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Hollow poly(m-phenylenediamine) (PmPD) microparticles were successfully synthesised with chemically oxidative polymerisation through rapidly mixing the persulphate oxidant solution with m-phenylenediamine solution at room temperature. In a further experiment, Na2CO3 was used to create a CO2 bubble to facilitate the formation of hollow PmPD microparticles. The morphology and molecular structure of the products were characterised with scanning electron microscopy, transmission electron microscopy and Fourier transmission infrared spectroscopy. The results showed that the PmPD possesses a mouth-like cave when synthesised without Na2CO3. More interestingly, using Na2CO3, the cave number and shape of PmPD microparticles change. The PmPD synthesised with or without Na2CO3 has similar functional groups but different oxidation state.