A high temperature in situ optical probe for colloidal nanocrystal synthesis

We report on the fabrication and utilization of a robust high-temperature (>300 °C), adjustable-path-length, vacuum-tolerant, configurable, in situ optical probe, which interfaces with widely used chemical glassware via a 14/20 ground glass joint. This probe allows for high-speed reaction monitoring of colloidal semiconductor nanocrystal solutions at temperatures that were previously inaccessible. We demonstrate this capability by monitoring the hot-injection synthesis of CdSe quantum dots via UV-Vis absorption spectroscopy at 380 °C with a time resolution of ∼10 ms, with the primary limitation being the acquisition and data saving rate of the commercial spectrometer used. We further demonstrate that this probe can also be used for in situ photoluminescence measurements. This system is generally applicable to harsh solution environments where optical monitoring of reaction progress is desirable and/or necessary.