Unveiling Non-isothermal Crystallization of CaO–Al(2)O(3)–B(2)O(3)–Na(2)O–Li(2)O–SiO(2) Glass via In Situ X-ray Scattering and Raman Spectroscopy

[Image: see text] The crystallization in glasses is a paradoxical phenomenon and scarcely investigated. This work explores the non-isothermal crystallization of a multicomponent alumino-borosilicate glass via in situ high-energy synchrotron X-ray diffraction, atomic pair distribution function, and Raman spectroscopy. Results depict the crystallization sequence as Ca(3)Al(2)O(6) and CaSiO(4) followed by LiAlO(2) with the final compound formation of Ca(3)B(2)O(6). These precipitations occur in a narrow temperature range and overlap, resulting in a single exothermic peak in the differential scanning calorimetry thermogram. The concurrent nucleation of Ca(3)Al(2)O(6) and CaSiO(4) is intermediated by their corresponding hydrates, which have dominantly short-range order. Moreover, the crystallization of LiAlO(2) and Ca(3)B(2)O(6) is strongly linked with the changes of structural units during the incubation stage in non-isothermal heating. These findings clarify the crystallization of multicomponent glass, which have been inferred from ex situ reports but never evidenced via in situ studies.