Dynamic nuclear polarization is combined with temperature-jump methods to develop a new 2D C-13-C-13 NMR experiment that yields a factor of 100-170 increase in sensitivity. The polaization step is performed at similar to 100 K, and the sample is subsequently melted with a 10.6 mu m laser pulse to yield a sample with highly polarized C-13 spins. C-13 detected 2D C-13-C-13 spectroscopy is performed in the usual manner.