Dynamic mechanical analysis: Difference between revisions

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'''Dynamic mechanical analysis''' (abbreviated '''DMA''') is a technique used to study and characterize materials. It is most useful for studying the [[viscoelastic|viscoelastic]] behavior of [[polymer|polymers]]. A sinusoidal stress is applied and the strain in the material is measured, allowing one to determine the complex modulus. The temperature of the sample or the frequency of the stress are often varied, leading to variations in the complex modulus; this approach can be used to locate the [[glass transition|glass transition]] temperature<ref>{{cite web |url=https://coventivecomposites.com/explainers/dynamic-mechanical-analysis-dma/|accessdate=2018-10-01|title=What is Dynamic Mechanical Analysis (DMA)?}}</ref> of the material, as well as to identify transitions corresponding to other molecular motions.
 
==Theory==
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The viscoelastic property of a polymer is studied by dynamic mechanical analysis where a sinusoidal force (stress σ) is applied to a material and the resulting displacement (strain) is measured. For a perfectly elastic solid, the resulting strain and the stress will be perfectly in phase. For a purely viscous fluid, there will be a 90 degree phase lag of strain with respect to stress.<ref name="Meyers1999">{{cite book|last=Meyers|first=M.A.|author2=Chawla K.K.|title=Mechanical Behavior of Materials|publisher=Prentice-Hall|year=1999}}</ref> Viscoelastic polymers have the characteristics in between where some [[phase lag]] will occur during DMA tests.<ref name=Meyers1999/> When the strain is applied and the stress lags behind, the following equations hold:<ref name="Meyers1999"/>
 
*Stress: <math> \sigma = \sigma_0 \sin(t\omega + \delta) \,</math> <ref name=Meyers1999/>
*Strain: <math> \varepsilon = \varepsilon_0 \sin(t\omega)</math>
 
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====Derivation of dynamic moduli====
 
Shear stress <math>\sigma(t)=\int_{-\infty}^t G(t-t') \dot{\gamma}(t')dt'</math> of a finite element in one direction can be expressed with relaxation modulus <math>G(t-t')</math> and strain rate, integrated over all past times <math>t'</math> up to the current time <math>t</math>. With strain rate <math> \dot{\gamma(t)}=\omega \cdot \gamma_0 \cdot \cos(\omega t)</math>and substitution <math>\xi(t')=t-t'=s </math> one obtains <math>\sigma(t)=\int_{\xi(-\infty)=t-(-\infty)}^{\xi(t)=t-t} G(s) \omega \gamma_0 \cdot \cos(\omega(t-s))(-ds)=\gamma_0\int_0^{\infty} \omega G(s)\cos(\omega(t-s))ds</math>. Application of the trigonometric addition theorem <math>\cos(x \pm y)=\cos(x)\cos(y) \mp \sin(x)\sin(y)</math> lead to the expression
:<math>
\frac{\sigma(t)}{\gamma(t)}=\underbrace{[\omega\int_o^{\infty}G(s)\sin(\omega s) ds]}_{\text{shear storage modulus }G'} \sin(\omega t)+\underbrace{[\omega\int_o^{\infty}G(s)\cos(\omega s) ds]}_{\text{shear loss modulus }G''} \cos(\omega t).
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===Measuring glass transition temperature===
One important application of DMA is measurement of the [[Glass transition#Transition temperature Tg|glass transition temperature]] of polymers. Amorphous polymers have different glass transition temperatures, above which the material will have [[rubber]]y properties instead of glassy behavior and the stiffness of the material will drop dramatically along with a reduction in its viscosity. At the glass transition, the storage modulus decreases dramatically and the loss modulus reaches a maximum. Temperature-sweeping DMA is often used to characterize the glass transition temperature of a material.[[File:2019-10-17 20 23 45-DMA Reference Measurements Linear Drive - Anton Paar RheoCompass™.png|alt=|thumb|325x325px|Figure 2. Typical DMA thermogram of an amorphous thermoplastic (polycarbonate). Storage Modulus (E’) and Loss Modulus (E’’) and Loss Factor tan(delta) are plotted as function of temperature. The glass transition temperature of Polycarbonate was detected to be around 151°C (evaluation according to ISO 6721-11)]]
===Polymer composition===
 
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[[Image:Schematic of DMA.png|thumb|Figure 3. General schematic of a DMA instrument.]]
 
The instrumentation of a DMA consists of a displacement sensor such as a [[linear variable differential transformer]], which measures a change in voltage as a result of the instrument probe moving through a magnetic core, a temperature control system or furnace, a drive motor (a linear motor for probe loading which provides load for the applied force), a drive shaft support and guidance system to act as a guide for the force from the motor to the sample, and sample clamps in order to hold the sample being tested. Depending on what is being measured, samples will be prepared and handled differently. A general schematic of the primary components of a DMA instrument is shown in figure 3.<ref>{{cite web|url=http://www.mse.iastate.edu/research/research-groups/gom/laboratory-facilities/charaterization-lab/dma.html|title=DMA|accessdate=2010-02-02|url-status=dead|archiveurl=https://web.archive.org/web/20100610052549/http://www.mse.iastate.edu/research/research-groups/gom/laboratory-facilities/charaterization-lab/dma.html|archivedate=2010-06-10}}</ref>
 
===Types of analyzers===