利用水热法制备了A0.925（MoO4）0.5（WO4）0.5∶Dy03.＋05（A=Ca、Sr、Ba）固溶体微晶。通过X射线衍射（XRD）、扫描电镜（SEM）、荧光分析（FA）等测试手段对微晶结构、形貌和发光性能进行了表征。结果表明A0.925（MoO4）0.5（WO4）0.5∶Dy03＋.05（A=Ca、Sr、Ba）复合钨钼酸盐微晶均呈现典型的四方晶相白钨矿结构。荧光光谱中的480nm处的偶合双峰和575nm处的锐而强的黄发射峰,分别对应于稀土离子Dy3＋的4F9/2→6 H15/2和4F9/2→6 H13/2跃迁。其中具有球状颗粒（尺寸为0.7μm）形貌的Ca0.925（MoO4）0.5（WO4）0.5∶Dy03.＋05微晶的发射峰强度最强,在光学材料中具有潜在应用。
A0.925（MoO4）0.5（WO4）0.5∶Dy3＋0.05（A=Ca,Sr,Ba） solid solution microcrystallines were synthesized by hydrothermal method;the crystal structure,surface morphology and room temperature photoluminescence properties of the microcrystallines were investigated by through X-ray diffraction（XRD）,scanning electron micrograph（SEM） and fluorescence analysis（FA）.The results show that the A0.925（MoO4）0.5（WO4）0.5∶Dy3＋0.05（A=Ca,Sr,Ba） microcrystallines all are typical scheelite structure with tetragonal symmetry.The emission peeks located at 480nm and 575nm respectively correspond to the transition of 4F9/2→6H15/2 and 4F9/2→6H13/2.The Ca0.925（MoO4）0.5（WO4）0.5∶Dy3＋0.05 microcrystallines with spherical morphology（grains size：0.7μm） give the maximum emission intensity,and it has wide potential application in optical materials.
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