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M
0.5+
x
Mg
x
Zr
2–
x
(PO
4
)
3
(M = Cd, Sr) phosphates have been synthesized via precipitation. In both systems, we have obtained limited solid solutions with the NaZr
2
(PO
4
)
3
(NZP) structure (in the range 0 ≤
x
≤ 0.6 for M = Cd and 0 ≤
x
≤ 0.5 for M = Sr). Structure refinement of SrMg
0.5
Zr
1.5
(PO
4
)
3
by the Rietveld method has shown that the Zr
4+
and Mg
2+
cations reside on framework sites, whereas Sr
2+
ions occupy structural voids. The thermal expansion of the M
0.5+
x
Mg
x
Zr
2–
x
(PO
4
)
3
(M = Cd, Sr) phosphates has been studied by X-ray diffraction in the temperature range 173–473 K. The results demonstrate that the incorporation of the larger (Sr
2+
) cations into voids in the NZP structure leads to a decrease in the magnitude of the axial linear thermal expansion coefficients. We have predicted and investigated a solid solution, Sr
0.7
Mg
0.2
Zr
1.8
(PO
4
)
3
, with a nearly zero thermal expansion anisotropy (0.55 × 10
–6
K
–1
) and a small average thermal expansion coefficient (3.92 × 10
–6
K
–1
).