In the present communication, we have successfully synthesized the efficient NLO material of glycine hydrofluoride (GHF) by conventional chemical reaction, and grown the single crystal by adopting slow evaporation solution growth technique. In order to know its suitability for device fabrication, different characterization analyses have been performed. The lattice constants have been determined from powder X-ray diffraction (PXRD) method and found that it crystallizes in orthorhombic crystal system. Its crystalline perfection was evaluated by high-resolution X-ray diffraction technique (HRXRD) and the value of FWHM indicates the presence of low angle structural grain boundaries. Its luminescence behaviour has been analysed by photoluminescence (PL) analysis and found maximum luminescence in the lower wavelength region. Its relative second harmonic generation efficiency was evaluated from Kurtz powder technique. The phase matching angle of GHF was determined by using Nd:YAG laser as a source. Its thermal, mechanical and electrical properties were examined by TG/DTA, Vickers microhardness tester and dielectric measurements, respectively.