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Here, for the first time, the development of graphitic structure in the hierarchal porous sulfonated\u2010PDVB microspheres without employing specific equipment or additives like metal catalysts, organic ingredients, or graphite particles, at 1100\u00b0C is reported. The abnormal additive\u2010free graphitic structure formation is confirmed by Raman spectroscopy (I<jats:sub>D<\/jats:sub>\/I<jats:sub>G<\/jats:sub> = 0.87), high\u2010resolution transmission electron microscopy (HRTEM), and selected area diffraction patterns (SAED), as well as x\u2010ray diffraction patterns (XRD), while preservation of aromatic compounds from the carbonization is detected by Fourier transform infrared (FTIR) analysis. Polymer evolution from room temperature to 1100\u00b0C is also studied by FTIR, Raman spectroscopy, and XRD\u00a0techniques. Based on the obtained results, it is suggested that the hierarchal and complicated ink\u2010bottle pore network with a high surface area besides super micropores in the sulfonated\u2010PDVB microspheres has served as nano\u2010sized reaction media. These pores, hereafter referred as \u201cdynamic nanoreactors\u201d, are expected to have confined the in\u2010situ produced thermal decomposition products containing broken bond benzene rings, while changing dimensionally and structurally during the designed carbonization regime. This confinement has led to the benzene rings fusion at 250\u00b0C, a remarkable extension of them at 450\u00b0C, their growth to graphene sheets at 900\u00b0C and finally, the stacking of curved graphene layers at 1100\u00b0C. The results of this research put stress on the capability of nanopores as nanoreactors to facilitate reactions of decomposition products at low temperatures and ambient pressures to form stacked layers of graphene; A transformation that normally requires catalysts and very high pressures for only specific polyaromatic hydrocarbons.<\/jats:p>","DOI":"10.1002\/smll.202308082","type":"journal-article","created":{"date-parts":[[2024,1,23]],"date-time":"2024-01-23T07:59:26Z","timestamp":1705996766000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Intervention\u2010Free Graphitization of Carbon Microspheres from a Non\u2010Graphitizing Polymer at Low Temperature: Nanopores as Dynamic Nanoreactors"],"prefix":"10.1002","volume":"20","author":[{"ORCID":"https:\/\/orcid.org\/0009-0004-5860-0233","authenticated-orcid":false,"given":"Aliyeh","family":"Afzalalghom","sequence":"first","affiliation":[{"name":"School of Metallurgy &amp; 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