Development of novel materials with advanced properties is one of the main research directions of chemistry. New substances are not only crucial for many current technological applications but also should satisfy the needs of tomorrow. Industry often requires reliable, economically effective methods that can provide high quality reproducible results. Here we propose an inexpensive synthesis method that is suitable for synthesis of many types of particles. In this work we focused on Gd₂O₃:Tm³⁺, Er³⁺, Nd³⁺ particles with luminescence and magnetic properties. Based on the analysis of morphology, structural and optical properties of particles prepared by the standard Pechini methods and its variations, we found that the method with K₂CO₃ as additive yields particles with smaller sizes (down to tens of nm), higher crystallinity, and up to 1.7 times increased luminescence intensity. We also demonstrate that the unique combination of the particles’ characteristics, for example, the intensity ratio of the luminescent bands corresponding to different REI and the mass susceptibility, strongly depends on the composition, synthesis method, and structure. The variety of the combination of the properties makes these particles a promising candidate for safety markers applications.