Using thickness-shear mode quartz resonator for characterizing the viscoelastic properties of PDMS during cross-linking, from the liquid to the solid state and at different temperatures
Introduction
The Quartz Crystal Microbalance (QCM) is a versatile tool, first described by Sauerbrey in his seminal work [15]. Due to its simplicity, this type of sensor has been widely used in various domains, enabling us to determine with accuracy measurands [5] such as mass density [19], viscosity [10] and pressure [18], in a continuous and non-destructive manner, with sample as small as a microliter. As illustrated in Fig. 1, it consists in a circular thin disk of piezoelectric AT-cut quartz, with metallic electrodes on both sides. The application of a voltage between them generates a shear deformation of the crystal, which can then be excited into resonance when its thickness is near an odd multiple of half the acoustic wavelength. The deposit of a material sample on the crystal changes the resonance properties, which are fundamentally dependent on the characteristics, either mechanical or electrical, of the sample. For all its applications, the QCM needs an electrical interface able to apply a sinusoidal voltage between its electrodes and to measure the resonance conditions. Among all the methods of read-out, the most used is the impedance analysis [1], which maps the electrical admittance of the QCM as a function of the frequency, giving access to a greater number of parameters than simpler methods such as the use of an oscillator circuitry.
In biology, where the QCM is increasingly used [2], the functionalization of the QCM surface with a definite substance enables us to measure active species absorption or deposition, and then to recognize specific pathologies like schistosomiasis [21] or Ebola fever [22]. In chemistry, with a similar method, such a sensor can detect presence of harmful molecules in the air, acting as an electronic nose [17]. In mechanics, finally, it is used for measuring complex shear modulus of polymers [12], [8], [16] or for following its evolution during a specific process, such as dissolution [7].
To our best knowledge, the QCM has never been used to characterize the viscoelastic properties of a rubber at different stages of the crosslinking, while it should provide additional information to better describe and understand crosslinking kinetics. This study aims at performing such measurements with a polydimethylsiloxane (PDMS), from the liquid to the solid state, at different temperatures.
The paper is organized as follows. Section 2 briefly describes the theory governing the behavior of the QCM and the measurement principle. Section 3 presents the application to the characterization of viscoelasticity of a polydimethylsiloxane: the experimental device, the measurement methodology and the material. Results obtained are analyzed in light of the aforementioned objectives. Concluding remarks close the paper.
Section snippets
Theoretical framework and measurement principle
On a fundamental point of view, the QCM is simply a transducer, linking its load impedance with its electrical impedance. The fundamental relations governing its behavior are briefly recalled hereafter. The reader can refer to [9] for further information.
Materials and methods
The quartz crystal and its holder used in the experiments are the commercially available QCM200 (Stanford Research Systems, CA, USA). The crystal has a resonance frequency near 5 MHz and a diameter of 2.54 cm. It is covered with circular electrodes of titanium and gold. It is physically maintained with one O-ring on both side and connected with the electrical interface via BNC connectors, which are then adapted to an SMA connection. The portable network analyzer is the miniVNA PRO (mini Radio
Conclusion
The present paper aimed at presenting the QCM as a relevant tool for measuring the viscoelastic properties of rubbers in the megahertz domain. The advantage of such a technique is that the measurement can be carried out for liquids and for solids as well, i.e. from the uncross-linked to the cross-linked state. The volume of the material needed is small compared to classical characterizations. This technique is well adapted to measurements in an oven, i.e. at different temperatures. It has been
Amaury Dalla Monta received his Master in Mechatronics in 2015. He is a PhD Student at the Institute of Physics at University of Rennes 1 since October 2015.
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2022, Biosensors and Bioelectronics: XCitation Excerpt :Meanwhile, in electrochemistry, data obtained from impedance measurements where sensing electrode of a QCM in liquid medium was used as a working electrode in a three electrode electrochemical setup, allowed monitoring of electron transfer on QCM (Gabrielli et al., 2007). Today, QCM is employed to monitor electropolymerization (Antonio et al., 2019; Ayankojo et al., 2018), ion intercalation (Narayanan et al., 2020), corrosion (Tang et al., 2021) and electrodeposition (Tesakova et al., 2020), thin film characterizations, such as, crosslinking (Dalla Monta et al., 2018; Galagedera and Flechsig, 2020), swelling (Hollingsworth et al., 2019; Qian et al., 2018) or any other structural changes, affinity measurements of binding events (Zhang et al., 2020), including interactions of proteins and hybridization events of DNA (Sun et al., 2017), RNA or chemical analogues thereof. There are several ways to measure parameters of QCM: impedance or network analysis, decay methods and oscillators are used by majority of the devices in the market due to having major advantages among others (Arnau, 2008; Alassi et al., 2017).
QCM modified with FAU zeolite nanostructures for analysis of temperature induced adsorbed mass changes
2021, Measurement: Journal of the International Measurement ConfederationCitation Excerpt :In other words, if an uniform layer is deposited on the surface of the QCM, the variation of the frequency is proportional to the deposited mass. In simple terms, the increment in the QCM thickness causes that acoustic waves travel over a “longer” distance than when there is no additional mass on the QCM [6]. In practice, when the mass is loaded on the QCM surface, the frequency generated by the QCM decreases.
Mechanical characterization of PDMS with different mixing ratios
2021, Procedia Structural IntegritySimple fabrication of highly sensitive capacitive pressure sensors using a porous dielectric layer with cone-shaped patterns
2021, Materials and DesignCitation Excerpt :When the periodic force is applied, the output signals generally follow the same shapes as that of the driving signals, showing a minimal delay (Fig. 7(b)). It was assumed that the reaction force would slightly decrease with time due to the viscoelastic properties of PDMS [35–37]. The robustness of the sensor is also an important factor.
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Amaury Dalla Monta received his Master in Mechatronics in 2015. He is a PhD Student at the Institute of Physics at University of Rennes 1 since October 2015.
Dr. Florence Razan received her Master in Physics in 2002 and PhD in microsensors from Bordeaux 1 University in 2005. Since 2006, she is an Associate Professor at ENS Rennes, Mechatronics Department. She has been working at the SATIE Laboratory, where her main interest is the development of microsensors for soft material characterization. Since 2015, she is the head of the Mechatronics Department.
Prof. Jean-Benoît Le Cam received his PhD from Ecole Centrale de Nantes in 2005 and has since worked on experimental characterization of the physical phenomena involved in the deformation of polymers. In 2006, he joined the French Institute of Advanced Mechanics as an Assistant Professor. In 2011, he joined the Institute of Physics at University of Rennes 1 (UR1) as a Professor in order to create the Quantitative Imaging Group on mechanics of elastomers. Since 2015, he holds the Cooper Standard Chair in mechanics of elastomers at UR1 and manages the LC-DRIME Research lab.
Dr. Grégory Chagnon is engineer of Ecole Centrale de Nantes in 2000 and received the M.Sc. degree in Mechanical Engineering from Nantes University, France, in 2000. He received the Ph.D. degree in Mechanical Engineering for his research in the field of mechanical analysis and modelling of rubber like materials in 2003. He is currently the head of the Biomedical and Mechanical engineering of Materials (BioMMat) team of the TIMC-IMAG laboratory (Grenoble), and he is specialist in Mechanics of soft materials and also works on the development of smart biomedical devices.