Zn–Al–NO3–LDH was synthesized using the co-precipitation method at different pH values of 6, 7, 8, 9 and 10 with Zn2+/Al3+ = 4. The structural, textural and morphological properties of samples were studied. All prepared samples were mesoporous materials. The dielectric response of Zn–Al–NO3–LDH samples can be described by anomalous low frequency dispersion (ALFD). Thermal diffusivity of samples has been measured as a function in in situ temperature at range 27 – 210°C. The optimized electrical conductivity and thermal diffusivity has been found with the synthesized Zn–Al–NO3–LDH sample at pH 8.