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• Azopolymer thin films doped with particles of biometals were prepared. • Polarization holographic gratings are recorded with a He-Cd gas laser with wavelength 442 nm in the composite films. • The influence of the dopants' composition and concentration on the polarization holographic gratings parameters is discussed. The paper presents a study of the diffraction efficiency of polarization holographic gratings recorded in thin films of the azopolymer PAZO (poly[1-[4-(3-carboxy-4-hydroxyphenylazo) benzenesulfonamido]-1,2-ethanediyl, sodium salt]) doped with Cu(II) 3-amino-5,5′-dimethylhydantoin (CLP) and Ni(II) 3-amino-5,5′-dimethylhydantoin (NLP) at three different concentrations, namely 1, 2 and 5 wt.%. The influence of the dopants composition and concentration on the parameters of the polarization holographic gratings recorded in the thin composite films has been discussed. The gratings are recorded with a He-Cd gas laser with wavelength 442 nm. The polarization of the recording beams was left and right circular and the recording angle was 20°. Along with the anisotropic grating in the volume of the media, surface relief is also formed. The diffraction efficiency kinetics is probed at 635 nm and the height of the relief gratings is determined by AFM. Diffraction efficiency (η) higher than 30 % was achieved for the hybrid samples, as well as 585 nm surface relief height. [ABSTRACT FROM AUTHOR]