The invention relates to a preparation method of metallographic samples of zirconium and zirconium alloy. The preparation method comprises the following steps: (a) sample pretreatment, namely sampling a to-be-tested material, ultrasonically cleaning to remove oil stain on the surface of a sample; (b) coarse grinding and fine grinding, namely grinding the sample processed in the step (a) on metallographic sand paper, wherein particle size marks of the utilized sand paper sequentially are 400#, 800#, 1200#, 2000# and 3000#; (3) chemical polishing, namely preparing a solution in a volume ratio that HF to HNO3 to H2O is 10 to 45 to 45, dipping the solution with an absorbent ball, and lightly wiping the surface of the sample with the absorbent ball for several times until the surface of the sample presents a polished surface as bright as a mirror; (d) cleaning, namely lightly wiping the surface of the polished sample in the step (c) by dipping absolute ethyl alcohol with the absorbent ball so as to remove complexes generated by chemical polishing; (e) oxidation cooling, namely dehydrating the cleaned sample, arranging the sample in a constant temperature region of a muffle furnace for oxidation for 2-10 minutes until the color of the surface of the sample is changed from bright white to faint yellow, taking out the sample, cooling, and carrying out metallographic observation and particle size evaluation.