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[Display omitted] • The KDP and MACKDP single crystals were grown by the slow evaporation method. • The UV–Vis-NIR spectrums reveal that the title compounds can be used as nonlinear optical materials. • KDP and MACKDP crystal belong to the soft material category. • Third-order nonlinear optical susceptibility (χ3) was found to be 5.391 × 10−8 esu and 5.412 × 10−8 esu for KDP and MACKDP, respectively. Potassium dihydrogen phosphate (KDP) and Methyl ammonium chloride doped KDP (MACKDP) were made into nonlinear optical single crystals using the ambient temperature slow evaporation method. An examination of powder X-ray diffraction reveals that the reflection lines of the doped KDP crystal are almost identical to those of the pure parent chemical KDP, with just a little difference in peak intensity. The space group and lattice parameters of the crystal structure were determined using XRD measurements on a single crystal. FTIR spectrum studies indicated the existence of numerous functional groups due to the shifting of peak positions. According to the results of UV–Vis-NIR testing, the UV cutoff wavelength for pure KDP is 381 nm and for methyl ammonium chloride doped potassium dihydrogen phosphate crystal is 383 nm. Growing crystals have reduced permittivity and dielectric loss tangent at increasing frequencies and temperatures. There were 1.12 times more correlated second harmonic (SHG) powers in the doped crystal than there were in pure KDP, according to the Kurtz and Perry approach. Thermogravimetric and differential thermal analysis were used to evaluate the thermal properties of an KDP doped MACKDP crystals. Vickers microhardness experiments have examined the impact of methyl ammonium chloride mixing on the hardness parameters of KDP crystal. The encouraging third-order nonlinear properties were examined employing a Z-scan technique using an Nd: YAG laser at 532 nm. To be considered a viable choice for nonlinear optical devices, the title material must exhibit a wide range of noteworthy physicochemical and optical nonlinear features. [ABSTRACT FROM AUTHOR]