EQCM Tutorial
EQCM Tutorial
EQCM Tutorial
EQCM Tutorial
Version 1.11.0
NOVA EQCM tutorial
2𝑓𝑓02
∆𝑓𝑓 = − ∙ ∆𝑚𝑚
𝐴𝐴�𝜌𝜌𝑞𝑞 𝜇𝜇𝑞𝑞
Where ∆𝑓𝑓 is the change in frequency, in Hz, 𝑓𝑓0 is the nominal resonant frequency
of the crystal (6 MHz), ∆𝑚𝑚 is the change in mass, in g/cm2, 𝐴𝐴 is the area of the crystal
in cm2, 𝜌𝜌𝑞𝑞 is the density of quartz, in g/cm3 and 𝜇𝜇𝑞𝑞 is the is the shear modulus of
quartz, in g/cm·s2.
More information about the EQCM module can be found in the EQCM user manual.
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2 – Hardware setup
In order to use the EQCM module, the hardware setup in NOVA must be configured
accordingly (see Figure 1).
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• EQCM(1).Temperature
• EQCM(1).Driving force
• EQCM(1).∆Frequency
Figure 2 – The signals provided by the EQCM are available in the sampler
The temperature signal is measured by the sensor located at the bottom of the
EQCM cell. This signal is provided in °C. The driving force signal corresponds to a
voltage value between 0 V and 2.5 V. This value represents the amount of energy
required to sustain the oscillation of the crystal. When the loading of the crystal
increases, the driving force also increases. In air, the typical driving force is close to
0 V. In water, the driving force is about 0.85 V. The ∆Frequency signal corresponds
to the relative change in oscillation frequency of the quartz crystal. This variation is
expressed with respect to an arbitrary, user-defined reference frequency (zero Hz).
Note
The electrochemical signals provided by the EQCM are not sampled through the
ADC164 module. These signals are directly provided by the EQCM module. This
means that these signals cannot be sampled in ‘optimized mode’.
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Warning
The highest possible sampling rate of the EQCM module is 50 samples/s (20 ms
interval time). If measurements with shorter interval times are performed, the last
values of the EQCM signals will be recorded multiple times until new samples are
obtained for these signals.
Figure 3 – The Autolab control window can be used to switch the EQCM module ON or OFF
Once the EQCM has been switched on, the electrochemical signals provided by the
EQCM module can be sampled, using any available measurement command (except
measurement commands using the FRA2/FRA32M module or the fast-sampling ADC
module 1).
1
ADC750 or ADC10M.
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Figure 4 – The Reset EQCM ∆Frequency command can be found in the Measurement –
General group
Note
This command can be added anywhere in a procedure. Whenever the Reset EQCM
∆Frequency command is used, a window allowing fine tuning of the EQCM driving
force and zeroing of the ∆Frequency value will be displayed (see Figure 5).
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The topmost section, shown in Figure 6, displays real time information on the
measured signals provided by the EQCM:
Figure 6 – The topmost section of the Determine EQCM zero frequency window displays the
measured values in real time
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The middle section, shown in Figure 7, displays the recorded values of the driving
force plotted versus time.
Figure 7 – The middle section of the Determine EQCM zero frequency window displays the
measured driving force plotted versus time
The bottom section, shown in Figure 8, displays a series of buttons that can be used
to control the behavior of the Determine EQCM zero frequency:
Figure 8 – The bottom section of the Determine EQCM zero frequency window displays the
measured values in real time
• Zero Δf: set the value of the measured ΔFrequency to zero. Setting the
value to zero requires several iterations. During this adjustment, the
button will be grayed out.
• Clear plot: this button can be used to clear the plot displayed in the
window. The measurement resumes after the button is pressed. The
values shown in the topmost part of the window are not cleared.
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Using the provided screw driver, the trimmer on the EQCM oscillator should always
be adjusted in order to minimize the driving force of the QCM crystal. This should
always be performed every time the environment of the crystal is changed. The
driving force value is displayed in the plot area of the Determine EQCM zero
frequency window.
The Clear plot button can be pressed at any time to clear the display. The
button can be used to zero the ∆Frequency signal. Pressing the Abort button stops
the measurement.
Note
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The EQCM tutorial contains two procedures that can be used as examples of
electrochemical quartz crystal microbalance measurements (see Figure 10).
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Load the Cyclic voltammetry with EQCM procedure in the procedure editor. This
procedure is designed to perform a cyclic voltammetry staircase measurement in
potentiostatic mode. At the beginning of the procedure, the EQCM module is
switched on, using the Autolab control command (see Figure 11).
During the cyclic voltammetry experiment, the three signals provided by the EQCM
module are sampled alongside the WE(1).Current signal. The measurement starts by
applying a pre-conditioning potential. Just before the cyclic voltammetry
measurement starts, the Reset EQCM ∆Frequency is used to fine tune the settings
of the EQCM module and to zero the ∆Frequency signal (see Figure 11).
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Figure 12 – An example of EQCM cyclic voltammetry recorded using the Cyclic voltammetry
with EQCM procedure (blue curve: current, red curve: ∆Frequency)
Load the Chrono amperometry with EQCM procedure in the procedure editor. This
procedure is similar to the previous one. It is designed to perform a potential step
experiment during which the signals provided by the EQCM module are sampled.
At the beginning of the procedure, the EQCM module is switched on, using the
Autolab control command (see Figure 13).
After the first potential value has been applied and the response of the cell has been
recorded using the Record signals (> 1 ms) command, the Reset EQCM ∆Frequency
is used to fine tune the settings of the EQCM module and to zero the ∆Frequency
signal (see Figure 13). After the ∆Frequency signal has been zeroed, the procedure
proceeds with the potential step and the response of the cell is sampled.
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Hardware specifications
The EQCM module is an option module for the modular Autolab PGSTAT, with the
exception of the PGSTAT100, PGSTAT100N and PGSTAT302F 2. The EQCM module
is fitted with a 6 MHz crystal oscillator and it can be used to monitor changes in
frequency, with a dynamic range of 80000 Hz.
The module is also fitted with a temperature probe, which can be connected to the
temperature sensor embedded in the standard electrochemical cell provided with
the module.
Specification Value
Oscillation frequency 6 MHz
Frequency resolution 0.07 Hz
Relative accuracy 1 Hz
Absolute accuracy 10 Hz
Frequency range 80 kHz
Temperature sensor accuracy 1 °C
Temperature sensor resolution 0.1 °C
Note
More information about the EQCM module can be found in the EQCM User
Manual.
2
The EQCM module cannot be fitted in the µAutolab II/III and in the PGSTAT101.
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