銣鎢氧化物RbxWOy已被發現其氧含量的變化會影響其物性,包括隨氧含量變化所發生的金屬-非金屬轉變,以及超導臨界溫度會隨銣、氧含量的變化而有所不同。基於RbxWOy的特性與其多晶樣品研究上之侷限性,開始著手於Rb0.23WOy在2.90≦y≦3.00範圍內單晶樣品的製備以及物性分析。Rb0.23WOy隨著氧含量的降低熔點逐漸變高,Rb0.23WO3.00單晶樣品燒結溫度為1190oC,Rb0.23WO2.90單晶樣品燒結溫度為1210oC,以及降溫速率影響單晶樣品的尺寸。結構分析採用後向反射勞厄法,不同氧含量的單晶樣品其(1 0 0)勞厄繞射圖皆呈現p2mm四角對稱,(0 0 1)勞厄繞射圖皆呈現p6mm六角對稱。對Rb0.23WO3.00單晶樣品在氧中退火過後的實驗發現超導臨界溫度隨著退火次數的增加隨之提升,以及晶格常數c縮短的現象。 Rubidium tungsten bronze RbxWOy (0.19< x< 0.33,2.9< y< 3.05) has been observed that the oxygen concentration dependent metal-nonmetal transition, and the rubidium and oxygen concentration dependent distribution for superconductivity critical temperature. In order to investigate the properties of RbxWOy more clearly, the preparation for single crystalline samples Rb0.23WOy (2.90≦y≦3.00) was carried out. The melting point of Rb0.23WOy increases as the oxygen concentration decreases. The melting point of Rb0.23WO3.00 is 1190oC and that of Rb0.23WO2.90 is 1210oC. And the size of single crystals affected by the cooling rate of calcination. The back-reflection Laue method presents p2mm symmetry along (1 0 0), and p6mm symmetry along (0 0 1) respectively for all single crystals with different oxygen concentration. The single crystalline Rb0.23WO3.00 was annealed in oxygen, and the superconductivity was observed above 3 K while the original material didn''t superconduct above 2 K, and the lattice parameter c decreased as the annealing times increased.