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Characterizations of nanomaterials and nano-process are essential studies in order to establish fabrication processes of the nanomaterials and to optimize their conditions. The structural and compositional characterization is considered to be a first step for this kind of study. Secondary ion massspectrometry (SIMS) is one of the useful methods to analyze the composition, particularly trace elements. Advantages and disadvantages of SIMS analytical technique are discussed, comparing with other methods. Nano-particles patterning process is explained, using zinc oxide nano-particles. Its evaluation is carried out by means of a static SIMS, as example. Finally, the recent development of the novel Nano-SIMS is briefly mentioned, and then its application is reported, concerning with the grain boundary analysis of ceramics consisted with fine grains.