An electrochemical quartz crystal microbalance study on adsorption of single walled carbon nanotubes onto poly[3,4-ethylenedioxythiophene] layers

Efimov, Igor; Gruia, Violeta-Tincuţa; Rumiche, Francisco; Bund, Andreas; Ispas, Adriana

doi:10.1007/s10008-015-2979-4

Cited by 5 publications

(7 citation statements)

References 38 publications

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“…This method provides noninvasive in situ real-time monitoring of these properties during long-term cycling of batteries and supercapacitor electrodes. The two output channels of EQCM-D, namely resonance frequency and dissipation, make it highly suitable for both gravimetric and combined gravimetric and mechanical characterization of thin battery and supercapacitor electrodes. − The dissipation factor D is defined as the ratio of the full-width at half-height of the resonance peak (i.e., bandwidth W ) to the resonance frequency, f : D = W / f. For brevity, we will refer to W as the “resonance width”.…”

Section: Introductionmentioning

confidence: 99%

“…As can be seen in Figure (bottom), the acoustic shear waves generated by a piezoelectric crystal, operating in horizontal-shear (or thickness-shear) mode, penetrate a thin electrode coating rigidly attached to a quartz crystal (QC) surface in contact with a gas or liquid (here “rigidly attached” means no-slipping condition at the interface). − The loading coating shifts the values of f and W from that typical for the pristine (uncoated) QC. Immersion of coated crystal into a liquid causes additional changes in f and W. The entire shifts of resonance frequency and resonance width (Δ f and Δ W , respectively) contain encoded information about the electrode material properties.…”

Section: Introductionmentioning

confidence: 99%

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In Situ Real-Time Mechanical and Morphological Characterization of Electrodes for Electrochemical Energy Storage and Conversion by Electrochemical Quartz Crystal Microbalance with Dissipation Monitoring

et al. 2018

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Quartz crystal microbalance with dissipation monitoring (QCM-D) generates surface-acoustic waves in quartz crystal plates that can effectively probe the structure of films, particulate composite electrodes of complex geometry rigidly attached to quartz crystal surface on one side and contacting a gas or liquid phase on the other side. The output QCM-D characteristics consist of the resonance frequency (MHz frequency range) and resonance bandwidth measured with extra-ordinary precision of a few tenths of Hz. Depending on the electrodes stiffness/softness, QCM-D operates either as a gravimetric or complex mechanical probe of their intrinsic structure. For at least 20 years, QCM-D has been successfully used in biochemical and environmental science and technology for its ability to probe the structure of soft solvated interfaces. Practical battery and supercapacitor electrodes appear frequently as porous solids with their stiffness changing due to interactions with electrolyte solutions or as a result of ion intercalation/adsorption and long-term electrode cycling. Unfortunately, most QCM measurements with electrochemical systems are carried out based on a single (fundamental) frequency and, as such, provided that the resonance bandwidth remains constant, are suitable for only gravimetric sensing. The multiharmonic measurements have been carried out mainly on conducting/redox polymer films rather than on typical composite battery/supercapacitor electrodes. Here, we summarize the most recent publications devoted to the development of electrochemical QCM-D (EQCM-D)-based methodology for systematic characterization of mechanical properties of operating battery/supercapacitor electrodes. By varying the electrodes' composition and structure (thin/thick layers, small/large particles, binders with different mechanical properties, etc.), nature of the electrolyte solutions and charging/cycling conditions, the method is shown to be operated in different application modes. A variety of useful electrode-material properties are assessed noninvasively, in situ, and in real time frames of ion intercalation into the electrodes of interest. A detailed algorithm for the mechanical characterization of battery electrodes kept in the gas phase and immersed into the electrolyte solutions has been developed for fast recognition of stiff and viscoelastic materials in terms of EQCM-D signatures treated by the hydrodynamic and viscoelastic models. Working examples of the use of in situ hydrodynamic spectroscopy to characterize stiff rough/porous solids of complex geometry and viscoelastic characterization of soft electrodes are presented. The most demonstrative example relates to the formation of solid electrolyte interphase on LiTiO electrodes in the presence of different electrolyte solutions and additives: only a few cycles (an experiment during ∼30 min) were required for screening the electrolyte systems for their ability to form high-quality surface films in experimental EQCM-D cells as compared to 100 cycles (200 h cycling) in conventi...

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

In Situ Real-Time Mechanical and Morphological Characterization of Electrodes for Electrochemical Energy Storage and Conversion by Electrochemical Quartz Crystal Microbalance with Dissipation Monitoring

et al. 2018

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“…However, the readers of this Perspective article should not be left with the opinion that only EQCM-D provides the assessment of dimensional, porous structure and viscoelastic changes in battery electrodes during their charging; utilization of network analyzers working on multiple harmonics results in essentially similar information . In recent work, it was nicely demonstrated that coupling of viscoelastic effects of different electrode hosts with the shallow roughness of their external surface can be rigorously quantified in terms of quartz crystal impedance analysis. − …”

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confidence: 99%

In Situ Monitoring of Gravimetric and Viscoelastic Changes in 2D Intercalation Electrodes

et al. 2017

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Viscoelastic properties of battery electrodes in contact with electrolyte solutions may affect the electrodes' cycling performance. However, they are not easily assessed by in situ measurements. Herein, we show that an electrochemical quartz-crystal microbalance with dissipation (EQCM-D) enables extraordinary sensitive probing of intrinsic electrodes materials' properties such as intercalationinduced gravimetric and viscoelastic changes, using Ti 3 C 2 (OH) 2 (MXene) as a classical 2D intercalation model material. The insertion of each Li-ion into thin electrodes comprising this MXene is accompanied by insertion of one water molecule. Solvent-dependent viscoelastic changes and periodic stiffening/softening upon fully reversible Li-ion intercalation/deintercalation into an MXene electrode correlates well with its excellent long-term cycling performance. The experimental platform based on a commercial instrument, EQCM-D monitoring, and advanced viscoelastic modeling (extended Voight-type model) can be used for in situ real time characterization of intrinsic materials' properties of practical composite battery electrodes important for a deeper understanding of the factors controlling their cycling performance.

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“…We have shown that the hydrodynamic factor affects both the frequency and resonance width changes in a rough/porous rigidly attached solid. Similar hydrodynamic corrections for a particular (shallow-type) roughness of viscoelastic deposits have been recently considered to provide good fitting to the experimental quartz-crystal impedance data. , …”

Section: Resultsmentioning

confidence: 97%

“…Similar hydrodynamic corrections for a particular (shallow-type) roughness of viscoelastic deposits have been recently considered to provide good fitting to the experimental quartz-crystal impedance data. 40,41 ■ CONCLUSIONS…”

Section: Analytical Chemistrymentioning

confidence: 99%

Electrochemical Quartz Crystal Microbalance with Dissipation Real-Time Hydrodynamic Spectroscopy of Porous Solids in Contact with Liquids

Sigalov

Shpigel

Levi³

et al. 2016

Anal. Chem.

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Using multiharmonic electrochemical quartz crystal microbalance with dissipation (EQCM-D) monitoring, a new method of characterization of porous solids in contact with liquids has been developed. The dynamic gravimetric information on the growing, dissolving, or stationary stored solid deposits is supplemented by their precise in-operando porous structure characterization on a mesoscopic scale. We present a very powerful method of quartz-crystal admittance modeling of hydrodynamic solid-liquid interactions in order to extract the porous structure parameters of solids during their formation in real time, using different deposition modes. The unique hydrodynamic spectroscopic characterization of electrolytic and rf-sputtered solid Cu coatings that we use for our "proof of concept" provides a new strategy for probing various electrochemically active thin and thick solid deposits, thereby offering inexpensive, noninvasive, and highly efficient quantitative control over their properties. A broad spectrum of applications of our method is proposed, from various metal electroplating and finishing technologies to deeper insight into dynamic build-up and subsequent development of solid-electrolyte interfaces in the operation of Li-battery electrodes, as well as monitoring hydrodynamic consequences of metal corrosion, and growth of biomass coatings (biofouling) on different solid surfaces in seawater.

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An electrochemical quartz crystal microbalance study on adsorption of single walled carbon nanotubes onto poly[3,4-ethylenedioxythiophene] layers

Cited by 5 publications

References 38 publications

In Situ Real-Time Mechanical and Morphological Characterization of Electrodes for Electrochemical Energy Storage and Conversion by Electrochemical Quartz Crystal Microbalance with Dissipation Monitoring

In Situ Real-Time Mechanical and Morphological Characterization of Electrodes for Electrochemical Energy Storage and Conversion by Electrochemical Quartz Crystal Microbalance with Dissipation Monitoring

In Situ Monitoring of Gravimetric and Viscoelastic Changes in 2D Intercalation Electrodes

Electrochemical Quartz Crystal Microbalance with Dissipation Real-Time Hydrodynamic Spectroscopy of Porous Solids in Contact with Liquids

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