采用泡生法生长了掺铥钨酸镱钾(KTm0.1Yb0.9 (WO4)2)激光晶体。利用X射线单晶衍射法和X射线粉末衍射法研究了KTm0.1Yb0.9(WO4)2晶体的物相与结构。采用X射线单晶衍射法并结合Diamond晶体结构绘图软件，获得了晶体内部结构模型图：该晶体是由WO6、TmO8/YbO8 和KO12基团组成。W2O10二聚体通过WOW单氧桥相连，在平行于c轴方向上形成(W2O8)n多重带。ReO8和 KO12多面体共顶相连，沿［101］和［110］方向形成了具有二维层结构的延长带。X射线粉末衍射分析表明：该晶体具有低温β相双钨酸盐结构，属于单斜晶系，空间群C2/c；计算了晶胞参数、晶粒尺寸和结晶度。测试了晶体的振动光谱，对各个峰值的红外和拉曼活性及分子振动情况进行了归属，进一步验证了晶体中WO6原子基团及单氧桥(WOW)和双氧桥(WOOW)的存在。

KTm0.1Yb0.9(WO4)2 laser crystal was grown by the Kyropoulos method. The phase and structure of the crystal were studied using the X-ray single crystal diffraction and X-ray powder diffraction. Combined with the X-ray single crystal diffraction method, the structure model of the crystal was obtained by the diamond crystal graphics software. It is indicated that the crystal consists of WO6, TmO8/YbO8 and KO12 groups. The W2O10 dimers, which are connected by the single oxygen bridge(WOW), have a formation of the(W2O8)n multiple bands in the direction of parallel to the c axis. TmO8/YbO8 and KO12 are connected with the same vertex, which can form an extension band along the ［101］ and ［110］ directions with a two-dimensional structure. X-ray powder diffraction analysis indicates that the crystal belongs to monoclinic system with a space group C2/c. It is verified that as-grown crystal is β-double tungstate with low temperature. The cell parameters, crystal grain size and crystallinity of the crystal were calculated as well. The vibration spectra of the crystal were investigated. The vibration modes and frequencies of infrared and Raman peaks were identified, which could further verify the presence of WO6 groups, single oxygen bridges(WOW) and double oxygen bridges(WOOW) in the crystal.