In-situ analyzation and detection of real-time chemical reactions can be a significant part in interpreting the underlying mechanism in very reactive chemical reactions. To do this, first we have designed a microfluidic device (MFD) pattern for observation of synthesis of hierarchical nanostructures based on graphene oxide (GO), conjugating the well-known coupling reaction by which the solution of 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC)-mediated coupling is enhanced in the presence of n-hydroxysuccinimide (NHS) to make amide bonding, hereafter called as the EDC coupling. Then, we have manufactured microfluidic devices with multiple tens of micrometer-sized channels that can circulate those nanomaterials to be chemically reacted in the channels. These microfluidic devices were made by negative photo lithography and soft lithography. We showed the possibility of using Raman spectroscopy to reveal the basic mechanism of the energy storage applications.