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Pb(Zr0.52Ti0.48)O3/polycarbonate (PZT/PC) composite films with different concentration of PZT ferroelectric nanocrystals are prepared. The polarization and dielectric relaxation behavior of PZT ferroelectric nanocrystals are characterized using in situ transmittance and X-ray diffraction (XRD) measurements for the first time. It’s found that 10% PZT/PC composite film has the largest orientation change and negligible dielectric relaxation after poling (the φ value of 13.8% is almost constant with time even for 168 h). Based on the XRD results, we consider that the preferential orientation of PZT nanocrystals to align in PC matrix after poling is [001] direction.