The invention discloses high-purity strontium-calcium-europium nitride solid solution powder and a preparation method thereof. The general formula of the high-purity strontium-calcium-europium nitridesolid solution powder is (Sr1-x-yCaxEuy)2N (x is more than or equal to 0 and less than or equal to 0.45, and y is more than or equal to 0.008 and less than or equal to 0.025). The preparation methodcomprises the steps that S1, Ca, Sr and Eu with the purity larger than or equal to 99.99% are weighed and placed in a vacuum smelting furnace, argon is introduced, melting and pouring are conducted atthe temperature of 700-880 DEG C, and an alloy cast ingot is obtained; S2, after the surface of the cast ingot is cleaned, the cast ingot is placed in a hydrogen decrepitation furnace, hydrogen withthe purity larger than or equal to 99.99% is introduced, the cast ingot is heated to 200-400 DEG C, and the cast ingot is broken and dehydrogenated to obtain alloy coarse powder; S3, the temperature is reduced, liquid nitrogen with the purity larger than or equal to 99.99% is introduced, the temperature is increased to 580 DEG C, the pressure ranges from 0.5 Mpa to 0.8 Mpa, heat preservation is conducted for 5 hours, and high-purity strontium-calcium-europium nitride solid solution coarse powder is obtained; and S4, the coarse powder is transferred into a glove box, and the coarse powder is crushed in a crusher coated with a tungsten carbide coating to obtain a powder finished product.