Use Of Dynamic Mechanical Analysis Research Articles

Advancing the dynamic mechanical analysis of organic semiconductor materials.

Dynamic mechanical analysis (DMA) is a powerful technique for characterizing the mechanical properties of a wide range of materials. However, the importance of DMA in studying organic/polymer semiconductors has not been fully appreciated. In this Highlight, we explore recent advancements in the use of DMA in understanding the viscoelastic and mechanical properties and thermal transitions of organic semiconductor materials. In particular, the insights gained from DMA can serve as new guides for the device optimisation of organic solar cells towards stable operation. Furthermore, we present key findings, challenges, and future directions to advance the application of DMA in organic electronics.

Investigation of frequency dependent mechanical properties of porous materials using dynamic mechanical analyzer and frequency-temperature superposition theory

In acoustic design of engineering applications - such as in the acoustic analysis of passenger vehicles - poroelastic materials are of great importance. One of the most influencing properties in determining their noise-reduction potential is the storage modulus. The purpose of this study is to examine the frequency dependence of storage modulus of selected porous acoustic materials at least up to 1000 Hz. This is executed by using the combined use of dynamic mechanical analyzer and frequency-temperature superposition theory. All other methods for measuring the storage modulus fall short in determining frequency-dependence above 100 Hz: quasi-static mechanical analyzer is mostly used for determining an averaged constant value deduced from low-frequency measurements, while the usage of an electromagnetic shaker capable for high-frequency excitation may include effects of fluid motion inside the pores, thus significantly modifying the results. Frequency-temperature superposition enables to determine the storage modulus values in a wide frequency range, based on low-frequency measurements, where fluid-structure interaction is negligible. It was found that the modulus varied significantly up to and beyond 1000 Hz, and thus, acoustical characterization of these materials can be significantly improved using the proposed method. The work concludes with recommendations to improve the accuracy of the results.

Use of Dynamic Mechanical Analysis (DMA) for Characterizing Interfacial Interactions in Filled Polymers

Dynamic mechanical analysis (DMA) provides reliable information about the viscoelastic behavior of neat and filled polymers. The properties of filled polymers are relevant to different industries as protective organic coatings, composites etc. Interfacial interactions in filled polymers play an important role in determining their bulk properties and performance during service life. In this brief review article, studies that used DMA to characterize the interfacial interactions in filled polymers have been reviewed. The available open literature provides a mixed opinion about the influence of interfacial interactions on the glass transition temperature of filled polymers. Nevertheless, it appears that in the case of strong interfacial interactions between the filler particles and the polymeric matrix, the peak value of tan δ is reduced in comparison to that of a filled polymer where these interactions are weak.

Comparison of Contemporary Elm (Ulmus spp.) and Degraded Archaeological Elm: The Use of Dynamic Mechanical Analysis Under Ambient Moisture Conditions.

This paper describes dynamic mechanical analysis (DMA) experiments on archaeological and contemporary elm tested under air-dry conditions, to explore the suitability of this technique for increasing understanding of the viscoelastic behaviour of archaeological wood. A strong reduction of storage modulus of archaeological elm (AE) was seen in comparison with contemporary wood (CE), resulting from the high degree of wood degradation, notably the reduction in hemicelluloses and cellulose content of AE, as demonstrated by Attenuated Total Reflection–Fourier Transform Infra-Red spectroscopy (ATR-FTIR). The γ relaxation peak was observed in all samples. The γ peak in AE shifted to a higher temperature, and the activation energy for γ-peak motions was lower in AE (29 kJ/mol) than in CE (50 kJ/mol) indicating that motion is less restricted within the degraded AE cell wall, or possibly a difference in the monomer undergoing rotation. Detection of changes in storage modulus are well known, but the DMA temperature scan technique proved to be useful for probing the degree of wood degradation, relating to the changes in location and intensity of secondary relaxation peaks. The γ peak in loss factor can be used to confirm that cell wall degradation is at an advanced stage, and to improve understanding of the internal spatial structure of the degraded wood cell wall.

Optimizing Viscoelastic Properties of Rubber Compounds for Ballistic Applications

Using interlayers of rubber adds a positive effect to the synergy of disruptor–absorber armors. Emerging from its viscoelasticity the material is able to transform mechanical stress into heat. The dynamic mechanical properties of elastomers depend on both ambient temperature and frequency of an applied mechanical load. The damping shows a maximum in the glass transition area. If the frequency of the glass transition is in the magnitude of the mechanical stress rate applied by ballistic impact, the elastomer will undergo the transition and thus show maximized damping. An ideal material for ballistic protection against small calibers is developed by making use of dynamic mechanical analysis and the time–temperature superposition principle. The material is later analyzed by ballistic experiments and compared to other nonideal rubbers with regard to glass transition temperature, hardness and damping. It is shown that by choosing a material correctly with certain glass transition temperature and hardness, the ballistic properties of a steel–rubber–aluminum armor can be enhanced. The chosen material (butyl rubber) with a hardness of 50 °ShA is able to enhance energy absorption during ballistic impact by around 8%, which is twice as good as other rubber with non-optimized properties.

Innovative strategy for designing proton conducting ceramic tapes and multilayers for energy applications

Aim of this work is to present, for the first time, the use of Dynamic Mechanical Analysis as a tool to characterize the thermo-mechanical behavior of green tapes defining the process conditions for the subsequent lamination step. This method was applied on tapes of protonic conductors, key-materials for different applications in the energy sector, from gas separation membranes to solid oxide fuel cells and electrolyzers. The pore former (rice starch) content was found to considerably affect the thermomechanical behavior (elastic and storage moduli, elongation to break, viscosity) of the tape and therefore the lamination process. The temperature required for a proper lamination increases from 50 up to 75 °C passing from the system without rice starch to the one with the highest pore former amount. This work identifies for the first time an optimal lamination viscosity (1010 Pa s), regardless the tapes formulation, required for a suitable adhesion among the layers.

The Potential of Agglomerated Cork for Sandwich Structures: A Systematic Investigation of Physical, Thermal, and Mechanical Properties.

Considering the major role played by sandwich structures in many fields where high stiffness-to-weight ratio is required, the selection of a suitable core material is of paramount importance. In order to face the environmental problems related to waste disposal, the selection of an eco-friendly core material is now included in the design criteria of sandwich structures. Agglomerated cork is recognized as a good solution that combines satisfactory mechanical performances and eco-sustainability. Many research studies individually addressed cork’s morphological, thermal, and mechanical features without providing a comprehensive overview of the relationships that exist between them. In this work, the investigation of the peculiar cork morphology allowed learning more about its good insulation capacity and its impressive recovery capability. The use of dynamic mechanical analysis (DMA) and thermogravimetric analysis (TGA) clarified the influence of temperature on both flexural and compressive performances. The effect of testing parameters such as temperature and speed on agglomerated cork properties was validated through statistical analysis. Moreover, to highlight agglomerated cork advantages and drawbacks, the work provides also a comparison with more traditional polyvinylchloride (PVC) foams commonly used in industrial applications.

Comparison of short and long term creep testing in high performance polymers

Abstract The creep behaviour of thermoplastics plays an important role in engineering design and especially the failure and lifetime prediction of structural components in a variety of industries. Often this mechanical property is determined with long-term creep tests. In order to reduce the development time of components made from such materials used in applications with conditions over 100 °C for long times, we propose the use of dynamic-mechanical analysis to predict long-term creep deformation through the stepped isothermal (SIM) and the stepped isostress methods (SSM). The present study aims to determine whether SIM and SSM can be generalised to material characterisation of advanced polymers at high temperature. Both methods are evaluated and verified by long-term measurements. Both amorphous and semi-crystalline polymers are studied and the influence of the glass transition temperature (Tg) on the accelerated test results is examined with tests conducted above and below the Tg region for PEEK. The results of our analysis show accelerated testing is an effective tool in predicting long term behaviour and comparing the creep response of thermoplastics. PAI exhibits a far superior creep response when compared to PEEK and PEI over 100 °C.

Self-powered pressure sensor based on the triboelectric effect and its analysis using dynamic mechanical analysis

Since 2012 there has been a rapid rise in the development of triboelectric nanogenerators due to their potential applications in the field of energy harvesting and self-powered sensors for vibrations, accelerations, touches, pressures and other mechanical motions. This study suggests a novel triboelectric nanogenerator based on the interaction between polyvinylidene fluoride and polyvinylpyrrolidone submicron fibers. Polyvinylpyrrolidone is introduced as a new material for the TENG because of its tendency of losing electrons easily, while polyvinylidene fluoride is selected for its strong-electron attracting ability. Electrospinning is suggested as a fabrication method for the nanofibers due to its simplicity, versatility and low-cost. Furthermore, the paper explores the possibility to use this triboelectric nanogenerator as a self-powered pressure sensor. For this purpose, the nanogenerator is subjected to dynamic mechanic analysis which produces controlled pressure forces applied with a certain frequency. This is the first work to suggest the use of dynamic mechanical analyzer to study the relation between the applied mechanical stimulus and the electric responses of the triboelectric nanogenerator. Eventually the sensitivity of the nanogenerator to different pressures is analyzed. A directly proportional relationship is found between the pressure applied and the resultant voltage and current amplitudes. The developed nanogenerator reacts to pressure in real time and as a sensor it exhibits a very high sensitivity and low experimental error for repeated measurements. The main contributions of this study are the development of a novel nanogenerator based on the triboelectric effect between polyvinylidene fluoride and polyvinylpyrrolidone electrospun fibers and the investigation for its potential use as a self-power pressure sensor. Eventually, the paper explores the advantages of dynamic mechanical analyzer for pressure analysis.

Assessment of the use of dynamic mechanical analysis to investigate initial onset of brown rot decay of Scots pine (Pinus sylvestris L.)

Microbiological degradation of wood by decay fungi can cause a rapid change in the structural properties of timber which can result in both strength and mass loss. Traditional techniques for the evaluation of decay (e.g. mass loss) lack the sensitivity to evaluate the effects of the very first stages of the decay process. This paper describes the effects of initial brown rot decay, defined by the amount of Poria placenta genomic DNA (gDNA) present in the samples, on the dynamic mechanical properties of the timber. It was found that there is a correlation between the mean storage modulus of the timber and the amount of P. placenta gDNA present, and therefore the level of decay. This shows that using dynamic mechanical analysis is a viable technique that can be used to study initial decay processes.

Wood quality assessment of Pinus radiata (radiata pine) saplings by dynamic mechanical analysis

The use of dynamic mechanical analysis was explored as a possible method of screening for wood quality in breeding programmes. Viscoelastic properties along the grain of wood from 18-month-old Pinus radiata saplings were measured using a humidity-controlled dynamic mechanical analyser. Storage modulus and tanδ were determined independently for opposite wood (OW) and compression wood (CW) in 25 trees in the temperature range from 10 to 45 °C at 5 °C intervals at three frequencies (0.1, 1 and 10 Hz) at constant moisture content of 9 %. Storage modulus and tanδ were frequency and temperature dependent. The two wood types did not differ significantly in their storage modulus. But OW exhibited significantly higher tanδ values than CW. The relationship of viscoelastic properties with physical (acoustic velocity, basic density and longitudinal shrinkage) and chemical wood properties was explored. There was a strong correlation (R = 0.76) between storage modulus and dynamic MOE (measured by acoustics). In addition, tanδ was positively correlated with longitudinal shrinkage. Monosaccharide compositions of the cell wall polysaccharides and lignin contents were determined and showed significant differences in the relative proportion of major cell wall components in OW and CW. Correlations between tanδ and xylose, originating from heteroxylans, and lignin content were found for CW, suggesting that the damping behaviour of cell walls is controlled by the matrix between cellulose fibril aggregates.

Determination of Glass Transition Temperature of Double-base Rocket Propellants with the Use of Dynamic Mechanical Analysis

The paper presents results of Dynamic Mechanical Analysis (DMA) of double-base (DB) solid rocket propellant with special attention paid to determining the glass transition temperature. The presented experiments were carried out with the use of Netzsch DMA 242C analyzer with the dual cantilever operation mode. Advantages and drawbacks of the DMA method, measured values, as well as important characteristics of solid double-base rocket propellants were briefly described. Obtained values of the storage modulus E', the loss modulus E, and tanδ were represented in dependence on temperature. The glass transition temperature of the tested propellant was determined according to NATO standard 4540 [7] at the peak of the loss modulus curve.

A Study of Isothermal Curing of PMI Using DMA

The isothermal curing of polymethacrylimide (PMI) is studied through the use of dynamic mechanical analysis (DMA). Based on the growth rate of measured dynamic mechanical property, the relative conversion is defined to investigate the evolution of storage modulusE′at different curing temperatures. Hsich’s nonequilibrium thermodynamic fluctuation theory, Avrami equation, and isoconversional methods are used to analyze isothermal cure kinetics of PMI. The results show that there are different increase modes ofE′at low temperature range and high temperature range, respectively. In low temperature range, the relative conversion curves include a transitional stage which is found to be strongly frequency-dependent, but this stage is not observed in the relative conversion curve in high temperature range. During the isothermal curing process, the relative evolution ofE′can be described by Hsich’s nonequilibrium thermodynamic fluctuation theory and Avrami equation. Moreover, the values and evolutions of activation energy are different in two temperature ranges, which suggest that the curing mechanism probably has changed.

Chitosan-dextran branched copolymers: Synthesis and properties

Chitosan-dextran branched copolymers have been synthesized, and the rheological properties of their aqueous acetic acid solutions have been studied. On the basis of the data of FTIR spectroscopy, the formation of chemical bonds between chitosan and dextran at the nitrogen atom has been confirmed. With the use of dynamic mechanical analysis and differential scanning calorimetry, the temperatures of relaxation transitions in the resulting branched copolymers have been determined. It is shown that, along with the formation of a branched copolymer, the chemical crosslinking of chitosan macrochains can occur. Mechanical properties of films formed from solutions of the obtained polymers have been studied.

A new method to predict optimum cure time of rubber compound using dynamic mechanical analysis

ABSTRACTThe degree of vulcanization of a rubber compound has a big influence on the properties of the final product. Therefore, precisely defining the curing process including optimum cure time is important to ensure the production of final products having high performance. Typically, vulcanization is represented using vulcanization curves. The main types of equipment used for producing vulcanization curves are the oscillating disc rheometer (ODR) and the moving die rheometer (MDR). These can be used to plot graphs of torque versus time at a constant temperature to show how cure is proceeding. Based on the results obtained, optimum cure time (t90) is calculated as the time required for the torque to reach 90% of the maximum achievable torque. In this study, the use of Dynamic Mechanical Analysis (DMA) for assessment of t90 was assessed. DMA was carried out using shear mode isothermal tests to measure the changes in material properties caused by vulcanization. The results revealed that the shear storage modulus (G′), shear loss modulus (G′′), and tan δ all reflect the vulcanization process, however, tan δ gave the best representation of level of vulcanization. Indeed, the curve of tan δ was able to be used to derive the t90 for rubber compounds and showed good agreement with the results from an MDR. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2014, 131, 40008.

Thermo-mechanical characterisation of in-plane properties for CSM E-glass epoxy polymer composite materials – Part 2: Young's modulus

The in-plane Young's modulus of a CSM E-glass/epoxy material is characterised through the use of dynamic mechanical analysis (DMA). The measured data is used to generate material models which describe the property behaviour as a function of conversion and temperature. Gelation of the epoxy resin plays a major role in the modulus development and is measured directly on the glass/epoxy material. The Young's modulus is described through a bi-functional model including the liquid/solid transition of the material. The evolution of Young's modulus is modelled by decoupling modulus increments caused by time and temperature, and is graphically illustrated through a Modulus-Temperature-Transformation (MTT) diagram. Based on the established material models presented in this paper and models in Part-1, it is feasible to assess residual stresses and shape distortions of composite parts made from this glass/epoxy material.

Preliminary studies for use of dynamic mechanical analysis (DMA) to verify intensity of thermal wood modifications

Colour change and/or mass loss due to thermal treatment are in direct relation to the performance of thermally modified wood. The application of techniques commonly used to characterise polymers may be used to study this relationship. A standard testing procedure in the field of plastics for the characterisation of bulk properties that directly affect material performance, is dynamic mechanical analysis (DMA). DMA indicates how a material will perform in a specific application. It can be used to identify the intensity of a thermal modification by evaluation of the viscoelastic response of wood. The paper presents the method together with results of preliminary tests with Norway spruce [Picea abies (L.) Karst.] and beech (Fagus sylvatica L.). The tests showed that it is possible to thermally modify small wood specimens directly inside the DMA equipment while, at the same time, getting real time mechanical and physicochemical information about the progress of the process.

The use of dynamic mechanical analysis (DMA) to evaluate plasticization of acrylic polymer films under simulated gastrointestinal conditions

Purpose Glass transition temperature ( T g) measurements of polymers are conventionally conducted in the dry state with little attention to the environment they are designed to work in. Our aim was to develop the novel use of dynamic mechanical analysis (DMA) to measure the T g of enteric polymethacrylic acid methylmethacrylate (Eudragit L and S) polymer films formulated with a range of plasticizers in the dry and wet (while immersed in simulated gastric media) states. Methods Polymer films were fabricated with and without different plasticizers (triacetin, acetyl triethyl citrate, triethyl citrate, polyethylene glycol, propylene glycol, dibutyl phthalate, dibutyl sebacate). T g was measured by a dynamic oscillating force with simultaneous heating at 1 °C/min. This was conducted on films in the dry state and while immersed in 0.1 M HCl to simulate the pH environment in the stomach. Results The T g of unplasticized Eudragit L and S films in the dry state was measured to be 150 and 120 °C, respectively. These values were drastically reduced in the wet state to 20 and 71 °C for Eudragit L and S films, respectively. The plasticized films showed similar falls in T g in the wet state. The fall in T g of Eudragit L films to below body temperature will have far-reaching implications on polymer functionality and drug release. Conclusions Immersion DMA provides a robust method for measuring T g of polymer films in the wet state. This allows better prediction of polymer behaviour in vivo.

Use of dynamic mechanical analysis (DMA) to determine critical transition temperatures in frozen biomaterials intended for lyophilization

Dynamic mechanical analysis is widely used to determine glass transitions in solid state materials. However, here we demonstrate the application of DMA for the determination of glass transitions (Tg ’) in the frozen liquid state by means of a steel sample pocket. The use of the pocket allows frozen material to be analysed and glass transition events demonstrated. In addition, it allows weak glass transitions to be detected clearly in some complex formulations where they can be obscured by eutectic and other strong thermal events when other methods such as DSC or DTA are used. Classical excipients (trehalose, lactose, dextran) were analysed and shown to give reproducible Tg ’ values, though with values slightly higher than those obtained by DSC. Finally, several complex real biological materials, typical of those encountered when freeze drying biological and biopharmaceutical materials, were analysed and the potential value of DMA demonstrated to determine the relevant glass transition temperatures for use in cryobiology and freeze drying.

Mechanical characterization of NiTi SMA wires using a dynamic mechanical analyzer

An investigation into the thermo-mechanical response of trained Ni–Ti shape memory alloy (SMA) wires with two-way shape memory effect (TWSME) induced into them was conducted in order to examine the influence of the cold work on quasi-static and fatigue behavior of SMAs. Use of dynamic mechanical analyzer (DMA) for such tests on thin wires was examined and successfully utilized. Quasi-static stress–strain responses of the wires at different temperatures were obtained to determine the critical stresses for forward as well as reverse transformations. Mechanical stress-controlled fatigue tests were conducted on the wires in the austenitic state (130°C). They showed a two-stage deterioration of fatigue life—a rapid decay when the maximum stress of the fatigue cycle is higher than the critical transformation stress, and a more gradual deterioration at stress levels considerably lower than the critical stress. The fatigue life of the wires was found to increase with the load ratio, R, whereas the frequency of cyclic loading had only a marginal effect. Differential scanning calorimetry (DSC) of the fatigued austenite specimens indicated the presence of residual stress-induced martensite in the austenitic state. The high concentration of the austenite–martensite interfaces act as potential sites for stress-concentration and are the main source of the drastic decrease of the fatigue life in the two-phase region.