Ammonium fluoride NH4F and antimony trifluoride SbF3 form many stoichiometric compounds, such as NH4SbF4, (NH4)2SbF5, NH4Sb2F7, (NH4)3Sb2F9, NH4Sb3F10, etc. Since (NH4)2SbF5 exhibits superionic conductivity and undergoes phase transitions, an attempt has been made to grow other stoichiometric compounds of this group. In this report, we deal with the growth and microhardness studies of NH4Sb3F10, single crystals. Crystals of size 60 x 25 x 35 mm3 were grown in a period of two months. Microhardness studies have been carried out using a Vickers diamond pyramid indenter. To study the anisotropy of this material, specimens cut in different orientations such as (001), (010), (100), (101), (101BAR) have been subjected to microhardness studies. The results show strong anisotropy in the work-hardening coefficient for different orientations. This anisotropy is explained on the basis of a plastic deformation model.