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Abstract  

Due to dynamic nature of processes taking place during the experiment (chemical reaction and physical processes, heat flow, gas flow, etc.) the results obtained by thermal methods may considerably depend on the conditions used during the experiment. Therefore, whenever the results of thermal analysis are reported, the experimental conditions used should be stated. In this paper we have studied the heat transfer from the furnace to the sample and through the sample during dynamic mechanical analysis measurements. Numerical modelling of the heat transfer was done using an own computer program based on the heat conduction equation, solved numerically applying the finite difference methods. The calculated values of the thermal lag between the furnace and the sample were compared with the values experimentally determined on samples of a composite polymeric energetic material (double-base rocket propellant). Also, the temperature distribution within the sample as a function of the heating rate was analysed using the same numerical model. It was found out that using this model and temperature dependent heat transfer coefficient, experimentally obtained values of the thermal lag between the furnace and the sample can be satisfactory described. It was also shown that even at slow heating rates, such is, e.g. 2 °C min−1, the thermal lag between the furnace and the sample can reach several degrees, while the thermal gradient within 3-mm thick rectangular sample can reach 0.4 °C.

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Abstract  

The aim of this paper is to describe how a dynamic mechanical analyser can be used together with the microwave coaxial line technique. This coupling enables the simultaneous recording of changes in the mechanical properties and moisture content of materials as a function of time or temperature at a selected frequency. The sample is placed either directly under the probe or clamped in the sample holder of the dynamic mechanical analyser. Sample positioning and heating is accurately controlled by the mechanical analyser and its temperature controller. Samples can be subjected to a constant static force, a frequency or both. A micro probe, recently designed for measurements on semi-rigid and rigid surfaces [1], and connected to a network analyser was used to monitor the moisture content of the samples.

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Abstract  

A description is given of modifications to a dynamic mechanical analyser (DMA) to allow controlled relative humidity (RH) experiments to be performed under isothermal or thermal scanning conditions. Free film samples of polyester melamine paints (under-cured, normal-cured and over-cured) were supplied and the viscoelastic properties measured in the tensile mode of the DMA. A reduction in the glass transition temperature (T g) of up to 10C was found as the controlled RH was increased.

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storage modulus calibration of dynamic mechanical analyzers . Annual book of ASTM standards, vol 14.02 . West Conshohocken PA : ASTM International (ASTM) . 5. E2425-06. Test method for loss modulus

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thermal characterization techniques are thermogravimetric analyzer (TG), differential thermal analyzer (DTA), differential scanning calorimeter (DSC), dynamical mechanical analyzer (DMA), and thermal constant analyzer (TCA) etc. Table 1 depicts the list

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Abstract  

Issues encountered with dynamic mechanical analysis of artists’ acrylic emulsion paint films are presented alongside modifications to improve controlled relative humidity (RH) experiments using isothermal and thermal scanning conditions. Free films of titanium white (PW6) artists’ acrylic emulsion paints were cast as free films and their viscoelastic properties measured using the tensile mode of the dynamic mechanical analyser (DMA). Artists’ acrylic emulsion paints are within their glass transition temperature region at room temperature and are highly responsive to changes in ambient temperature and relative humidity, hence controlling relative humidity during analysis is vital to the successful analysis of these paints.

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Abstract  

The activation energy associated with the glass transition relaxation of an epoxy system has been determined by using the three-point bending clamp provided in the recently introduced TA Instruments DMA 2980 dynamic mechanical analyzer. A mathematical expression showing the dependency of modulus measurements on the sample properties and test conditions has also been derived. The experimental results showed that the evaluation of activation energy is affected by the heating rate and test frequency, as well as the criterion by which the glass transition temperature (T g) is established. It has been found that the activation energy based on the loss tangent (tanδ) peak is more reliable than on the loss modulus (E 2) peak, as long as the dynamic test conditions do not cause excessive thermal lags.

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Abstract  

A description is given how the dielectric coaxial technique measuring in the microwave region has been used for monitoring drying processes in leather samples. It is also shown how the coupling of this technique together with dynamic mechanical analysis enables the simultaneous recording of changes inthe dielectric properties, related to the moisture content of the material, together with the mechanical properties as a function of time or temperature. The samples studied include unaged and artificially aged goat and calf leathers. Measurements using the dynamic mechanical analyser are presented over a range of temperature which includes the shrinkage temperature. During the drying process, values of mechanical modulus or displacement and dielectric permittivity are recorded as a function of time or temperature which includes the temperature range of leather shrinkage, and from previous research report of Larsen [1] this has been associated with the chemical state of the leather samples.

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A new high molecular weight polyimide based on 4,4′-oxidiphthalic anhydride (ODPA) dianhydride and 2,2′-dimethyl-4,4′-diaminobiphenyl (DMB) diamine has been synthesizedvia a one-step polymerization method. This polyimide is soluble in phenolic solvents. Films from 7 to 30 μm thick were cast from the polymer solution and show in-plane orientation on a molecular scale detected by Fourier transform infrared spectroscopy experiments. This anisotropic structure leads to anisotropic optical properties arising from two different refractive indices along the inplane and out-of-plane directions. ODPA DMB possesses high thermal and thermo-oxidative stability. The glass transition temperature has been determined to be 298 °C. Dynamic mechanical analyses show two relaxation processes appearing above room temperature: the β- and the α-relaxation processes. The α-relaxation corresponds to the glass transition while the β-relaxation is a secondary relaxation process associated with the non-cooperative subsegmental motion.

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Applications of the new 980 Dynamic mechanical analyser (DMA) to the study of thermoplastic polymers, thermosetting polymers and metal glasses have been discussed in this paper. This instrument has also been used to study impact modified thermoplastics [2] elastomers [3] and metals. DMA is one of the thermo-analytical thechniques available to the research or quality control chemist for evaluating the mechanical properties of materials. With the introduction of the 980 it is anticipated that the disadvantages due to long operation time and complexity inherent in older instrumentation will no longer hold back progress towards the full realisation of the technique.

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