Short‐beam three‐point bend tests in syntactic foams. Part II: Effect of microballoons content on shear strength

Epoxy binders containing microballoons ranging from 38.5 to 57.7% by volume were cast in a mold and cured, and the resulting slabs were sectioned to yield short‐beam test coupons. The strength changes with microballoons content were noted. These reveal an increase from 3.87 to 5.79 MPa for a decrease in microballoons content from 57.7 to 38.5%. Mechanical data were correlated with fractographic features employing scanning electron microscope. The failure features involving the microballoons and interface regions are highlighted in this article. The works show the existence of a dependence of strength parameters on the inter‐microballoon distances. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 680–686, 2005     

Short beam three point bend tests in syntactic foams. Part I: Microscopic characterization of the failure zones

Scanning Electron Microscopic (SEM) studies were carried out on the failure surface of syntactic foam material tested in a short beam three point bend test (SBT) by employing 21 × 15 × 3 mm³ dimension bearing specimens. The syntactic foams were fabricated using glass microballoons in epoxy binder. The failure of the tensile, compression, and shear dominated regions were studied by SEM at different magnifications. The tensile region had characteristic features, such as partial debonding of the microballoons from the matrix and cracking of glass microballoons, apart from matrix cracking and some river pattern features. The compression side was characterized by crushing and collapsing of microballoons, resulting in accumulation of debris with no apparent river pattern for matrix‐rich regions. The midway positions of the SBT failed surface comprised of deformation bands in the matrix and occasional debonding of microballoons. The morphology recorded in the tensile and compression regions corroborated well with the results obtained on these foam samples in those specimens that were subjected to pure uniaxial tension and compression, respectively. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 673–679, 2005     

Encapsulation of air‐filled poly(dimethylsiloxane) microballoons in polyimide as a polymeric low ε dielectric

Air‐filled microballoons of poly(dimethylsiloxane), ie PDMS, have been encapsulated in polyimide. The molecular assembly so formed has shown surface dominance by PDMS while analytical techniques, such as X‐ray photoelectron spectroscopy and infrared spectroscopy, have confirmed a similar distribution in the bulk. The electrical properties of the resultant polymer have been studied and the relative permittivity has been found to be very low while other beneficial attributes of the polyimide have been retained. Copyright © 2004 Society of Chemical Industry     

Rheokinetic studies and compressive response of high performance polybenzoxazine syntactic foams

Polybenzoxazines are finding increasing usage in demanding applications where high temperature stability is required, especially in the field of aerospace. In this work, thermally stable bisphenol F-based polybenzoxazine [poly(BF-a)] syntactic foams containing varying volume fractions (30–60%) of hollow glass microballoons (HGMs) were prepared and their mechanical response in the quasi-static regime was established. The effect of introducing glass microballoons on the curing profile of benzoxazine resin was studied using both nonisothermal differential scanning calorimetry and rheometry. Temperature-sweep experiments were performed to arrive at the optimal processing window of the benzoxazine-glass microballoons formulations, particularly in terms of viscosity, gelation temperature, and time. Thermally accelerated ring-opening polymerization of the benzoxazine resin led to complete curing of the syntactic foam formulations, as assessed by calorimetric studies. The thermal degradation behavior of the poly(BF-a)/HGM was studied using thermogravimetric analysis. As expected, the density of the syntactic foam specimens decreased with increasing microballoon content. Maximal increase in the specific compressive properties of the poly(BF-a)/HGM samples was observed in formulations containing 40% volume fraction of glass microballoons. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47234.     

Influence of chopped strand fibres on the flexural behaviour of a syntactic foam core system

The comparative performance in a three point bending test of syntactic foam comprising epoxy resin and glass microballoons with and without the inclusion of glass fibre in the form of chopped strands is reported. Test samples having a span‐to‐depth ratio of 16:1 were used. The data show that the glass fibre reinforced foam system had a higher strength compared to the unreinforced system. Resorting to light macroscopic and scanning electron microscopic examinations on mechanically tested samples expanded the scope of the work for a structure–property correlation to emerge. © 2000 Society of Chemical Industry     

Rheology of Nano‐Scale Aluminum Suspensions

Nano‐scale aluminum particles are innovative materials which are used increasingly in energetic formulations. In this contribution, the rheological behavior of suspensions with either paraffin oil or HTPB as the matrix fluid and nano‐scale aluminum (ALEX) as the dispersed phase is described and discussed. The paraffin oil/aluminum suspensions exhibit non‐Newtonian flow behavior over a wide range of concentrations, whereas the HTPB/aluminum suspensions exhibit Newtonian behavior (i.e. the viscosity is independent of shear stress) up to a concentration of 50 vol.% aluminum. Both systems have unusual viscoelastic properties in that their elastic moduli are independent of the solids concentration.     

Effect of filler‐to‐matrix blending ratio on the mechanical strength of palm‐based biocomposite boards

The effect of the blending ratio of a polyurethane matrix and oil‐palm empty fruit bunch (EFB) fibers on the mechanical properties of biocomposite boards has been studied. The PU matrix and EFB fibers were used at blending ratios of 25:75, 30:70 and 35:65 (by weight). The mechanical property of hardness was studied. The intention of this study was to produce fiberboard from a vegetable oil‐based polyester as the matrix and biomass from the palm oil industry, namely EFB. It was found that the blending ratio with a lower filler loading (35:65) gave higher impact and flexural strengths due to better fiber encapsulation which enhanced the fiber–matrix interfacial adhesion. Copyright © 2005 Society of Chemical Industry     

PEG 400/Paraffin oil non‐aqueous emulsions stabilized by PBut‐Block‐P2VP block copolymers

For the preparation of PEG 400 in paraffin oil non‐aqueous biocompatible emulsions, the stabilization efficiency was compared for two well‐defined poly(butadiene)‐block‐poly(2‐vinylpyridine) (PBut‐block‐P2VP) block copolymers, with similar molecular weights but different compositions. The PBut₁₂₈‐block‐P2VP₅₀ and PBut₁₈₉‐block‐P2VP₃₇ samples, designated as copolymer A and B, respectively, are self‐organized in paraffin oil as micelles with a P2VP core and a PBut corona. The PEG 400/paraffin oil emulsion characteristics were determined as a function of the copolymers concentrations and phase ratios. Higher static and shear stabilities were obtained for emulsions stabilized by copolymer B than for those obtained in the presence of copolymer A . A further difference concerns the droplet size, relative viscosity, and loss modulus values obtained at a given dispersed phase volume fraction. At constant copolymer concentrations, it appeared that copolymer B , with a longer PBut sequence, is a more efficient emulsifier and stabilizer than copolymer A . © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41390.     

Development of potentially biodegradable polyamide‐6 and polyvinyl alcohol blends: Physico‐mechanical properties,thermal properties,and soil test

Blends of polyamide‐6 with 5, 7.5, 10, 15, and 20 wt % of polyvinyl alcohol (PVA) were prepared by the extruding in a corotating twin‐screw extruder. The extrudate strands were cut into pellets and injection‐molded to make test specimens. These specimens were tested for physico‐mechanical properties such as tensile strength, impact strength, density, water absorption, hardness, and thermal characteristics by differential scanning calorimetry, heat distortion temperature (HDT), vicat softening point (VSP), and melt flow index. The prepared blends show enhanced biodegradation, water absorption, and density, but it is observed that the introduction of PVA into the polyamide–6 matrix shows considerable reduction in tensile strength, impact strength, HDT, VSP, and hardness initially, but subsequent addition does not show significant reduction because of the enhanced interaction between amide groups of polyamide‐6 and hydroxyl groups of PVA. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2339–2346, 2005     

Tensile properties of glass microballoon‐epoxy resin syntactic foams

The effect of hollow glass particle (microballoon) volume fraction in the range of 0.3–0.6 on the tensile properties and fracture mode of syntactic foams is characterized in the present research. Sixteen types of syntactic foams have been fabricated and tested. Four types of glass microballoons, having 220, 320, 380, and 460 kg/m³ density, are used with epoxy resin matrix for making the syntactic foam samples. These foams contain 30, 40, 50 and 60% microballoons by volume. All types of microballoons have the same size but different wall thickness, which reflects as a difference in their density. It is observed that the tensile strength increases with a decrease in the volume fraction of microballoons. All types of syntactic foams showed 60–80% decrease in the tensile strength compared with that of the neat resin. The foams containing low strength microballoons showed lower tensile modulus compared with that of the neat resin, but the presence of high strength microballoons led to an increase in the tensile modulus of the composites. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 1254–1261, 2006     

Effects of geometry and injection‐molding parameters on weld‐line strength

Polymeric flows in microchannels are found to differ significantly from those in macrogeometries. Increasing the mechanical properties of microstructures is one of the most important issues in injection‐molding processes. Weld‐line characteristics of structures with different cross‐sections are investigated in this study. The effects of process parameters and cross‐sectional dimensions on the tensile strength of a weld line are discussed. A mold was designed in such a way that specimens with and without weld lines can be developed separately. Five specimens, with different cross‐sections, are injection‐molded simultaneously. Both polypropylene (PP) and high density polyethylene (HDPE) are used in this study. With the Taguchi method, four process variables: melt temperature, mold temperature, injection speed, and packing pressure were found to be the most influential. Experimental results show that the weld‐line strength from a standard test is not applicable in microinjection molding. The microstructure of weld lines is clearly observed from the micrographs. POLYM. ENG. SCI., 45:1021–1030, 2005. © 2005 Society of Plastics Engineers     

The synthesis and application of Pb‐doped GLYMO/chelated‐zirconium complex coating materials for UV‐light absorption

New glass coating materials containing γ‐glycidoxypropyltrimethoxy‐silane/zirconium(IV)‐n‐propoxide(2‐methoxyethylacetoacetate)/lead(II) nitrate were developed for UV‐light absorption by sol‐gel process. The effect of agitation time, temperature, and Zr complex and Pb²⁺ ion concentrations on UV light absorption were investigated. Zr complex was characterized by using ¹H‐NMR, ¹³C‐NMR, and FTIR spectroscopy. Ultraviolet visible spectroscopy was utilized to determine the optical properties of coating materials. Results showed that coated glass has very low transmission in the UV region (300–400 nm) relative to uncoated glass, especially at 150°C for 15 h agitation. UV light transmission of coated glasses treated at 80, 100, 450, or 500°C was not different from uncoated glass. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1175–1179, 2006     

Strain rate effect in the single‐fiber‐fragmentation test

The single fiber fragmentation test (SFVU) has been widely used to characterize the interface it fiber‐reinforced polymers. The purpose of the work reported here was to determine the effect of strain rate on the fiber fragment lengths obtained in the SFFT. Three materials systems were used to make single‐fiber‐composite specimens: E‐glass fiber/polycarbonate matrix, AS4‐carbon fiber/polycarbonate matrix, and AS4‐carbon fiber/polycarbonate matrix. The fiber‐matrix adhesion in all three systems is based on physisorption rather than chemisorption. Each system was tested at strain rates ranging over four orders of magnitude. Results are reported in terms of fragment length, the dependent variable in this study, which is inversely related to the quality of the Interface. It was expected that the fragment length would show a systematic decrease with Increasing strain rate, but the expected trend was not found. Although the polycarbonate matrix exhibited rate‐dependent viscoelastic behavior typical of amorphous polymers below T_g, the fragment length at saturation did not show a statistically significant variation with strain rate for any of the three materials systems. A major contributor to the lack of observed effect was the inherent random variability associated with the SFFT; random variability in average fragment length was equal or greater than the 19% effect of rate predicted for ideal elastic systems with no debonding at the interface. In addition, considerable interfacial debonding occurred during the SFFT, not surprising for Interfaces based on physisorption alone. Debonding Interferes with transfer of applied load from matrix to fiber, and would thus interfere with transfer of the effect of rate from matrix to fiber. A tensile Impact test developed previously was also performed on single‐fiber composite specimens made from the same three materials systems. The results of the Impact tests differed from those obtained at controlled strain‐rates for only two of the materials systems.     

Flow improvement of Liaohe extraheavy oil with comb‐type copolymers

Liaohe extraheavy oil is a kind of special crude oil with high paraffin and asphaltene contents and a pour point of up to 60°C. To improve its flowability, comb‐type poly(maleic alkylamide‐co‐α‐octadecene) copolymers (MACs) with various amidation ratios were synthesized and used. Model oils containing paraffin mixtures with the same average carbon number to Liaohe extraheavy oil with and without asphaltene were prepared to explore the effect of the MACs on paraffin crystallization and asphaltene dispersion, respectively. We found that MACs reduced the yield stress, changed the size and shape of the paraffin crystals, and obstructed the paraffin crystallization for both model oils and extraheavy Liaohe oils as observed by rheology, polarizing light microscopy, X‐ray diffraction, and differential scanning calorimetry. The MACs seemed to be an ideal candidate for improving the flowability of Liaohe extraheavy oils. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40082.     

Characterization of paraffin oils and petrolatum using LDI‐TOF MS and principle component analysis

Laser desorption/ionization time‐of‐flight mass spectrometry (LDI‐TOF MS) followed by evaluation of the mass spectra with principal component analysis (PCA) was used for the in‐depth characterization of paraffin oils (mineral oils) and petrolatum (paraffin jelly) samples. These raw materials are liquid and semisolid mixtures of hydrocarbons obtained from petroleum. Mass spectrometric analysis was done using a solvent‐free sample preparation with silver trifluoroacetate. The analysis was carried out on a commercially available matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometer. Mass spectra were evaluated using parameters calculated from the areas of different alkane and cycloalkane species and by PCA. The ratios between specific peak areas were chosen as PCA‐input data instead of the less reproducible absolute peak areas. The principal components enable comparison of a large number of samples and can also be used for visualization of data. In this work, it is clearly demonstrated that combining LDI‐TOF MS and PCA provides a fast and efficient tool for the characterization of paraffin oils and petrolatum. Petrolatum and four different kinds of paraffin oil were analyzed and the results compared with other analytical methods.     

Synthesis and chain extension of poly(L‐lactic acid‐co‐succinic acid‐co‐1,4‐butene diol)

L ‐Lactic acid (LA) was copolymerized with succinic acid (SA) and 1,4‐butenediol (1,4‐BED) in bulk state with titanium(IV) butoxide as a catalyst to produce poly(LA‐co‐SA‐co‐1,4‐BED) (PLASBED). Poly(L ‐lactic acid) (PLLA) homopolymer obtained from a direct condensation polymerization of LA had weight average molecular weight (M_w) less than 4.1 × 10⁴ and was too brittle to prepare specimens for the tensile test. Addition of SA and 1,4‐BED to LA produced PLASB with M_w as high as 1.4 × 10⁵ and exhibited tensile properties comparable to a commercially available high‐molecular‐weight PLLA. Chain extension by intermolecular linking reaction through the unsaturated 1,4‐BED units in PLASBED with benzoyl peroxide further increased the molecular weight and made PLASBED more ductile and flexible to show elongation at break as high as 450%. Biodegradability of PLASBED measured by the modified Sturm test was nearly independent of the 1,4‐BED content. Gel formation during the chain extension did not exert any significant influence on the biodegradability either. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1116–1121, 2005     

Polysilazane‐based heat‐ and oxidation‐resistant coatings on carbon fibers

Carbon fibers must be protected from a high‐temperature oxidizing environment because, at approximately 500°C and above, the fibers exhibit reduced mass and strength stability. The fibers can be protected by the application of thermal coatings, which simultaneously improve the adhesive properties of the carbon fibers in the composite materials. Polysilazanes are a new family of heat‐resistant polymer coatings that are converted into silicone carbide or silicone nitride ceramic structures at high temperatures. The converted ceramics are resistant to the effects of high temperatures. In this research work, polysilazane‐based coatings were applied to carbon filament (CF) rovings with the dip‐coating method. Tensile testing at room temperature and under thermal stress was carried out to assess the mechanical and thermomechanical properties of both coated and uncoated rovings. Scanning electron microscopy and energy‐dispersive X‐ray analysis were performed to evaluate the surface topographical properties of the coated and uncoated rovings. Thermogravimetric analysis was executed to determine the thermal stability of the polymer coatings. The coating performance on the CF rovings was determined by assessment of the test results obtained. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Soil burial test for poly(ethylene‐co‐vinyl alcohol)‐graft‐polycaprolactone

The ring‐opening polymerization of ε‐caprolactone was carried out with poly(ethylene‐co‐vinyl alcohol) as a macroinitiator to synthesize poly(ethylene‐co‐vinyl alcohol)‐graft‐polycaprolactone (EVOH‐g‐PCL). A simple low‐density polyethylene (LDPE)/polycaprolactone (PCL) (64/36) blend lost 5.3 wt % of its original weight after 90 days of a soil burial test. However, the elongation at break of the LDPE/PCL blend remained almost invariable even after the solid burial test because the tensile properties depended mostly on the LDPE phase on account of the poor interaction between the continuous LDPE matrix and the dispersed PCL phase. For EVOH‐g‐PCL, the elongation at break decreased drastically as a result of the soil burial test, and the reduction of the elongation at break was more pronounced for EVOH‐g‐PCL with a higher PCL concentration, even though the weight loss of EVOH‐g‐PCL after the soil burial test was as low as 1.2–1.3% and was nearly independent of the PCL concentration. Few holes were observed in EVOH‐g‐PCL when the PCL concentration was less than 26 wt % after an accelerated hydrolysis experiment at 60°C for 7 days in a 0.1M KOH solution. In contrast, the hydrolysis formed small holes in EVOH‐g‐PCL with a PCL concentration of 36 wt %. The LDPE/PCL blend was much better percolated, as a result of the hydrolysis, than EVOH‐g‐PCL with the same PCL concentration; the soil burial test showed the same results. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 1064–1071, 2005     

Production and Sensitivity Evaluation of Nanocrystalline RDX‐based Explosive Compositions

The initiation sensitivity of cyclotrimethylenetrinitramine (RDX) was investigated as a function of crystal size. For this study, RDX powders with mean crystal sizes of ca. 200 and 500 nm were prepared by rapid expansion of supercritical solutions (RESS) with carbon dioxide as the solvent. Initiation sensitivity testing to impact, sustained shock, and electrostatic discharge stimuli was performed on uncoated as well as wax‐coated specimens. The test data revealed that in a direct comparison to coarser grades the nanocrystalline RDX‐based samples were substantially less sensitive to shock and impact stimuli. Furthermore, the 500 nm RDX‐based specimens exhibited the lowest sensitivity values, an indication that minima in shock and impact sensitivities with respect to crystal size exist.     

Heat‐damage assessment of carbon‐fiber‐reinforced polymer composites by diffuse reflectance infrared spectroscopy

Diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy was used to assess the effects of heat damage on carbon‐fiber‐reinforced polymer composites. Moisture‐saturated graphite–epoxy laminates with a quasi‐isotropic lay‐up were heat‐damaged above their upper service temperatures. The loss of matrix‐dominated mechanical properties due to heat exposure was investigated in the laboratory under environmental testing conditions with mechanical tests, ultrasonic C‐scanning, and DRIFT spectroscopy. The reduction of the mechanical strength of the composite materials was accompanied by an increase in the carbonyl band integral and a decrease in the phenyl ratio and hydroxyl and hydrocarbon band integrals, as shown by the DRIFT spectra. DRIFT was confirmed to be more effective than ultrasonic inspection in evaluating the extent of heat damage, and a good correlation was found between the mechanical test results and DRIFT spectra. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 1222–1230, 2005