We applied fluctuation microscopy technique to study medium-range order in tetrahedral semiconductor materials, such as amorphous silicon, amorphous diamond-like carbon films. It is shown that this technique is very sensitive to local structure changes in the medium range order and promises solutions to open questions that cannot be answered by current techniques. For asdeposited amorphous germanium and silicon, we previously identified a fine-grain para-crystallite structure [1, 2], which will be relaxed into a lower-energy continuous random network structure after thermal annealing. With the same fluctuation microscopy technique, we however found that thermal annealing introduces medium-range order in amorphous diamond-like carbon films. Future studies will be focused on modeling and systematic exploration of annealing effects.