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We report the sol–gel synthesis of Cu2V2O7 fine particles, in which some of the constituent Cu is replaced with other elements. The sintered body of Zn substituted β-Cu1.8Zn0.2V2O7 shows a large negative thermal expansion (NTE) over a wide temperature range due to microstructural effects peculiar to a ceramic body. Using the sol–gel method, we successfully produced β-Cu1.8Zn0.2V2O7 ceramic fine particles that retain the same level of thermal expansion suppression capabilities as the bulk with a size of about 1 μm. We also succeeded in performing rare earth metal (Ce, Sm, Yb) substitutions, which might be a clue for improving NTE performance. These achievements provide particulate filler for thermal expansion control of a micrometer region, which has been earnestly sought in many fields of technology.