Instructions for Quartz Crystal Microbalance (QCM)

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Introduction: The QCM is a very precise balance that operates on the basis of the piezoelectric effect. A potential is applied across the quartz crystal by two electrodes mounted on either side of the crystal. When the correct frequency of alternating current is applied, the crystal starts vibrating in its fundamental resonant mode. For the crystals we are using this mode is approximately 8 or 10MHz. The crystal is set up in a cell with one electrode surface exposed and the other protected. The crystal reacts quickly and precisely to changes at its surface, such as the formation of thin films, deposits, and so on. The resonant frequency of the crystal will decrease with additional mass, and from these changes, we can determine the mass change with the Sauerbrey equation:
f=2f 2 0 m / A

or
m= fA / 2f 2 0

where f = frequency, m = mass, = density of quartz (2.648 g/cm3), = shear modulus of quarts (2.947x1011 dyne/cm2) and A = active electrode area. The guide below is for the set up and use of the QCM with the LabView interface. For a more detailed discussion of theory, applications and equipment, please see the papers and other materials in the binder near the machine or on the web.

Set-Up: The first step is to ensure that the crystal is inserted into the cell properly.

-The large electrode must be up. If the other face of the crystal was up, the edges of the electrode would experience some interference through interactions with the liquid in the cell.

-Place the crystal in the bottom of the cell as shown. Be sure to use the extender (shown on the left) so that the electrodes will reach out of the cell.

-Place the cell on top of the bottom, and flip the cell over keeping the two pieces together. Insert the four screws in the slots in the bottom of the cell. Tighten the screws in a crosswise fashion to ensure even distribution of pressure (for instance, using the picture below, tighten #1, #3, #4, and then #2). This should be done gradually. That is, tighten each screw a small amount, then tighten the others a small amount and continue in the above pattern until all screws are sufficiently tight. Avoid excessive force as this may damage the cell and adversely effect the vibrations of the crystal.

Once the crystal is properly inserted in the cell, it is ready to be plugged in. Flip the cell over so that the cell opening is facing up. It should look like this:

-Plug the cell into lever oscillator 35366 as shown. The green dot on the cell corresponds to the electrode that will be facing solution. The black dot on the 35366 corresponds to the ground.

-Now plug the 35366 into the frequency counter using a coaxial cable. The terminal on the oscillator is labeled frequency counter.

-Plug the oscillator in using the transformer provided, and switch on the frequency counter. A frequency should appear on the counter screen somewhere in the vicinity of 10Mhz (or 8Mhz), depending on the crystal used), when clean and dry.

The apparatus is now set-up and ready to collect data. However, it is recommended that one allow the crystal AT LEAST HALF AN HOUR TO EQUILIBRATE. Temperature changes in the crystal due to the vibrations will cause fluctuation during the warm-up period. When the crystal has stabilized such that its fluctuations are not more than 5Hz around some point near 10MHz, it is ready for use. This point will vary from experiment to experiment due to differences in temperature, pressure, crystal position and screw tightness in the cell.

Data Acquisition: Log in to the computer next to the apparatus under the Ward Group account. On the desktop, there is an icon labeled QCM. Click on this icon and LabView will open and display the QCM interface pictured below.

This interface will control the data acquisition for the rest of the experiment. To begin collecting data click on the arrow in the tool bar across the top (you may also push Ctrl+R). Once the instrument is collecting data, it must be calibrated. To do this, click the Set Base Frequency button. This will cause the delta frequency and delta mass fields to display zero (or a value quit near zero). If you notice a drift in the delta fields, please allow more time for the crystal to warm up before proceeding. If a medium, such as water, is added to the cell, please allow 5-10 more minutes for the system to reach and equilibrium and reset the base frequency before continuing.

Aside from the delta mass and delta frequency fields, there is also a plot of the frequency change versus time on the display. The default bounds are from -200Hz to 2000Hz along the Y-axis and the most recent 30 seconds along the x-axis. -To adjust the graph, simply highlight the bound that you would like to change and enter a new value using the keyboard -This graph is for instantaneous display only. If a print out is required, please see the instructions below. The default interval for data acquisition is 500ms. If you would like to lengthen this you may add additional ms to the interval with the counter on the interface. This value can be typed in or you can adjust it using the arrows.

Saving Data: Once you have started collecting data, LabView will continue to read from the frequency counter and display results until you press the stop button. Do not press stop without confirming your data saving preference. If you would like to save your results, make sure that the switch marked save is in the on position before pressing stop. Once the data collection has halted a dialog asking where you would like to save your data will appear.

Choose a place where you would like to save your data and name the file *.txt. It is important that you add the .txt suffix to the file name so that it will be in the proper format for use with excel. Now you are done. Please close the program after stopping it, and leave the Oscillator and crystal cell as you found them.

Analyzing and Printing Results: If you wish to print your results, but do not plan on doing an manipulation of them with Excel, simply open the *.txt file that you saved in the above procedure. If you would like to import your data to Excel for graphing or calculation purposes, please follow the procedure below. Using Excel: Theses instructions are based on the newest version (2007), but should be rather similar for other versions. 1) 2) 3) 4) Open the Excel program and a new worksheet (one may open automatically). Click on the Data tab on the top menu bar. From the far right select from text. When prompted to input a file location, point the program to the output saved above. 5) On the first screen when prompted for data type choose delimited. Also, ensure that import will start at row 1. Push next.

6) On the next screen, confirm that the delimiters are Tab. Push Next. 7) On the next screen choose the general radio button for data format. This should be the default value. Click finish. 8) Excel will now prompt you for a location to place this new data. Choose a cell that you would like to be the upper left corner of your data table. Click OK. 9) Your data has now been imported into Excel and can be manipulated as any other data.