Incorporation of nano-sized mesoporous MCM-41 material used as fillers in natural rubber composite

The nano-sized mesoporous MCM-41 (without template), and the modification of MCM-41 (without template) were used to prepare natural rubber (NR) composites. The effects of coupling agents γ-aminopropyltriethoxysilane (KH-550), γ-methacryloxypropyltrimethoxysilane (KH-570), bis-(γ-triethoxysilylpropyl)-tetrasulfide (Si-69), isopropyl tri-(dioctylpyrophosphate)titanate (NDZ-201) on the mechanical properties of the composites were also investigated. The results showed that the tensile properties of Natural rubber/mesoporous MCM-41 nanocomposite were improved as compared with those of NR compound. KH-570 had good effect on enhancing the overall properties of the composites. Scanning electron microscopy (SEM) observations revealed that the modified nano-sized MCM-41 material was well dispersed in the polymer matrix and the enhancement of the interface between the matrix and fillers was obtained.     

Functionalization of mesoporous MCM-41 for the delivery of curcumin as an anti-inflammatory therapy

In this study, mesoporous silica nanoparticles (MSNs) composed of MCM-41 were synthesized and modified with amine groups (i.e., NH₂) to form NH_2/MCM-41, which was loaded with curcumin (CUR) to form CUR@NH₂/MCM-41 to create an efficient carriers in drug delivery systems (DDSs). The three samples (i.e., pure MCM-41, NH₂/MCM-41, and CUR@NH₂/MCM-41) were characterized using X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area, Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transition electron microscopy (TEM), and a thermogravimetric analyzer (TGA). The study investigated the effect of the carrier dose, CUR concentration, pH, and contact time on the drug loading efficiency (DLE%) by adsorption. The best DLE% for MCM-41 and NH₂/MCM-41 was found to be 15.78 and 80%, respectively. This data demonstrated that the Langmuir isotherm had a greater correlation coefficient (R²) of 0.9840 for MCM-41 and 0.9666 for NH₂/MCM-41 than the Freundlich and Temkin isotherm models. A pseudo-second-order kinetic model seems to fit well with R² = 0.9741 for MCM-41 and R² = 0.9977 for NH₂/MCM-41. A phosphate buffer solution (PBS) with a pH of 7.4 was utilized to study CUR release behavior. As a result, the full release after 72 h was found to have a maximum of 74.1% and 29.95% for pure MCM-41 and NH₂/MCM-41, respectively. The first-order, Weibull, Hixson-Crowell, Korsmeyer-Peppas, and Higuchi kinetic release models were applied to releasing CUR from CUR@MCM-41 and CUR@NH₂/MCM-41. The Weibull kinetic model fit well, with R² = 0.944 and 0.96912 for pure MCM-41 and NH₂/MCM-41, respectively.     

Steam-assisted crystallization of TPA+-exchanged MCM-41 type mesoporous materials with thick pore walls

Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, ¹H–¹³C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show that the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.     

Influence of reduced graphene oxide on mechanical behaviors of sodium carboxymethyl cellulose

Sodium carboxymethyl cellulose/reduced graphene oxide (NaCMC/rGO) nanocomposite films were prepared by a simple solution mixing-evaporation method. The NaCMC/rGO nanocomposite films were characterized and compared with sodium carboxymethyl cellulose/graphene oxide (NaCMC/GO) nanocomposite films. The stability of the rGO dispersion, and the structural and mechanical properties of the composite films were investigated by UV–Vis spectrophotometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, and using a universal testing machine (UTM). The results revealed that CMC and rGO were able to form a homogenous mixture. Compared with pure CMC, the tensile strength and Young's modulus of the CMC/rGO nanocomposite films were considerably enhanced (by 72.52% and 131.79%, respectively) upon incorporation of 2 wt% rGO.     

Development and characterization of the composites based on mesoporous MCM-41 and polyethylene glycol and their properties

Novel MCM-41/polyethylene glycol composites have been synthesized using different ratios of MCM-41. The structure of the different composites was confirmed by using various characterization tools, including: thermal analyses (TGA and DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and field emission scanning electron microscopy (FE-SEM). The XRD and FT-IR results indicated that PEG interacts with MCM-41 via the formation of hydrogen bonds where no new phase was detected. The TGA analysis results demonstrated that the presence of MCM-41 practically affects the temperature of the main step of degradation. The DTA analysis demonstrated that an increase in the MCM-41 content up to 30 wt.% is accompanied by a continuous decrease in the melting point of PEG.     

Thermal and mechanical properties of phenolic-based composites reinforced by carbon fibres and multiwall carbon nanotubes

The thermal, mechanical and ablation properties of carbon fibre/phenolic composites filled with multiwall carbon nanotubes (MWCNTs) were investigated. Carbon fibre/phenolic/MWCNTs were prepared using different weight percentage of MWCNTs by compression moulding. The samples were characterized by scanning electron microscopy (SEM), flexural tests, thermal gravimetric analysis and oxyacetylene torch tests. The thermal stability and flexural properties of the nanocomposites increased by increasing MWCNTs content (wt% ⩽1), but they decreased when the content of MWCNTs was 2 wt%. The linear and mass ablation rates of the nanocomposites after modified with 1 wt% MWCNTs decreased by about 80% and 52%, respectively. To investigate the material post-test microstructure, a morphological characterization was carried out using SEM. It was shown that the presence of MWCNTs in the composite led to the formation of a strong network char layer without any cracks or opening.     

Synthesis of MCM-41 nanoparticles from stem of common reed ash silica and their application as substrate in electrooxidation of methanol

In this work, stem of common reed ash (SCRA) is introduced as a new source of silica in the preparation of mesoporous materials. Mesoporous silicate MCM-41 nanoparticles were synthesized hydrothermally using sodium silicate prepared from SCRA as a silica source. The characterization of MCM-41was carried out by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), N\(_{2}\) adsorption/desorption (BET) and transmission electron microscopy (TEM). SEM shows that MCM-41 nanoparticles are sphere-like with size in the range of 30–50 nm with some degree of agglomeration. TEM image of the synthesized sample shows the open framework structure of MCM-41. A type IV isotherm can be observed from adsorption/desorption curves, which is the characteristic of mesoporous materials. The prepared MCM-41 nanoparticles were used as substrate to facilitate the oxidation of methanol through the modification with an electroactive species. The modification was achieved by impregnation of MCM-41 pores with \(\hbox {Ni}^{2+}\) ions (Ni-doped MCM-41). A modified carbon paste electrode (CPE) was prepared by mixing Ni-doped MCM-41 with carbon paste (NiMCM-41CPE). Cyclic voltammetry of NiMCM-41CPE shows an increment in current density of methanol oxidation in comparison with CPE in alkaline solution. Moreover, a decrease in the overpotential of methanol oxidation occurred on the surface of modified electrode. The effects of some parameters such as scan rate and methanol concentration are also investigated on the behaviour of NiMCM-41CPE. Also, the heterogeneous electron transfer rate for the catalytic reaction (k) of methanol is calculated.     

A facile approach to prepare regenerated cellulose/graphene nanoplatelets nanocomposite using room-temperature ionic liquid

This study presents the preparation of regenerated cellulose (RC)/graphene nanoplatelets (GNPs) nanocomposites via room temperature ionic liquid, 1-ethyl-3-methylimidazolium acetate (EMIMAc) using solution casting method. The thermal stability, gas permeability, water absorption and mechanical properties of the films were studied. The synthesized nanocomposite films were characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The T20 decomposition temperature of regenerated cellulose improved with the addition of graphene nanoplatelets up to 5 wt%. The tensile strength and Young's modulus of RC films improved by 34 and 56%, respectively with the addition of 3 wt% GNPs. The nanocomposite films exhibited improved oxygen and carbon dioxide gas barrier properties and water absorption resistance compared to RC. XRD and SEM results showed good interaction between RC and GNPs and well dispersion of graphene nanoplatelets in regenerated cellulose. The FTIR spectra showed that the addition of GNPs in RC did not result in any noticeable change in its chemical structure.     

Study on synthesis of poly(GMA)-grafted Fe3O4/SiOX magnetic nanoparticles using atom transfer radical polymerization and their application for lipase immobilization

Functionalized superparamagnetic particles were prepared by atom transfer radical polymerization of glycidyl methacrylate onto the surface of modified Fe₃O₄/SiO_X nanoparticles. The obtained particles were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Candida rugosa lipase was covalently immobilized on the magnetic particles in mild condition via covalent binding with a higher activity recovery. The resulting immobilized lipase had better resistance to pH and temperature inactivation in comparison to free lipase, the adaptive pH and temperature ranges of lipase were widened, and it exhibited good thermal stability and reusability.     

Ultrasonic-assisted synthesis and magnetic studies of iron oxide/MCM-41 nanocomposite

Iron oxide nanoparticles were stabilized within the pores of mesoporous silica MCM-41 amino-functionalized by a sonochemical method. Formation of iron oxide nanoparticles inside the mesoporous channels of amino-functionalized MCM-41 was realized by wet impregnation using iron nitrate, followed by calcinations at 550 °C in air. The effect of functionalization level on structural and magnetic properties of obtained nanocomposites was studied. The resulting materials were characterized by powder X-ray diffraction (XRD), high-resolution transmission electron microscopy and selected area electron diffraction (HRTEM and SAED), vibrating sample and superconducting quantum interface magnetometers (VSM and SQUID) and nitrogen adsorption–desorption isotherms measurements. The HRTEM images reveal that the most of the iron oxide nanoparticles were dispersed inside the mesopores of silica matrix and the pore diameter of the amino-functionalized MCM-41 matrix dictates the particle size of iron oxide nanoparticles. The obtained material possesses mesoporous structure and interesting magnetic properties. Saturation magnetization value of magnetic iron oxide nanopatricles stabilized in MCM-41 amino-functionalized by in situ sonochemical synthesis was 1.84 emu g⁻¹. An important finding is that obtained magnetic nanocomposite materials exhibit enhanced magnetic properties than those of iron oxide/MCM-41 nanocomposite obtained by conventional method. The described method is providing a rather short preparation time and a narrow size distribution of iron oxide nanoparticles.     

Effect of nanoclays on physico-mechanical properties and adhesion of polyester-based polyurethane nanocomposites: structure–property correlations

Polyester–polyurethane nanocomposites based on unmodified and modified montmorillonite clays were compared in terms of their morphology, mechanical, thermal, and adhesive properties. Excellent dispersion of the modified nanoclay in polymer with 3 wt% loading was confirmed from X-ray diffraction, and low-, and high-magnification transmission electron micrographs. The properties of the clay-reinforced polyurethane nanocomposites were a function of nature and the content of clay in the matrix. The nanocomposite containing 3 wt% modified clay exhibits excellent improvement in tensile strength (by ~100%), thermal stability (20 °C higher), storage modulus at 25 °C (by ~135%), and adhesive properties (by ~300%) over the pristine polyurethane.     

In situ production of Al–TiB<Subscript>2</Subscript> nanocomposite by double-step mechanical alloying

An in situ Al–TiB₂ nanocomposite was synthesized by mechanical alloying (MA) of pure Ti, B and Al powder mixture in a planetary ball mill. A double-step process was used to prevent the formation of undesirable phases like Al₃Ti intermetallic compound. In the first step, a powder mixture was tailored to obtain nominal Al–90 wt% TiB₂ composition and the second step involved the addition of Al to the mixture in order to achieve Al–20 wt% TiB₂. The structural and thermal characteristics of powder particles were studied by X-ray diffractometry (XRD), scanning electron microscopy (SEM), differential scanning calorimetery (DSC), and transmission electron microscopy (TEM). The results showed that the MA process leads to the in situ formation of nanosized TiB₂ particles in an Al matrix with a uniform distribution. It was also found that the double stage addition of aluminum can prevent the formation of undesirable compounds even after annealing at high temperatures_.     

Poly (3,4-ethylenedioxythiophene) (PEDOT) and poly (3,4-ethylenedioxythiophene)-few walled carbon nanotube (PEDOT-FWCNT) nanocomposite based thin films for Schottky diode application

Transparent, conductive films of poly (3,4-ethylenedioxythiophene) (PEDOT) and poly (3,4-ethylenedioxythiophene)-few walled carbon nanotube (PEDOT-FWCNT) nanocomposite were synthesized by in-situ oxidative polymerization and investigated for their Schottky diode property. The prepared films were characterized by UV–Vis spectroscopy, thermal gravimetric analysis (TGA), surface resistivity, cyclic voltametery, scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). SEM reveals the formation of homogeneous and adhesive polymer films while HRTEM confirms the uniform wrapping of polymer chains around the nanotube walls for PEDOT-FWCNT film. Improved thermal stability, conductivity and charge storage property of PEDOT in the presence of FWCNT is observed. Among different compositions, 5 wt. % of FWCNT is found to be optimum with sheet resistance and transmittance of 500 Ω sq⁻¹ and 77%, respectively. Moreover, the electronic and junction properties of polymer films were studied and compared by fabricating sandwich type devices with a configuration of Al/PEDOT or PEDOT-FWCNT nanocomposite/indium tin oxide (ITO) coated glass. The measured current density-voltage characteristics show typical rectifying behavior for both configurations. However, enhanced rectification ratio and higher forward current density is observed in case of PEDOT-FWCNT based Schottky diode. Furthermore, reliability test depicts smaller hysteresis effect and better performance of PEDOT-FWCNT based diodes.     

A mechanistic study on electromagnetic shielding effectiveness of polysulfone/carbon nanofibers nanocomposites

The present study aims to produce a light weight electromagnetic interference (EMI) shielding material from carbon nanofibers (CNFs)-based polysulfone (PSU) nanocomposites. EMI shielding effectiveness (EMI SE) was studied by analyzing the electromagnetic wave transmission, reflection, and absorption characteristics of nanocomposites. The electrical conductivity and EMI SE of the nanocomposite with different weight percentage of CNFs (3–10 wt%) were investigated at room temperature and the measurement of EMI SE was carried out in a frequency range of 8.2–12.4 GHz (X-band). The mechanism of EMI shielding of PSU/CNFs nanocomposite has been well explained by comparing the contribution of reflection and absorption to the total EMI SE. The state of dispersion of CNFs and PSU–CNFs interaction was studied by high resolution transmission electron microscopy and scanning electron microscopy. The thermal stability of nanocomposite studied from thermogravimetric analysis was increased after addition of CNFs to PSU matrix. Electrical conductivity of nanocomposite followed power law model of percolation theory having a percolation threshold Φ_c = 0.0079 vol% (0.9 wt%) and exponent t = 1.73. The EMI SE of nanocomposites with thickness of 1 mm was 19–45 decibel (dB) at 3–10 wt% CNFs loading. This high thermal stability and high EMI SE suggest the potential use of PSU/CNFs nanocomposite as effective lightweight EMI shielding material in different electronic applications.     

Investigation of physical and chemical properties of polypropylene hybrid nanocomposites

Hybrid nanocomposites fabricated based on an optimized physical and chemical properties modified polypropylene (PP)/polypropylene grafted maleic anhydride (PP-g-MA) with varied concentrations (1–7 wt% at a step of 2 wt%) of organoclay, montmorillonite (MMT). The morphology of the nanocomposites was studied by scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). It was found that partly intercalated and partly exfoliated structure (intercalated–exfoliated structures) existed in the system. The degree of exfoliation is a key factor to determine the reinforcement efficiency. The ratio of exfoliation to intercalation plays an important role in determining the properties of PP nanocomposites and only completely exfoliated silicate layers can significantly improve the properties. PP hybrid nanocomposites showed good thermal stability in the thermogravimetric analysis (TGA). Introduction of ∼3% MMT in the nanocomposites increased the onset temperature of degradation by 27.5 °C compared to that of pure PP, while the 5 wt% MMT resulted the maximum hardness in these nanocomposites. The solvent resistance of PP hybrid nanocomposites slightly increased with increasing the clay content.     

Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica

Synthesis of mesoporous MCM-41 materials at room temperature using less expensive polymeric version of ethyl silicate (40 wt% SiO₂) as a source of silica was established. The influence of crucial synthesis parameters such as molar ratios of H₂O/NH₄OH, NH₄OH/SiO₂ and CTMABr/SiO₂ in gel on the quality of the phase formed was investigated. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and low temperature N₂ adsorption-desorption isotherms have been employed to characterize the products. The magnitude of orderness, textural properties and thermal stability of the Si-MCM-41 samples prepared under identical judiciously pre-controlled synthesis conditions using ethyl silicate and conventional tetraethyl orthosilicate (TEOS) were assessed. Even though, ethyl silicate has proved to be suitable source for the preparation of MCM-41 at room temperature, there exists an optimum value of H₂O/NH₄OH for different NH₄OH/SiO₂ molar ratios in the gel. Changes in the morphology were observed when NH₄OH/SiO₂, H₂O/NH₄OH molar ratios in the gels were changed.     

Synthesis and characterization of super-microporous material with enhanced hydrothermal stability

Super-microporouos silicon material with high hydrothermal stability denoted as MCM-41-T has been prepared from mesoporous MCM-41 by high temperature treatment. The structural and chemical property of MCM-41-T has been characterized by X-ray diffraction, transmission electron microscopy, N₂ adsorption-desorption, infrared spectroscopy and ²⁹Si MAS NMR. The characteristic results show that Si-OH groups are forced to condense by high temperature treatment, and the pore size of MCM-41-T is around 1.5 nm in the super-microporous range. Compared with the original material MCM-41, the hydrothermal stability of MCM-41-T has been significantly enhanced.     

Nanodiamond/poly (lactic acid) nanocomposites: Effect of nanodiamond on structure and properties of poly (lactic acid)

Nanodiamond (ND)/poly (lactic acid) (PLA) nanocomposites with potential for biological and biomedical applications were prepared by using melting compound methods. By means of transmission electron microscopy (TEM), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Thermogravimetric analyses (TGA), Dynamic mechanical analyses (DMA), Differential scanning calorimetry (DSC) and Tensile test, the ND/PLA nanocomposites were investigated, and thus the effect of ND on the structural, thermal and mechanical properties of polymer matrix was demonstrated for the first time. Experimental results showed that the mechanical properties and thermal stability of PLA matrix were significantly improved, as ND was incorporated into the PLA matrix. For example, the storage modulus (E′) of 3 wt% ND/PLA nanocomposites was 0.7 GPa at 130 °C which was 75% higher than that of neat PLA, and the initial thermal decomposition was delayed 10.1 °C for 1 wt% ND/PLA nanocomposites compared with the neat PLA. These improvements could be ascribed to the outstanding physical properties of ND, homogeneous dispersion of ND nanoclusters, unique ND bridge morphology and good adhesion between PLA matrix and ND in the ND/PLA nanocomposites.     

Fabrication of thermoplastic polyester elastomer/layered zinc hydroxide nitrate nanocomposites with enhanced thermal,mechanical and combustion properties

The objective of this study is to explore the potential of layered zinc hydroxide nitrate modified with sodium benzoate as nanoparticle in thermoplastic polyester elastomer (TPEE). The organically modified zinc hydroxide nitrate was compounded with TPEE using solution blending method. The nanocomposite structure was characterized by means of X-ray diffraction and transmission electron microscopy. The results showed that the nanoparticle was homogenously dispersed in TPEE matrix, and partially exfoliated structure was formed. The thermal behavior, mechanical and thermal combustion properties of the novel nanocomposite were studied respectively through differential scanning calorimeter (DSC), dynamic mechanical analysis (DMA) and microscale combustion calorimeter (MCC). For the nanocomposite containing 7 wt% nanoparticle, the crystallization temperature evaluated by DSC was increased by 10 °C. The storage modulus at −95 °C measured by DMA was improved by around 26%. The heat release capacity (an indicator of a material fire hazard) from MCC testing was reduced by about 56% (compared to the results of neat TPEE).     

酞菁钴/MCM-41的制备及其可见光催化性能

以MCM-41分子筛为载体,采用浸渍法将酞菁钴负载到分子筛上以氙灯为光源降解甲基橙溶液。对负载型酞菁钴催化剂进行FT-IR、XRD、SEM表征,结果表明所制催化剂负载效果良好,且分子筛结构未发生改变。以甲基橙溶液为模拟处理对象,研究催化剂的催化性能,考察了光照、酞菁钴负载、催化剂用量等因素对催化效果的影响。结果表明,氧气充足时,在光照条件下、0.04g负载型酞菁钴催化剂处理200mL的0.05g/L甲基橙溶液能够有很好的处理效果,2h降解率能够达到98.3%,且重复利用4次后降解率仍能达到90%。