Akao A, Aoki H, Innami Y, Minamikata S, Yamada T
Tokyo Ika Shika Daigaku Iyo Kizai Kenkyusho Hokoku. 1989;23:25-9.
Single crystals of pyromorphite, Pb5(PO4)3Cl, were grown by standard flux growth technique with excess lead chloride used as the flux. Pyromorphite was first prepared by heating an intimate mixture of lead hydrogen phosphate and lead chloride in the molar ratio 6:4 at 100 degrees C for 1 h. A mixture of 60 wt% of pyromorphite and 40 wt% of lead chloride was heated at 850 degrees C for 15 h and then cooled at the rate of 3.4 degrees C/h. Hexagonal prismatic crystals of length 1 mm were obtained. The chemical composition has close to the theoretical value. The crystal is hexagonal, space group P6(3)/m with a = 9.9981(8), c = 7.344(1) A and Z = 2. The structure was refined to R = 0.058 and Rw = 0.053 with 502 independent reflections. The structure is in principal the same as that of barium chlorapatite; the chlorine ions occupy the (0, 0, 0) position.
采用标准助熔剂生长技术,以过量的氯化铅作为助熔剂,生长出了磷氯铅矿(Pb5(PO4)3Cl)单晶。首先,通过将磷酸氢铅和氯化铅按摩尔比6:4的均匀混合物在100℃加热1小时来制备磷氯铅矿。将60 wt%的磷氯铅矿和40 wt%的氯化铅的混合物在850℃加热15小时,然后以3.4℃/小时的速率冷却。获得了长度为1毫米的六方柱状晶体。其化学成分接近理论值。该晶体为六方晶系,空间群为P6(3)/m,a = 9.9981(8),c = 7.344(1) Å,Z = 2。利用502个独立反射将结构精修至R = 0.058,Rw = 0.053。该结构与氯钡磷灰石的结构基本相同;氯离子占据(0, 0, 0)位置。