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The crystal-chemical approach has been applied to design materials with regulated thermal expansion. To that end, model simulations have been performed for compositions of phosphates that yield solid solutions of the following type Na
1 + 2
x
Zr
2 –
x
Cu
x
(PO
4
)
3
and Ca
0.5 +
x
Zr
2 –
x
Cu
x
(PO
4
)
3
, 0.1 ≤
x
≤ 0.5 with the expected structure of NaZr
2
(PO
4
)
3
(NZP). The new phosphates have been prepared by solid-state reactions and characterized by X‑ray diffraction, IR spectroscopy, and scanning electron microscopy. The compounds have been shown to crystallize in the NZP structure, with a particle size from 0.1 to 1 μm. The thermal expansion of the compounds has been studied by high-temperature X-ray diffraction in the temperature range from 25 to 700°C. Linear, average, and volume coefficients of thermal expansion and anisotropy of thermal expansion have been calculated and analyzed in relation to composition of Na, Zr, Cu and Ca, Zr, Cu phosphates in the studied sets.