The invention discloses a nano (Ti, M) C solid solution crystal whisker and a preparation method thereof. The nano (Ti, M) C solid solution crystal whisker is prepared from the following components: 40-79.9% of Ti, 0.1-40% of M and the balance of C, wherein M is at least one of W, Mo, V, Cr, Ta and Nb. Preparation raw materials comprise a component precursor of (Ti, M) C, a halogenating agent and a catalyst. The preparation method comprises the following steps: preparing a precursor mixed solution from all raw materials with distilled water, and drying so as to obtain precursor mixed powder; putting the precursor mixed powder into a reaction furnace, performing carbon-thermal reaction at 1100-1300 DEG C, firing the obtained nano (Ti, M) C solid solution crystal whisker for 4-6 hours at 350-400 DEG C in the presence of air for decarbonization, washing, performing eccentric separation, and finally drying, thereby obtaining the nano (Ti, M) C solid solution crystal whisker. The nano (Ti, M) C solid solution crystal whisker can be used as a nano ceramic phase crystal whisker toughening reinforcing metal based and ceramic based composite material, and is in good interface combination with a substrate.