Time-Domain Thermoreflectance Protocol (solid-liquid)

1. Turn on the laser and let the laser warm up for 10 15 minutes. Confirm the
mode-locking by connecting the photo-diode to the oscilloscope
2. The pump beam is separated by ~ 3mm from the top of the probe beam
when viewed at the back of the objective lens
3. Check for parallelism of the pump and probe beams at the back of the
objective lens
4. Mount the sample on the holder. Turn off the lights and block the pump and
probe beams. Turn on the circular light in the objective lens. With the help of
the CCD camera, focus on the sample. Focus cannot be achieved if there are
irises in the camera path. Note that occasionally the glass will come into
focus and will be indistinguishable from
5. Ensure that moving the sample to the left and right does not result in the
objective lens losing focus on the surface. This can lead to refraction of the
probe beam and at long delay times lead to discrepancies in the data
6. Remove the beam blocker in the probe beam path. Use the polarizer to locate
the probe beam on the monitor. Center the probe beam on the scale (on the
monitor) using the beam splitter on in probe beam path. Center the pump
beam on the monitor using the polarizing beam splitter (PBS) on the pump
path
7. Turn on the photodetector and position it to let the reflected probe beam fall
on the photodiode. Use an iris in front of the photodetector to block the
pump beam from corrupting our signal.
8. Open the ensemble application (delay stage controlling software) on the data
collection computer and move the delay stage to positive time delay. There
should be a signal on the lock-in amplifier
9. Block the probe beam and zero the lock-in amplifier. The X (Vinphase) and Y
(Voutofphase) should read zero.
10. Open the probe beam path and check the signal on the lock-in amplifier.
Maximize this signal by overlapping the pump beam on the probe beam by
using the x-y stage on the polarizing beam splitter. These should ideally be
very fine adjustments
11. Open the labview program and adjust the out-of-phase signal such that its
fairly constant at short delay times before and after t = 0s. This can be done
by using the phase adjustment.xls spreadsheet.

12. Collect the Vin/Vout for an Al-Fused Silica reference sample to begin with. The
data collection template should have a Reference Sample spreadsheet. Copy
and paste your data into the reference sample section of the spreadsheet. The
data should match data that has been collected earlier
13. When working with metal-monolayer samples, first collect data for all
samples in air. This should give the exact same signal for all the samples you
have. The ones that do not provide you with the same signal should not be
used.
14. Flush the fluid cell with liquid of choice using a luer-lock syringe.
15. To change out a sample to do another TDTR measurement, take fluid cell to
the interfacial engineering lab remove the sample and then flush the luers
and the section the sample sits on with the liquid that is being used. Finally,
blow dry with a nitrogen gun and set next sample onto fluid cell for analysis.