Samarium doped calcium hydrogen phosphate was synthesized as single crystal by room temperature solution growth technique, namely, silica gel technique. The kinetics of the growth parameters was studied with regard to variation of pH, dopant concentration, gel ageing, and upper reactant concentration. The optimum conditions for the growth of good quality single crystal were worked out. Single crystal X-ray diffraction analysis establishes that the crystal belongs to monoclinic system. The density observed by the flotation method is greater than the density of the reported pure calcium hydrogen phosphate thereby suggesting the incorporation of the dopant (Sm) ion into the lattice of host (CHP). Thermal analysis gave two sharp endothermic peaks which are due to partial dehydration and phase transition, respectively. Dielectric studies establish a shift in the Curie temperature from 355 to 370°C only at higher frequencies thereby suggesting the relaxational behavior of the material.