener sustainable route toward the synthesis of NIPHUs. We report a highly efficient solvent-free process to produce [4,4′-bi(1,3-dioxolane)]-2,2′-dione (BDC), involving CO2, as renewable feedstock, and bis-epoxide (1,3-butadiendiepoxide) using only metal–organic frameworks (MOFs) as catalysts and cetyltrimethyl-ammonium bromide (CTAB) as a co-catalyst. This synthetic procedure is evaluated in the context of reducing global emissions of waste CO2 and converting CO2 into useful chemical feedstocks. The reaction was carried out in a pressurized reactor at pressures of 30 bars and controlled temperatures of around 120–130 °C. This study examines how reaction parameters such as catalyst used, temperature, or reaction time can influence the molar mass, yield, or reactivity of BDC. High BDC reactivity is essential for producing high molar mass linear non-isocyanate polyhydroxyurethane (NIPHU) via melt-phase polyaddition with aliphatic diamines. The optimized Al-OH-fumarate catalyst system described in this paper exhibited a 78% GC-MS conversion for the desired cyclic carbonates, in the absence of a solvent and a 50 wt % chemically fixed CO2. The cycloaddition reaction could also be carried out in the absence of CTAB, although lower cyclic carbonate yields were observed.
Ethylenediamine-modified graphene oxide-based three-dimensional aerogels were fabricated by one-step hydrothermal technique. The influence of oxidation conditions and starting graphite material was studied by elemental analysis, X-ray photoelectron spectroscopy, Raman spectroscopy and Scanning electron microscopy. The CO2 adsorption properties of modified aerogels were tested. The results show the distribution of oxygen groups and type of GO altered by oxidation conditions and graphite nature induce a different N doping configuration in the modified aerogel and a higher surface utilization factor for the CO2 capture. The GO-based aerogel obtained from expanded graphite exhibited the best performance (2-fold the un-modified one), reaching a value of 1.18 mmol g(-1) at 1 bar and 298 K, thus indicating the high potential of the present approach towards enhancing the CO2 capture.
Low-density three-dimensional (3D) N-doped graphene aerogels by a one-step solvothermal method in the presence of ethylenediamine (EDA) are reported. The gelation, formation, and properties of the aerogels were studied with solvothermal conditions, namely, operating temperature, time, graphene oxide (GO) concentration, and the GO/EDA w/w ratio. Two ranges of solvothermal conditions are employed: one involving an operating temperature below 100 °C and a conventional chemical reduction of GO with EDA at atmospheric pressure and a second one employing a higher temperature range up to 165 and a high pressure reduction with EDA. The results show that both solvothermal approaches allow for the fabrication of homogeneous N-doped 3D graphene aerogels with density values close to 10 mg cm−3. The measurements indicated that low values of GO concentration, temperature, and EDA are optimum for obtaining low-density 3D aerogels. N doping is improved with an EDA amount in lower temperature conditions. The N doping mechanism below 100 °C is dominated by the epoxy ring opening while at temperatures up to 165 °C both epoxy ring opening and amidation take place. The CO2 adsorption properties are strongly controlled by the nitrogen configuration, namely, pyridinic nitrogen in terms of its density.
Ultra-light eco-friendly graphene oxide (GO)-based aerogels are reported by simple one-step solvothermal self-assembly. The effect of varying parameters such as C/O ratio of GO; reducing agent amount; temperature; and duration on the properties of the aerogels was studied. The structural and vibrational features and hydrophobic surface properties of the obtained aerogels were obtained by XRD; FTIR; XPS; Raman; SEM; and contact angle measurements. The effect of synthesis conditions on the engine oil and organic solvent absorption properties was assessed. The results indicated that the lower the C/O ratio of GO, the better the absorption properties, with the best performance for oil uptake reaching 86 g g−1. The obtained results indicate the approach based on ice-templating and the tailoring of oxygen content in GO make the resulting aerogels potential candidates for use in oil spill and organic solvent treatments.
Multiwall carbon nanotubes (MWCNT) and multilayer graphene (MLG) were studied as microwave susceptor additives for polymers. Different percentages of both nanoparticles were added to polypropylene by melt compounding in order to study the microwave absorption and the polymer heating. Polypropylene was selected as polymer matrix due to its unpolar nature to avoid the influence of polymer polarity and evaluate the influence of the nanoparticles. Electrochemical spectroscopy impedance measurements were carried out to evaluate the conductive and dielectric properties of nanocomposites. Results showed that nanocomposites with higher electrical conductivity have better capacity of absorbing microwave radiation. High values of permittivity and loss tangent also increases the microwave radiation absorption and the ability of the material to convert this electromagnetic radiation into heat. Carbon nanotubes showed better microwave susceptor behavior than graphene multilayer. Nanocomposites with 1% w/w of carbon nanotubes can be compared with the heating efficiency of a polypropylene filled with 10% w/w of multilayer graphene. The higher efficiency of carbon nanotubes it is explained by their higher electrical conductivity and optimal dielectric properties of the nanocomposites compared to multilayer graphene polymer systems.
Carbon nanotubes dispersion within the polymer matrix is a very important factor to take into account when developing new nanocomposites with optimized properties. In this article, dispersion studies have been carried out with polypropylene filled with 1% of multiwall carbon nanotubes. The nanocomposites were obtained by melt compounding in a corotative twin screw extruder. Processing parameters as screw speed, screw configuration and feeding technology were modified to analyse their effect onto carbon nanotubes dispersion. Developed nanocomposites were exposed to microwave heating (5.8 GHz, 700 W, 60 min) and heating temperature was monitored. The relation between dispersion level of carbon nanotubes and heating effectiveness was studied. Microwave heating efficiency of carbon nanotubes was increased as dispersion was improved. Electrical conductivity of nanocomposites was measured and used as indirect variable of microwave heating susceptor of carbon nanotubes nanocomposites. Higher electrical conductivity indicates a better microwave susceptor propertiy of the nanocomposite. POLYM. ENG. SCI., 56:1321–1329, 2016. © 2016 Society of Plastics Engineers
ABSTRACTIn this work, we present thermoplastic nanocomposites of polycarbonate (PC) matrix with hybrid nanofillers system formed by a melt‐mixing approach. Various concentrations of multi‐walled carbon nanotubes (MWCNT) and graphene nanoplatelets (GnP) were mixed in to PC and the melt was homogenized. The nanocomposites were compression molded and characterized by different techniques. Torque dependence on the nanofiller composition increased with the presence of carbon nanotubes. The synergy of carbon nanotubes and GnP showed exponential increase of thermal conductivity, which was compared to logarithmic increase for nanocomposite with no MWCNT. Decrease of Shore A hardness at elevated loads present for all investigated nanocomposites was correlated with the expected low homogeneity caused by a low shear during melt‐mixing. Mathematical model was used to calculate elastic modulus from Shore A tests results. Vicat softening temperature (VST) showed opposite pattern for hybrid nanocomposites and for PC‐MWCNT increasing in the latter case. Electrical conductivity boost was explained by the collective effect of high nanofiller loads and synergy of MWCNT and GnP. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 42536.
ABSTRACTIn this work, nanocomposites of polycarbonate/acrylonitrile‐butadiene‐styrene (PC/ABS) with various loads of multiwall carbon nanotubes (MWCNT) are investigated. Material is previously formed by masterbatch dilution approach and further processed by injection molding at various velocities. Microscopic characterization of nanocomposites morphology reveals stronger dependence of MWCNT dispersion on processing parameters at higher nanofiller load. Dispersion of carbon nanotubes at various distances from the injection gate is studied by Raman spectroscopy showing lower deviation at elevated injection velocity. Nanoindentation results that are in agreement with uniaxial tensile testing show a slight decrease of nanocomposites' mechanical performance at 3.0 wt % MWCNT in samples injected at reduced velocity. This is explained by the increase of agglomeration behavior at these conditions. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 42014.
In this study, nanocomposites of polypropylene (PP) with various loadings of multi-wall carbon nanotubes (MWCNT) and graphene nanoplatelets (GnP) were formed by masterbatch dilution/mixing approach from individual masterbatches PP-MWCNT and PP-GnP. Melt mixing on a twin-screw extruder at two different processing temperatures was followed by characterization of morphology by transmitted-light microscopy including the statistical analysis of agglomeration behavior. The influence of processing temperature and weight fractions of both nanofillers on the dispersion quality is reported. Thermal properties of the nanocomposites investigated by DSC and TGA show sensitivity to the nanofillers weight fraction ratio and to processing conditions. Electrical conductivity is observed to increase up to an order of magnitude with the concentration of each nanofiller increasing from 0.5 wt % to 1.0 wt %. This is related with a decrease of electrical conductivity observed for unequal concentration of both nanofillers. This particular behavior shows the increase of electrical properties for higher MWCNT loadings and the increase of thermo-mechanical properties for higher GnP loadings. (c) 2015 Wiley Periodicals, Inc.
ABSTRACTThe influence of injection molding parameters on electrical properties and morphology of PC/ABS‐MWCNT nanocomposites is presented in this article. Investigation is based on the masterbatch of 5.0 wt % carbon nanotubes obtained by melt‐mixing. Further processing includes dilution of this nanocomposite to desired concentrations on twin‐screw extruder and injection molding or direct dilution of masterbatch in injection molding. Additionally, reprocessing of materials formed by compression and injection molding is presented along with the change in electrical conductivity. Morphology differs strongly between the two processing paths showing change in agglomeration behavior between nanotubes concentrations. Electrical properties show dependence on injection velocity and melt temperature in both applied processing paths. Moreover, electrical conductivity recovery is proved after injection and compression molding. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 2152–2158, 2013
Nanocomposites of polycarbonate/acrylonitrile-butadiene-styrene (PC/ABS) with multiwall carbon nanotubes (MWCNT) prepared by masterbatch dilution are investigated in this work. Melt compounding with twin screw extruder is followed by complete characterization of morphology, rheological-, mechanical-, and thermal-properties of the nanocomposites. Light-transmission- and scanning electron microscopy shows the preferential location of MWCNT in the PC. Nevertheless, relatively good dispersion in the whole matrix is achieved, what is corroborated with the specific mechanical energy. The study of viscoelastic properties of PC/ABS-MWCNT shows the fluid-solid transition below 0.5 wt % MWCNT. Beyond this point the continuous nanofiller network is formed in the matrix promoting the reinforcement. Addition of 0.5 wt % MWCNT reduces ductility of PC/ABS and enhances Young's modulus by about 30% and yield stress by about 20%. Moreover, theoretical values of stiffness calculated within this work agree with the experimental data. Electrical conductivity, showing percolation at 2.0 wt % MWCNT, are influenced by processing temperature. (c) 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40271.
4 wt% multiwalled carbon nanotubes (MWCNTs) were incorporated into a miscible blend of polyphenylenether/polystyrene (PPE/PS) on a twin-screw extruder at a screw speed of 600 rpm. The masterbatch obtained was diluted at 400 and 600 rpm to obtain lower MWCNT loadings in PPE/PS. Electron microscopy & optical microscopy images show very good MWCNT dispersion even at high filler loadings of 4 wt%, but slightly larger agglomerate size fractions are observable at higher screw speeds. While MWCNT addition enhanced the thermal stability of PPE/PS, a small change in glass transition was observed on the composites at different filler concentrations compared to PPE/PS. The specific heat capacity at glass transition decreases considerably until 2 wt% MWCNT and levels down thereafter for both processing conditions pointing to enhanced filler-matrix interaction at lower loadings. Storage modulus of the nanocomposites was enhanced significantly on MWCNT incorporation with reinforcing effect dropping considerably as a function of temperature, especially at lower filler contents. The modulus and the tensile strength of PPE/PS were only marginally enhanced in spite of excellent MWCNT dispersion in the matrix. Electrical percolation occurs at 0.4 wt% MWCNT content, and the electrical conductivity of 0.5 wt% MWCNT reinforced PPE/PS was close to 12 orders in magnitude higher compared to PPE/PS.
Composites of thermoplastic polyurethane (TPU) and ultra-thin graphite (UTG) with concentrations ranging from 0.5 wt.% to 3 wt.% were prepared using a solution compounding strategy. Substantial reinforcing effects with increased loadings are achieved. Compared to neat TPU, values for storage modulus and shear viscosity are enhanced by 300% and 150%, respectively, for UTG concentrations of 3 wt.%. Additionally, an enhancement of thermal properties is accomplished. The crystallization temperature and thermal stability increased by 30 °C and 10 °C, respectively, compared to neat TPU. Furthermore, the use of oxidized UTG (UTGO) with its added functional oxygen groups suggests the presence of chemical interactions between UTG and TPU, which additionally impact on the thermal properties of the corresponding composites. Controlling the oxidation degree, thus offers further possibilities to obtain composites with tailored properties. The presented approach is straightforward, leads to homogeneous TPU-UTG composites with improved materials properties and is especially suitable for commercial UTG materials and further up-scaled production.
Summary: Nanocomposites of commercial PC/ABS matrix filled with multi-walled carbon nanotubes (MWCNT) suspended in ethyl alcohol were compounded on twin-screw co-rotating extruder and subsequently injection molded varying injection speed and temperature. Optical microscopy (OM) and scanning electron microscopy (SEM) were used to characterize the morphology of nanocomposites. A presence of fine agglomerates of carbon nanotubes was observed. The elastic modulus and stress at yield point increased with MWCNT content for all nanocomposites. However, higher values of yield stress were obtained for lower injection velocities, due to more homogeneous dispersion at mild injection molding conditions.
The dispersion of multiwalled carbon nanotubes (MWCNT) in thermoplastic polyurethanes (TPUs) was evaluated in a corotative twin-screw extruder through a melt-blending process. A specific experimental design was prepared with different parameters, such as screw speed, screw design, and carbon nanotube loading, taken into account. The obtained samples were characterized by thermogravimetric analysis, light transmission microscopy, field emission scanning electron microscopy, dynamic rheometry, dynamic mechanical analysis, and electrical conductivity. This work focuses on the influence of the compounding parameters in the dispersion quality of MWCNTs in a TPU matrix to optimize them for an industrial scaleup. (C) 2011 Wiley Periodicals, Inc. J Appl Polym Sci 122: 3745-3751, 2011
The dispersion of multi-walled carbon nanotubes in thermoplastic polyurethanes has been done in co-rotative twin screw extruder through a melt blending process. A specific experimental design was prepared taking into account different compounding parameters such as feeding, temperature profile, screw speed, screw design, and carbon nanotube loading. The obtained samples were characterized by thermogravimetric analysis (TGA), light transmission microscopy, dynamic rheometry, and dynamic mechanical analysis. The objective of this work has been to study the dispersion quality of the carbon nanotubes and the effect of different compounding parameters to optimize them for industrial scale-up to final applications.