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The LiZr
2
(AsO
4
)
3
arsenate and LiZr
2
(AsO
4
)
x
(PO
4
)
3 −
x
solid solutions have been prepared through precipitation followed by heat treatment, and characterized by X-ray diffraction, X-ray structure analysis, IR spectroscopy, and impedance spectroscopy. We have established conditions for the crystallization of the arsenate and a continuous series of arsenate phosphate solid solutions (0 ≤
x
≤ 3), which have been obtained as two polymorphs: monoclinic and hexagonal. Using the Rietveld method, we have refined the crystal structures of the polymorphs of LiZr
2
(AsO
4
)
3
(sp. gr.
P
2
1
/
n
,
a
= 9.1064(2),
b
= 9.1906(2),
c
= 12.7269(3) Å, β = 90.844(2)°,
V
=1065.03(5) Å
3
,
Z
= 4; sp. gr.
R
c
,
a
= 9.1600(4),
c
= 22.9059(13) Å,
V
= 1664.44(14) Å,
Z
= 6) and LiZr
2
(AsO
4
)
1.5
(PO
4
)
1.5
. Their structural frameworks are built up of AsO
4
tetrahedra—or (As,P)O
4
tetrahedra occupied by arsenic and phosphorus atoms at random—and ZrO
6
octahedra, with the lithium atoms in between. The ionic conductivity of the materials has been measured. The cation conductivity of monoclinic LiZr
2
(AsO
4
)
x
(PO
4
)
3 −
x
with 0 ≤
x
≤ 1 has been shown to exceed the conductivity of lithium zirconium phosphate.