Abstract Synthesis mechanism and phase stability analysis of square z‐Y2Si2O7 was studied in this research by using Y(NO3)3·6H2O and tetra ethoxy orthosilicate as precursors. The concentration of the precursor directly affects the degree of hydrolysis of tetra ethoxy orthosilicate and the uniformity of the gel by Fourier transform infrared spectral analysis. The thermogravimetric analysis shows that the crystallization temperature of the precursor decreases gradually with the decrease of precursor concentration. Because the low precursor concentration is beneficial to the formation of the homogeneous molecular level of yttrium silica network gel. Finally, the crystallized z‐Y2Si2O7 was detected by X‐ray diffraction and further verified by a transmission electron microscope after calcining at 800°C. The maximum stable temperature of z‐Y2Si2O7 was less than 1050°C. The microscopic morphology of z‐Y2Si2O7 is square nanoparticles. The grain size of z‐Y2Si2O7 increases with the decrease of precursor concentration.
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