The invention discloses a preparation method of a Si-C-N ceramic precursor. The preparation method comprises the following steps of: dissolving silicon-containing chlorosilane in an organic solvent which in immiscible with water, carrying out ammonolysis by virtue of aqueous alkali of a compounding containing -NH-, separating oil phase from water phase, and rotatably evaporating the oil phase at the boiling temperature of the organic solvent, to obtain liquid polysilazane; and putting the liquid polysilazane in a three-opening flask, and in the presence of N2, Ar or vacuum atmosphere, and continuously carrying out curing reaction for 12-72 hours at the temperature of 50-250DEG C, wherein the obtained solid product is the Si-C-N ceramic precursor. According to the preparation method, interfacial polymerization is adopted, so that the influence of byproducts on the purification and yield of polysilazane can be avoided, the reaction working procedures can be simplified, and the reaction time can be shortened; and the reaction process is easy to control, the synthesis yield reaches up to 90%, the product is high in purity, and a pyrolysis product is good in high temperature resistance and oxidation resistance.