Dynamic Mechanical Analysis Tests Research Articles

A numerical and experimental identification of crystallinity gradients in carbon fiber reinforced thermoplastic composites obtained by laser assisted filament winding

The presence of temperature and crystallinity gradients in carbon fiber–reinforced PolyEtherEtherKetone (PEEK) composite laminates, produced via laser-assisted tape placement, is investigated in this paper. The manufacturing process takes place with high deposition speed and using localized laser source for heating, therefore enhancing the formation of temperature and crystallinity gradients through the laminate thickness. A previously validated thermal model coupled with a non-isothermal crystallinity model and a fusion model are used to simulate the temperature and crystallinity distributions through the laminate thickness. The results from the model are correlated with Dynamic Mechanical Analysis (DMA) tests and Differential Scanning Calorimetry (DSC) tests since a crystallinity gradient is difficult to monitor experimentally. The simulated gradients suggested the presence of an amorphous layer between two consecutive plies and an increase in the crystallinity through the material’s thickness. This observation is correlated with the behavior reported for the semi-crystalline laminates during the DMA test, where the modulus drops abruptly during the glass transition, a typical behavior for an amorphous material.

Effect of α-methyl on the performance of photocurable 3D printing polyurethane materials

For photosensitive polyurethane systems, reactive diluents are indispensable components whose main role is to reduce the viscosity of the polyurethane prepolymer to meet the requirements of the photocurable 3D printing technology for high fluidity of the precursor solution. Generally, the reactive diluent would be involved in the photocuring reaction, which in turn has a remarkable impact on the mechanical, reaction kinetics, and thermodynamic characteristics of the photosensitive polyurethane system. However, this feature is usually neglected in the study of photosensitive urethane acrylate (PUA) systems, so there is a considerable necessity to investigate the mechanism of active diluents in the photocured reaction of PUA systems. In this work, the effects of α-methyl groups along the chains of diluent molecules on the photoreaction kinetics, photocurable 3D printing, mechanical and mechanical properties, and thermodynamic characteristics of PUAs were investigated employing hydroxyethyl methacrylate and hydroxyethyl acrylate as active diluents, respectively. The relationship between chemical structure and kinetics of PUA systems was also elucidated by using dynamic mechanical analysis tests. The results demonstrated that the α-methyl group blocks the migration of reactive radicals, reduces the efficiency of the photoreaction, and causes an increase in the rigidity and strength of the molecular chain. This study not only revealed the effect of α-methyl on the kinetic mechanical and thermal performance of PUA systems but also paves the way for the development of a new class of photosensitive PUA materials used for the photocurable 3D printing technology.

Nonlinear behaviour of epoxy and epoxy-based nanocomposites: an integrated experimental and computational analysis

The focus of this study is on the nonlinear mechanical properties of epoxy and epoxy-based nanocomposites, exploring frequency and strain amplitude dependency. Nanocomposite samples of epoxy are reinforced with fumed silica (FS), halloysite nanotubes (HNT) and Albipox 1000 rubber (Evonik) nanoparticles. Considering these particles have different geometries and stiffnesses, they are expected to have significantly different influences on the mechanics of the resulting composite. To enhance the reliability of the results and to reveal the impact of nanofillers on the mechanics of the material more distinctly, the manufacturing process is designed to be the same for all the specimens within the same material groups to eliminate the effects of the manufacturing process. The comprehensive characterization process consists of Fourier-Transform InfraRed Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and Dynamic Mechanical Analysis (DMA). The DMA tests are designed so that the material properties are measured depending on the vibration frequency and strain amplitude. Finally, the characterized nonlinear dynamic properties of these nanocomposites are used as the input material properties into a numerical model. In this simulation, a cantilever beam with representative nonlinear material properties, for these nanocomposites, is created, as example and its forced response is plotted under the same levels of excitation in the frequency domain. Key effects of the different nanofillers are identified using the resonance behavior, primarily focusing on the stiffness and damping of the epoxy-based nanocomposites. These experimental and numerical procedures followed show the significant impact of the nanoparticle reinforcements on the nonlinear nature of these epoxy-based composites.

Insights on the J‐integral expression of pure shear carbon black filled natural rubber specimen and predicting the crack growth rate using finite element method

AbstractThe J‐integral approach manifests itself in an efficient way to determine the crack growth and failure mechanism of tread and sidewall compounds used in tyres. Therefore, for a pure shear (PS) specimen of carbon black filled natural rubber, the J‐integral formula was vivisected, and the material parameters were defined using the concepts of solid mechanics considering the planar stress conditions. Theoretical calculations, experimental observations, and finite element analysis were executed to calculate the J value for different strain percentages. Different hyperelastic material models were used to understand the hyperelastic behavior of the test compound, but Yeoh model was found to be the best fit with the least error against the experimental test data. The frequency sweep dynamic mechanical analyzer test was done to observe the viscoelastic response of the material. It was observed that the J value decreased with decreasing contour radius and had exhibited stark difference with the global tearing energy values, indicating the effects of stress softening and the dependence of J value on the elastic characteristics of the material. Further, the J value attained from finite element methods for a random strain 22% was used to predict the crack growth rate of the pre‐notched PS specimen.Highlights J‐integral formula for pure shear specimen using solid mechanics approach. J value comparison of theoretical, experimental, and finite element methods. Dependence of J value on the elastic characteristics of the material. Different hyperelastic models compared and Yeoh model chosen for analysis. Prediction of crack growth rate at a random strain percentage.

Preparation of polylactic acid (PLA) films plasticized with a renewable and natural Liquidambar Orientalis oil

Polylactic acid (PLA) is a brittle biodegradable thermoplastic due to its relatively high glass transition temperature (Tg ∼ 60 °C). This Tg limits the using of PLA in flexible applications, for example packaging films. In this study, it has been shown for the first time that the Liquidambar Orientalis (LO) oil as a nontoxic, environmentally friendly, and green additive can be successfully used as a natural, renewable, and sustainable plasticizer to produce flexible PLA parts and improve its thermal and physical properties and application potential. Natural oil obtained from Liquidambar Orientalis tree was introduced into PLA (as 10, 20, and 30 phr) by melt compounding (MC) and solution mixing (SM) methods. Effect of LO oil amount on the glass transition temperature, melt and cold crystallization behaviors, and degree of crystallinity values of samples were determined with differential scanning calorimetry (DSC). In addition, solid state viscoelastic properties of PLA films were also characterized with dynamic mechanical analysis (DMA) tests. Results showed that LO oil significantly reduced the Tg and storage modulus (E') value of PLA and LO oil showed an excellent plasticizing effect for PLA due to reducing strong hydrogen bonds and secondary interactions between PLA chains.

Investigation of Creep Failure in Ag-4Pd Bonding Wire Under Dynamic Mechanical Analysis Tests

Investigation of Creep Failure in Ag-4Pd Bonding Wire Under Dynamic Mechanical Analysis Tests

Experimental characterization and numerical analysis of CFRPs at cryogenic temperatures

The thermo-mechanical performance of carbon fiber reinforced polymers (CFRPs) is affected by temperature changes due to the dissimilar nature of the constituents and dissimilar properties. For instance, under cryogenic conditions, the effective mechanical performance of the composite system can be significantly reduced. In this work, dynamic mechanical analysis (DMA) tests and coupon mechanical tests at room and cryogenic temperatures (through immersion in liquid nitrogen), are combined with computational micromechanics to analyze the development of micro-residual stresses from curing to cryogenic conditions, and their influence on the mechanical performance of a unidirectional CFRP. The results confirm the stiffness increase in the matrix and in the composite under cryogenic conditions, but the high tensile triaxial stress state that is developed during cooling reduces the overall composite strength, despite the increase of the matrix strength with decreasing temperature. To capture the failure modes and the evolution of the properties appropriately, the elastic-plastic response and the pressure dependent failure model are formulated to appropriately represent the shear response of the composite system and matrix failure under complex triaxial stress states, enabling a complete analysis and the identification of effective material properties, based on a reduced number of simple tests on the neat resin and on the composite system at different temperatures, which otherwise would be impossible to obtain considering the dimensional and technological restrictions of performing mechanical tests at cryogenic conditions.

Mechanical Recycling of Waste PLA Generated From 3D Printing Activities: Filament Production and Thermomechanical Analysis

AbstractThere is a growing need to address waste generated from Fused Filament Fabrication (FFF) 3D printing activities. This study explores the mechanical recycling of waste polylactic acid (PLA) accumulated from failed 3D printing operations and PLA biocomposite filaments containing nanocellulose fibres. FFF 3D printable filaments were produced via melt mixing and extrusion of virgin PLA containing varying amounts of waste PLA. The chemical, thermal and thermomechanical characterisation of each specimen was evaluated using Fourier‐transform infrared spectroscopy (FTIR), simultaneous thermal analysis (SDT), dynamic mechanical analysis (DMA), and uniaxial tensile analysis (UTA). A desktop FFF 3D printer was used to fabricate UTA and DMA test specimens. The thermal stability of the filament specimens containing waste derived from the failed 3D prints were comparable with that of the commercial filaments. However, a 11% decrease in the onset of thermal degradation is observed for the filament containing waste biocomposites. The specimens containing waste PLA exhibited higher crystallinity and storage modulus. UTA results revealed similar tensile strength and % elongation, except for the specimen containing 50% waste PLA which exhibited a 29% decrease in tensile strength. This work successfully demonstrates mechanical recycling as a viable waste management strategy for waste materials generated during FFF 3D printing.

Nanoscale dynamic mechanical analysis of a viscoelastic matrix inclusion within an elastic substrate

Advanced composite materials incorporate viscoelastic matrix inclusions in designated locations within elastic substrates, which grant them specialized energy dissipation capabilities of dynamic loadings. Identifying the local nanomechanical properties of the matrix-substrate complex within the composite is critical to its design and adaptation toward a specific target function. Here, we conduct FE simulations of nanoscale dynamic mechanical analysis (DMA) testing on hemispherical matrix inclusions within elastic substrates and analyze the variations in its indentation storage loss moduli measures for different matrix-substrate configurations. Then, we describe the mechanical system by simple spring models, identify the dominating parameters at different contact states of the nanoscale DMA testing, and obtain highly accurate analytical formulae that link the indentation measures of the matrix-substrate complex to the individual mechanical properties of the matrix and substrate parts. Our analysis can be directly integrated into benchmark nanomechanical testing methodologies of composite materials and promotes the local dynamic-mechanical characterization of complex materials systems, including nanomaterials, micro-architected structures, and bio-inspired designs.

Effect of plasticizer composition on the properties of injection molded cassava starch-based bioplastics

Sustainability has led to an exponential increase in the interest for using renewable resources. The abundance of starch in nature has promoted the production of starch-based bioplastics through widespread industrial techniques employed for conventional polymers, such as injection molding (IM). This research specifically aims to assess the effect of different plasticizers (i.e., glycerol, glycerol/water) on the properties of cassava (Manihot esculenta) starch bioplastics obtained through IM. Through dynamic mechanical analysis (DMA) and tensile tests, viscoelastic and mechanical properties of the bioplastics at different plasticizer to starch ratios (30–40 %, w/w) were analyzed. Other properties, such as water uptake capacity (WUC) or soluble matter loss were studied and related to the structure of the materials analyzed via scanning electron microscopy and X-ray diffraction. The effect of relative humidity (RH) on dynamic mechanical response of bioplastics was explored. Mixed plasticizer fractions, including glycerol and water, gave rise to hardened materials with rougher surfaces that were dramatically softened at both low and high RH. The low WUC and uniform structure displayed by materials produced from cassava starch and 30 % of glycerol might be of interest for its application in food packaging due to their optimal performance with temperature at high RH (80 %).

Comprehensive investigation into the thermal rheological behavior and relaxation characteristic of single/composite polymers in laminated glass

Polymeric interlayers are of significance for the structural capability of thin-walled laminated glass members both before and after glass fracture. Polymers present evident temperature and time dependence, which should be carefully assessed in the design process. To improve mechanical properties dependent on the temperature and time, novel interlayers including modified ethylene-vinyl acetate (PVE®) and composite PVE/PC (SGE®), have been developed along with the sound resistance of the interfacial adhesion to aging. In this work, dynamic mechanical thermal analysis tests were carried out to investigate the thermal rheological behavior and relaxation characteristic of polyvinyl butyral (PVB), ionomer (SentryGlas®, SG), PVE, PC and SGE. The results show that PVE and SGE follow the complex thermal rheological behavior as a result of the existence of two different types of relaxation transitions, whilst PVB, SG, and PC are thermorheologically simple materials. The arctangent function was introduced to describe the temperature dependence of PVB and SG. The relaxation modulus of polymers was subsequently derived based on the approximation equation and inverse Fourier transform. The results of the inverse Fourier transform indicate that vertical shift might need to be considered for PVE and SGE. The application of the approximation equation was assessed and its limitation was discussed. Finally, the relaxation characteristics of five polymers were described using the generalized Maxwell model based on the weighted least squares method.

N-doped-GO@Zn nano-layers filled epoxy composite with superior mechanical and anti-corrosion properties

Fabrication of a durable corrosion-resistant epoxy coating with superior active and passive preservation features along with improved mechanical properties is the major target of this study. For this, the Nitrogen (N)-doped graphene oxide (NGO) nano-sheets were obtained in two conditions (I: plane and II: edge) and then modified with zinc ions as an inhibitor. The chemistry of the NGO-Zn nano-sheets was surveyed by FTIR and TGA methods. It was discovered from the EIS test outcomes that the entrance of 0.2 wt% of NGO-Zn nano-sheets into the epoxy coating supplied a strong protective system with considerably improved barrier properties and the emergence of active features. The hindrance properties of these nano-composite coatings were so excellent that the log |Z|10 mHz value experienced little changes even after 147 days of electrolyte attack. The active protection feature of the EP/NGOU-Zn and EP/NGU-Zn nano-containers in reference to Rt values after 48 h of immersion was concluded, displaying 1.3 and 1.7 times improvement. The Raman and FTIR test outcomes of the cured epoxy composites showed that the incorporation of fillers into the coating has no adverse effect on its curing behavior. Results disclosed that the NGO constructed with method II (NGU) greatly improved the mechanical properties of the polymeric matrix by about 50 %, recording maximum storage modulus (2021 MPa) in the dynamic mechanical thermal analysis (DMTA) test among all samples.

Evaluation of photopolymer resins for dental prosthetics fabricated via the stereolithography process at different polymerization temperatures—Part I: Conversion rate and mechanical properties

Improvement in the mechanical properties of 3-dimensional (3D) printed dental prostheses is necessary to prevent wear caused by an antagonist or fracture. However, how different printing temperatures affect their mechanical properties is unclear. The purpose of this in vitro study was to evaluate the mechanical properties of 3D printed parts fabricated at different printing temperatures. Photopolymer specimens were fabricated at 3 different temperatures (room temperature, 50°C, and 70°C) using a stereolithography 3D printer. After rinsing to remove the residual monomer, the specimens were divided into 2 groups: with or without postprocessing. The viscosity of the photopolymerization resin was measured while the temperature was increased. Furthermore, the double-bond conversion (DBC) of the printed part was evaluated (n=3). Mechanical properties were investigated via dynamic mechanical analysis (n=1) and tensile testing (n=5). Statistical comparisons were performed via 1-way analysis of variance, followed by the Tukey honestly significant difference test (α=.05). The DBC rates of the green condition group increased from 66.67% to 86.33% with increasing temperature. In addition, these specimens exhibited improved mechanical properties and reduced residual monomer levels. Specimens fabricated at a temperature of 70°C exhibited mechanical properties suitable for clinical application.

Fatigue S-N curve approach for impact loading of hyper- and visco-elastic leading edge protection systems of wind turbine blades

Computational evaluation of leading edge erosion remains challenging due to the high-strain rate loading conditions caused by impact of the wind turbine blade leading edge with rain droplets and other environmental particles. Here, a methodology is proposed for obtaining an S-N curve which can be used for impact fatigue evaluation of hyper- and viscoelastic leading edge protection systems for wind turbine blades, in the relevant strain rate domain. Two material systems (hard and soft polyurethane (PU)) are characterised experimentally by dynamic mechanical analysis (DMA) and static tensile tests. Time-temperature superposition is applied to the raw DMA data in order to obtain the material’s mastercurve, describing its visco-elastic behaviour in an expanded strain rate domain. The Yeoh (hyperelastic) and prony series (vis-coelastic) material model parameters are calibrated and form the input for a 2D-axisymmetric finite element model, in which Single Point Impact Fatigue Test (SPIFT) testing conditions are simulated. The stress field experienced by the coating during SPIFT testing is obtained and combined with the experimental measurements, allowing the determination of the material systems S-N curve, in the relevant strain rate domain. Results for a hard and soft PU coating system are compared with rain erosion test (RET) data. The RET data shows higher lifetime for the hard PU systems, a tendency that can be predicted when comparing the S-N curve for the hard and soft PU system. This methodology can be utilised in computational lifetime evaluation of leading edge coating systems. Furthermore, the methodology has the potential to partly alleviate the need of RET in the development and comparison of next-generation leading edge protection systems.

Investigating the effect of cure schedules and cure initiators on sustainable composites for large offshore structures

This study evaluates the effect of post-cure schedules and cure initiator form on the mechanical properties of Glass fibre reinforced polymer (GFRP) laminates manufactured using an infusible reactive thermoplastic resin. Tensile, flexural, shear and dynamic mechanical analysis tests were conducted. Fractography was also performed. Specimens fabricated using liquid cure initiator and subjected to an elevated temperature post-cure were the control specimens. Ambient cured specimens decreased by no more than 12% in the case of tensile properties (modulus of 90° specimens) and by < 14.3% in the case of flexural properties (also modulus in 90° specimens). Furthermore, the difference in mechanical properties of 0° specimens fabricated using a powder cure initiator was observed to be within ≈ 7% of respective properties of control specimens. In the context of fabricating thick laminates for large-size offshore structures, the results suggest that an extended ambient post-cure cycle in conjunction with an initiator in powder form can be employed instead of an elevated temperature post-cure schedule with initiator in liquid form. This is economically beneficial since it eliminates infrastructure required for elevated temperature curing/post-curing. The risk of porosity induced due to liquid-based initiators is also avoided.

The Development of a Novel Thin Film Test Method to Evaluate the Rain Erosion Resistance of Polyaspartate-Based Leading Edge Protection Coatings

The relationship between the bulk thermomechanical properties and rain erosion resistance of development polyaspartate-based coatings as candidate leading edge protection (LEP) materials for wind turbine blades is investigated by the combined application of dynamic mechanical analysis (DMA) and rain erosion testing (RET) within a novel test method (DMA+RET). This method introduces the use of DMA+RET to both monitor the change in thermomechanical properties with respect to raindrop impact and subsequently rationalise differences in rain erosion resistance between coating formulations of comparable composition. The application of this combined process has demonstrated the importance of relatively high viscoelastic moduli at increased strain rates and creep recovery after RET as key material properties to be considered for LEP material development, whereas previous research presented in the scientific literature has primarily focussed on the use of routine characterisation procedures by tensile testing or stand-alone DMA to evaluate coating formulations prior to rain erosion testing. This journal article therefore presents a novel method to evaluate key material properties relevant to rain erosion resistance before and after subjection to raindrop impact using standard ASTM G73 RET equipment. The test method is demonstrated on a novel polyaspartate-based coating, PA-U, that exhibits notable rain erosion resistance in comparison to commercial LEP products. PA-U exhibited negligible mass loss after 30 h of rain erosion testing and favourable thermomechanical properties (E″ = 35 MPa at critical strain; equilibrium recoverable compliance of 0.05 MPa−1) in comparison to alternative formulations.

Hydrogel Membranes from Chitosan-Fish Gelatin-Glycerol for Biomedical Applications: Chondroitin Sulfate Incorporation Effect in Membrane Properties.

Chondroitin sulfate (ChS), chitosan (Chi), and fish gelatin (FG), which are byproducts of a fish-treatment small enterprise, were incorporated with glycerol (Gly) to obtain dense hydrogel membranes with reduced brittleness, candidates for dressing in wound healing applications. The mechanical properties of all samples were studied via Dynamic Mechanical Analysis (DMA) and tensile tests while their internal structure was characterized using Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR) and X-ray Diffraction (XRD) instruments. Their surface morphology was analyzed by ThermoGravimetric Analysis (TGA) method, while their water permeability was estimated via Water Vapor Transmission Rate (WVTR) measurements. Wettability and degradation rate measurements were also carried out. Characterization results indicated that secondary interactions between the natural polymers and the plasticizer create the hydrogel membranes. The samples were amorphous due to the high concentration of plasticizer and the amorphous nature of the natural polymers. The integration of ChS led to decreased decomposition temperature in comparison with the glycerol-free sample, and all the materials had dense structures. Finally, the in vitro endothelial cell attachment studies indicate that the hydrogel membranes successfully support the attachment and survival of primary on the hydrogel membranes and could be appropriate for external application in wound healing applications as dressings.

Bio-inspired metallic cellular material with extraordinary energy dissipation capability

Graphene coating on the skeleton of porous material opens the door to simply achieving high-performance composites. In this study, relying on the adhesive properties of polydopamine (PDA), PDA modified reduced graphene oxide (PDA-rGO) is adhered to the skeleton of nickel foam, of which the mechanical properties as well as the vibration damping and sound absorption performances are investigated. The mechanical test results reveal that the existence of coating leads to 240% and 59% increments of the compressive modulus and the yield strength, respectively. The enhancement of dynamic mechanical properties is also verified by dynamic mechanical analysis (DMA). Moreover, in DMA tests, the loss factors of nickel foam coated with PDA-rGO are found to achieve up to 170% growth, and show excellent stability with increasing temperature, indicating the reliability of loss factor enhancement in harsh environment. The superior vibration damping performance of nickel foam coated with PDA-rGO is further confirmed by vibration tests. Furthermore, the coating is found to effectively boost the flow-resistance and improve the sound absorption capability of nickel foam in turn, this synergy results in a significant increase in the noise reduction coefficient for up to 73.3%. Hence, adhering PDA-rGO to nickel foam in the present study provides a promising strategy for the development of multi-functional and versatile metallic foam.

Multifunctional Modifying Systems Based on Ionic Liquids for Epoxy Resin Systems and Composites

The continuous development of the industry of composite materials and epoxy resins requires the development of components that modify these systems. It is extremely beneficial to modify functionality by using one or two substances instead of modifying only one system parameter. Typically, this end-use will determine the key parameters of the resin system that should be modified and the modification systems designed as such. In this study, we introduce novel systems utilizing ionic liquids, strategically designed to concurrently alter multiple system parameters, including: (i) flexibility, (ii) crosslinking density, and (iii) fire resistance. The following techniques were used in the research: (i) Differential Scanning Calorimetry (DSC), (ii) Thermogravimetric Analysis (TGA), (iii) Dynamic Mechanical Analysis (DMA) and (iv) fire performance tests (UL-94, Limiting Oxygen Index and Mass loss type cone calorimetry (MLC)) to show as much dependence of material parameters on the type of modifying additive as possible. Both the cured resin and the curing process as well as a single-layer composite reinforced with carbon fiber were tested. The results show that properly designed ionic liquids are able to perform many functions in the composite material and simultaneously affect several parameters, both by lowering and increasing them. In addition, they can exhibit activity in the field of flame-retardant composites.

An acrylic resin system for in‐situ pultrusion: Curing performances and rheology

AbstractIn recent years, the use of low viscosity and in‐situ polymerizable thermoplastic acrylic resins for advanced fiber reinforced composites has grown, specially to address the difficulty of fiber impregnation with high‐melt viscosity thermoplastic polymers. The present work investigated the curing kinetics, chemo‐rheology of an acrylic resin system for in‐situ pultrusion, and proposed the corresponding constitutive models. First, the curing kinetics was studied with the differential scanning calorimetry experiments. The viscosity development was obtained by a rheometer as functions of the degree of cure (DOC) and temperatures. The gelation point was acquired from the intersection point of storage and loss modulus curves through dynamic mechanical analysis test, which occurs at DOC of 0.65 determined by the cure kinetics model. Through the dynamic mechanical analysis, a four step cure hardening modulus model (modified CHILE approach) was proposed. The aforementioned models were applied in a case study to evaluate the influence of process parameters on the DOC, viscosity and physical behavior of the acrylic resin system in the pultrusion die.Highlights Material characterizations of an acrylic resin system are investigated. The cure kinetics and viscosity and elastic modulus models are proposed. A pultrusion case study is given.