With the rapid development of science and technology in micro/nanofield, it is urgent to carry out the research on new technology of micro/nanomechanics test and multiscale-related experimental mechanical analysis method. There is still a lot of work to be done in the basic theory and analysis method of micro-Raman spectroscopy as a new microscale mechanical test method applied to the experimental research of material mechanics. Based on the above background, the purpose of this paper is the application of spectrochemical technology in the preparation of nanomaterials and art identification technology. In this paper, different morphologies of SiO2 nanomaterials, such as crystalline nanoparticles, amorphous nanowires, nanospheres, and nanonets, were prepared by a simple hot steaming method in the presence of argon. The samples were characterized by Raman spectroscopy. In addition, this paper also carried out art identification work, using spectral technology to detect some paintings and calligraphy. The experimental results show that the Raman spectra of these paintings and calligraphy papers are in the visible region because their fluorescence is too strong, and almost all the peaks are submerged. In the near-infrared region (1064 nm), their peaks are also very weak, but they can be distinguished by fluorescence and scanning electron microscopy.