Synthesis of hybrid ZnO/CNTs nanoparticles and their reinforcement in nylon‐6 polymer fibers

In this investigation, in situ synthesis of zinc oxide nanoparticles in the presence of multiwalled carbon nanotubes (CNTs) have been carried out using a sonochemical technique. Zinc(II)acetate was used as a source of ZnO in the presence of ethylene glycol (EG) to obtain zinc oxide (ZnO) nanoparticles. The synthesized hybrid ZnO/CNTs nanoparticles were used as reinforcements to enhance the mechanical, thermal and UV absorbing properties of Nylon‐6 composite fibers. The polymer nanocomposites (PNC) were fabricated by dry mixing Nylon‐6 polymer powder with the ZnO/CNTs hybrid nanoparticles as the first step, then followed by the drying and melt extrusion process of fiber materials in a single‐screw extruder. The extruded fibers were stretched and stabilized using a godet set‐up and wound on a Wayne filament winder machine. The hybrid ZnO/CNTs infused Nylon‐6 composite fibers were compared with commercial ZnO, CNTs infused Nylon‐6 composite fibers and neat Nylon‐6 fibers for their structural and thermal properties. The morphological characteristics of ZnO/CNTs nanoparticles were carried out using X‐ray diffraction and transmission electron microscopy (TEM) techniques. The Nylon‐6 PNC fibers which were of ～80 μ size were tested mechanically. The tensile tests revealed that failure stress of the 1% infused ZnO/CNTs Nylon‐6 PNC fibers is about 73% higher than the neat extruded Nylon‐6 fiber and the improvement in the tensile modulus is 377.4%. The DSC results show an increase in the glass transition temperature and crystallization for ZnO/CNTs infused Nylon‐6 PNC fibers. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effects of interface bonding properties on cyclic tensile behavior of unidirectional C/Si3N4 and SiC/Si3N4 composites

In this paper, the effect of fiber/matrix interface bonding properties on the cyclic loading/unloading tensile stress?strain hysteresis loops of 2 different ceramic‐matrix composites (CMCs), ie, C/Si₃N₄ and SiC/Si₃N₄, has been investigated using micromechanical approach. The relationships between the damage mechanisms (ie, matrix multicracking saturation, fiber/matrix interface debonding and fibers failure), hysteresis dissipated energy and internal frictional damage parameter have been established. The damage evolution processes under cyclic loading/unloading tensile of C/Si₃N₄ and SiC/Si₃N₄ composites corresponding to different fiber/matrix interface bonding properties have been analyzed through damage models and interface frictional damage parameter. For the C/Si₃N₄ composite with the weakest fiber/matrix interface bonding, the composite possesses the lowest tensile strength and the highest failure strain; the hysteresis dissipated energy increases at low peak stress, and the stress?strain hysteresis loops correspond to the interface partially and completely debonding. However, for the SiC/Si₃N₄ composite with weak interface bonding, the composite possesses the highest tensile strength and intermediate failure strain; and the hysteresis dissipated energy increases faster and approaches to a higher value than that of composite with the strong interface bonding.     

Preparation and characterization of nano/micro‐calcium carbonate particles/polypropylene composites

A new kind of polypropylene (PP)/CaCO₃ composites was prepared on a twin screw extruder with the nanoparticle content of 5 wt % and the 2500 mesh microparticle content of 15 wt %. The mechanical property of four different samples [pure PP (1) , PP filled with 15 wt % microCaCO₃ particle composites (2) , PP filled with 5 wt % nanoCaCO₃ particle composites (3) and PP filled with micro/nano‐CaCO₃ complex size particle composites (4) ] was investigated through tensile tests, notched Izod impact tests and SEM. The results indicated that the sample 4 had the best mechanical property. The proofs of SEM showed that the high impact energy could lead to debonding and creating microcavitation between the nanoparticle and polymer interface if the polymer was filled with the nanoparticles. This process could absorb a lot of mechanical failure energy, but too much mechanical failure energy would lead to the enlargement of microcavitation and the destruction of the composites in sample 3 . In sample 4 , the microparticle could be used to prevent the enlargement of microcavitation in the matrix polymer under the higher impact failure energy. In this article, the model of the impacting failure process of micro/nanoCaCO₃/PP composites was established. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Fabrication and properties of high performance PEEK/Si3N4 nanocomposites

The crystallization, morphology, microhardness, scratch hardness, dynamic modulus, and wear behavior of high performance poly(ether‐ether‐ketone) (PEEK) matrix nanocomposites reinforced with 0 to 30 wt % silicon nitride (Si₃N₄) nanoparticles were reported. The crystallinity of PEEK nanocomposites increases at 2.5 wt % Si₃N₄ but, thereafter it decreases with increasing Si₃N₄ content due to the hindrance to the ordering of PEEK chains. The crystallization peak temperature and crystallization onset temperature increases by 14°C for 10 wt % nanocomposite. The melting temperature does not vary significantly with Si₃N₄ content. SEM shows almost uniform distribution of Si₃N₄ in the PEEK matrix. The Vickers microhardness and scratch hardness increases significantly up to 10 wt % Si₃N₄ content.The dynamic modulus of nanocomposites increases below and above T_g of PEEK. The specific wear rate of nanocomposites with 2.5 wt % Si₃N₄ is reduced significantly and it is lowest at 10 wt % Si₃N₄. However, the coefficient of friction of nanocomposites is more than that of pure PEEK. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Promotion of the mechanical properties and thermal conductivity of epoxy by low Si3N4 whisker content and its mechanisms

Si₃N₄ whisker (Si₃N_4w) is selected as epoxy filler. The influence of filler content on the bulk density, porosity, bending strength, Young's modulus, critical stress intensity factor, work of failure, morphologies of fracture surface, and thermal conductivity of Si₃N_4w/epoxy is investigated. The bending strength is 82.63 MPa at a Si₃N_4w content of 5 vol% and increases to 25.29% more than that of neat epoxy. Compared with that of neat epoxy, the work of failure and thermal conductivity increase by 455% and 34.78% to 18 248.92 J·m⁻² and 0.31 W·m⁻¹·K⁻¹, respectively, at a Si₃N_4w content of 7 vol%. However, Si₃N_4w/epoxy becomes sensitive to precrack due to a weak C N bond and residual tensile stress at the interface, thereby resulting in the decline of critical stress intensity factor. The coexistence of various energy dissipation mechanisms, namely, steps, craters or depressions, stress whitening, plastic flow, pull out of Si₃N_4w, and rough fracture surface, is observed in Si₃N_4w/epoxy. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48721.     

Microstructure,high-temperature mechanical and dielectric properties of novel Si3N4 f/SiNO wave-transparent composites

Continuous Si₃N₄ fiber reinforced SiNO matrix composites (Si₃N_4 f/SiNO composites) were innovatively prepared for long-time high-temperature resistant wave-transparent materials of hypersonic aircraft. The microstructure, high-temperature mechanical and dielectric properties of Si₃N_4 f/SiNO composites were investigated in detail. The as-fabricated Si₃N_4 f/SiNO composites have homogeneous SiNO matrix distribution for the special winding process, which is beneficial for the mechanical strength and wave-transparent properties. The average tensile strength and flexural strength at room temperature is 87.8 MPa and 171.2 MPa respectively, which suggests Si₃N_4 f/SiNO composites have excellent mechanical strength. The tensile strength value decreases to 54.6 MPa after heat-treated at 1000 ℃ for the surface reactions between the SiNO matrix and Si₃N₄ fibers. After heat-treated at 1550 ℃, the composites have the tensile strength value of 24.2 MPa for the high strength retention rate of Si₃N₄ fibers at this temperature. Si₃N_4 f/SiNO composites have excellent room temperature dielectric properties and excellent dielectric stability in different frequency bands (7–18 GHz). The dielectric constant values vary from 3.69 to 3.75 while the dielectric loss attains the order of 10^?3. The dielectric constants and dielectric loss of Si₃N_4 f/SiNO composites are relatively stable from RT to 800 ℃. The as-fabricated Si₃N_4 f/SiNO composites that have excellent high temperature resistance and dielectric properties are the ideal high temperature wave-transparent composites.     

A Novel Hot Pressing Flowing Sintering for Preparation of Texturing Ceramics

In this paper, we proposed a novel hot‐pressing flowing sintering (HPFS) for texturing ceramics. The perfectly two‐dimensional textured Si₃N₄ ceramics were fabricated by HPFS. The Lotgering orientation factor f_L for Si₃N₄ texture was 0.9975. During earlier sintering stage, the specimen flowed along the plane which perpendicular to the hot‐pressing direction under pressure, through the controlling of the graphite die movement. The rod‐like β‐Si₃N₄ nuclei was easily to texture during the flowing process, due to the small size of the β‐Si₃N₄ nuclei and the high porosity of the flowing specimen. As a result, the perfectly two‐dimensional textured Si₃N₄ was obtained. After aligned, the β‐Si₃N₄ grains grew along the materials flowing direction with little constraint, which accelerated the growth of the grains extensively. So, in addition to texture, the Si₃N₄ ceramics by HPFS also showed high aspect ratio. The present study indicated that the HPFS would be more simple and low‐cost method for texture of Si₃N₄, compared with conventional hot‐forging which contained the sintering and forging.     

High-temperature microstructural evolution of SiCN fibers derived from polycarbosilane with different C/N ratios

Research into the high-temperature microstructural evolution of SiCN ceramic fibers is important for the aerospace application of advanced ceramic matrix composites in harsh environments. In this work, we studied the microstructural evolution of SiCN fibers with different C/N ratios that derived from polycarbosilane fibers at the annealing temperature range of 1400∼1600 °C. These results showed that the phase separation of SiC_xN_y phase and the two-dimension grain growth process of free carbon nanoclusters could be processed at the researched temperature range. As the annealing temperature increased to 1600 °C, the crystallization of amorphous SiC and Si₃N₄ could be detected. SEM and Raman analysis showed that the decomposition and carbothermal reduction of the Si₃N₄ phase at high temperatures played primary roles in contributing to the fiber strength degradation. Thus, a higher C/N ratio, which is beneficial for inhibiting the decomposition of amorphous Si₃N₄, helps SiCN fibers retain high tensile strength at high temperatures.     

Interfacial effects in polypropylene–silica nanocomposites

Grafted inorganic nanoparticles can greatly improve the mechanical performance of polymers. To examine the effects of the interfacial characteristics generated by the grafting polymer bonded to nanoparticle surfaces, we chemically grafted nano‐silica with different polymers and then melt‐mixed it with polypropylene (PP). We extracted the homopolymers produced during the graft polymerization from the grafted products before the composites were manufactured to get rid of the side effects of the nongrafting polymers. We tailored the interfacial interaction between the grafted nano‐SiO₂ and PP matrix by changing the amount of the grafting polymers on the nanoparticles, that is, the grafting percentage. Mechanical tests indicated that all the composites incorporated with grafted nano‐SiO₂ particles possessed much higher impact strength than untreated SiO₂/PP composites and neat PP. The greatest contribution of the particles was made at a low grafting percentage. Tensile measurements showed that the treated nanoparticles could provide PP with stiffening, strengthening, and toughening effects at a rather low filler content (typically 0.8 vol %) because of the enhanced interfacial adhesion resulting from molecular entanglement and interdiffusion between the grating polymers on the nanoparticles and matrix macromolecules. The presence of grafting polymers on the nanoparticles provided the composites with a tailorable interphase. The tensile performance of the composites was sensitive to the nature of the grafting polymers. Basically, a hard interface was beneficial to stress transfer, whereas a soft one hindered the development of cavities in the matrix. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1771–1781, 2004     

Synthesis and growth mechanism of single crystal β‐Si3N4 particles with a quasi‐spherical morphology

Single‐crystal β‐Si₃N₄ particles with a quasi‐spherical morphology were synthesized via an efficient carbothermal reduction‐nitridation (CRN) strategy. The β‐Si₃N₄ particles synthesized under an N₂ pressure of 0.3 MPa, at 1450°C and with 10 mol% unique CaF₂ additives showed good dispersity and an average size of about 650 nm. X‐ray photoelectron spectroscopy analysis revealed that there was no SiC or Si–C–N compounds in the β‐Si₃N₄ products. Selected‐area electron‐diffraction pattern and high‐resolution image indicated single crystalline structure of the typical β‐Si₃N₄ particles without an obvious amorphous oxidation layer on the surface. The growth mechanism of the quasi‐spherical β‐Si₃N₄ particles was proposed based on the transmission electron microscopy and energy dispersive X‐ray spectroscopy characterization, which was helpful for controllable synthesis of β‐Si₃N₄ particles by CRN method. Owing to the quasi‐spherical morphology, good dispersity, high purity, and single‐crystal structure, the submicro‐sized β‐Si₃N₄ particles were promising fillers for preparing resin‐based composites with high thermal conductivity.     

High-strength superparamagnetic composite fibers

The polymer composites of magnetic nanoparticles can be possibly used in a bulk form by preserving all the novel characteristics of magnetic nanoparticles such as superparamagnetic behavior. By introducing magnetic properties of Fe₃O₄ nanoparticles into polymer fibers, novel magnetic properties combine with the advantages of composite fibers such as light-weight and ease-of-use. Using dry-jet-wet fiber spinning technology, we have successfully fabricated iron oxide/polyacrylonitrile (Fe₃O₄/PAN) composite fibers with 10 wt% nanoparticle in the polymer matrix. Composite fiber with a diameter as small as 15 μm can achieve tensile strength and tensile modulus values as high as 630 MPa and 16 GPa, respectively. Superparamagnetic properties of Fe₃O₄ nanoparticles were preserved in the composite fibers with saturation magnetization at 80 emu/g and coercivity of 165 G.     

Mechanical and thermal properties of polypropylene nanocomposites using organically modified Indian bentonite

We report preparation and characterization of nanoclay from Indian bentonite and imported nanoclays, and their compounding with polypropylene (PP) and maleic anhydride‐grafted PP (MA‐g‐PP) in twin screw extruder. The compounded polymer/nanoclay nanocomposites (PNCs) are molded into a standard specimen for studying its tensile, flexural and impact strength. A wide angle X‐ray diffraction (WAXD) and transmission electron microscopy (TEM) study demonstrates intercalation of PP in nanoclays rather than exfoliation for both, indigenous and imported nanoclays. The tensile modulus increased by 41 and 39% for PNC1 (PNC with imported nanoclay) and PNC2 (PNC with indigenous nanoclay) with respect to PP. The flexural modulus for PNC1 and PNC2 also increases by 23 and 22% due to incorporation of 5% nanoclay in PP along with 5% MA‐g‐PP. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

High-temperature electromagnetic wave absorption properties of Cf/SiCNFs/Si3N4 composites

Carbon fibers reinforced Si₃N₄ composites with SiC nanofiber interphase (C_f/SiCNFs/Si₃N₄) were prepared by combining catalysis chemical vapor deposition and gel-casting process. Microstructures, mechanical properties, and electromagnetic wave absorption properties within X-band at 25°C-800°C of C_f/SiCNFs/Si₃N₄ composites were investigated. Results show that SiC nanofibers are combined well with Si₃N₄ matrix and carbon fibers, the fracture toughness is thus increased more than double from 3.51 MPa·m^1/2 of the Si₃N₄ ceramic to 7.23 MPa·m^1/2 of the as-prepared composites. As the temperature increases from 25°C to 800°C, C_f/SiCNFs/Si₃N₄ composites show a temperature-dependent complex permittivity, attenuation constant, and impedance. The relatively high attenuation capability of C_f/SiCNFs/Si₃N₄ composites at elevated temperature results in a great minimum reflection loss of −20.3 dB at 800°C with a thin thickness of 2.0 mm. The superior electromagnetic wave absorption performance mainly originates from conductive loss, multi-reflection, and strong polarization formed by the combined effects of carbon fibers and SiC nanofibers.     

Electrokinetic properties of polypropylene‐layered silicate nanocomposite fibers

Nanocomposite fibers based on polypropylene (PP) polymer were prepared with different content of nanofiller. Filaments were spun from an isotactic iPP homopolymer. Montmorillonite modified by N,N‐dimethyl‐N,N dioctadecylammonium cations was used for preparation of PP nanocomposite fibers. A PP grafted with acrylic acid was added as a coupling agent. Nanocomposite fibers were characterized, i.e., the surface morphology of PP nanocomposite fibers was observed and surface properties were defined by electrokinetic properties determination by zeta potential measurements. For particle distribution observation the plasma etching was involved as a method for sample preparation. The addition of nanoparticles has an impact on ZP value of nanofilled fibers, however, isoelectric point IEP is not significantly influenced by different concentrations of nanofiller. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Improvement of thermal and fire properties of polypropylene

In the present research, the thermal stability and fire properties of polypropylene (PP) have been improved through direct melt intercalation of PP, organically modified montmorillonite (OMMT), calcium carbonate (CaCO₃) nanoparticles, and conventional flame retardants, i.e., decabromodiphenyl oxide (DB) and antimony trioxide (AO). The morphology of the compound was characterized by means of X‐ray diffractometry and transmission electron microscopy. Thermogravimetry analysis (TGA), cone‐calorimetry, limiting oxygen index, UL‐94, and tensile tests were also employed to investigate thermal and mechanical properties as well as the flammability of the compounds. Data, obtained from TGA, indicated that simultaneous incorporation of both OMMT and CaCO₃ nanoparticles forms a synergistic effect to improve both the thermal and thermo‐oxidative stability. The kinetic analysis of polymer degradation showed that the presence of nanoparticles hindered the thermal degradation of PP. The combination of OMMT and CaCO₃ was more effective to improve fire properties than OMMT and DB/AO. The experimental results indicated that the incorporation of OMMT and CaCO₃ improved both the tensile (i.e., the increase of yield strength, tensile strength, and Young's modulus) and thermal properties. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Preparation and characterization of aqueous polyurethane dispersions with well‐defined soft segments

Novel aqueous polyurethane (PU) hybrid dispersions were successfully prepared with 5–15 mol % functionalized hexamethylene diisocynate trimer modified by N‐(n‐butyl)‐3‐aminopropyltriethoxysilane and dihydroxylpropyl‐terminated siloxane oligomers (TS). The results of the differential scanning calorimetry and X‐ray diffraction tests show that the degree of segment order was reduced by the introduction of TS. The hybrid polymer films with TS introduced into the PU backbone displayed excellent water and xylene resistance. Atomic force microscopy showed that the films had a smooth surface. It was noticeable that the tensile strength (σ_b) and Young's modulus of the films increased simultaneously when TS was incorporated into PU; σ_b of the PU15 film with 15 mol % TS was much higher than that of the neat PU0 film, and the breaking elongation of the film with 10 mol % TS was clearly higher than that of the other films. The results indicate that an appropriate content of TS significantly improved the properties of the aqueous PU hybrids. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Polypropylene Filled With Glass Spheres in Extrusion‐Based Additive Manufacturing: Effect of Filler Size and Printing Chamber Temperature

A challenge in extrusion‐based additive manufacturing of polypropylene (PP) filled with spherical particles is the combination of decent processability, excellent warpage control, and the retention of the tensile strength of neat PP. This study addresses this issue by adopting two approaches. Firstly, different size fractions of borosilicate glass spheres incorporated into PP are compared. Secondly, the temperature of the printing chamber (T_Ch) is varied. The effects of these features on the thermal, crystalline, morphological, tensile, impact, and warpage properties of 3D‐printed parts are examined. Smaller glass spheres (<12 µm) are found to be superior to larger fractions in all investigated aspects. Notably, the corresponding composites show higher tensile strengths than neat PP. An increase in T_Ch results in a more homogeneous temperature distribution within the printing chamber and promotes annealing during printing. Consequently, the dimensional accuracy of printed parts is improved. Additionally, β‐crystals and larger spherulites are formed at a higher T_Ch.     

Local Fracture Toughness of Si3N4 Ceramics Measured using Single‐Edge Notched Microcantilever Beam Specimens

Local fracture toughness gives us useful and important information to understand and improve mechanical properties of bulk ceramics. In this study, the local fracture toughness of silicon nitride (Si₃N₄) ceramics was directly measured using single‐edge notched microcantilever beam specimens prepared by the focused ion beam technique. The measured fracture toughness of grain boundary of the Si₃N₄ ceramics is higher than the fracture toughness of SiAlON glass, which exists in the grain boundaries of Si₃N₄ ceramics. It is also shown that the fracture toughness of grain boundary depends on the rare earth oxide added as a sintering aid, which is expected in terms of the difference in the grain‐boundary structure. The fracture toughness of a single β‐Si₃N₄ grains is higher than the grain‐boundary fracture toughness. It was also higher than the value estimated from ab initio calculations and surface energy, which means that any dissipative energy should be included in the fracture toughness of a grain in spite of the brittle fracture in Si₃N₄. The fracture toughness of polycrystals of Si₃N₄ ceramics measured using single‐edge notched microcantilever beam specimens is intermediate between those of grains and grain boundaries, and it agrees with the estimated initial value of the Rcurve, K_I0, in Si₃N₄ ceramics.     

Study on depositing SiO2 nanoparticles on the surface of jute fiber via hydrothermal method and its reinforced polypropylene composites

To improve the interfacial compatibility of jute fiber reinforced polypropylene (PP) composites, hydrothermal method was used to deposit SiO₂ nanoparticles on the surface of pretreated jute fibers and the effect of reaction factors (tetraethoxysilane [TEOS] concentration, ammonia concentration, and reaction temperature) on the deposition of SiO₂ nanoparticles were evaluated. The results of FTIR, XRD, SEM, and TEM showed that the amorphous SiO₂ nanoparticles with an average particle size of 65.0 nm were successfully deposited on the surface of jute fibers at the TEOS/H₂O volume ratio of 1:2, ammonia of 0.55 M, reaction temperature of 100 °C (0.15 MPa) for 5 h. Compared with the sol–gel method, SiO₂ nanoparticles obtained by the hydrothermal method possessed smaller particle size and were less agglomerated, which can better fill in the surface defects of the jute fibers and result in a 12.9% increase in the tensile strength. The study on the mechanical properties and interface performance of the jute fiber reinforced PP composites indicated that the interfacial compatibility between jute fibers and PP was obviously improved. The tensile and impact strength of the composites reinforced with nano‐SiO₂ deposited jute fibers were increased by 26.87% and 25.65%, respectively, compared with the untreated jute fibers. J. VINYL ADDIT. TECHNOL., 26:43–54, 2020. © 2019 Society of Plastics Engineers     

Ultralight Silicon Nitride Ceramic Foams from Foams Stabilized by Partially Hydrophobic Particles

Ultralight Si₃N₄ ceramic foams have been successfully prepared through particle‐stabilized foams method, which is based on the adsorption of in situ hydrophobized Si₃N₄ particles to the liquid/air interface of the foams. Here, we firstly used a long‐chain surfactant cetyltrimethylammonium chloride to render the Si₃N₄ particles partially hydrophobic. By tailoring the surfactant concentration and pH values of the suspensions, the wet foams were stabilized to avoid coarsening and coalescence. SEM results show that the Si₃N₄ ceramic foams possess single strut walls with elongated β‐Si₃N₄ grains interlocking with each other, and their pores are uniform with an average pore size of 95 μm. The obtained ceramic foams maintain compressive strength of 1.34 ± 0.13 MPa with porosity of 92.0%, when the suspension contains 3 mmol/L surfactant at the pH of 11.0.